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    • 专利摘要:
    The present invention includes a first step of mechanically grinding a tablet and a second step of shifting to obtain a powder (the resulting powder comprises less than 4% of particles per 150 micrometers of particles passing through a 150 μm sieve). Characterized in that the present invention relates to a method for producing a powder from tablets having a tensile strength of at least 5 KPa and at least 2% by weight of a surfactant.
    公开号:KR20010070974A
    申请号:KR1020017000691
    申请日:1999-07-16
    公开日:2001-07-28
    发明作者:올레로노보마리아델마르；반디예크폴이르마알베르투스；베가호세루이스
    申请人:데이비드 엠 모이어；더 프록터 앤드 갬블 캄파니；
    IPC主号:
    专利说明:

    Process for producing a powder from a tablet
    [1] The present invention relates to a process for preparing powder from detergent tablets, in particular tablets adapted for use in washing.
    [2] Detergent tablets are widely used for different types of washing or cleaning applications. When applied to automatic dishwashing, these tablets are prepared from the original high compression powder with the provided chemical composition, and therefore the high compression tablets are not sensitive to mechanical stress because they are solids, so the tablets are in order to produce an aqueous solution comprising a surfactant. Dissolve immediately in the dishwasher. In the manufacturing process of such tablets, a small proportion of the tablets produced are not suitable for use due to, for example, unsuitable chemical composition or immediately destroyed. In such cases, tablets that are unsuitable for use typically can be recycled by grinding and dissolving them to form a solution, whereby a powder can be obtained from this solution, which powder is suitable for use by adding to the original powder in small proportions. Compress again to produce.
    [3] The present invention relates to a method for producing a powder from tablets having a tensile strength of at least 5 KPa and containing at least 2% by weight of a surfactant.
    [4] Among the advantages of this method is that it can be used to reduce waste in the environment while maintaining satisfactory quality for the tablets used.
    [5] Existing methods for preparing powders from tablets, in particular methods for recycling tablets for automatic dishwashing, have these and other advantages, but have disadvantages. For example, the granular structure of the recycle powder is different from the original powder due to the grinding and dissolution of the tablet made from the original powder.
    [6] The present invention seeks to provide a method of the kind mentioned above which satisfactorily controls the granular structure of the recycle powder while allowing to obtain the recycle powder.
    [7] Summary of the Invention
    [8] According to the present invention, an object of the present invention is achieved by a method of the above kind comprising a first step of mechanically grinding a tablet and a second step of sifting to obtain a powder, the powder thus obtained Silver contains less than 4% by weight of particles passing through a 150 μm sieve.
    [9] The method according to the invention has a number of advantages. Since the recycling of tablets is accomplished using mechanical stirring and shifting, the recycled powder can be obtained without passing through the dissolution step, but under certain conditions it may be desirable to add to this step. In addition, the shifting taken with mechanical agitation allows to control the granular structure of the product, keeping the level of particulates through the 150 μm sieve to a minimum. It is to be noted that 150 μm seeds are introduced to define the level of particulates obtained in the recycle powder obtained, which differs from the means used for the second step of shifting.
    [10] Detailed description of the invention
    [11] The present invention relates to a process for preparing powder from tablets having a tensile strength of about 5 KPa or more. In a preferred embodiment according to the invention, the tensile strength of the tablets is at least 10 KPa, preferably at least 15 KPa, more preferably at least 20 KPa so that the tablets dissolve immediately but have sufficient mechanical resistance. Tablets also contain 2% by weight of surfactant. In a preferred embodiment according to the invention, the tablet comprises at least 5% by weight, preferably at least 10% by weight, more preferably at least 15% by weight and most preferably at least 20% by weight of surfactant. Indeed, the present invention more particularly relates to laundry tablets, particularly comprising high concentrations of surfactants. The method according to the invention comprises a first step of mechanically grinding a tablet. Mechanical grinding can be achieved through different means, with preferred means for mechanical grinding using centrifugation, preferably centrifugal shifters, in particular KEK manufactured by KEMUTEC, more preferably K650 manufactured by KEMUTEC. Is provided. The second step of the process consists in the process of shifting to obtain powder. In fact, the tablet consists of a plurality of grains having a particular granular structure, rather than a solid block, after being mechanically ground. When shifting, a part of the granular structure can be selected. In a preferred embodiment according to the invention, the shifting is obtained as a mesh having a plurality of apertures of 5 mm diameter. The remaining granular structure is not included in the powder obtained by discharge. Typically, the remaining particulate structure, not introduced into the second stage, represents less than 1% per weight of the total particulate structure. Preferably, the remaining particulate structure is reinserted at the start of the process with the tablet to be processed to access the process loop. According to the present invention, the powder obtained comprises less than 4% by weight of particles passed through a 150 μm sieve. In a preferred embodiment, the powder obtained comprises less than 3.5% by weight of particles passing through 150 μm sieve. It is to be noted that the 150 μm sheave is usually different from the weaving means used in the second step according to the invention, which is mentioned for the purpose of providing a means for analyzing the granular structure of the powder obtained. Minimizing the level of fine particles improves the hygiene and environmental properties of the powders obtained. This applies more particularly to tablets comprising enzymes, so that the enzyme components of the tablets are preferably not milled during the process. The percarbonate component should not be crushed because the stability of the processed product may be affected. Indeed, in a preferred embodiment, the present invention relates to a tablet comprising a percarbonate. In addition, by limiting the level of particulates, when preparing tablets comprising the powder obtained, it is possible to obtain good solubility for the tablets in a washing environment.
    [12] The present invention applies in particular to re-blending the unsatisfactory tablets with the original powder, thus adding the obtained powder to the original powder to form a mixture, wherein the added powder is 1 per weight of the mixture. And 20% and the mixture is compressed to form tablets. Preferably, in this case, the powder obtained comprises particles passing through the 150 μm sieve at a ratio by weight that is less than twice the percentage by weight of the particles passing through the 150 μm sieve and contained in the original powder. In fact, especially with regard to the fine particles, the more powders obtained have a granular structure close to the original powder, the more reliable the recombination process is. In this case, the original tablets to be introduced into the process according to the invention are typically produced by themselves by compacting the original powder and with or without paint. Typically, the present invention relates to tablets having a tensile strength of less than 100 KPa. Tablets with a tensile strength of less than 80 KPa are more preferred, tablets with a tensile strength of less than 50 KPa are even more preferred, and tablets with a tensile strength of less than 30 KPa are most preferred. In fact, the tablets according to the invention should dissolve immediately in a washing environment so that the tablets are not over compressed. The process according to the invention can be considered for the preparation of powders from tablets typically used for automatic dish washing, but the dissolution properties are not very stringent for laundry tablets, which makes them more advantageous when applied to laundry tablets. It should be noted that
    [13] For industrial applications, the process according to the invention allows for the treatment of multiple tablets at a rate of 3 to 8 tons per hour and per mechanical grinding and shifting means. Even more preferred is a speed of 7 to 8 tons per hour.
    [14] Highly soluble compounds
    [15] Tablets according to the invention may further comprise highly soluble compounds which promote dissolution. Such compounds may be formed from mixtures or from single compounds. Highly soluble compounds are defined as follows:
    [16] A solution containing deionized water and 20 g / l of a specific compound is prepared as follows.
    [17] 1.Put 20 g of the specific compound into a Sotax Beaker. This beaker is placed in a constant temperature bath fixed at 10 ° C. The stirrer with the ship propeller is placed in a beaker so that the base of the stirrer is 5 mm above the base of the stack beaker. The mixer is set at a rotational speed of 200 revolutions per minute.
