• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A process is provided for the manufacture of fibrils of short length by suddenly releasing the pressure acting on a two-phase liquid mixture of molten polymer and solvent and which is at a high pressure and a high temperature. The two-phase liquid mixture is ejected through a pressure release orifice so as to vaporize the solvent instantaneously and solidify the polymer, and the flow path of the two-phase liquid mixture is perturbed at the instant when it enters the pressure release orifice.
    公开号:SU816405A3
    申请号:SU752099765
    申请日:1975-01-17
    公开日:1981-03-23
    发明作者:Плеска Жан-Пьер；Марешаль Мишель
    申请人:Солвэй Э Ко (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a method for the manufacture of fibrils of short length, and also to a device intended for its implementation. ,
    A known method of producing fibrils · throttling a mixture of a molten polyolefin with a solvent at 140-220’s [1].
    However, this method requires an increased consumption of solvent in order to achieve sufficient loosening, prolonged thorough mixing of the mixture into which water is added at very high temperatures (230280 ° C) and a pressure of more than 100 kg / cm *. 15 In addition, at the moment before expanding the volume of the mixture, it is necessary to pump additional water into it at high temperatures and pressures.
    It is also necessary to use expensive equipment that requires the use of a special extruder and includes a die, a chamber with coaxially located inlet and throttle openings with a ratio of the distance between these openings to the diameter of the chamber exceeding 8.
    The purpose of the invention is the simplification of the process, reducing economic costs.
    The goal is achieved by the fact that in the method for producing fibrils, the mixture is throttled by lowering the mixture of the polyolefin melt with the solvent at 140-220 ° С and the mixture is throttled in the form of separate vortex jet flows of iodine at an angle of 46-120 ° to the axis of the throttling hole.
    To implement the method for producing fibrils, a device is used that contains a die, a chamber with inlet and coaxially arranged inputs and throttling holes, the ratio of the distance between these holes to the diameter of the chamber being selected within 0.187-2.5.
    In FIG. 1 shows a device for implementing the method; in FIG. 2-6 embodiments of the end part of the device; in FIG. 7 is an embodiment with several perturbation chambers arranged in series; in FIG. 8-device using a metal mesh; in FIG. 9 and 10 - device options with two feed holes; in FIG. 11 is a section AA in FIG. 9; in FIG. 12 is an embodiment of a die that allows formation of a continuous film of a lubricant at the level of the wall of the hole for punching,
    The die .1 (FIGS. 1-6) comprises a hole 2 for punching and a device for pre-punching t . This punching device Ιηογο comprising a overflow 3 having a central opening 4 is not necessary. Its meaning is to provide a pressure drop in the mixture of the molten polymer and the solvent, which is in liquid single-phase form, crossing the die for the purpose of causing the formation of a two-phase mixture.
    In addition, the die contains a perturbation chamber 5 bounded by a wall having holes for pushing through and an upper flat wall 6 containing a supply hole 7 in the center. The holes for pressing and feeding are opposite and coaxial. The perturbation chamber is cylindrical with a circular cross section. The holes are located in the centers of the bases. The distance between the holes (height) is preferred to spill spills. The distance between the holes of the perturbation chamber (chamber height) should be greater than the diameter of the feed hole. When the height of the perturbation chamber is small, the lateral deflected jets cannot be effectively directed across the central jet.
    On the contrary, when the height of the disturbing camera becomes very large, in the pope TO P echnye deflected jets tend to connect with the central jet and become parallel to them before they reach the hole punching. The height that the perturbation chamber may have is related to the diameter of this chamber.
