Process and Apparatus for The Production of A Detergent Composition

专利摘要:
A method of forming a detergent bar by injection molding in which pressure is applied to deliver a detergent composition with some structure to the mold. The detergent composition can be delivered to the mold in substantial semisolid state at temperatures below 70 ° C. and pressures above 20 psi at the point of injection. An apparatus for forming a detergent bar according to the present invention is also described.
公开号:KR20010012621A
申请号:KR1019997010582
申请日:1998-05-04
公开日:2001-02-26
发明作者:피터 스튜어트 앨런；존 마틴 코어델；그래머 네일 어빙；수레쉬 무리게파 나다카티；비자이 무쿤드 나익；크리스틴 앤 오버톤；프레더릭 에드먼드 스톡커；카닉 타베르디；존 콜린 왈러스
申请人:알 브이 테이트 (로드니 비버스 테이트)；유니레버 엔.브이.；에이치 드로이. 씨. 지. 오닌크；이. 에디；산드라 웨드워즈 (에스 제이 에드워즈)；
IPC主号:

专利说明:

Process and Apparatus for The Production of A Detergent Composition
Detergent bars are conventionally used in one of two methods: (i) post-milling extrusion ("plodding") and stamping (often called "milling" processes), or (ii) casting. Is manufactured by.
In the milling process, the preformed solid composition comprising all of the components of the bar is typically floated. That is, extruded through a nozzle to form a continuous rod and cut into smaller pieces of a predetermined length, commonly referred to as billets. The billet is then fed into the stamper or otherwise stamped on one or more surfaces, or simply cut, using, for example, a die or roller shaped die of the same value as the bar surface striking with a mallet.
There are several drawbacks involved in the milling method of detergent bar production.
The problem encountered in the stamping method is die-blocking, in which the amount of residual detergent remaining on the die halves accumulates during the continuous use of the die. Die blocking may deteriorate or even not release the bar from the die surface and / or cause visible defects on the bar surface. Extrusion and stamping also require the extruded billet to be in a substantially hard form at processing conditions. Die blocking and soft billets can be caused, for example, by a soft detergent composition comprising a large proportion of components that are liquid at process conditions and / or also by a milling process, for example extrusion and / or stamping. It may be a result of the shear and stretching forces applied to the.
Milling is therefore only suitable for compositions that are plastic and otherwise not ductile or that are not ductile or sticky by shear decomposition at the operating temperature of the production apparatus, typically in the range of room temperature ± 30 ° C.
Milled bars also tend to have an oriented structure, aligned along the axis from which they are extruded. They also tend to form cracks in the bars that weaken the bars due to repeated wetting and drying in use, which may cause wet-cracking depending on the sides. Wet-cracking is very undesirable because it makes the bar unsightly and causes bar fragmentation.
Another typical method for the production of detergent bars is casting. In the case of casting, the detergent composition is introduced into the top of a closed cavity (i.e., a mold) of the desired shape in a heated, mobile and easily pourable state and the temperature of the composition is lowered to solidify the composition. The mold can then be opened to remove the bar.
To be cast, the detergent composition must be mobile at the elevated temperatures used and readily pourable. Certain detergent compositions are not suitable for casting as they are viscous liquids or semi-solids at elevated temperatures that are commercially realistic.
Moreover, in the casting process, the detergent melt tends to cool slowly and unevenly. This can lead to undesirable structural orientation and separation of components. Certain active cooling systems are often used to obtain satisfactory process time. Even when a cooling system is used, still generally the detergent composition in the mold is cooled evenly throughout.
The main problem with the casting process is that the detergent composition in the mold tends to shrink as it cools. This is very undesirable when the mold is intended to impart unusual shapes and / or specific kinds of logos on the bars. Shrinkage can cause depressions in the form of dimples, wrinkles, or pores, or at the point of filling of the bars.
Thus, forming the detergent composition into good quality bars (i.e., with good appearance and physical properties), which overcomes the identified problems and disadvantages involved in the milling process and also avoids the problems associated with casting. There is a need for a method and apparatus.
U.S. Patent No. 2987484 (Procter & Gamble) discloses an original non-soap fluid mixture of synthetic detergents and binder-vehicles, which can be solidified in shape-retaining form, through small orifices. A closed die forming process is disclosed which rapidly injects into a substantially closed die.
This process includes heating the composition to a temperature in the range of 70 ° C. to 150 ° C. such that the composition melt is in a fluid-injectable state. In all embodiments, the temperature is in the range of 82-150 ° C. The melt includes a cruncher in which the fluid mixture is mixed and heated, a conduit in one loop with the crusher, a heat exchanger in the conduit to stabilize the temperature of the melt, and a pump to maintain circulation and injection pressure It is circulated through a continuous injection circuit.
The viscosity of the melt heated under the conditions of injection is 2 to 50 Pa · s. This is described as dependent on the strength and temperature of the shear and the action of the composition. However, no shear rate is shown for this viscosity range. Melts with a viscosity of 2 to 50 Pa · s under injection conditions are sufficiently concentrated to not splatter, contain air or escape into the mold vents, and completely fill the mold before any composition solidifies in the mold. And lean enough to avoid excessive injection pressure. Suitable injection pressures are about 1 to 20 psi, but are preferably in the range of 2 to 10 psi. In all examples, the injection pressure is 5-8 psi. Too high a pressure is described as splashing in the mold and increasing the density of the melt.
U.S. Patent No. 2987484 also teaches that in a work process the fluid mixture must be cooled through a crystalline phase in addition to Nigre (isotropic liquid), which is a property of the claims. Moreover, detergent fluid mixtures in pure or intermediate (anisotropic liquid) phases are not suitable for closed die forming due to excessive viscosity of these phases and the tendency of undesirable complexes to form on them. In addition, US Pat. No. 2987484 mentions that cooling through pure and intermediate phases should be avoided (columns 4, lines 8 to 27) for successful closed die molding.
U.S. Patent No. 2989484 describes that the problems associated with conventional methods of bar manufacture and in particular in milling are overcome. However, the described solutions have several inherent drawbacks, which are mostly common in casting and framing processes. It is a very strong energy, which is required to heat the detergent composition to a high temperature, at which temperature the mold is injected and the mold is subsequently cooled to reduce the solidification time to a satisfactory level. Moreover, by injecting the composition as a hot fluid, the process causes the problem of shrinking as the bars solidify. It also failed to address the problem of component separation as the detergent composition cooled in the mold. In the device the detergent composition is pumped through a conduit or permanently sheared by a mixer in the crusher.
A typical process of detergent bar manufacture is to allow the detergent composition to be entirely structured (eg casting) in the mold, which requires initially high thermal energy input, or to process (eg extrusion and stamping) a hard solid material prior to molding. The detergent composition is operated to be structured entirely outside the mold / bar-shaped means. The latter type of process applies high shear energy (eg in stamping) to the structured material. In an attempt to overcome this process, in particular the disadvantages of milling and flaming, the process described in US Pat. No. 2987484 does not deviate from this general pattern. That is, high energy is input using relatively high temperature. In view of this, U.S. Patent No. 2987484 provides only another casting process in that the detergent material is injected into the mold instead of pouring.
The inventors have found that the problem present in the prior art methods can be overcome by working with a processing window which forms the structure partly at the outside of the mold and partly at the inside. In this way, the bursting shear effect present in the process will only affect the partially formed structure and sufficient structure will be formed in the mold to produce a good quality bar. In this way, the structure of the detergent composition can be damaged to a very low degree during bar formation and withstand higher injection pressures without rupturing the partial structure.
<Summary of invention>
By structuring the detergent composition in part before delivery of the detergent composition to the mold in the injection molding process, good quality bars can be obtained, and problems of shrinkage, orientation of the oriented structure and component separation are significantly reduced. In addition, manufacturing advantages such as shorter bar release times can also be obtained.
Accordingly, according to a first aspect, the present invention includes applying pressure to a detergent composition to deliver the detergent composition to the mold, wherein the detergent composition is at least partially structured when the detergent composition is introduced into the mold. Provide a method of forming a detergent bar.
Preferably, the continuous phase of the detergent composition is at least partially structured.
In the present invention, the detergent composition is considered to be at least partially structured when the detergent composition includes certain molecular structures that will affect its viscosity. In addition or alternatively, the detergent composition may be considered at least partially structured when the detergent composition comprises a structuring agent that increases its viscosity.
Preferably the detergent composition is in a semisolid state when delivered to the mold.
In a second aspect, the present invention is characterized in that the pressure at the point where the detergent composition is introduced into the mold at least partially during its introduction into the mold exceeds 20 psi. It provides a method for forming a detergent bar comprising applying.
In a third aspect, the present invention provides a method for forming a detergent bar, comprising applying pressure to the detergent composition to deliver the detergent composition to the mold, wherein the temperature of the detergent composition when introduced into the mold is less than 70 ° C. do.
By delivering the detergent composition to the mold at a temperature lower than that described in the prior art, the process requires less intense energy and cools to a temperature at which the solid is discharged more quickly from the mold.
The inventors have devised an apparatus for forming the detergent bar by injection mold. More specifically, the inventors have provided a means for supplying the detergent composition to a means for applying pressure.
Accordingly, the present invention provides a detergent bar forming apparatus comprising means for applying pressure to the detergent composition to deliver the detergent composition to the mold and substantially individual means mounted to supply the detergent composition to the means for applying the pressure. do.
The detergent composition may be introduced into the supply means in any suitable state, for example in the form of a fluid, semisolid or particulate.
The inventors have found that particularly efficient means of supplying the detergent composition, including the composition supplied in fluid form in the injection molding process of the detergent composition, is provided by means of a screw extruder.
Thus, the supply means preferably comprises a screw feeder.
In another aspect, the present invention provides a detergent bar obtainable by the method of the present invention.
The inventors have found that the method of the present invention is very suitable for introducing additives or benefit agents of a nature not mixed with the detergent composition. Accordingly, the present invention provides a detergent bar obtainable by the method of the present invention comprising a detergent composition and components present in the non-spherical domain that are not mixed with the detergent composition.
In another aspect, the present invention includes adding an additive or benefit agent to an at least partially structured detergent composition and applying pressure to the detergent composition comprising the additive or benefit agent for delivery to a mold. Or a method of introducing a benefit agent.
In one preferred embodiment, the additive or benefit agent is of a nature that does not mix with the detergent composition.
Unless further specified, references to the invention or any desirable feature apply to all aspects of the invention.
The present invention relates to a method and apparatus for forming a detergent bar and a detergent bar produced thereby. The detergent bar may be of the body or fabric cleaning type.
1 shows an apparatus used in the process of the invention (side view, reciprocating single screw extruder).
Figure 2 shows another device according to the invention (top view, twin screw extruder).
Figure 3 shows another apparatus according to the present invention (side view, in-line low shear injection head, degassing zone and twin screw extruder with solid feed stuffer).
FIG. 4 shows the end of the device of FIG. 2 (apparatus for movement of the mold during filling).
Figure 5 shows a device (top view, simple ram extruder) used in the method of the present invention.
6 shows the internal structure of a mold die according to the present invention.
7 shows the external structure of the mold.
8 shows another embodiment of a mold.
9 schematically shows a detergent forming system.
<Detailed description of drawing>
Figure 1 shows an injection molding apparatus ('Sandretto' series 7 HP 135 injection molding machine) for detergent materials for use in the present invention, generally indicated by (1).
The apparatus comprises a typical means (2) for supplying the particulate solid detergent composition. The means shown are generally known as stuffing pots and comprise a piston 3 which presses loose particulate detergent material. Particulate material flows from the stuffing pod to the screw feeder. The screw feed device comprises a barrel 4 with a cylindrical inner bore 5. Inside the barrel 4 there is a single screw 6 (50 mm diameter dough molding compound screw). Means (not shown) for continuously rotating the screw 6 are provided. The screw rotates at 80-100 rpm. Rotation of the screw 6 causes the detergent composition to flow in the direction indicated by the arrow. Independently controlled heating means 7 in the form of a duck for the liquid are provided around the barrel 4. The heating means 7 raises the temperature of the detergent composition to the extent that it can be delivered under pressure without sticking. According to the barrel 4 the temperature profile is staged.
At the end of the barrel 4 the bore 5 is reduced to the diameter of the nozzle 8 and can be fixed to a two-part aluminum mold 9 with a mold cavity shaped in the form of a detergent bar (the fixing means is Not shown).
During operation, the screw 6 can move inside the barrel 4 so that its end can withdraw from the accumulation zone 10 of the cylindrical bore 5.
In operation, the detergent composition may be prepared into small particles (average diameters of 1 to 10 mm) using devices already known in the art, such as floaters with chill rolls, noodler plates and the like. Can be. The particulate detergent composition is fed to the stuffing pot 2 and thereby into the screw feeder. Screw 6 rotates continuously to transfer detergent composition along bore 5. During the transfer, the temperature of the detergent composition is raised to the heating means 7 so that the temperature at the injection point is from room temperature to 70 ° C.
A means (not shown) is provided to move the feed screw 6 along the axis of the cylindrical bore 5.