    [18] 2. Introduce 980 g of deionized water into a sock beaker.
    [19] 3. 10 seconds after introducing water, measure the conductivity of the solution using a conductivity meter.
    [20] 4. Repeat step (3) 20 seconds, 30 seconds, 40 seconds, 50 seconds, 1 minute, 2 minutes, 5 minutes and 10 minutes after performing step (2).
    [21] 5. The measured value measured at 10 minutes is used as the rising value or the maximum value.
    [22] Certain compounds are very soluble in accordance with the present invention starting from when the addition of deionized water to the compound is complete and the conductivity of the solution reaches 80% of its maximum value within 10 seconds. In fact, when monitoring the conductivity in this manner, the conductivity rises after a certain time, and this rise is considered as the maximum value. Such compounds are preferably in the form of a flowable material consisting of solid particles at temperatures of 10 to 80 ° C. for ease of handling, but other forms such as pastes or liquids may also be used.
    [23] Examples of highly soluble compounds include sodium diisoalkylbenzene sulfonate or sodium toluene sulfonate.
    [24] Coagulation effect
    [25] Tablets according to the invention may also comprise compounds or mixtures of compounds with an aggregation effect, which may be mechanically stronger at constant compressive forces. The flocculating effect of the detergent mixture on the particulate matter is characterized by the force required to grind the tablets based on the detergent matrix under test, which is pressed under controlled compression conditions. For a given compressive force, high tablet strength indicates that the granules stick together strongly when compressed, resulting in a strong cohesive effect. Means for assessing tablet strength (also called radial fracture stress) are described in the literature. Pharmaceutical dosage forms: tablets volume 1 Ed. H.A, Lieberman et al., Published in 1989].
    [26] The flocculation effect induced by the highly soluble compound is obtained by comparing the tablet strength of the original base powder without the highly soluble compound to the tablet strength of the powder mixture comprising 97 parts of the original base powder and 3 parts highly soluble compound. It is measured according to the invention. Highly soluble compounds are added to the matrix in the form of substantially anhydrous (less than 10% water content, preferably less than 5%). The addition temperature is 10-80 degreeC, More preferably, it is 10-40 degreeC.
    [27] Highly soluble compounds have a tablet tensile stress of 50 g of detergent granular material and 55 mm diameter at a given 3000 N compressive force of greater than 30% due to the presence of 3% highly soluble compound having a cohesive effect in the base granular material. If increased (preferably 60%, more preferably 100%), it is defined according to the invention to have a cohesive effect on the particulate matter.
    [28] It should be noted that the solubility of tablets in aqueous solutions is significantly increased when incorporating highly soluble compounds having a cohesive effect on tablets formed by compacting particulate matter, including surfactants. In a preferred embodiment, at least 1% per weight of the tablet is formed from highly soluble compounds, more preferably at least 2%, even more preferably at least 3%, most preferably at least 5% of the granular material per weight of the tablet. It is formed from a very soluble compound having a cohesive effect on.
    [29] It is to be noted that a composition comprising highly soluble compounds and surfactants is described in EP 0 524 075, which is a liquid composition.
    [30] Highly soluble compounds having a cohesive effect on particulate matter allow to obtain tablets with higher tensile strength at constant compressive force or the same tensile strength at lower compressive force as compared to conventional tablets. Typically, tablets have a tensile strength greater than 5 KPa, preferably greater than 10 KPa, more preferably greater than 15 KPa, even more preferably greater than 30 KPa, less than 100 KPa, even more preferably less than 80 KPa, especially when used in laundry applications, Most preferably less than 60 KPa. In fact, for laundry applications, the tablets should be compressed less than for example for automatic dishwashing applications, so that dissolution is achieved more quickly, so in laundry applications, the tensile strength is most preferably less than 30 KPa.
    [31] This allows tablets to be produced that are less compacted and dissolve more quickly with coagulation and mechanical resistance similar to conventional tablets. In addition, because the compounds are very soluble, the dissolution of the tablets is further promoted, creating a synergy that promotes the dissolution of the tablets according to the invention.
    [32] Tablet manufacturing
    [33] The present invention seeks to yield less compact and less dense tablets at a constant compression force when compared to conventional detergent tablets.
    [34] Detergent tablets of the invention can be prepared simply by mixing the solid components together and compacting the mixture in the conventional, for example, tablet presses of the pharmaceutical industry used. Preferably the main component, in particular the gelling surfactant, is used in particulate form. Any liquid component may be incorporated into the solid particulate component, for example, in a conventional manner by surfactants or antifoams.
    [35] Especially in the case of laundry tablets, components such as enhancers and surfactants can be spray dried in a conventional manner and then compressed at a suitable pressure. Preferably, the tablets according to the invention are compressed using a compressive force of less than 100000 N, more preferably less than 50000 M, even more preferably less than 5000 N, most preferably less than 3000 N. Indeed, the most preferred embodiment is a tablet suitable for laundry compressed using a compressive force of less than 2500N, however, automatic dishwashing tablets may be considered such that, for example, such automatic dishwashing tablets are typically more compact than laundry tablets.
    [36] The granular material used to prepare the tablets of the present invention can be prepared by any granulation method or granulation method. Examples of such methods are spray drying methods (performed in air or countercurrent spray drying towers) which typically provide low bulk densities of up to 600 g / l. Higher density granular materials can be manufactured by assembling and densifying in high shear batch mixers / assemblies or by continuous assembly and densification processes (eg Lodige). CB and / or Lodige Using a KM mixer. Other suitable methods include particulate materials made by any chemical process, such as fluidized bed methods, compression methods (eg roll compaction), extrusion, and flocculation, crystallization centering, and the like. Each particle may also be any other particle, granule, sphere or grain.
    [37] The particulate material components may be mixed together by any conventional means. The arrangement is suitable for example in concrete mixers, Nauta mixers, ribbon mixers and the like. Alternatively, the mixing process can be carried out continuously by metering each component by weight relative to the moving belt and blending them in one or more drum (s) or mixer (s). The non-gelling binder can be sprayed onto a mixture of some or all of the particulate material components. The other liquid components may also be sprayed individually or premixed into the mixture of components. For example, a slurry of perfume and optical brightener can be sprayed. Finely divided flow aids (dusting agents such as zeolites, carbonate silica, etc.) can be sprayed onto the binder and then added to the particulate material, preferably at the end of the process, making the mixture less sticky.
    [38] Tablets may be prepared using any compression method, for example tabletting, briquetting or extrusion, preferably tableting. Suitable devices include standard single stroke or rotary presses (eg Courtoy). , Coach , Manesty Or Bonals ] Is included. The tablets prepared according to the invention preferably have a diameter of 20 to 60 mm, preferably 35 to 55 mm and a weight of 25 to 100 g. The height to diameter (or width) ratio of the tablets is preferably greater than 1: 3, more preferably greater than 1: 2. The compression pressure used to make these tablets needs to exceed 100000 kN / m 2, preferably 30000 kN / m 2, more preferably 5000 kN / m 2, even more preferably 3000 kN / m 2 and most preferably 1000 kN / m 2. none. In a preferred embodiment according to the invention, the tablet has a density of at least 0.9 g / cc, more preferably at least 1.0 g / cc, preferably less than 2.0 g / cc, more preferably less than 1.5 g / cc, most preferably Is less than 1.1 g / cc.