    The die 1 for abrupt punching (Fig. 8) is equipped with a metal mesh 12 located in the perturbation chamber 5. The perturbation chamber 5 is bounded by a wall containing a hole 2 for punching,. and an upper flat wall 6 having a feed hole 7 in its center. The burst hole 2 and the feed hole 7 are opposite and coaxial. The side wall of the perturbation chamber 5 having a cylindrical shape is bounded by a ring 13. The perturbation chamber may be of another shape, in particular a parallelepiped. The function of the ring 13 is double, on the one hand, this ring determines the height of the perturbation chamber 5 and, on the other hand, it supports a grid with small cells 12 located in the perturbation chamber against the wall 6 containing the supply hole.
    The dies shown in FIGS. 9, 10 and 11 are of the same type as the die shown in FIG. 8, except that it does not contain a metal mesh located in a perturbation chamber. In addition, the communication between the supply chamber 8 and the perturbation chamber 5 is provided by two supply holes 7, the axes of which are inclined with respect to each other and which are connected in one hole of the side of the perturbation chamber. In these dies, ring 13 defining the cylindrical side wall of the perturbation chamber serves only to control the height of this chamber.
    usually less than 10 cm and, especially, 7.5 cm.
    The inlet and outlet of the pressure opening 2 (Figs. 2-6) are possible profiles.
    When the chamber 8 of the die is supplied with a two-phase mixture of molten polymer and solvent, this mixture, due to the straight line arrangement of the hole 7 of the wall 6 and the hole 2 for bursting, flows through the perturbation chamber through the central fluid stream 9 and along the side streams 10, which, being located close to the hole 2 for punching, directed across the Central jet walls of the perturbation chamber. The angle of incidence of these side jets can be changed by changing the profile of the wall containing the burst hole 2, as shown in FIG. 2-6. The angle formed by the axis of the punch hole and the wall of the chamber in which this hole is made determines the angle of incidence of the lateral most eccentric jets, which are the most deflected.
    In the die (Fig. 7), several perturbation chambers 5 are arranged in series.
    In addition, it is desirable that the perturbation chamber meet various criteria to achieve maximum efficiency.
    It is necessary that the perturbation chamber has a sufficient transverse dimension in order for the formation of side jets that can disrupt the central jet at the entrance level of the opening 2 for selling
    The dies, (Fig. 9, 10 and 11) are equipped with a metal mesh located in the perturbation chamber, and / or may have two or more holes, the axes of which are parallel.
    As shown in FIG. 1,2,3,4,7 and
    11, it is possible to provide an expansion chamber 11 l at the outlet, punching holes, the expansion angle being preferably greater than 150 °
    The die 1 (FIG. 12), comprising a pre-punch chamber 8, a feed hole 7 of the perturbation chamber 5 and a punch hole 2, is provided with a peripheral chamber 15 that surrounds the perturbation chamber 5, and the partition 14 separating these chambers is interrupted at the level of the inlet opening for pushing 2 in such a way as to create a round slot 47 coaxial with the hole for pushing. The peripheral chamber 15 is further provided with an opening 16 for connecting to a source of liquid lubricant.
    Example 1. Prepare a two-phase mixture by bringing to a temperature of 195 ° C and a pressure of 63 kg / cm ^ containing. 15% by weight of high density polyethylene with a melting index of 5 and 85% by weight of technical hexane. These conditions correspond to the onset of two liquid phases. This mixture is forced through a die with a perturbation chamber having the following geometric characteristics: the ratio between the diameter of the perturbation chamber and the diameter of the perturbation hole 7 is 16; the ratio between the height, the perturbation chamber and the diameter of the supply opening 7 is 5; the ratio between the height of the perturbation chamber and the diameter of this chamber is 0.313; diameters and heights of the feed hole 7 and the hole for bursting 1 mm
    The expanding device extending the sharp-forcing hole is 150 °. The angle of deviation of the flow of the mixture subjected to throttling, 90 °.
    The biphasic mixture is consumed at 21.4 kg / h. polymer. Get short fibrils with an average length equal to. Noah 1.7 mm. The specific surface of these fibrils rose to 35 m / g.