During operation, a flowable detergent composition at elevated temperature is supplied to the zone 10. When the detergent composition accumulates in this zone, the screw 6 is removed from the nozzle 8 so that the volume of the space 10 increases.
Once accumulated to a sufficient volume in the space 10, the screw 6 is driven towards the nozzle 8 by hydraulic means (not shown), so that the detergent composition is at a elevated temperature to transfer the detergent composition through the nozzle to the mold 9. Pressure is applied to the composition. A check valve (not shown) is provided to prevent backflow along the screw.
As soon as the mold is filled, the mold can be pressurized if necessary while cooling. This maintains the volume of detergent in the mold as it shrinks as it cools.
The mold can then be removed from the installation and, if necessary, cooled before opening.
Mold cooling means can be used to promote cooling of the detergent composition in the mold. For example, solid phase carbon dioxide, ice / water baths or cold water can be used to precool the mold or post-cool the mold before deforming.
2 shows a side view of one embodiment of the present invention. Generally represented by (11). Apparatus 11 is preferred to supply a detergent composition which is supplied in liquid form. However, the device 11 can be used to supply a detergent composition which is supplied in solid form if a suitable supply means is provided.
Duct 12 is provided to accommodate the supply of liquid detergent composition, for example, from individual steps in the manufacturing process. The duct 12 is connected to the extruder 13. In the extruder 13 there are two intermeshed co-rotating feed screws 14, 15 each with a single vane. At the end of the screw, a series of media shear mixing elements are provided comprising three tri-lobe paddles 26 and three melt disks 27 for providing back pressure and some mixing. Temperature control means are provided in the jacket zone 16 around the barrel of the extruder 13. The temperature control means comprises a channel for the liquid coolant and an electrical installation for heating. The temperature control means in zone A of the extruder is maintained at a low temperature of, for example, 30 ° C., so that a solid detergent composition is formed so that the shaft ends of the screws 14, 15 are sealed. The temperature control means in the zone marked B is hot to keep the detergent composition molten to prevent containment at the feed point. In the zone indicated by C (ie the rest of the extruder length) the temperature control means 16 is for gradually conditioning the detergent composition to the desired temperature.
A valve connection 17 is provided through which the detergent composition is supplied to an injection head 18 comprising two injection chambers 19. The injection chamber 19 comprises a cylinder with a retractable piston 20. The injection head 18 has a nozzle 21 to be described in FIG. 4 below. Both the connecting portion 17, the injection head 18 and the injection chamber 19 are provided with an electric heater (not shown) for temperature control.
In operation, the molten feed of detergent composition is fed to the feed cavity 13 and into the injection chamber 19 via the connecting portion 17 by means of a screw which co-rotates in the direction of the arrow in a region where the temperature is between 90 and 95 ° C. Drive it in. At this point the temperature is below 70 ° C. During the first phase of operation, detergent material accumulates in the injection chamber as the piston 20 pushes simultaneously. Once the proper volume of detergent composition has accumulated, the piston 20 is actuated by hydraulic pressure (not shown) such that the resulting pressure is applied to the composition to advance through the nozzle 21 into the mold and will be described further below. .
3 shows a side view of one embodiment of the present invention. Generally represented by (28). The apparatus comprises two intermeshed co-rotating feed screws, each with a single vane as described in FIG. The general shape of the two intermeshing screws can be selected to suit the particular application. At the end of the screw, a series of media shear mixing and kneading elements are also provided as described in FIG. Mixing and kneading elements can be interspersed between conveying screw elements of various pitches. Temperature control means comprising channels for liquid coolant and electrical heating means are provided in the jacket zone around the barrel of the extruder (as in FIG. 2).
The device may accept liquid, semisolid or solid material as the feed, depending on the feed arrangement selected. The particular detergent material is fed to zone D of the extruder through solid feeder 29. The fluid material is supplied to zone E of the extruder by liquid supply means 30. The exhaust port 31 is shown in zone H of the extruder. In zone J of the extruder, solid supply means 32 for the solids delivery accompanying the extruder are shown. In zone K, a duct 33 for the inflow of liquid additives by a pump (not shown) is shown. It is to be understood that the extruder zones can be interchanged so that the solid, liquid, and additive feed can be introduced at any location along the length of the screw. One or multiple feeds may be supplied for a particular product.
At the outlet of the extruder is a three-way valve 34 which is used for sampling and recirculation. When this valve is in the straight passage position, the conditioned material from the extruder passes into the accumulator 36 comprising the cylindrical chapter 37 and the piston 38. The position of the piston 38 in the cylinder 37 changes with the material flow into and out of the accumulator. The piston back air pressure maintains a constant pressure on the material in the accumulator and thus provides a buffer between the continuous flow rate from the extruder and the interstitial demand of the injection head 39. Provide a temperature control jacket to the three-way valve 34 and the accumulator 36.
The injection head is located perpendicular to the extruder so that its axis is perpendicular. Means (not shown) for temperature control are provided.
The injection head 39 is a hydraulic actuator 40, a spindle 41 connected to the actuator, an inlet chamber 42, an injection chamber 43, a non-return ring check valve 44 and an injection valve 45 ). In addition, the nozzle 46 and the metal mold | die 9 are shown. The nozzle and mold can be preheated before injection if necessary.
In the filling mode, the injection valve 45 is closed. The pressure above the ring check valve is greater than the pressure below, and the valve moves to its lower position. In this position the material can flow through the ring check valve between the injection spindle and the cylinder wall. When the injection spindle is hydraulically moved upward by the movement of the actuator, the material to be produced flows into the injection chamber. The filling process is complete when the spindle is fully raised.
Minimizing the spindle diameter (within the limits of mechanical strength) provides the maximum area for flow, resulting in minimal extension shear on the flowing material.
When the pressure at the bottom of the valve exceeds the pressure at the top, the valve moves to its upper position to isolate the injection chamber from the inlet chamber. At this point the machine is filled for injection. This manual valve system eliminates the need for an inlet control valve and allows first-in, first-out material to flow into the mold.
In the injection mode, the injection valve 45 is opened, the cylinder is hydraulically driven downward, and the pressure in the injection chamber rises above the pressure in the inlet chamber. This closes the ring check valve. As the spindle moves downward with the actuator, the material flows from the injection chamber through the nozzle 46 through the open injection valve into the mold.
The volume of material delivered to the mold is measured by the stroke of the hydraulic actuator. The speed of the material delivered to the mold is measured by hydraulic pressure.
The application pressure is measured at the appropriate position in the injection head 39. When using the device according to FIG. 3, the applied pressure was measured via an actuator. Moreover, the pressure was also measured at the point just before the nozzle. This is expressed as injection pressure as mentioned in Tables 3-5.
4 shows the end of the device of FIG. 2. However, the nozzle and mold shape can be equally applied to the apparatus of FIG. 3. The nozzle 46 can be seen from the top, along with the injection chamber 19 and the piston 20.
The mold 9 can also be seen. The nozzle extension 47 extends through the hole in the top to the mold cavity 48 of the mold 9. The mold 9 is mounted on a hydraulic system 50 or a plate 49 that can be moved up and down manually.
In use, when the piston 20 is activated to deliver the detergent composition under pressure from the injection cylinder, the detergent composition flows through the nozzle 46 and the nozzle extension 47 to the mold cavity 48. The forward speed of the piston 20 is followed by the withdrawal speed of the plate 49. As a result, the mold 9 is lowered while the mold cavity 48 is filled with the detergent composition. The detergent composition flowing under pressure tends to fill the bottom of the mold cavity. The withdrawal speed of the plate 49 is adjusted such that the tip of the nozzle extension 47 is always just below the mold cavity 48. This provides good fillability.
In addition, the same good filling is obtained by moving the nozzle 46 instead of the plate 49. The nozzle moves to the base of the mold cavity 48 and rises out of the mold as the mold cavity is filled with the detergent composition.
In one preferred embodiment, the nozzle is grooved by providing a series of vertical grooves 51 of depth about 1 mm. They extend from the top of the nozzle to about 10 mm from the tip. If the nozzle is in the mold, air may escape from the mold through the groove. When the nozzle retracts, the mold is blocked by the nozzle to maintain the pressure in the mold.
5 shows a simple ram extruder device for use in the method of the present invention. The simple reservoir or barrel 52 has a facility 53 capable of heating and maintaining the temperature of the sample from room temperature (RT) to 100 ° C. The plunger 54 is provided with a drive mechanism and a speed controller 55. Pressure indicator-transmitter 56 is provided at the bottom of the reservoir. One end of the mouthpiece 57 is screwed to the bottom of the reservoir. The other end of the mouthpiece is connected to the gate 58 on the mold 59 using a screw bolt. A vacuum pump is connected to the outlet capillary 60 to degas the mold before filling.
6 shows a die 61 of a mold made from aluminum. The die is provided with a cavity 62 in a volume of about 60 ml. The inner surface of the cavity is convex and a projection is provided which provides a mirror image 63 of the desired name on the molding of the injection molded bar. The inner surface of the cavity is coated with PTFE 64 having a thickness of 35 μ. Corresponding to the final shape of the injection molded tablet, the cavity formed by combining the two dies is opened through the gate 65. This gate jointly connects the supply reservoirs through the spouts. Leakage of material from the mold is prevented by providing a gasket 66 along the connecting surface of the die. Capillary tube 67, 1.5 mm in diameter, connects the mold to the vacuum pump. The capillary end 68 away from the cavity is screwed in and connected to the valve and then to the vacuum pump. Closing the valve helps the mold interior to reach a high injection pressure after the mold is evacuated. The die is provided with holes 69 for bolting the two dies to each other.
FIG. 7 shows the outer surface of a mold including two dies joined together in FIG. 5. The die is provided with fins / ribs 70 to increase cooling efficiency.
8 shows another embodiment of the mold of the present invention, wherein the outer surface of the die 71 is inclined so that the die of the mold can slide on the surface erased into the interior of the housing 72 to withstand the injection pressure. Achieve.
9 shows a detergent forming system according to the invention comprising a plurality of said molds 74 mounted on a feed reservoir 73 and a conveyor 75, whereby the method of the invention is carried out via a reservoir. Performed by circulating the mold, the detergent composition is injected into the mold under pressure and subsequently solidified, deformed (76) again through a cooling step and recycled again.
The invention is further illustrated by the following non-limiting examples.
By "detergent bar" is meant a tablet, cake or bar having a concentration of at least 5% based on the bar of the surfactant, including soap, synthetic detergent actives or mixtures thereof. The detergent bar may also include a benefit agent for imparting or maintaining the desired properties of the skin. For example, a humectant may be included.
The detergent composition may comprise a homogeneous component or a mixture of components, or may comprise a material suspended or dispersed in a continuous phase.
The detergent composition delivered to the mold can be in any form that can be delivered to the mold. For example, as long as the composition is plastically sufficient to allow the pressure application means to deliver the composition to the mold, as will be appreciated by those skilled in the art, the composition may be a substantial fluid (eg, melt, melted dispersion, liquid ), Substantially semisolid or substantially solid form.
<Structure>
The detergent composition should be compared with the detergent composition at the same temperature as the detergent composition under consideration of substantially the same composition, except that there is no structure and / or structure agent, thereby confirming an increase in viscosity.
For example, the structure may be provided by liquid crystal formation, polymer structuring agent or clay, or a sufficient volume of dispersed solid component that will affect the viscosity. The solid components can interact to form a network within the detergent composition to provide the structure, or provide the structure through simple physical interaction / contact of each other or the continuous phase and the solid particles.
In detergent compositions, especially detergent compositions in substantial fluid or liquid state, there are two general separate classes of compositions that are structurally isotropic and structurally anisotropic. These phase states that are structurally isotropic are liquid, cubic liquid crystal phases, and cubic crystal phases. All other phases are structurally anisotropic.
Structural liquids may be internally structured in which the structure is formed by a main component, preferably a surfactant material (ie with an anisotropic or liquid crystal phase), and / or the three-dimensional matrix structure is for example a polymer (eg , Carbopols), clay, silica and / or silicate materials (including aluminosilicates formed in situ) may be externally structured.
Such additives may be present in 1 to 10% by weight of the detergent composition.
In detergent compositions the internal structure may be present by the components used, their concentration, the temperature of the composition and the shear present or exposed in the composition.
In general, the degree of alignment of the surfactants included in the system increases with increasing surfactant and / or electrolyte concentration. If the concentration of the surfactant and / or electrolyte is very low, the surfactant may be present in the molecular solution, or in the solution of spherical micelles, both of which are isotropic, i.e. without structure. The addition of additional surfactants and / or electrolytes may form the structure of the surfactant material. Various forms of such structures exist, for example, in two layers. These are referred to in various terms, such as rod- micelles, anisotropic surfactant phases, planar lamellar structures, lamellar droplets and liquid crystalline phases (which can be mostly anisotropic or isotropic). Various examples of fluid compositions internally structured with surfactant materials are described in H.A. Barnes, "Detergents", Ch.2. in K. Walters (Ed), "Rheometry: Industrial Applications", J. Wiley & Sons, Letchworth 1980. Often different researchers actually use different terms to refer to the same structure. For example, lamellar droplets are referred to as sherulite in European Patent No. 0151884.