    [39] Hydrotrope compounds
    [40] In a preferred embodiment of the invention, the tablets also include hydrotropes, which are specific compounds defined as hydrotropes as follows, which further assist in dissolving the tablets in aqueous solution. See S.E. Friberg and M. Chiu, J. Dispersion Science and Technology, 9 (5 & 6), pages 443 to 457, (1988-1989)]:
    [41] 1. Prepare a solution comprising 25% by weight of a specific compound and 75% of water.
    [42] 2. Octanoic acid is then added to a solution having a temperature of 20 ° C. at a rate of 1.6 times the weight of the specific compound in the solution. The solution is mixed in a sock beaker with a ship propeller equipped with a marine propeller, with the propeller positioned about 5 mm above the base of the beaker and the mixer set at a rotational speed of 200 revolutions per minute.
    [43] 3. Certain compounds are hydrotrope when the octanoic acid is fully solubilized and when the solution contains only one phase, the phase is liquid.
    [44] In a preferred embodiment of the present invention, it should be noted that the hydrotrope compound is a flowable material made of solid particles at operating conditions of 15 to 60 ° C.
    [45] Hydrotrope compounds include the compounds described below:
    [46] A list of commercial hydrotropes can be found in the literature. McCutcheon's Emulsifiers and Detergents published by the McCutcheon division of Manufacturing Confectioners Company. Main compounds also include:
    [47] 1.Nonionic hydrotropes having the following structure:
    [48]
    [49] Wherein R is a C 8 to C 10 alkyl chain, x is 1 to 15 and y is 3 to 10
    [50] 2. Anionic hydrotropes such as alkali metal aryl sulfonates. This includes alkali metal salts, naphthoic acids and various hydroaromatic acids of benzoic acid, salicylic acid, benzenesulfonic acid and many derivatives thereof. Examples of these include sodium, potassium and ammonium benzene sulfonate salts derived from toluene sulfonic acid, xylene sulfonic acid, cumene sulfonic acid, tetralin sulfonic acid, naphthalene sulfonic acid, methyl naphthalene sulfonic acid, dimethyl naphthalene sulfonic acid, trimethyl naphthalene Sulfonic acid.
    [51] Other examples include salts of dialkyl benzene sulfonic acids such as diisopropyl benzene sulfonic acid, ethyl methyl benzene sulfonic acid, salts of alkyl benzene sulfonic acid having an alkyl chain length of 3 to 10 (preferably 4 to 9), alkyl Linear or branched alkyl sulfonates having 1 to 18 carbon atoms in the chain.
    [52] 3. For example, solvent hydrotropes such as alkoxylated glycerin and alkoxylated glycerides, ester alkoxylated glycerin, alkoxylated fatty acids, esters of glycerin and polyglycerol esters. Preferred alkoxylated glycerin has the following structure:
    [53]
    [54] Wherein l, m and n are each a number from 0 to about 20, provided that l + m + n is from about 2 to about 60, preferably from about 10 to about 45, and R is H, CH 3 or C 2 H 5 )
    [55] Preferred alkoxylated glycerides have the following structure:
    [56]
    [57] [Wherein R 1 and R 2 are each C n COO or — (CH 2 CHR 3 —O) l —H {where R 3 is H, CH 3 or C 2 H 5 , and l is from 1 to about 60 Number, n is a number from about 6 to about 24}.
    [58] 4. Polymeric hydrotropes as described, for example, in EP 636687:
    [59]
    [60] Wherein E is a hydrophilic functional group, R is H or a C 1 -C 10 alkyl group or a hydrophilic functional group, R 1 is H, a lower alkyl group or an aromatic group, and R 2 is H, a cyclic alkyl or an aromatic group Is a group)
    [61] The molecular weight of the polymer is typically about 1000 to 1000000.
    [62] 5. 5-Carboxy-4-hexyl-2-cyclohexan-1-yl octanoic acid [Deacid] ] Specially designed hydrotropes.
    [63] The use of such compounds in the present invention further increases the dissolution rate of the tablets, for example, because the hydrotrope compound promotes dissolution of the surfactant. Such compounds may be formed from mixtures or single compounds.
    [64] film
    [65] The coagulation of the tablets according to the invention can be further improved by making coated tablets, where the coating covers the uncoated tablets according to the invention, so as to maintain dissolution while further improving the mechanical properties of the tablets or Make further improvements.
    [66] In one embodiment of the invention, the tablet may then be coated so that the tablet does not absorb moisture or only absorbs moisture at a very slow rate. The coating is also strong so that only a very low degree of breakage or wear will occur even if a moderate mechanical impact is applied to the tablet during handling, packaging and transportation. Finally, the coating is preferably brittle so that the tablet breaks when subjected to a stronger mechanical impact. In addition, the coating material is advantageously dissolved under alkaline conditions or emulsified immediately by the surfactant. This avoids the problem of visible residue in the windows of the front load washing machine during the wash cycle, and also helps to avoid the deposition of undissolved particles or lumps of the coating material during laundry loading.
    [67] Water solubility is measured according to the test protocol of ASTM E1148-87 entitled "Standard Test Method for Measurements of Aqueous Solubility."
    [68] Suitable coatings are dicarboxylic acids. Particularly suitable dicarboxylic acids are oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, subberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and mixtures thereof It is selected from the group consisting of.
    [69] The coating material has a melting point of preferably 40 to 200 ° C.
    [70] The coating can be applied in a number of ways. Two preferred coating methods are the method of coating with a molten material (a) and the method of coating with a solution of the material (b).
    [71] In (a), the coating is applied at a temperature above its melting point and then solidified on the tablet. In (b), a coating material is apply | coated as a solution, a solvent is dried, and it is left to stand by an aggregation film. Substantially insoluble material may be applied to the tablet, for example by spraying or dipping. Typically, when spraying molten material onto a tablet, it solidifies rapidly to form a cohesive film. If the tablet is immersed in the molten material and then removed, rapid cooling again results in rapid solidification of the coating. Obviously it has been found that materials with a melting point below 40 ° C. that are substantially insoluble are not sufficiently solid at ambient temperature, and materials with a melting point above about 200 ° C. are not practical for use. Preferably, the material melts at 60 to 160 ° C, more preferably at 70 to 120 ° C.
    [72] By "melting point" is meant the temperature at which a substance becomes a transparent liquid when it is heated slowly, for example in a capillary.
    [73] Coatings of any desired thickness may be applied according to the invention. For most purposes, the coating forms 1 to 10%, preferably 1.5 to 5%, of the tablet weight.
    [74] The tablet coating of the present invention is very hard and provides additional strength to the tablet.
    [75] In a preferred embodiment of the present invention the breaking properties of the coating upon washing are improved by adding a disintegrant to the coating. These disintegrants, once in contact with water, swell and break down the coating into small pieces. This improves the solubility of the coating in the wash solution. Disintegrants are suspended in the coating melt at levels of up to 30%, preferably from 5 to 20%, most preferably from 5 to 10%. Possible disintegrants are described in Handbook of Parmaceutical Excipients (1986). Examples of suitable disintegrants include starch (natural starch, modified starch or pregelatinized starch, sodium starch gluconate), gum (agar gum, guar gum, locust bean gum, karaya gum, pectin gum, tragacanth gum), Salts thereof, including croscarmellose sodium, crospovidone, cellulose, carboxymethyl cellulose, alginic acid and sodium alginate, silicon dioxide, clay, polyvinylpyrrolidone, soy polysaccharides, ion exchange resins and mixtures thereof do.
    [76] The tensile strength
    [77] Depending on the composition of the starting material and the shape of the tablet, the compressive force used can be adjusted so as not to affect the tensile strength and the disintegration time in the washing machine. Such methods can be used to produce homogeneous or laminated tablets of any size or shape.
    [78] For columnar tablets, the tensile strength corresponds to the radial breaking stress (DFS), a method of indicating the strength of the tablet, and is determined by the following equation:
    [79]
    [80] [Where F is the maximum force (Newtons) causing tensile failure (break) measured by a VK 2000 tablet hardness tester (Van Kell industries Inc.), D is the diameter of the tablet, and T is the thickness of the tablet. ] (See Method Parmaceutical Dosage Forms: Tablets Volume 2 page 213 to 217)
    [81] Tablets with a radial breaking stress of less than 20 KPa are considered brittle and may cause some broken tablets to be delivered to the consumer. A radial breaking stress of 25 KPa or more is preferable. Typically, tablets according to the invention have a tensile strength in the normal direction to the main axis of more than 5 KPa, preferably more than 10 KPa, more preferably more than 15 KPa, even more preferably more than 20 KPa, especially when used in laundry applications. The tablets according to the invention also dissolve immediately so that the tensile strength is preferably less than 75 KPa, more preferably less than 50 KPa.
    [82] It is similarly applied to non-circular tablets to define tensile strength, so that the cross section perpendicular to the height of the tablet is non-circular, and therefore the force is applied along the direction perpendicular to the height direction of the tablet and normal to the face of the tablet, The face is perpendicular to the non-circular cross section.
    [83] Tablet dispense
    [84] The partition ratio of disintegrated tablets can be measured by the following method.
    [85] Weigh two tablets, nominally 50 g each, and then dispense the device (Bauchnecht). WA9850 washing machine). The water supply to the washing machine is set at a temperature of 20 ° C. and a hardness of 21 grains per gallon and the distribution device water inlet flow rate is set to 8 l / min. Purified residue levels remaining in the dispensing device are inspected by changing the laundry and set to washing program 4 (white / color, short cycle). The distribution residue ratio is measured as follows:
    [86] % Dispensing = Residual Weight × 100 / Original Tablet Weight
    [87] The level of residue is determined by repeating the process ten times and the average residue level is calculated based on each of the ten measurements. It is considered that in this stress test a residue of 40% of the starting tablet weight is allowed. Less than 30% residue is preferred, and less than 25% residue is more preferred.
    [88] It should be noted that the measurement of the number hardness, indicative of the concentration of Ca 2+ ions in solution, is given in conventional “grains per gallon”, so 0.001 mol per liter = 7.0 grains per gallon.
    [89] Effervesent
    [90] In another preferred embodiment of the invention the tablet further comprises a boiling agent which is a compound that further promotes the solubility of the tablet in aqueous solution.
    [91] Boilability as defined herein means that as a result of the chemical reaction between the soluble acid feedstock and the alkali metal carbonate, carbon dioxide gas is produced, releasing gas bubbles from the liquid:
    [92] That is, C 6 H 8 O 7 + 3 NaHCO 3 → Na 3 C 6 H 5 O 7 + 3CO 2 ↑ + 3H 2 O
    [93] Further examples of acid and carbonate feedstocks and other effervescent systems can be found in Pharmaceutical Dosage Forms: Tablets Volume 1 page 287 to 291.
    [94] The boiling agent can be added to the tablet mixture in addition to the detergent components. Adding such boiling agents to the detergent tablets improves the disintegration time of the tablets. The amount is preferably 5 to 20%, most preferably 10 to 20%, based on the weight of the tablet. Preferably the boiling agent should be added as coagulant of different particles or as a compact, but in the form of not individual particles.
    [95] Due to the gas produced by boiling in the tablets, the tablets may be identical to tablets with high D.F.S but still without disintegration time. If the D.F.S of the tablet with boiling is kept the same as the tablet without boiling, the disintegration of the tablet with boiling will be faster.
    [96] Further dissolution aids may be provided using compounds such as sodium acetate or urea. A list of suitable dissolution aids can be found in Pharmaceutical Dosage Forms: Tablets, Volume 1, Second edition, Edited by H.A. Lieberman et all, ISBN 0-8247-8044-2.
    [97] Cleaning surfactant
    [98] Surfactants are included in the tablets according to the invention. Solubility of the surfactant is promoted by adding highly soluble compounds.
    [99] Non-limiting examples of surfactants useful herein typically used at levels of about 1 to about 55% by weight include conventional C 11 -C 18 alkyl benzene sulfonates (“LAS”) and primary side chains and random C 10. -C 20 alkyl sulfates ( "AS"), the general formula CH 3 (CH 2) x ( CHOSO 3- M +) CH 3 and CH 3 (CH 2) y ( CHOSO 3- M +) for CH 2 CH 3 C 10 —C 18 secondary (2,3) alkyl sulfates wherein x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water soluble cation, in particular sodium, unsaturated sulfate, for example For example, oleyl sulfate], C 10 -C 18 alkyl alkoxy sulfate (“AE x S”, in particular ethoxy sulfate of EO 1 to 7), C 10 -C 18 alkyl alkoxy carboxylate (especially of EO 1 to 5 ethoxy carboxylates), C 10-18 glycerol ether, C 10 -C 18 alkyl poly glycoside and their corresponding sulfated polyglycosides side, and the C 12 -C 18 alpha-sulfonated fatty acid to sulfonic Include a hotel. If desired, conventional nonionic and amphoteric surfactants such as C 12 -C 18 alkyl ethoxylates (“AEs”) and C 6 -C 12 alkyls, including so-called narrow peaks of alkyl ethoxylates Phenol alkoxylates (especially ethoxylates and mixed ethoxy / propoxy), C 12 -C 18 betaines and sulfobetaines ("sultaines"), C 10 -C 18 amine oxides, and the like, may also be included in the overall composition. Can be. C 10 -C 18 N-alkyl polyhydroxy fatty acid amides may also be used. Typical examples include C 12 -C 18 N-methylglucamide. See WO 9,206,154. Other sugar derived surfactants include N-alkoxy polyhydroxy fatty acid amides such as C 10 -C 18 N- (3-methoxypropyl) glucamide. N-propyl to N-hexyl C 12 -C 18 glucamide can be used for low foaming. C 10 -C 20 Conventional soaps may also be used. For the purpose of generating a lot of foam, branched C 10 -C 16 soaps can be used. Especially useful are mixtures of anionic and nonionic surfactants. Other conventional useful surfactants are described in the standard literature. In a preferred embodiment, the tablet comprises at least 5%, more preferably at least 15%, even more preferably at least 25%, most preferably 35 to 45% surfactant by weight.
    [100] Non-gelling binder
    [101] Non-gelling binders can be incorporated with the particles to form tablets to further promote dissolution. Such compounds further promote dissolution of the tablets in aqueous solution.
    [102] Where non-gelling binders are used, suitable non-gelling binders include synthetic organic polymers such as polyethylene glycol, polyvinylpyrrolidone, polyacrylates and water soluble acrylate copolymers. The handbook of Pharmaceutical Excipients second edition describes the following binder types: acacia, alginic acid, carbomer, sodium carboxymethylcellulose, dextrin, ethylcellulose, gelatin, guar gum, hydrogenated vegetable oil type I, hydroxy Ethyl cellulose, hydroxypropyl methylcellulose, liquid glucose, magnesium aluminum silicate, maltodextrin, methylcellulose, polymethacrylate, povidone, sodium alginate, starch and zein. Most preferred binders, for example cationic polymers, ie ethoxylated hexamethylene diamine quaternary compounds, bishexamethylene triamine or others, for example pentaamine, ethoxylated polyethylene amines, maleic acrylic polymers It has an active cleaning action.