The presence of such internal structuring, alignment or anisotropy is typically revealed by the temperature / viscosity / shear profile of the composition in a manner known to those skilled in the art. Often, the presence of molecular structures causes non-Newtonian fluid behavior.
The presence and identity of the surfactant structuring system in the detergent composition can be measured by means known to those skilled in the art, such as, for example, optical techniques, various flow measurements, X-ray or neutron diffraction methods, and sometimes electron microscopy. have.
As is known to those skilled in the art, molecular structures can be detected using polarization microscopy. The isotropic phase has no effect on the polarization, but the structured phase affects the polarization and can be birefringent. Isotropic liquids cannot expect any kind of periodicity in X-rays or neutron diffraction micrographs, while molecular structures can generate primary, secondary or even tertiary periodicity in a manner known to those skilled in the art. Can be.
Preferably the detergent composition is in a semisolid state when delivered to the mold. As will be appreciated by those skilled in the art, a detergent composition can be considered semisolid if sufficient structure is present in the composition and no longer behaves as a simple liquid.
In contrast to the prior art, the inventors have found that a detergent bar with good physical properties can be obtained by cooling the detergent composition from or through pure and / or intermediate liquid crystal phases. Moreover, the inventors have found that it is not necessary to cool the detergent composition through the crystalline phase other than Nigre in order to achieve successful bar formation by the injection molding process.
Thus, the detergent composition introduced into the mold is preferably cooled from and / or through the anisotropic liquid crystal phase.
Thus, the methods and apparatus of the present invention are, for example, compositions, in particular body cleansing compositions having a high concentration of components that are liquid at ambient conditions, compositions having a solid structure sensitive to shear, and compositions that are too viscous to cast. As such, it provides a means for producing a detergent bar of good quality from a detergent composition that cannot be prepared by a milling or casting method.
One of the advantages provided by the present invention is that as the bar cools, it reduces the problems associated with shrinking the bar in the mold. This makes the reproduction of the surface contour and shape of the cavity more accurate. In particular, good logo reproduction can be obtained.
To overcome the problems associated with prior art processes, the detergent compositions of the present invention are typically more viscous than prior art detergent compositions. As a result, the pressure required to deliver the detergent composition to the mold is greater.
<Pressure>
The pressure applied to the detergent composition in contact with the pressure application means is referred to herein as "applied pressure," and the term "apply" and "apply" the pressure to the detergent composition means the application pressure. Since the detergent composition may be relatively viscous, the pressure received by the composition may be lower toward the bottom of the flow path.
"Injection pressure" is the pressure on the detergent composition at the point of introduction into the mold.
The inventors have found that pressures higher than those of the prior art can be used to deliver the detergent composition to the mold without damaging the final molecular structure of the detergent bar. As in the second aspect of the present invention, injection pressures in excess of 20 psi may be used to supply a relatively viscous composition to the mold.
The application pressure may be on the order of 10 to 50 psi. However, higher application pressures can be used to deliver relatively viscous (eg, semisolid) detergent compositions to the mold, for example 1000 psi or less. The application pressure typically does not exceed 750 psi and more typically does not exceed 500 psi. Excessive shear at this pressure can be avoided by controlling process parameters such as temperature, flow rate and device design.
The injection pressure is typically above 20 psi, preferably above 29.4 psi, more preferably above 50 psi. Since the detergent composition to be injected and molded is at least partially structured and / or relatively low temperature, injection pressures significantly higher than those reported in US Pat. No. 2,987,784 may be used. For example, the detergent composition may be in substantially semisolid form. Injection pressures above 200, above 400 and even above 700 psi may be used.
The inventors have found that the problem with bar shrinkage in the mold can be reduced, if necessary, by transferring additional detergent composition to the mold once the capacity in the mold cools or becomes solid. To accomplish this, a "holding pressure" is applied on the detergent composition in the mold. In this way, the total volume in the mold can be maintained so that regeneration of the shape can be further improved.
Moreover, the use of holding pressure minimizes weld lines (ie, the interface between the flow fronts of the detergent material inside the mold) and improves the clarity of the logo.
Thus, a detergent bar with reduced shrinkage and good physical properties can be obtained by applying pressure to the detergent composition to deliver the detergent composition to the mold and continuously applying pressure on the detergent composition for a period of time after the mold is filled.
The pressure generated in the mold by continually applying pressure to the detergent composition introduced into the mold after the mold is filled is referred to herein as the holding pressure. The detergent composition may be under high holding pressure in the mold. For example, this pressure can be 1000 psi or less.
All pressure values are in psi gauge (psig), above or below atmospheric pressure.
The time during the holding pressure resulting from the continuous application of pressure to the detergent composition after the mold is filled is referred to herein as the holding time. The retention time will vary depending on the nature of the detergent composition delivered to the mold. For example, a composition delivered to the mold at the molten state and at a high temperature will require a longer retention time than the composition delivered to the mold at the semisolid state and / or at a lower temperature.
In general, the retention time is less than 2 minutes, preferably less than 1 minute, more preferably less than 30 seconds, most preferably less than 10 seconds. The retention time can be very short, for example less than 1 second.
<Temperature>
The inventors have found that at temperatures below those typically used in the prior art, the detergent composition can be delivered to the mold under pressure without damaging the final molecular structure of the detergent bar. If the presence of the structure can be clearly identified in the detergent composition delivered to the mold, it may be satisfactory to bring the detergent composition at a temperature of 100 ° C. or higher when the detergent composition is introduced into the mold. However, as in the third aspect of the invention, the detergent composition can be delivered to the mold under pressure at temperatures below 70 ° C. when introduced into the mold. Excessive shear at these temperatures can be avoided by controlling process parameters such as flow rate and device design.
Detergent compositions generally do not have a simple melting point and, as the temperature increases, from solid form to semisolid form and then to fluid (or molten) form. Any actual detergent composition in the form of a bar will be substantially solid at ambient or general storage and / or use temperatures, generally in the range of 30 to 40 ° C. or less.
Thus, the detergent composition is preferably introduced into the mold at a temperature above ambient temperature, for example, preferably above 30 ° C., more preferably above 40 ° C.
Of course, the lower the temperature, the less energy is required to heat the composition from ambient temperature, and the faster the bar cools and the less the bar tends to shrink.
A particular advantage of the present invention is that the detergent composition can be introduced into the mold at lower temperatures in a simple casting technique. When heating the solid detergent composition, less heat (ie energy) may be needed as the operating temperature may be lower. When cooling the liquid detergent, no heating may be necessary. Thus, the present invention works economically.
Typically, the detergent composition may be at or below 60 ° C.
The present invention is particularly suitable for detergent compositions in which subcooling, ie thermal energy can be removed out of the mold without the final bar structure being formed.
<Injection molding apparatus>
Injection molding is a method currently used prominently in the molding of synthetic polymeric thermoplastic articles, in particular thermoplastic articles having thin cross sections and complex shapes.
In essence, an injection molding apparatus for a plastic material includes a substantially closed mold and means for delivering the plastic material under elevated pressure into the substantially closed mold. Preferably there is a means for raising the temperature of the plastic material to a temperature at which the material can flow under pressure. The process of the invention can be carried out using such known injection molding apparatus in the presence or absence of any means for heating the feed. Preferred variants according to the invention are discussed below.
The detergent composition of the present invention may be injection molded using a device comprising means for applying pressure to the detergent composition to drive the detergent composition into a mold. "Means for applying pressure" is defined as a device that includes a material and is capable of applying pressure to the material to insert the material into the mold.
Suitable types of devices for driving the detergent composition into the mold include positive displacement pumps such as, for example, piston pumps (which may include extruders), gear pumps and lobe pump-type equipment. -type) There is a facility.
A suitable device is a simple ram extruder in contact with the mold. Such devices typically include a reservoir or barrel of detergent composition, a plunger for applying pressure to the material in the reservoir and an outlet port through which the detergent composition is pushed through the mold directly or indirectly. The simple ram extruder device is particularly suitable for injection molding of detergent compositions, for example in semisolid form.
Injection molding apparatus as described above can be used for the method of the present invention.
In one preferred embodiment, the detergent composition is preferably at least partially structured when delivered to the mold. Preferably, the detergent composition is in semisolid form when delivered to the mold. Of course, the present invention also provides that the detergent composition is injection molded in substantial fluid form.
Some detergent compositions may be permanently sticky when they are injection molded under inadequate conditions. That is, some solid detergent compositions have complex molecular structures that can collapse when the solid is exposed to excessive shear stress. The molecular structure may not be rebuilt after this shear, leaving the detergent composition in a sticky and unusable state.
It is therefore desirable to ensure that such detergent compositions are not exposed to excessive shear during delivery to the mold.
In order to control the shearing experience of the detergent composition, it is necessary to consider the properties of the detergent composition itself, in particular its viscosity and molecular structure at various temperatures. To control shear, process parameters such as temperature, pressure applied to the composition, flow rate of the detergent composition in the device, and configuration of the device can be controlled. Shapes such as severe bending, compression, and fast moving portions can exert high shear on the detergent composition.
The inventors have found that by delivering the detergent composition to the mold at an appropriate temperature, no shear sensitive structure can be formed completely and no loss of structure of the composition at room temperature. Any suitable method may be used to control the temperature of the detergent composition injected into the mold. It can be supplied at a suitable temperature for delivery to the mold and need not be changed to its temperature. In addition, the temperature of the detergent composition is preferably altered using heating or cooling means to raise or lower the temperature of the composition as appropriate before or during delivery of the detergent composition to the mold.
Preferably, the state of the detergent composition is changed before or during the supply. For example, it can change from the liquid phase to the semisolid state. In addition, it can change from solid to semisolid state.
Any suitable cooling or heating means can be applied to the injection molding apparatus in which the detergent composition is included / passed during the injection molding process.
Suitable heating and cooling means are well known to those skilled in the art. For example, a suitable cooling means is a cooling jacket comprising a cooling medium, and a suitable heating means is, for example, an electric heating jacket comprising a heating medium or various types of heat exchangers.
In order to prevent blockage by solidification, a high temperature can be maintained near the point where the detergent composition is fed into the mold.
Multiple individual controllable heating means or cooling means may be provided at different locations of the device. A stepped temperature profile can then be provided in the direction in which the detergent composition flows. For example, the temperature may increase or decrease step by step.
Detergent compositions are often in the form of solid particulates (eg pellets), which are then extruded and stamped in the milling process or melted and cast in the casting process. Known injection molding apparatuses used in the plastics industry generally use particulate plastic starting materials that easily flow out of the hopper. In contrast, the detergent composition in particulate form can be sticky and flow relatively poorly. Thus special means may be necessary to ensure a good supply of detergent composition to the device.
We also observed that some detergent compositions were prepared and supplied in a hot molten state. Accordingly, there is a need for means for supplying a liquid detergent composition to a means for applying pressure to the detergent composition.
Accordingly, the present invention forms a detergent bar comprising means for applying pressure to the detergent composition to deliver the detergent composition to the mold and substantially individual means mounted for supplying the detergent composition to the means for applying pressure to the detergent composition. Provide the device.
The supply means are substantially individual in that no part of the supply means plays any important role in applying pressure to the detergent composition. Of course, the supply means is suitably fluidly connected to the means for applying pressure to the detergent composition, whereby the detergent composition can be easily supplied as a means for applying pressure.
Examples of suitable feeding means are conveyors, containers with tapered lower sections, stirrers, ram feeders, screw feeders or any number of combinations thereof.
In one preferred embodiment, the detergent composition is supplied to the supply means in substantially solid (eg particulate) or semisolid form. “Particulate forms” include pellets, flakes, noodle, granules and chips, as is well known in the art.
When the detergent composition is supplied in a substantially solid form, heating means may be required to heat the material in the device (eg, reservoir in the case of a lap extruder device) to be fluid and / or maintained under pressure.
If the detergent composition is supplied in substantial fluid form, a cooling zone may be used instead of or in addition to the heating zone. If the molten feed is fed at a temperature above 70 ° C., it is preferably cooled before being delivered to the mold. Of course, it is appreciated that the detergent composition can be introduced into the mold at temperatures above 100 ° C. Moreover, heating devices can be used to maintain these high temperatures.