    [103] The non-gelling binder material is preferably sprayed to bring the melting point below 90 ° C., preferably below 70 ° C., even more preferably below 50 ° C., so as not to damage or degrade other active ingredients in the matrix. Most preferred are non-aqueous binders (i.e. not in an aqueous state) that can be sprayed in molten form. However, it may be a dry binder, incorporated into the matrix, but may also be a solid binder with binding properties in the tablet.
    [104] The non-gelling binder material is preferably used in an amount of less than 0.1 to 15% of the composition, more preferably less than 5% based on the weight of the tablet, especially less than 2% for non-washing active material.
    [105] It is desirable to avoid gelling binders, such as nonionic surfactants, in their liquid or molten form. Nonionic surfactants and other gelling binders are not excluded from the composition, but are preferably processed into detergent tablets as components of particulate matter rather than as liquids.
    [106] Enhancer
    [107] Detergent enhancers can optionally be included in the compositions herein to assist in controlling mineral hardness. Inorganic enhancers as well as organic enhancers can be used. Enhancers are typically used in fabric laundry compositions to help remove particulate dirt.
    [108] Enhancer concentrations can vary very widely depending on the final purpose of the composition.
    [109] Inorganic or P-containing detergent enhancers include, but are not limited to, alkali metals, ammonium and alkanolammonium salts of polyphosphates such as tripolyphosphate, pyrophosphate and glassy polymeric meta-phosphate, phosphonates, phytic acid , Silicates, carbonates (including bicarbonates and sesquicarbonates), sulfates and aluminosilicates. However, non-phosphate enhancers are needed in some areas. Importantly, the compositions herein surprisingly work well in the presence of so-called "weak" enhancers such as citrate or even in the so-called "underbuilt" cases, which can occur with zeolite or laminated silicate enhancers.
    [110] Examples of silicate enhancers are alkali metal silicates, especially silicates and laminated silicates having a SiO 2 : Na 2 O ratio of 1.6: 1 to 3.2: 1, for example, HP Rieck, dated May 12, 1987. Laminated sodium silicate as described in US Pat. No. 4,664,839. NaSKS-6 is the trade name of the crystalline laminated silicate sold by Hoechst (commonly abbreviated herein as "SKS-6"). Unlike zeolite enhancers, Na SKS-6 silicate enhancers do not contain aluminum. NaSKS-6 has a delta-Na 2 SiO 5 form in the form of laminated silicates. It can be prepared by the method as described in German patent applications 3,417,649 and 3,742,043. SKS-6 is a highly preferred laminated silicate for use herein, but a silicate of formula NaMSi x O 2x + 1 yH 2 O, wherein M is sodium or hydrogen, x is a number from 1.9 to 4, preferably 2 And y is a number from 0 to 20, preferably 0). Various other laminated silicates prepared by Hoechst include NaSKS-5, NaSKS-7 and NaSKS-11 in alpha, beta and gamma forms. As noted above, delta-Na 2 SiO 5 (NaSKS-6 form) is most preferred for use herein. Other silicates such as, for example, magnesium silicate may also be useful, which may act as crispening agents in granular formulations as stabilizers for oxygen bleach and as components of foam control systems.
    [111] Examples of carbonate enhancers are alkaline earth metals and alkali metal carbonates as described in German Patent Application No. 2,321,001 published November 15, 1973.
    [112] Aluminosilicate enhancers are useful in the present invention. Aluminosilicate enhancers are of great importance in the most commonly sold strong granular detergent compositions and may also be important enhancer components in liquid detergent formulations. Aluminosilicate enhancing agent has a structure of formula M z (zAlO 2) y] · xH 2 O ( Here, z and y are at least 6 constant, the molar ratio of z for y in the range of 1.0 to about 0.5, x is from about 15 To an integer from about 264).
    [113] Useful aluminosilicate ion exchange materials are commercially available. These aluminosilicates can be structurally crystalline or amorphous and can be natural aluminosilicates or synthetic derived aluminosilicates. Methods for preparing aluminosilicate ion exchange materials are described in US Pat. No. 3,985,669, issued to Krummel et al. On October 12, 1976. Preferred synthetic crystalline aluminosilicate ion exchange materials useful herein are commercially available under the trade names Zeolite A, Zeolite P (B), ZeoliteMAP and Zeolite X. In a particularly preferred embodiment, the crystalline aluminosilicate ion exchange material is of the structure:
    [114] Na 12 [(AlO 2 ) 12 (SiO 2 ) 12 ] · xH 2 O
    [115] Where x is from about 20 to about 30, in particular about 27
    [116] This material is known as zeolite A. Dehydrated zeolites (x = 0-10) may also be used herein. Preferably, the aluminosilicates have a particle size of 0.1 to 10 microns in diameter.
    [117] Organic detergent enhancers suitable for the purposes of the present invention include, but are not limited to, a wide variety of polycarboxylate compounds. As used herein, "polycarboxylate" refers to a compound having a plurality of carboxylate groups, preferably three or more carboxylates. Polycarboxylate enhancers can generally be added to the composition in acid form, but may also be added in the form of neutralizing salts. When used in salt form, alkali metals such as sodium, potassium and lithium or alkanoaluminum salts are preferred. Polycarboxylate enhancers include various categories of useful materials. One important category of polycarboxylate enhancers is U.S. Patent No. 3,128,287 issued to Berg on April 7, 1964 and U.S. Patent issued to Lamberti et al. On January 18, 1972. As described in US Pat. No. 3,635,830, ether polycarboxylates including oxydiisuccinates are included. See also "TMS / TDS" enhancer in US Pat. No. 4,663,071 to Bush et al., May 5, 1987. Suitable ether polycarboxylates also include cyclic compounds, especially cycloaliphatic compounds such as those described in US Pat. Nos. 3,923,679, 3,835,163, 4,158,635, 4,120,874 and 4,102,903.
    [118] Other useful detergent enhancers include ether hydroxypolycarboxylates, copolymers of maleic anhydride with ethylene or vinyl methyl ether, 1,3,5-trihydroxy benzene-2,4,6-trisulfonic acid and carboxymethyl Oxysuccinic acid, substituted ammonium salts of various alkali metals, ammonium and polyacetic acid (such as ethylenediamine tetraacetic acid and nitriloacetic acid), and polycarboxylates such as melic acid, succinic acid, oxydisuccinic acid, Polymaleic acid, benzene 1,3,5-tricarboxylic acid, carboxymethyloxysuccinic acid and soluble salts thereof.
    [119] Citrate enhancers such as citric acid and soluble salts thereof (particularly sodium salts) are polycarboxylate enhancers of particular importance for strong liquid detergent formulations, due to their recoverable raw materials and their effectiveness due to their biodegradability. Citrate may also be used in particulate compositions, in particular with zeolites and / or laminated silicate enhancers. Oxydisuccinates are also particularly useful in such compositions and combinations.