Being able to supply a continuous supply of detergent composition is a desirable property of the supply device.
The means for supplying the detergent material may supply the composition to a means for applying pressure or to a zone before the means for applying pressure, such as a heating or cooling zone. In one preferred embodiment, the means for supplying the detergent material feeds the composition into the accumulator zone which provides an interface between the continuous operation of the feeder and the discontinuous injection cycle of the means of applying pressure.
Means for controlling the temperature of the detergent composition may be provided at any location within the injection molding apparatus. For example, such heating or cooling means may be provided in the means for applying pressure, in the supply means or in the individual zones, or in any combination thereof. Individual heating zones may be located, for example, between the means for supplying detergent material and the means for applying pressure.
The present invention provides the use of a screw extruder as part of supply, pressure application or both as part of an injection molding apparatus. In a reciprocating injection molding machine, the means for applying pressure to the prepared (eg heat heated) material is provided by the screw itself. Typically, the screw can move along its axis away from the mold. As the flowable material is transferred into the accumulation zone at the end of the screw barrel, the resulting pressure causes the screw to push back. In order to apply pressure to the accumulated molten material ("shot"), the screw is directed towards the accumulation zone (typically using hydraulic pressure) whereby pressure is applied on the material there and the nozzle is inserted into the mold. Move through. A check valve or specially designed strand tip prevents material from flowing back into the screw vanes.
Means for applying pressure to the detergent composition may include a tip of a screw extruder, as described above for known injection molding apparatus. In addition, individual means for delivering the detergent under pressure can be used and are described below.
Preferably, the means for supplying the detergent composition comprises a feeder in the form of a screw feeder. This has been found to provide particularly smooth feeding.
Screw geometry can be designed to suit the composition to be processed. The speed of rotation of the screw or screws can be controlled to provide a satisfactory flow rate of material to the means for applying the accumulation zone or pressure without applying undesirable shear to the detergent.
There is a particular problem with fluid detergent compositions. Single screw extruders rely on drag flow for conveying, so in order to convey fluids they are specially designed to have a close clearance and / or incline to assist gravity in the forward flow of the material. Need to be. It is therefore desirable to have two swollen screws with self-wiping blades intermeshing, preferably providing a positive displacement for the detergent composition to move forward. The screw can rotate in the opposite direction (reverse rotation) but preferably rotates simultaneously to reduce the reverse pressure flow. Such twin screw extruders with interlocking wings for delivering liquids or solids are known to the skilled person.
It may be desirable not to use a displacement screw to apply pressure to the detergent composition to deliver the detergent composition to the mold. Instead, a pressure chamber can be provided that includes one or more walls defined by a piston that can accumulate and move the volume of the pressure chamber to increase or decrease its volume.
In one preferred embodiment, in addition to the feed material for injection molding in the means for applying pressure, the screw extruder also performs the function of preconditioning the material in the desired physical state for injection. By providing one or more heating and / or cooling zones in the screw extruder, and selecting the appropriate screw, screw arrangement and screw speed, for example, the material fed into the extruder can be characterized by the particular injection molding process used and the properties of the product to be sought. It can be mixed uniformly and structured to the extent necessary for For example, one preferred embodiment of the present invention requires the material to be injected in a substantially semisolid state.
In addition, the feeder, preferably the screw extruder, may comprise an intermediate port for adding degassing and / or additional components. For example, additives such as dyes and fragrances and other benefit agents may also be added through the intermediate pot, depending on the length of the screw feed.
Using a screw feed with a temperature profile, the components and / or additives and / or benefit agents can be added to the bulk flow rate of the material in the feeder at a particular temperature. In addition, the materials in the screw feed moving inside the screw feed may be mixed or / or structured large or small, depending on the apparatus and processing parameters used. Thus components and / or additives and / or benefit agents may be added to the bulk flow rate of the material at selected degrees of viscosity and / or mixing and / or structuring.
Moreover, soap formation (eg saponification) or soap detergent surfactant formation (eg neutralization of anionic surfactant acid precursors) occurs in the screw extruder, more specifically in the first part of the screw extruder. Can be.
In addition to degassing, gas (eg air) may also be added to the detergent composition that is injection molded, for example to produce reduced density or floating bars. Preferably, gas is added at the screw extruder stage.
<Injection nozzle>
The means for applying pressure to the detergent composition can be connected to the mold by simple passages or passages with connections to the backflow prevention means or bypass ducts for rapid withdrawal of the pressurizing means and smooth operation of the device after the mold has been filled. have.
However, in one preferred embodiment, the detergent composition is fed through a nozzle whose length is a significant proportion of the length of the internal volume of the mold (1/2 or more, preferably 3/4 or more). The inventors have found that simply filling may be problematic by jetting or snaking the material in the mold. It has been found that good filling is possible by extending the nozzle substantially to the distal end of the mold. Preferably, the nozzle and the mold move relative to each other while the detergent composition is supplied. The mold may move relative to the means for applying pressure while the detergent composition is being supplied and / or the nozzle may move relative to the mold. The speed at which the nozzle and the mold move relative to each other is preferably matched to the detergent delivery rate such that the nozzle is directly below the surface of the detergent composition in the mold. It was found that this leads to particularly good filling. In one preferred embodiment, the nozzle moves relative to the mold.
The nozzle may be neatly heated or preheated, for example, to prevent a portion of the detergent composition from solidifying (invading) in the nozzle to prevent smooth delivery of the composition to the mold.
Preferably, the diameter of the injection nozzle for use with the means for delivering the detergent composition under pressure is small. Preferably the diameter is a circular cross section as 1 to 20 mm, preferably 5 to 10 mm, most preferably about 8 mm.
<Mold>
The mold of the present invention may be made of any suitable material, for example a rigid material having good mechanical strength. For the purpose of rapid cooling, materials with high thermal conductivity may be desirable. Preferably the mold is a metal and its alloys (for example steels comprising aluminum, brass and other copper alloys, carbon and stainless steel), sintered forms of metals or metal composites, ceramics, composites and porous or foam forms And a material selected from nonmetallic materials such as thermoset plastics.
The mold can be made of rigid and non-rigid material, for example non-rigid plastic can be used. The mold may form part or all of the packaging of the detergent bar product. In this regard, the packaging may be rigid or may be non-rigid, such as, for example, a wrapper. For example, the inner lining of the rigid mold may include a packaging for the detergent bar product such that the packaged bar is released from the mold. The mold may also include an expandable lining in the cavity defined by the mold, and the lining expands to fill the cavity as the detergent composition is delivered to the mold. Such linings and packaging materials that can be released with the bar can be a necessary part of product packaging, or can be removed when the bar is released, for example they can only be used to facilitate easy release of the bar from the mold. .
The mold may be precooled or preheated before delivering the detergent composition to the mold. The inner surface of the mold can be preheated, for example, to a temperature above the delivery temperature and / or melting temperature of the composition. It has been found that this preheating of the mold gives the bars a flatter and more polished finish.
After detergent delivery, the mold can be cooled to promote rapid solidification of the detergent. For example, any suitable coolant such as air, water, ice, solid carbon dioxide or combinations thereof may be used depending on the cooling rate and the final temperature required. Preferably, at least a portion of the outer surface of the mold is provided with means for improving the cooling efficiency of the mold after injection. In a preferred embodiment of the invention, such means comprises a jacket for the circulation of fins or ribs or coolant liquid for air cooling.
The mold suitably includes two or more complementary rigid dies suitable for each other and mounted to withstand injection and holding pressures, each die corresponding to each part of the desired shape of the molded article, defining a cavity The die corresponds to the overall shape of the molded article when engaged along the contact portion of its edge. Multiple part molds comprising two or more die parts can be used to produce a wide variety of three-dimensional shapes, such as circular, elliptical, square, rectangular, concave or any other desired shape.
In a mold comprising two or more die portions, one or more said dies may be provided with sealing means along the contact portions of their edges. More specifically, the sealing means comprises an elastomeric gasket.
Provide the mold with a size and shape that can vary depending on the interior surface, ie the shape of the final product. The inner surface of the mold may be partially or fully coated with a material having good release properties, such as low surface energy, or other properties, as described, for example, in International Patent Application Publication No. 97/20028. Examples of such materials are fluoroplastics and fluoropolymers, silicones, and other elastomeric materials. The thickness of the coating is preferably less than 1 mm, more preferably less than 50 μ. The inner surface of the mold can be flat, concave, convex or any other shape desired. It may be shaped to comply with bar shrinkage without damaging the final bar appearance, for example a very convex surface may be used.
The inner surface of the mold is optionally provided with a mirror image of the desired name or logo or number on the surface of the molded article as protrusions or settlements.
In order to ensure easy removal of the article from the mold without twisting or damaging the article on the article, it may be devised to properly tilt the mirror image edge of the article without being exactly perpendicular to the die surface. In order to further prevent distortion or damage to the name or logo or number, there should be no burrs and blemishes on the inner die surface and preferably be carefully polished.
Leakage of material from the mold comprising the die portion can be prevented by, for example, lapping or providing a gasket to tightly match the bonding surface of the die. For high viscosity materials, a flat surface contact is sufficient. The two dies may be joined to each other using nuts and bolts or by some kind of clamping mechanism, for example a hydraulic mechanism. In addition, the outer surface of the die portion can slide along the inclined surface into individual housing means allowing the mold to withstand lateral forces. Good sealing is important when high application and holding pressures are used.
Typically, the mold has a gate through which the opening in the mold through which the detergent composition can be delivered to the mold cavity. Here, the gate may be open on one side towards the mold cavity and the other side may be engaged directly or indirectly with the pressure application means.
The detergent composition may be delivered from the pressure application means through the spout (or infusion) channel. Here, it may be advantageous to heat or cool the mouth channel. The detergent composition can be delivered directly to the mold without any hot channel. For example, the detergent composition can be delivered directly through the nozzle.
The mold may comprise a neck, ie a short channel separated from the mold cavity by a gate. The detergent composition can be delivered through the mold neck. In addition, a nozzle may be introduced into the mold cavity through the neck and the gate to deliver the detergent composition.
In a mold comprising a die portion, the gate and / or neck may be entirely present in one die portion or formed over the engagement of two or more die portions. The gate is open on one side towards the cavity and the other side is mounted to engage the means for applying pressure as appropriate by a nozzle introduced into the mold through the neck.
The mold can be designed so that it can be closed as soon as it is filled or as soon as the material in the mold solidifies to the extent that the outer cell is formed. By manufacturing the mold so that air does not leak out, the shrinkage effect is controlled. In one preferred embodiment, the gate is open while pressure is continuously applied by means of applying pressure. The mold can be closed at the gate while the material inside the mold is still under pressure.
The process is continued by circulating a plurality of molds throughout a feed station, which leads to a step in which the detergent composition is injected into each mold under pressure and subsequently cooled to solidify the material and then deformed before recycling. It can be done in a manner.
In a mold comprising a die portion, the die portion may be designed to be of a different degree to the adhesion of the solidified detergent bar. This gives flexibility to the means by which the bar is released from the mold as the die cracks. Differential attachment to the solidified bar to the die can be achieved, for example, by coating a particular die portion without coating other portions as described above, or by using coatings with different release properties.
<Exhaust ball>
In an injection molding process, it is generally necessary to provide means for venting, ie removing air from the mold as it is filled. Mold evacuation is, for example, a technique used in various known injection molding processes in the thermoplastic industry, and such techniques may also be suitably used in the present invention as will be appreciated by those skilled in the art.
In the present invention, mold evacuation can be achieved by simply providing an evacuation means such as, for example, small pores (s) or slit (s) in the mold. The vent hole may be formed by joining two or more die portions of the mold.
In addition, the vent hole may be an integral part of the mold or die. The vent hole may be closed at the point where the detergent composition filled in the mold solidifies. In addition, a small amount of detergent material may exit the mold through the vent hole, which is subsequently removed. The venting means are also openable and open while the mold is being filled and closed as soon as the mold is filled. Adopting a suitable shape for molding and logo can also facilitate air flow from the mold.
The present invention can also provide exhaust by introducing a porous material inside the mold. Porous material herein is any material that is porous or permeable with pores in the range of 2 to 500 μm in diameter. Preferably the pore is in the range from 5 to 50 μ, in particular from 10 to 20 μ.
The porous material may form part or all of the mold or die portion. For example, only the logo can be made of porous material. Molds made of a porous material can be used to form the bars from the detergent composition delivered in a molten and unmelted state.
A porous material suitable for use in the mold as the exhaust means is Metapor F100 AL, microporous air permeable aluminum (manufactured by Portec, North America, a division of NEST Technologies or Portec, Ltd., Switzerland). Another porous die material may be Porcerax II, Porous Steel (Mold Steel, Inc., Erlanger, KY). The mold release can also be facilitated by, for example, pressing the porous die after the mold has been filled and the detergent composition has solidified to an appropriate degree.
In one other embodiment, the present invention removes the air present in the mold with a vacuum or partial vacuum during filling, or more preferably before filling.
In one preferred embodiment of the invention, the nozzle is equipped with means to allow air to escape from the mold when the nozzle delivers material to the mold. Preferred means are channels that extend parallel to the length of the nozzle. This channel is suitably extended to most of the length of the nozzle, but preferably does not extend directly to the tip of the nozzle. As the nozzle delivers the detergent composition into the mold cavity, air can flow out of the mold along these channels. In one preferred embodiment, the nozzle is withdrawn from the mold cavity when the cavity is filled. When the nozzle reaches a point at substantially the same height as the gate of the mold, the channelless portion of the nozzle tip provides an effective air seal. This allows the holding pressure to be applied as required.
<Bar composition>
Suitable detergent compositions for injection molding are
(A) 10 to 60% by weight of synthetic soap detergent,
(B) 0 to 60% by weight of a water-soluble structural agent having a melting point of 40 to 100 ° C,
(C) 5 to 60% by weight of a water-insoluble structuring agent having a melting point of 40 to 100 ° C,
(D) 1 to 25% by weight of water,
(E) 1 to 20% by weight of one or more amphoteric and / or zwitterionic surfactants (based on the total composition),
(F) 0 to 20% by weight of one or more nonionic surfactants (based on the total composition),
(G) 0-60 wt% soap,
(H) other optional ingredients as described below,
(I) 0 to 10% by weight total electrolyte.
Synthetic detergents suitable for use in the process of the invention include C ₈ -C ₂₂ aliphatic sulfonates, aromatic sulfonates (eg alkyl benzene sulfonates), alkyl sulfates (eg C ₁₂ -C ₁₈ alkyl sulfates) Pate), alkyl ether sulfates (eg, alkyl glyceryl ether sulfates).
Suitable aliphatic sulfonates are, for example, primary alkanes sulfonates, primary alkanes disulfonates, alkenes sulfonates, hydroxyalkanes sulfonates or alkyl glyceryl ether sulfonates (AGS).
Other anionic surfactants that may also be used include alkyl sulfosuccinates (including mono- and dialkyls, such as C ₆ -C ₂₂ sulfosuccinates), alkyl and acyl taurates, alkyl and acyl sarcosinates , Sulfoacetates, alkyl phosphates, alkyl phosphate esters, alkoxy alkyl phosphate esters, acyl lactates, monoalkyl succinates and maleates, sulfoacetates.
Another surfactant that can be used is acyl isethionate (eg C ₈ -C ₁₈ ). These esters are prepared by reaction between mixed aliphatic fatty acids having 6 to 18 carbon atoms and less than 20 iodine levels and alkali metal isethionates. At least 75% of the mixed fatty acids have 12 to 18 carbon atoms and up to 25% have 6 to 10 carbon atoms. Acyl isethionate may be an alkoxylated isethionate as described in US Pat. No. 5,337,466 (Ilardi et al.), Which is incorporated herein by reference.
The anionic surfactants used are preferably mild, ie strarum corneum, surfactants which do not damage the outer skin layer. Rough surfactants such as primary alkanesulfonates or alkyl benzene sulfonates are generally avoided.
Suitable water soluble structuring agents include moderately high molecular weight polyalkylene oxides and especially polyethylene glycols or mixtures thereof having a suitable melting point (eg 40 to 100 ° C., preferably 50 to 90 ° C.). Polyethylene glycols (PEG's) used have molecular weights of 2,000 to 25,000. Water soluble starch is also included.
Suitable insoluble structurants are generally unsaturated and / or branched long chain (C ₈ -C ₂₄ ) liquid fatty acids or ester derivatives thereof, and / or unsaturated and / or branched long chain liquid alcohols or ether derivatives thereof. It may also be a short chain saturated fatty acid such as capric acid or caprylic acid. Examples of liquid fatty acids that can be used are oleic acid, isostearic acid, linoleic acid, linolenic acid, ricinoleic acid, elideic acid, arycitonic acid, myristolic acid and palmitolic acid. Ester derivatives include propylene glycol isostearate, propylene glycol oleate, glyceryl isostearate, glyceryl oleate and polyglyceryl diisostearate.
Examples of alcohols are oleyl alcohol and isostearyl alcohol. Examples of ether derivatives are isosteareth or oleth carboxylic acid, or isosteareth or oleth alcohol. Examples of suitable zwitterionic surfactants for use in the composition may be broadly described as derivatives of aliphatic quaternary ammonium, phosphonium, and sulfonium compounds, and the aliphatic radicals may be straight, branched, aliphatic alicyclic One has from about 8 to about 18 carbon atoms and includes, for example, anionic groups such as carboxy, sulfonate, sulfate, phosphate, or phosphonate.
Amphoteric surfactants that may be used in the present invention include one or more acid groups. It may be a carboxylic acid or sulfonic acid group. These include quaternary nitrogen and consequently quaternary amido acids. They should generally contain alkyl or alkenyl groups having 7 to 18 carbon atoms. Suitable amphoteric surfactants are simple betaines or sulfobetaines.
Ampoacetates and diampoacetates are also intended to be included in the possible zwitterions and / or amphoteric compounds that may be used.
In addition to the one or more anionic and amphoteric and / or zwitterions, the surfactant system may optionally include nonionic surfactants in amounts of up to 20% by weight.
Nonionics that can be used are, in particular, reaction products of ethylene oxide and alone ethylene oxide with compounds having hydrophobic groups and reactive hydrogen atoms such as, for example, aliphatic alcohols, acids, amides or alkyl phenols, with alkylene oxides, in particular propylene oxide There is this. Certain nonionic detergent compounds include alkyl (C ₆ -C ₂₂ ) phenol-ethylene oxide condensates, condensation products of aliphatic (C ₈ -C ₁₈ ) primary or secondary linear or branched alcohols with ethylene oxide, and propylene oxide And a product produced by a condensation reaction of a reaction product with ethylenediamine and ethylene oxide. Other so-called nonionic detergent compounds include long chain tertiary amine oxides, long chain tertiary phosphine oxides and dialkyl sulfoxides.
Nonionics may also be sugar amides such as polysaccharide amides. Specifically, the surfactant may be one of the lactobionamides described in US Pat. No. 5,538,279 (Au et al.) And may be one of the sugar amides described in US Pat. No. 5009814 (Kelkenberg), supra. Are incorporated herein by reference.
Other surfactants that may be used are alkyl polysaccharide nonionic surfactants as described in US Pat. No. 3,373,325 (Parran Jr.) and as described in US Pat. No. 45,656,47 (Llenado), which documents are described herein. Cited by reference.
The nonionic surfactant may also be a water soluble polymer chemically modified with a hydrophobic moiety or residues. For example, hydrophobically modified PEGs such as EO-PO block copolymers, POE (200) -glyceryl-stearate can be included in the compositions claimed by the present invention. The composition may further optionally comprise up to 60% soaps prepared by the general soap making procedure. For example, saponification products of natural materials can be used, such as animal oil, coconut oil, palm oil, rice bran oil, fish oil or any other suitable source of long chain fatty acids. The soap may be pure soap or medium phase soap.
In addition, the compositions of the present invention may be used in organic solvents such as ethanol or propylene glycol, carboxymethylcellulose, magnesium aluminum silicate, hydroxyethylcellulose, methylcellulose, carbopol, glucamide, or antyl (Antil®, Rhone Poulenc). Secondary viscous agents, such as fragrances, tetrasodium ethylenediaminetetraacetate (EDTA), EHDP or metal sequestering agents such as mixtures in amounts of 0.01 to 1%, preferably 0.01 to 0.05%, and colorants, Opaques, and any such as pearlizers such as zinc stearate, magnesium stearate, TiO ₂ , EGMS (ethylene glycol monostearate) or Litron 621 (styrene / acrylate copolymer) Components may be included, all of which are useful for improving the appearance or aesthetics of the product.
The composition may further comprise antibacterial agents such as 2-hydroxy-4,2 ', 4'-trichlorodiphenylether (DP300), preservatives such as dimethyloldimethylhydantoin (glydant XL1000), parabens, sorbic acid, and the like. .
The composition may also include coconut acyl mono- or diethanol amides as suds accelerators, and strong ionizing salts such as sodium chloride and sodium sulfate may also be used advantageously. Preferably such electrolyte is present at 0 to 5% by weight, preferably less than 4% by weight.
For example, an antioxidant such as butylated hydroxytoluene (BHT) may advantageously be used in an amount of about 0.01% or higher where appropriate.
Cationic modifiers that may be used include Quatrisoft LM-200 Polyquaternium-24, Merquat Plus 3330-Polyquaternium 39, and Jaguar®. ) There is a type regulator.
Polyethylene glycols that can be used include Polyox WSR-205 PEG 14M, Polyox WSR-N-60K PEG 45M, Polyox WSR-N-750 PEG 7M and Carbowax Sentry (CARBOWAX SENTRY, Union Carbide) PEG having a molecular weight of 300 to 10,000 Daltons, such as those sold under the trade name.
Thickeners that can be used include Amerchol Polymer HM 1500 (nonoxynyl hydroethyl cellulose), glucam DOE 120 (PEG 120 methyl glucose dioleate), Revoderm® from Rewo Chemicals (PEG) Modified glyceryl cocoate, palmate or tallowate), Antil® 141 (Goldschmidt), clay and paraffin wax.
Another optional component that may be added is a polymer for deagglomeration, such as that taught in US Pat. No. 5,514,76, incorporated herein by reference.
Other ingredients that may be included are exfoliants such as polyoxyethylene beads, walnut shells and apricot seeds. Detergent compositions of the present invention may include typically known additives such as perfumes and colorants.
<Additives and benefit agents>
In order to improve the consumer perception of the bars, it may be desirable to introduce benefit agents and / or other additives into the composition. A skin benefit agent is defined as a product that can be included in a detergent composition that, when applied to the skin, deposits on the skin to impart or maintain the desired properties to the skin.
It is particularly preferable that the detergent composition used in the present invention include a benefit agent such as, for example, a moisturizing component.
Typically, such beneficial ingredients are of a nature that is substantially incompatible with the detergent composition and are preferably present in the form of separate zones. If the detergent composition is in a fluid state, such as in the casting process, any density difference between the beneficial component and the fluid detergent mixture may cause phase separation present in the molding after casting in the control system. The benefit agent may be present on a single component or with some components of the composition.
One of the problems with benefit agents is that the benefit agents are washed off by the bubbles of surfactant before they are deposited on the skin. One way to avoid this is to disperse the benefit agent in the bar unevenly, such as, for example, so that the benefit agent is directly transferred when the bar is rubbed onto the skin. It is widely accepted that more benefit agents are deposited on the skin when the benefit agents are disproportionately dispersed.
Moreover, in order to provide optimal deposition to the skin during the cleaning process, it may be desirable to control the size of the zone occupied by the beneficial component in the finished bar product. In fluid systems, it is difficult to stabilize droplets of a particular size.
Such zones may be between 1 μ and 5 mm in size. Preferably, the zone is 15 to 500 microns in size, as described, for example, in WO 96/02229. More preferably, the zones are 50 to 200 microns in size.
The inventors have found that the method of the present invention is particularly suitable for introducing a benefit agent into the detergent composition, especially when the detergent composition is in a semisolid state. Preferably, the benefit agent is added to the detergent composition in a means for supplying the detergent composition. If the means for supplying the detergent composition comprises a screw feeder, the benefit agent may be added at any suitable position along the screw feeder. Using the device of the present invention, if a temperature profile is present in the device, the temperature at which the benefit agent is added can be selected. Thus, beneficial components can be introduced into the bulk flow of the selected viscosity. By using appropriate apparatus and process parameters, benefit agents may also be introduced into the bulk flow of material with a selected degree of mixing and structuring.
The shear (mixing) the material undergoes after blending can also be controlled and used to control the size of the benefit agent zone. We have found that the benefit agent added by the method of the present invention may appear as a non-spherical domain in the final detergent composition bar. In general, the domain is extended.
For example, what is produced that includes materials such as benefit agents that are substantially incompatible with the detergent composition will be essentially a two-phase system. One phase will simply consist of a benefit agent and the other phase will consist of a detergent composition. In addition, benefit agents may interact with one or more components of the detergent composition to form individual benefit agent containing phases.
Thus, in another aspect, the present invention provides a detergent bar which can be obtained by the process of the present invention and comprises a component of a property such as detergent composition and benefit agent that is not mixed with the detergent composition, wherein the non-mixable component is It exists as a nonspherical domain. Other ingredients, such as perfumes or colorants, can be introduced in the same way.
Benefits include ingredients that moisturize, condition or protect the skin. Suitable benefit agents include, for example, moisturizing ingredients such as emollients / oils. Emollient oil means a substance that softens the skin, retards the decrease in the moisture content of the skin, and / or keeps it soft by protecting the skin.
Preferred benefit agents
Silicone oils such as linear and cyclic polydimethylsiloxanes, gums and variants thereof, amino, alkyl, alkylaryl and aryl silicone oils (the silicone oils used may have a viscosity of 1 to 100,000 centistokes),
Jojoba, soybean, rice bran, avocado, almond, olive, sesame, persic, castor, coconut, mink, peanut, wheat, cottonseed, palm kernel, rapeseed, safflower seed and sunflower oil, cocoa butter, Bovine oil, lard, natural fats and oils such as light oil obtained by hydrogenating the oils, and fats and oils comprising synthetic mono, di and triglycerides such as glycerides and 2-ethylhexanoic acid glycerides,
Waxes such as carnauba, spermaceti, beeswax, lanolin and derivatives thereof,
Hydrophobic plant extract,
Hydrocarbons such as liquid paraffin, petrolatum, microcrystalline wax, sericin, squalene and mineral oils,
Higher alcohols and fatty acids such as behenic acid, palmitic acid, stearic acid, lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, cholesterol alcohol and 2-hexadecanol alcohol,
Cetyl octanoate, cetyl lactate, myristyl lactate, cetyl palmitate, butyl myristate, butyl stearate, decyl oleate, cholesterol isostearate, myristyl myristate, glyceryl laurate, glyceryl ricinolate Glyceryl stearate, alkyl lactate, alkyl citrate, alkyl tartrate, glyceryl isostearate, hexyl laurate, isobutyl palmitate, isocetyl stearate, isopropyl isostearate, isopropyl laurate, iso Esters such as propyl linoleate, isopropyl myristate, isopropyl palmitate, isopropyl stearate, isopropyl adipate, propylene glycol monolaurate, propylene glycol ricinolate, propylene glycol stearate and propylene glycol isostearate,