    [120] 3,3-dicarboxy-4-oxa-1,6-hexanedioate and related compounds described in US Pat. No. 4,566,984, issued January 28, 1986 to Bush, are also suitable for the detergent compositions of the present invention. . Useful succinic acid enhancers include C 5 -C 20 alkyl and alkenyl succinic acids and salts thereof. Particularly preferred compounds of this type are dodecenyl succinic acid. Specific examples of succinic acid enhancers include lauryl succinate, myristyl succinate, palmity succinate, 2-dodecenyl succinate (preferably), 2-pentadecenyl succinate, and the like. Laurylsuccinate is also a preferred enhancer among these groups and is described in European Patent Application No. 86200690.5 / 0,200,263, published November 5, 1986.
    [121] Other suitable polycarboxylates are U.S. Patent Nos. 4,144,226 to Crutchfield et al., March 13, 1979 and U.S. Patent No. 3,308,067, issued to Diehl, March 7, 1967. It is described in. See also US Patent No. 3,723,322 to Dile.
    [122] Fatty acids, such as C 12 -C 18 monocarboxylic acids, may also be incorporated alone or in combination with the above-mentioned enhancers, in particular citrate and / or succinate enhancers, to provide further enhancer activity. This use of fatty acids generally reduces foaming, so manufacturers should take this into account.
    [123] Where phosphorus enhancers can be used, in particular for bar formulations used in hand washing operations, various alkali metal phosphates such as the well known sodium tripolyphosphate, sodium pyrophosphate and sodium orthophosphate can be used. . Phosphonate enhancers such as ethane-1-hydroxy-1,1-diphosphonate and other known phosphonates (see, eg, US Pat. Nos. 3,159,581, 3,213,030, 3,422,021) , 3,400,148 and 3,422,137) may also be used.
    [124] bleach
    [125] The detergent composition herein may optionally contain a bleach, or a bleach composition containing a bleach and one or more bleach activators. When present, bleach is typically at a concentration of about 1 to about 30%, more typically about 5 to about 20% of detergent compositions, particularly detergent compositions for fabric washing. If present, the amount of bleach activator is typically from about 0.1 to about 60%, more typically from about 0.5 to about 40% of the bleach composition comprising the bleach + bleach activator.
    [126] As used herein, the bleach can be any bleach that is useful for fabric cleaning, hard surface cleaning or other cleaning purposes that are currently known or known. These include oxygen bleach, and other bleaches. Perborate bleaches such as sodium perborate (eg mono- or tetra-hydrate) can be used herein.
    [127] Another category of bleaches that can be used without limitation includes percarboxylic acid bleaches and salts thereof. Suitable examples of preparations of this kind include magnesium salts of magnesium monoperoxyphthalate hexahydrate, metachloro perbenzoic acid, 4-nonylamino-4-oxoperoxybutyric acid and diperoxydodecanedioic acid. Such bleaches are U.S. Patent No. 4,483,781 to Hartman on November 20, 1984, and U.S. Patent No. 740,446 to Burns et al., June 3, 1985, 1985 European Patent Application No. 0,133,354 to Banks et al., Published February 20, and US Patent No. 4,412,934 to Chung et al., Issued November 1, 1983. . Highly preferred bleaches also include the 6-nonylamino-6-oxperoxycaproic acid described in US Pat. No. 4,634,551 to Burns et al. On January 6, 1987.
    [128] Peroxygen bleach can also be used. Suitable peroxy bleach compounds include sodium carbonate peroxyhydrate and equivalent "percarbonate" bleaches, sodium pyrophosphate peroxyhydrate, urea peroxyhydrate and sodium peroxide. Persulfate bleach (OXONE, commercially available from DuPont) can also be used.
    [129] Preferred percarbonate bleaches include dry particles having an average particle size range of about 500 to about 1,000 μm, wherein up to about 10 wt% of the particles are up to about 200 μm and another up to about 10 wt% are greater than about 1,250 μm. to be. Optionally, the percarbonate can be coated with a silicate, borate or water soluble surfactant. Percarbonates are available from various sources such as FMC, Solvay and Tokai Denka.
    [130] Mixtures of bleaches can also be used.
    [131] Peroxy bleach, perborate, percarbonate and the like are preferably combined with a bleach activator, which leads to the preparation of the peroxy acid corresponding to the bleach activator in aqueous solution (ie during the washing process). Various non-limiting examples of activators are described in US Pat. No. 4,915,854, and US Pat. No. 4,412,934, issued April 5, 1990 to Mao et al. Nonanoyloxybenzene sulfonate (NOBS) and tetraacetyl ethylene diamine (TAED) activators are typical and mixtures thereof may be used. See also US Pat. No. 4,634,551 for other typical bleaches and activators useful herein.
    [132] Highly preferred amino derived bleach activators have the structure:
    [133] R 1 N (R 5 ) C (O) R 2 C (O) L or R 1 C (O) N (R 5 ) R 2 C (O) L
    [134] Wherein R 1 is an alkyl group of about 6 to about 12 carbon atoms, R 2 is an alkylene of 1 to about 6 carbon atoms, and R 5 is H or an alkyl, aryl, or alkaryl having about 1 to about 10 carbon atoms , L is any suitable leaving group)
    [135] Leaving group is any group that is substituted from a bleach activator as a result of a nucleophilic attack on bleach activation by perhydrolyzed anions. Preferred leaving group is phenyl sulfonate.
    [136] Preferred examples of bleach activators of the above formulas include (6-octaneamido-caproyl) oxybenzenesulfonate, (6-nonanamido) as described in US Pat. No. 4,634,551, which is incorporated herein by reference. Caproyl) oxybenzenesulfonate, (6-decaneamido-caproyl) oxybenzenesulfonate and mixtures thereof.
    [137] Another class of bleach activators includes benzoxazine type activators described in US Pat. No. 4,966,723 to Hodge et al., Filed October 30, 1990, incorporated herein by reference. Very preferred benzoxazine type activators are as follows:
    [138]
    [139] Another class of preferred bleach activators includes acyl lactam activators, in particular acyl caprolactam and acyl valerolactam of the formula:
    [140] ,
    [141] Wherein R 6 is H or an alkyl, aryl, alkoxyaryl or alkaryl group having 1 to about 12 carbon atoms
    [142] Highly preferred lactam activators include benzoyl caprolactam, octanoyl caprolactam, 3,5,5-trimethylhexanoyl caprolactam, nonanoyl caprolactam, decanoyl caprolactam, undecenoyl caprolactam, benzoyl valerolactam, octa Noil valerolactam, decanoyl valerolactam, undecenoyl valerolactam, nonanoyl valerolactam, 3,5,5-trimethylhexanoyl valerolactam and mixtures thereof. See also US Pat. No. 4,545,784 (Sanderson), issued Oct. 8, 1985, which is incorporated herein by reference to adsorbing acyl caprolactam, including benzoyl caprolactam, to sodium perborate. . Bleaches other than oxygen bleaches are known in the art and can be used herein. One type of particularly important non-oxygen bleach includes photoactivating bleaches such as sulfonated zinc and / or aluminum phthalocyanine. See, US Pat. No. 4,033,718 to Holcombe et al., Issued July 5, 1977. Detergent compositions, when used, typically contain about 0.025 to about 1.25 weight percent of such bleach, particularly sulfonate zinc phthalocyanine.