Fish oil, menha, jasmine, camphor, white ginseng, bitter orange peel, ryu, terebin, cinnamon, bergamont, citrus unshiu, irises, sol, lavender, laurel, cloves , Hiba, eucalyptus, lemon, cranberry, thyme, peppermint, rose, sage, menthol, cineole, eugeniol, citral, citronelle, bro Essential oils such as renol, linalool, geraniol, primrose, camphor, thymol, spirantol, pinene, limonene and terpenoid oil,
Lipids such as cholesterol, ceramides, sucrose esters and pseudo-ceramides as described in EP 556 957,
Vitamins such as vitamins A and E, and vitamin alkyl esters including vitamin C alkyl esters,
Sunscreens such as octyl methoxyl cinnamate (Parsol MCX) and butyl methoxy benoylmethane (Parsol 1789), phospholipid and mixtures of any of the above ingredients.
If the softener can also serve as the structuring agent, the softener (which acts as softener or structuring agent) must not exceed 20% by weight, preferably 15% by weight of the composition, so that the structuring agent is 15% oleyl alcohol. In this case, it should be understood that oleyl alcohol as an emollient should be added up to 5% so as not to be included in duplicate.
Softeners / oils are generally used in amounts of 1 to 20% by weight, preferably 1 to 15% by weight of the composition. Generally, it should be included up to 20% by weight of the composition.
The invention is further described by the accompanying drawings.
<Example 1>
SANDRETTO series 7 HP135 with three temperature controlled zones was purchased and used as a reciprocating screw injection molding facility according to FIG. 1. The machine was equipped with a 50 mm diameter dough molding compound screw and barrel. The supply means included conventional stuffing pots, or manual feeders suitable for the material. Screw rotation speed was 80-100 rpm.
The mold 9 consisted of a pair of aluminum mold parts defining a bar shape. It was the same as conventionally used in die stamping of detergent bars, which was adapted by providing a feed hole that was as large as the nozzle was taken, and the pore at the proper location in the mold caused the air to escape during filling. Detergent compositions A, B and C were injection molded.
Composition A was as shown in the table below.
Net weight% Directly esterified fatty isethionate27.00 Palmitic / Stearic Acid Blend17.00 Coco Amido Profile Betaine5.00 Maltodextrin10.00 Sodium stearate6.00 PEG 800021.62 PEG 3002.05 PEG 14504.95 water4.50 Sodium isethionate2.16 Hydrophobic additives (preservatives, colorants, pigments, etc.)1.72 all100.0
Composition B included a ground commercial UK Lux white soap dated September 1996.
Composition C included a milled commercial Dove cosmetic bar dated June 1996.
The detergent composition was fed to the stuffing pot in the form of small particulates (grain size approximately 1-10 mm). Such particulate material could be obtained by slicing a commercial bar or using a commercially available chill roll or plotter / noodle device. In the same apparatus, the detergent composition was fed into the installation by hand. The detergent composition was then injected into the mold using an injection molding apparatus. The detergent composition was semisolid when the detergent composition was introduced into the mold. The mold was precooled in ice / water and dried before filling. After a few minutes at ambient conditions, the mold was removed from the injection molding machine and opened. The properties of the bars were evaluated in terms of ease of release from the mold and appearance of the surface. The results are shown in Table 1 below. It has been found that the injection molding apparatus of FIG. 1 is suitable for preparing a detergent bar with a good surface appearance which is easily released from the mold after a short time and satisfactory.
<Example 2>
The apparatus according to FIG. 2 was used comprising a 40 mm diameter screw and a BETOL co-rotating twin screw extruder with eight temperature controlled zones. The temperature of the connecting valve 17 and the injection head assembly 18, 19, 20 was also controlled.
A new piston type injection plant according to the invention was mounted at the end of a screw extruder. The detergent composition as described below was in molten form and fed to the extruder using a Bran and Luebbe metering pump. The molten feed had a temperature of 90-95 ° C. It was kept in a feed pot that was stirred and heated.
During filling, the mold was moved manually or hydraulically using the mold mechanism according to FIG. 4 herein.
Detergent compositions D and E were injection molded.
Composition D was shown in the table below.
Net weight% Directly esterified fatty isethionate38.0 Propylene glycol21.5 Sodium stearate12.2 Sodium palmitate12.2 water16.1 all100.0
Composition E was shown in the table below.
Net weight% Directly esterified fatty isethionate27.8 Sodium stearate14.6 Propylene glycol17.8 Stearic acid12.8 PEG 80009.7 Coco Amido Profile Betaine4.9 Paraffin wax2.9 Sodium isethionate0.4 water5.6 Small amount additives (preservatives, fragrances, pigments, etc.)2.5 all100.0
The apparatus was used to form a detergent bar at any temperature range and subsequently release from the mold and check mold release properties and surface quality. The results are shown in Table 2. It became clear that the apparatus of FIG. 2 can be used to produce good detergent bars.
CompositionZone Temperature (℃) Inlet Middle OutletCharge temperature (℃)Mold volume (ml)Mold temperature before filling (℃)Ease of ReleaseSurface appearance A40 50 5050To 7510-15Very easyExcellent B45 55 6560.6To 7510DragonSatisfied; flowline visible; good gloss C40 50 5046.8To 10011DragonSatisfaction, somewhat visible flow line
CompositionZone temperature (℃) ( ^* 1)Charge temperature (℃)Mold volume (ml)Mold temperature before charging (℃) ( ^* 2)Ease of ReleaseSurface appearanceRemarks D32, 100, 80, 70, 70, 70, 70, 70, 45, 45491007DragonGood; slight flow lineMove the mold manually E30, 100, 80, 70, 70, 70, 65, 35, 55, 554710010Sticky or DeformedsatisfiedHydraulically move the mold E30, 100, 80, 70, 70, 70, 62, 47, 60, 606075-5DragonGoodHydraulically move the mold E27, 100, 80, 73, 65, 61, 37, 45, 60, 60617520Very little adhesiveGoodHydraulically move the mold^* 1 temperature zones were 1, 2 (supply), 3, 4, 5, 6, 7, 8 (mixing elements), 9 (valve connection and injection head), 10 (cylinder). ^* 2 by cooling the mold is in contact (for temperatures in excess of 10 ℃) (for the temperature in the -5 ℃ zone) Mold solid carbon dioxide, ice / water bath (for temperatures below 10 ℃) and water or ambient air, and Accomplished.
<Example 3>
A device comprising a Betol co-rotating twin screw extruder with a 40 mm diameter screw, eight temperature control zones, and a low shear inline injection head was used as depicted in FIG. 3. Detergent composition E was made into molten form (95 ° C.) and placed in a stirred heating feed pot. It was then fed into zone E of the extruder using a Bran and Lueve metering pump. Detergent composition B was fed to Zone D as a 4 mm diameter noodle using a Ktron feeder at room temperature. Maximum injection pressure and retention time were recorded. The results are shown in Table 3.
The detergent composition was semisolid when the detergent composition was introduced into the mold. In all experiments, the mold was at room temperature before filling and cooled by keeping the mold at room temperature for an additional 5 minutes in addition to the packing of solid phase CO ₂ around the outside of the mold for the specified time.
It has been found in these experiments that the surface quality of the bar can be improved without damaging the release of the bar from the mold by using the holding pressure after filling.
CompositionZone temperature (℃) ( ^* 1)Charging temperature (℃)Mold volume (g)Solid phase CO ₂ cooling (min)Ease of ReleaseRetention time (s)Injection pressure (psig)Exterior E70, 70, 70, 70, 70, 70, 70, 70, 70, 70701002Dragon644Slippery surface; good bar E31, 95, 80, 70, 60, 50, 45, 55, 55, 55531250.5Slight adhesion on one side0206Mainly ripples on one side E31, 95, 80, 70, 60, 50, 45, 55, 55, 55531250.5DragonOne260Very small ripples E31, 95, 80, 70, 60, 50, 45, 55, 55, 55521250.5Dragon6204Ripple member; very good surface E31, 95, 80, 70, 60, 50, 45, 55, 55, 55531250.5Dragon6234Ripple member; very good surface B50, 50, 50, 50, 50, 50, 50, 50, 50, 50501000.5Dragon6771Satisfaction; some streamline^* 1 temperature zones were 1, 2 (supply), 3, 4, 5, 6, 7, 8 (mixing elements), 9 (valve connections and accumulators) and 10 (injection heads).
<Example 4>
Detergent composition E was injection molded with simultaneous addition of benefit agents.
Using the apparatus of FIG. 3, two silicone oils (viscosities 100 and 60000 centistokes) were introduced into the twin screw extruder in separate experiments. The flow rate of the silicone oil was controlled by a Seepex pump such that the concentration of the silicone oil in the final bar was approximately 2% / 15% by weight. For some experiments, dyes could be added to the silicone oil stream to visually confirm their presence in the bar during the experiment. It was semisolid when the detergent composition was introduced into the mold. The formed bar was easily released from the mold under similar conditions as its control without oil.
The mold was at room temperature before filling and cooling was performed as described in Example 3.
High resolution proton NMR was used to determine the distribution of silicone oil in the bar. NMR measurements were performed on the targets extracted from six different locations in the bar (three internals and three surfaces). The results are shown in Table 4.
Subsequent microscopic analysis showed that silicone oil was present in the bars as zones of irregular shape rather than droplets. Indicators of the average volume of the zones were obtained by warming the sample and letting the oil run through the droplets and measuring their diameter. This was dependent on the viscosity of the oil (the lower the viscosity, the smaller the zone) and the mixing zone of the metering zone (the monotonous helical screw blades provide zones larger than the kneading / mixing components), which allowed control of the size of the zone. Indicates.
CompositionZone temperature (℃)Charging temperature (℃)Silicone oil (cSt)Oil Metering (Zone)Injection pressure (psig)Retention time (s)Solid phase CO ₂ cooling (min)Remarks E32, 95, 80, 72, 65, 60, 55, 55, 55, 555560,00010 weight / wt%G2996OneFlat and dry surface; good filament; slight ripple; easy release E32, 95, 80, 72, 65, 60, 55, 55, 55, 555560,0005 wt /%G3236OneGood to good bar; easy release; oil on mold surface E32, 95, 80, 72, 65, 60, 55, 55, 55, 555560,0002 weight / wt%G3326OneGood to excellent; H ¹ -NMR indicates that silicone oil is present in 1.69-1.95 weight percent (average 1.85 weight percent) E32, 95, 80, 72, 65, 60, 55, 55, 55, 555510015 weight / wt%K3586OneEasy release; good surface; somewhat sticky touch; H ¹ -NMR indicates 14.2-17.7 weight percent (average 15.8 weight percent) of silicone oil E32, 95, 80, 72, 65, 60, 55, 55, 55, 555310010 weight / wt%K3766OneEasy release; slippery residue on mold surface; excellent bar E30, 100, 80, 70, 70, 60, 55, 45, 50, 5050100K Absence of mixing elements; dispersion of mobile phase in bars measured using H ¹ -NMR
<Example 5>
The bars of composition F were formed by injection molding using the apparatus of FIG. 3.
Composition F was as shown in the table below.
Net weight% Directly esterified fatty isethionate7.60 Sodium stearate4.75 SLES-3EO11.87 fatty acid4.26 PEG 80009.49 Coco Amido Profile Betaine11.87 Glycerol Monostearate20.64 Glycerol Monolaurate20.64 water3.79 Sunflower oil4.75 Small amount of additiveresidual all100.00
The detergent composition was semisolid when introduced into the mold. The temperature of the mold at the time of filling was room temperature.
CompositionZone temperature (℃)Charging temperature (℃)Mold volume (g)Solid phase CO ₂ cooling (min)Ease of ReleaseRetention time (s)Injection pressure (psig)Exterior F24, 55, 55, 50, 50, 45, 45, 40, 40, 40401005Difficult to release6232Good bar F31, 70, 70, 55, 45, 35, 35, 35, 35, 3535100OneSlight adhesion to logo0138Good bar
<Example 6>
Two representative body wash detergent compositions G and H were injection molded using a ram extruder as shown in FIG. 5.
Composition G was as shown in the table below.
Net weight% Soap ^* 76.7 water22.0 TiO ₂ 0.3 Spices1.0 all100.0^* Chain length distribution of fat filling of soap is shown in Table 3
Composition H was as shown in the table below.
Net weight% Sodium cocoyl isethionate49.5 Stearic acid20.0 Coconut fatty acid3.0 Sodium isethionate4.7 Linear Alkylbenzene Sulfate (LAS)2.0 Sodium chloride0.4 Soap ^** 8.3 Sodium stearate3.0 Spices1.3 Miscellaneous goods0.7 water7.1 all100.0^** Sodium Tallowate and Sodium Cocoate 82/18 Blend
Chain Length Dispersion of Fat Filler of Soap in Composition G Chain lengthweight% C80.81 C101.06 C1215.70 C145.80 C1638.22 C16: 10.07 C187.05 C18: 126.30 C18: 24.01 C200.19 Etc0.79 all100
The detergent composition was filled into the reservoir and the reservoir was heated until the feed material reached the desired temperature. The die was assembled and the sprue was connected to the gate of injection molding. The other end of the mouthpiece was screwed into the bottom of the reservoir. The spout and mold were heated and maintained at the desired temperature using a blanket-type heater. The temperature of the outer surface of the mold was measured using a washer Fe / K thermocouple.
As soon as the feed temperature and mold temperature reached the desired values, a vacuum pump was connected to the threaded portion of the outlet capillary 60 of the mold and a vacuum was applied to the mold before filling. A moisture trap was provided to the vacuum pump line to prevent moisture from entering the vacuum pump oil. In the vacuum pump line, the vacuum gauge measured the vacuum in the mold cavity.
The plunger 54 was then switched on and the hot feed was injected into the mold at a controlled rate and the speed displayed on the machine panel was mm / min. The rated pressure capacity of the plunger unit was 735 psi and if the pressure exceeded this value, the shutoff system of the unit automatically stopped the plunger.
The pressure measured by the indicator-transmitter 56 was displayed on the machine panel in mV units ranging from 0 to 1013 mV, corresponding to 0 to 735 psi on the injection molding facility. The inline computer recorded the pressure transmitter output in mV over time.
After the mold was filled and the plunger was switched off, the mold still attached to the spout was removed from the reservoir and cooled. Two dies of the mold were opened and the cured detergent bar was expelled.
The mold was cooled with air at about 27 ° C. and 3.6 ms ⁻¹ wind speed under forced circulation air cooling conditions. The feed introduced into the mold was a partially structured semisolid state containing a liquid crystalline phase.
Table 7 shows the preferred operating conditions for injection molding of these compositions.
Optimal operating conditions CompositionFeed temperature (℃)Mold temperature before filling (℃)Measured pressure (psi)Cooling time (min) G909073520 H604073520
It has been found that tablets with good surface finish and satisfactory logo stamp quality can be obtained using the method of the invention discussed above.
The properties of the injection molded compositions for conventional shear applied and extruded detergent bar controls were compared to the end use properties of H. Injection molded and controlled bars were the same weight (about 75 g) and similar shapes (rectangular). Table 8 shows the end use characteristics such as abrasion rate, mush, bubbles, and cracking of the two bars.
Wear rates were similar for the two tablets. The bubble volume for the injection molded bars was larger than for the control. The mash evaluation for injection molded bars was poor. No cracking was observed for both bars.
Evaluation of Injection Molded (I-M) Composition G Compared to Conventional Shear Extruded Balance StandardssizeControl Standard TabletI-M TabletCalc. 't'Table 't'Remarks attritiong28.331.931.92.78Not noticeable attrition%-27.825.125.42.78Not noticeable Depth after 4 daysmm2.74.89.22.78Outstanding Cracking0-14 scale numberNo cracking found on any tablet Bubble in soft water Bubble in hard waterml4133394363849.212.72.782.78Remarkable

权利要求:
Claims (25)
[1" claim-type="Currently amended] A method of forming a detergent bar that delivers a detergent composition to a mold by applying pressure to the detergent composition, wherein the detergent composition is at least partially structured when introduced into the mold.
[2" claim-type="Currently amended] A method of forming a detergent bar for applying pressure to a detergent composition to deliver the detergent composition to the mold, characterized in that the pressure at the point at which the detergent composition is introduced into the mold is at least partially greater than 20 psi during the time it is introduced into the mold.
[3" claim-type="Currently amended] A method of forming a detergent bar in which a temperature of the detergent composition introduced into the mold is less than 70 ° C., applying pressure to the detergent composition and delivering the detergent composition to the mold.
[4" claim-type="Currently amended] The method according to claim 1, wherein the detergent composition introduced into the mold is cooled from and / or through the liquid crystal phase.
[5" claim-type="Currently amended] The method of claim 1, wherein the detergent composition is in a nearly semisolid form when introduced into the mold.
[6" claim-type="Currently amended] The method according to claim 1, wherein the temperature is 40 ° C. to 70 ° C. when the detergent composition is introduced into the mold.
[7" claim-type="Currently amended] The method according to claim 1, wherein the detergent composition is heated during or before being fed into the mold.
[8" claim-type="Currently amended] The method of claim 1, wherein the detergent composition is cooled during or before being fed to the mold.
[9" claim-type="Currently amended] The method of claim 1, wherein the detergent composition is mixed with a component, such as a benefit agent, before the detergent composition is introduced into the mold.
[10" claim-type="Currently amended] 10. The method of claim 9 wherein mixing is performed in a screw extruder.
[11" claim-type="Currently amended] The method of claim 1, wherein the pressure is continuously applied to the detergent composition for a period of time after the mold is filled.
[12" claim-type="Currently amended] The method according to claim 1, wherein the mold is heated before the detergent composition is introduced into the mold.
[13" claim-type="Currently amended] The method according to any one of claims 1 to 12, wherein the mold is degassed before the detergent composition is introduced into the mold.
[14" claim-type="Currently amended] a) a mold for containing the detergent composition,
b) a reservoir for supplying a detergent composition to the mold, and
c) means for delivering the detergent composition to the mold, the detergent bar forming apparatus being capable of delivering the detergent composition at a pressure greater than 20 psi at the point of introduction into the mold.
[15" claim-type="Currently amended] 15. The feed station of claim 14, wherein the detergent composition is delivered under pressure to each mold and subsequently the detergent composition in each mold undergoes a step of cooling and deforming before the mold is recycled again. An apparatus designed to carry out a process in a continuous manner by circulating a plurality of molds throughout.
[16" claim-type="Currently amended] 12. Apparatus for forming a detergent bar comprising substantially individual means mounted to supply the detergent composition to the means for applying pressure to the detergent composition for delivering the detergent composition to the mold and to the means for applying the pressure.
[17" claim-type="Currently amended] 17. The apparatus of claim 16, wherein the feeder comprises a screw feeder.
[18" claim-type="Currently amended] 18. The apparatus of claim 17 wherein the screw feeder comprises two parallel screws with interlocking wings.
[19" claim-type="Currently amended] 19. The apparatus of any one of claims 14-18, further comprising means for adjusting the temperature of the detergent composition.
[20" claim-type="Currently amended] The device of claim 16, wherein the means for supplying the detergent composition further comprises means for mixing the detergent composition with a benefit agent or other additives.
[21" claim-type="Currently amended] 21. The detergent composition of any one of claims 14-20, wherein the length of the nozzle is a substantial proportion of the length of the internal volume of the mold, the nozzle and the mold may move relative to each other while the detergent composition is introduced into the mold, Wherein the detergent composition is fed from the device for applying pressure to the nozzle.
[22" claim-type="Currently amended] 22. The apparatus of claim 21 wherein the nozzle is grooved.
[23" claim-type="Currently amended] A detergent bar obtainable by the method of claim 1.
[24" claim-type="Currently amended] 14. A detergent bar obtainable by the method of any one of claims 1 to 13, comprising a detergent composition and a component present in the non-spherical domain that is incompatible with the detergent composition.
[25" claim-type="Currently amended] A method of introducing an additive or benefit agent into a detergent bar, the method comprising adding an additive or benefit agent to at least partially structured detergent composition and applying pressure to a detergent composition comprising the additive or benefit agent to the mold. .