    [143] The bleaching composition can be catalyzed by a manganese compound, if desired. Such compounds are well known in the art and are described, for example, in US Pat. No. 5,246,621, US Pat. No. 5,244,594, US Pat. No. 5,194,416, US Pat. No. 5,114,606 and European Patent Application No. 549,271A1, Manganese-based catalysts described in 549,272 A1, 544,440 A2, and 544,490 A1. Preferred examples of such catalysts are Mn IV 2 (uO) 3 (1,4,7-trimethyl-1,4,7-triazacyclononane) 2 (PF 6 ) 2 , Mn III 2 (uO) 1 (u- OAc) 2 (1,4,7-trimethyl-1,4,7-triazacyclononane) 2- (ClO 4 ) 2 , Mn IV 4 (uO) 6 (1,4,7-triazacyclononane) 4 (ClO 4 ) 4 , Mn III Mn IV 4 (uO) 1 (u-OAc) 2- (1,4,7-trimethyl-1,4,7-triazacyclononane) 2 (ClO 4 ) 3 , Mn IV (1,4,7-trimethyl-1,4,7-triazacyclononan)-(OCH 3 ) 3 (PF 6 ) and mixtures thereof. Other metal based bleach catalysts include those described in US Pat. No. 4,430,243 and US Pat. No. 5,114,611. Methods of enhancing bleaching using manganese bound to various complex ligands are also described in the following U.S. patents: 4,728,455, 5,284,944, 5,246,612, 5,256,779, 5,280,117, 5,274,147, 5,153,161 And 5,227,084.
    [144] As a practical matter, although not intended to be limiting, the compositions and methods herein may be adjusted to provide at least 1 part per 10 million active bleaching catalyst species in an aqueous laundry solution, preferably from about 0.1 to about 700 ppm, more preferably, of catalyst species in the laundry solution Preferably about 1 to about 500 ppm.
    [145] enzyme
    [146] Enzymes can be included in the formulations herein for a wide variety of fabric laundry, including, for example, removal of protein based, carbohydrate based or triglyceride based stains, and refugee dye transfer and fabric recovery. Enzymes to be incorporated include proteases, amylases, lipases, cellulases and peroxidases as well as mixtures thereof. Other types of enzymes can also be included. It may be any suitable raw material such as enzymes of vegetable, animal, bacterial, fungal and yeast raw materials. However, its selection depends on several factors, such as pH activity and / or stability optimals, thermal stability, stability versus active detergents, enhancers and the like. In this regard, bacterial or fungal enzymes such as bacterial amylases and proteases, and fungal cellulase are preferred.
    [147] Enzymes are typically incorporated at levels sufficient to provide about 5 mg, more typically about 0.01 to about 3 mg, of active enzyme per gram of the composition. In other words, the compositions herein typically comprise from about 0.001 to about 5%, preferably 0.01 to 1%, by weight of a commercial enzyme preparation. Protease enzymes are typically present in such commercial formulations at levels sufficient to provide 0.005 to 1 AU (Anson unit) per gram of composition.
    [148] Suitable examples of proteases are B. a. B. subtilis and b. Subtilisin obtained from certain strains of B. Licheniforms. Another suitable protease is obtained from strains of Bacillus with maximum activity over pH 8-12 and developed by Novo Industries A / S and sold under the trade name ESPERASE. Methods for preparing such enzymes and homologue enzymes are described in British Patent No. 1,243,784 to Novo. Proteolytic enzymes suitable for removing protein-based stains on the market include the trade names ALCALASE and SAVINASE manufactured by Novo Industries A / S, Denmark, and International Bio-Synthetics, Netherlands. Inc. under the trade name MAXATASE. Other proteases include Protease A (see European Patent Application No. 130,756, published January 9, 1985) and Protease B (European Patent Application No. 87303761.8, filed April 28, 1987 and January 9, 1985). Published European Patent Application No. 130,756 (Bott et al.).
    [149] Amylases include, for example, α-amylase described in British Patent Application No. 1,296,839 (Novo), RAPIDASE manufactured by International Bio-Synthetics and TERMAMYL manufactured by Novo Industries.
    [150] Cellulase usable in the present invention includes both bacterial or fungal cellases. Preferably, it has an optimal pH of 5 to 9.5. Suitable cellulases are described in US Pat. No. 4,435,307 to Barbesgoard et al., On March 6, 1984, which discloses Humicola insolens and Humicola strain DSM1800. Or fungi cellulase prepared from cellulase 212 producing fungi belonging to the genus Aeromonas, and cellulases extracted from hepatopancreses of the marine molluscs (Dolabella Auricula Solander). Suitable cellulases are also described in British Patent No. 2.075.028, British Patent No. 2.095.275 and German Patent No. 2.247.832. CAREZYME (Novo) is particularly useful.
    [151] Lipase enzymes suitable for use in detergents include enzymes produced by Pseudomonas stutzeri ATCC 19.154, such as the Pseudomonas group microorganisms, for example, described in British Patent No. 1,372,034. See also lipase of Japanese Patent Application No. 53,20487, which was published on February 24, 1978. Such lipases are available under the trade name Lipase P "Amano", manufactured by Amano Pharmaceutical Co. Ltd., Nagoya, Japan, and referred to as "Amano-P". Other commercial lipases are from Chromobacter viscosum, such as the Chromobacter biskosium strain Lipoliticum NRRLB 3673, available from Toyo Jozo Co., Dagata, Japan. Lipazane, Amano-CES, and further U.S. based in the United States. Chromobacter biskosium lipases manufactured by U.S. Biochemical Corp. and Deisoynth Co., The Netherlands, and lipases from Pseudomonas gladiolus. LIPOLASE enzymes derived from Humicola Lanuginosa and commercially available from Novo (see also European Patent No. 341,947) are preferred lipases for use herein.
    [152] Peroxidase enzymes are used with oxygen sources such as percarbonate, perborate, persulfate, hydrogen peroxide and the like. This is used to "bleach the solution", ie to prevent the dye or pigment removed from the substrate during the laundry operation from transferring to other substrates in the laundry solution. Peroxidase enzymes are known in the art and include, for example, horseradish peroxidase, reginase and haloperoxidases such as chloro- and bromo-peroxidase. Peroxidase containing detergent compositions are described, for example, in PCT International Patent Application WO89 / 099813, published October 19, 1989, invented by Kirk and assigned to Novo Industries A / S. have.
    [153] A wide range of enzymatic materials and their means of incorporation into synthetic detergent compositions are also described in US Pat. No. 3,553,139, issued to McCarty et al. On January 5, 1971. Enzymes are further described in both US Pat. No. 4,101,457 to Place et al. On July 18, 1978 and US Pat. No. 4,507,219 to Hughes on March 26, 1985. It is described in. Enzyme materials useful in liquid detergent formulations and methods for incorporation into such formulations are described in US Pat. No. 4,261,868, issued to Hora et al. On April 14, 1981. Enzymes for use in detergents can be stabilized by a variety of techniques. Enzyme stabilization techniques are described, for example, in U.S. Patent Nos. 3,600,319 to Gedge et al. On August 17, 1971, and the European patent of Vengas, published on October 29, 1986. Published Patent Publication No. 0 199 405 and Patent Application No. 86200586.5. Enzyme stabilization systems are also described, for example, in US Pat. No. 3,519,570.
    [154] Other ingredients that are commonly used in detergent compositions and may be incorporated into the detergent tablets of the present invention include chelating agents, antifouling agents, antifouling agents, dispersants, brighteners, antifoams, fabric softeners, dye transfer inhibitors and perfumes. .
    [155] Example
    [156] The following process is carried out in accordance with the invention: Purification is introduced into the feed auger through the shifter inlet at a rate of 7 ton / h. The feed auger moves the tablets to the columnar shifting chamber. The tablet is lifted into a rotating paddle assembly and centrifuged against a sieve screen with a mesh size of 5 mm. The blades on the paddle assembly are installed in a spiral shape to carry material along the entire length of the sieve screen. Pass the powder obtained through the sieve screen and collect at the main shifter outlet. The remaining material is conveyed to the end of the shifting chamber and discharged through individual inlets.