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同族专利:

---

公开号 | 公开日

---

AU7764598A|1998-12-11|

---

CN1242040C|2006-02-15|

---

IN190299B|2003-07-12|

---

HU0002997A2|2001-02-28|

---

CN1264421A|2000-08-23|

---

AU742860B2|2002-01-17|

---

BR9808811A|2000-07-18|

---

CA2289944C|2005-08-23|

---

ID22987A|1999-12-23|

---

US20010011067A1|2001-08-02|

---

KR100355171B1|2002-10-11|

---

JP2001525881A|2001-12-11|

---

BR9809823A|2000-06-27|

---

EA199901038A1|2000-04-24|

---

WO1998053038A1|1998-11-26|

---

KR100353785B1|2002-09-27|

---

HU0002997A3|2003-02-28|

---

RU2220192C2|2003-12-27|

---

JP2001525880A|2001-12-11|

---

ES2186169T3|2003-05-01|

---

DE69823027D1|2004-05-13|

---

AU7530698A|1998-12-11|

---

JP3633632B2|2005-03-30|

---

CA2289944A1|1998-11-26|

---

ES2217556T3|2004-11-01|

---

EA001627B1|2001-06-25|

---

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---

AU726769B2|2000-11-23|

---

US6800601B2|2004-10-05|

---

PL336976A1|2000-07-31|

---

US20010016566A1|2001-08-23|

---

CZ297819B6|2007-04-04|

---

CA2289762A1|1998-11-26|

---

PL192004B1|2006-08-31|

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CN1262705A|2000-08-09|

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DE69809226T2|2003-07-24|

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EP0983337B1|2002-11-06|

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PL336795A1|2000-07-17|

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US6224812B1|2001-05-01|

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CA2289762C|2003-04-29|

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IN189614B|2003-03-29|

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CN1137982C|2004-02-11|

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EP0985022B1|2004-04-07|

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EP0985022A1|2000-03-15|

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PL189056B1|2005-06-30|

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KR20010012622A|2001-02-26|

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CZ9904044A3|2001-01-17|

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EP0983337A1|2000-03-08|

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WO1998053039A1|1998-11-26|

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DE69809226D1|2002-12-12|

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ID24359A|2000-07-13|

引用文献:

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公开号 | 申请日 | 公开日 | 申请人 | 专利标题

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法律状态:
1997-05-16|Priority to GB9710048.1

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1997-05-16|Priority to GBGB9710048.1A

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1997-12-19|Priority to GBGB9726972.4A

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1997-12-19|Priority to GB9726972.4

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1998-05-04|Application filed by 알 브이 테이트 (로드니 비버스 테이트), 유니레버 엔.브이., 에이치 드로이. 씨. 지. 오닌크, 이. 에디, 산드라 웨드워즈 (에스 제이 에드워즈)

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2001-02-26|Publication of KR20010012621A

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2002-10-11|Application granted

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2002-10-11|Publication of KR100355171B1

优先权:

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申请号 | 申请日 | 专利标题

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GB9710048.1|1997-05-16|

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GBGB9710048.1A|GB9710048D0|1997-05-16|1997-05-16|Process and apparatus for the production of a detergent composition|

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GBGB9726972.4A|GB9726972D0|1997-12-19|1997-12-19|Injection moulding of detergent bars|

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GB9726972.4|1997-12-19|