    [157] Device Details: The shifter casing is processed from coated carbon steel epoxy resin. Motors, couplings and bearings are placed outside the process area to make contact with the product. The drive shaft is made of stainless steel and carries both supply augers and paddle assemblies. The design of the sieve screen frame is a welded or bolted tricyclic three strut structure, all of carbon steel or stainless steel.
    [158] Centrifugal shifters are used for round purification. Dimensions are as follows: weight: 53 +/- 2 g, diameter: 54 mm, height: 21.5 +/- 0.25 mm, tensile strength of tablets: 35 +/- 4 Kpa
    [159] The chemical composition (A) of the uncoated tablet is as follows:
    [160] Composition (A) (% by weight) Anionic Aggregates 121.45 Anionic Aggregates 213.00 Cationic aggregates5.45 Laminated silicate10.8 Sodium percarbonate14.19 Bleach activator aggregates5.49 Sodium carbonate13.82 EDDS / Sulfate Particles0.47 Tetrasodium salt of hydroxyethane diphosphonic acid0.73 Antifouling polymer9,33 Fluorescent0.18 Zinc Phthalocyanide Sulfonate Encapsulant0.025 Soap powder1.40 Foam inhibitor1.87 Citric acid7.10 Protease0.79 Lipase0.28 Cellulase0.22 Amylase1.08 Binder spray system1.325 Sum100.00
    [161] Anionic aggregate 1 comprises 40% anionic surfactant, 27% zeolite and 33% carbonate.
    [162] Anionic aggregate 2 comprises 40% anionic surfactant, 28% zeolite and 32% carbonate.
    [163] Cationic aggregates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate.
    [164] Laminated silicates include SKS 6 95% and silicates 5%.
    [165] Bleach activator aggregates comprise 81% TAED, 17% acrylic / maleic acid copolymer (acid form) and 2% water.
    [166] The ethylene diamine N, N-disuccinate sodium salt / sulfate particles comprise 58% ethylene diamine N, N-disuccinate sodium salt, 23% sulfate and 19% water.
    [167] Zinc phthalocyanine sulfonate encapsulant is 10% active.
    [168] Foam inhibitors include 11.5% silicone oil (Dow Corning), 59% zeolite and 29.5% water.
    [169] The binder spray system comprises 50% Lutensit K-HD 96 and 50% PEG (polyethylene glycol).
    [170] Preparation of tablets:
    [171] (i) A detergent base powder of composition (A) is prepared as follows: A homogeneous granular mixture is carried out by carrying out all spraying processes on the granular material of base composition (A) in a spray drum and then mixing together in a mixing drum. To form.
    [172] (ii) The tablets are then prepared by the following method: 53 g of the mixture are introduced into a suitable circular or rectangular shaped mold and compressed.
    [173] (iii) The tablets are immersed in a bath containing 80 parts of sebacic acid mixed with 20 parts of Nymcel zsb16. 3 g of the described mixture is applied to it, adjusting the time the tablet is immersed in a heating bath. The tablets are then cooled for 24 hours at room temperature at 25 ° C.
    [174] The granular structure of the obtained powder is compared with the granular structure of the original matrix A as follows:
    [175] Mesh size (μm)Original mixture (% by weight attached to each seed)Powder obtained (% by weight attached to each seed) 11809.6618.6 85024.5931.3 45064.6577.6 25091.2991 15096.6497 Up to 1503.363 Average particle size500 ㎛638 ㎛
    [176] The above table should be interpreted as follows:
    [177] The powder obtained is 18.6% per weight of material remaining on 1180 μm sheaves, which is compared to 9.66% per weight of the original mixture obtained after step (i) above on 1180 μm sheaves. Six sieves (1180, 850, 450, 250 and 150 μm) can be placed with the larger mesh size up and the smaller mesh size down so that the granular structure can be analyzed. The percentage by weight of particles that passed through all the sieves, i. The table above also shows the average particle size for the materials considered.
    [178] The measurements most relevant to the present invention are those wherein the level of particles passing through 150 μm sheave is less than 4% per weight of the powder obtained and the ratio of the weight per particle of particles passing through the 150 μm sheave and contained in the original powder or original mixture. Less than twice. It is noted that the tablets according to the invention and treated by the method described in this example have a coating, and the powder obtained is similar to the original powder or mixture used for the preparation of the coating without tablets. The method also applies to uncoated tablets.
    权利要求:
    Claims (10)
    [1" claim-type="Currently amended] A first step of mechanically grinding the tablets and a second step of sifting to obtain a powder (the powder thus obtained comprises less than 4% by weight of powder passing through a 150 μm sieve) To produce a powder from tablets having a tensile strength of at least 5 KPa and at least 2% by weight of a surfactant.
    [2" claim-type="Currently amended] The method of claim 1 wherein the tablet is obtained by compacting the original powder.
    [3" claim-type="Currently amended] The powder obtained according to claim 2, wherein the obtained powder comprises particles which have passed through the 150 mu m sieve at a percentage by weight which is less than twice the percentage by weight of the particles passing through the 150 mu m sieve and contained in the original powder. Way.
    [4" claim-type="Currently amended] The method of claim 1, wherein the obtained powder is added to the original powder to form a mixture, wherein the added powder constitutes 1 to 20% per weight of the mixture, and the mixture is compressed to form tablets.
    [5" claim-type="Currently amended] The method of claim 1, wherein the tablet has a tensile strength of less than 100 KPa.
    [6" claim-type="Currently amended] The method of claim 1, wherein the tablet comprises a coating.
    [7" claim-type="Currently amended] The method of claim 1, wherein the purification comprises an enzyme.
    [8" claim-type="Currently amended] The method of claim 1 wherein the mechanical grinding is provided by centrifugation.
    [9" claim-type="Currently amended] The method of claim 1, wherein the shifting is obtained by a mesh having a plurality of apertures having a diameter of 5 mm.
    [10" claim-type="Currently amended] The method of claim 1 wherein the method is applied to multiple tablets at a rate of 3 to 8 tons per hour.
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    公开号 | 公开日
    AU5105399A|2000-02-07|
    MA24935A1|2000-04-01|
    AT264909T|2004-05-15|
    AR019927A1|2002-03-27|
    CA2336957A1|2000-01-27|
    CN1309695A|2001-08-22|
    DE69823343D1|2004-05-27|
    EP0972827A1|2000-01-19|
    WO2000004126A1|2000-01-27|
    BR9912084A|2001-04-10|
    JP2002520480A|2002-07-09|
    EP0972827B1|2004-04-21|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    法律状态:
    1998-07-16|Priority to EP98202401.0
    1998-07-16|Priority to EP98202401A
    1999-07-16|Application filed by 데이비드 엠 모이어, 더 프록터 앤드 갬블 캄파니
    1999-07-16|Priority to PCT/US1999/016076
    2001-07-28|Publication of KR20010070974A
    优先权:
    申请号 | 申请日 | 专利标题
    EP98202401.0|1998-07-16|
    EP98202401A|EP0972827B1|1998-07-16|1998-07-16|Process for producing a powder from a tablet|
    PCT/US1999/016076|WO2000004126A1|1998-07-16|1999-07-16|Process for producing a powder from a tablet|
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