    Example 2, The process of Example 1 is carried out, except that preliminary punching is carried out at a pressure of 12 kg / cm 2 . Short fibrils with an average length of 1.9 mm are also obtained. The specific surface of the product rose to 23 m 2 / g.
    Example 3. The process of example 2 is carried out, but using a die with a perturbation chamber (Fig. 3), the geometric characteristics of which are identical to those indicated in example 1. Short fibrils with an average length of 1.8 mm are obtained. Their specific surface area is 21 m 2 / g.
    Example 4 .. The process of example 4 is carried out, taking into account that the die has the following modified geometric characteristics: the ratio between the height of the perturbation (0 chamber and the diameter of the perturbation hole 7 is 40; the ratio between the height of the perturbation chamber and its diameter is 2.5 The angle of deviation of the flow of the mixture 90 ^.
    Again, short fibrils 1 with an average length of 2.3 mm are obtained, the specific surface of which is 26 m a / g.
    Example 5 The process of example 2 is carried out, but using (die (Fig. 6), the geometric characteristics of which are as follows: the ratio of the diameter of the perturbation chamber and the diameter of the perturbation hole 7 is 6; the ratio between the height of the perturbation chamber and the diameter of the perturbation hole 7 is 3; the ratio between the height of the perturbation chamber and its diameter is 0.5, the diameters and heights of the feed hole 7 and the hole for bursting 1 mm, the Angle of deviation of the flow of the mixture 60 °.
    Short fibrils with an average length of 2.1 mm are obtained. and with a specific surface of 30 m 2 / g.
    PRI me R 6. Carry out the process according to example 2, but using a die equipped with an expansion chamber with an aperture of 150 °.
    The geometric characteristics are changed as follows: the ratio between the diameter of the perturbation chamber and the diameter of the feed hole 7 is 13.3; the ratio between the high β hundredth of the perturbation chamber and the diameter of the feed hole 7 is 4.16; the ratio between the height of the perturbation chamber and its diameter is 0.313; the diameters of the feed hole 7 and the hole for punching 1.2 mm; the height of the feed hole 7 and the hole for punching 1 mm The deviation angle of the mixture flow is 90 “. The polymer flow rate reaches ZOkg / h. In addition, fibrils with an average length of 2.2 nost of 30 m ^ / g are obtained.
    An example from the previous geometrical ry as follows: between the diameter of the perturbation chamber and the diameter of the feed hole 7 is 10.7; the ratio between the height of the perturbation chamber and the diameter of the perturbation hole 7 is 3.34; the diameters of the perturbation 55 holes 8 and holes for bursting 1.5 mm; the height of the perturbation hole 7 and the hole for punching 1 mm The deviation angle of the mixture flow is 90 °. The polymer flow rate reaches 49 kg / h. Get co and mouth fibrils
    2.6 mm. Specific mm. Specific Over 45
    7, Carry out the process' for example, but changing the characteristics of the film ratio with an average surface length of 23 m 2 / g.
    8. Carry out a process example, but O 'use, having
    Example <according to the previous yawning of the die (Fig. 7) three perturbation chambers arranged in series.
    The diameters of the holes following the direction of flow of the mixture are 2 mm, 1.5 mm, 1.2 mm, and 1 mm, respectively. The expansion chamber has an opening of 150.
    Short fibrils with an average length of 1.9 mm are obtained. the specific surface of which is 10 m 1 / g.
    PRI me R 9. A mixture containing 10 wt.% Prolipropylene with a melting index of 2.9 6501 and 90 wt.% Technical pentane, brought to 195 ° C and a pressure of 83 kg / cm 2 . This mixture is pressed by passing through a die with a perturbation chamber equipped with a metal mesh having the following geometric characteristics: the ratio between the diameter of the perturbation chamber and the diameter of the feed hole 7 is 6; the ratio between the height of the perturbation chamber and the diameter of the supply opening 7 is 2; the ratio between the height of the perturbation chamber and the diameter of this chamber is 0.333; diameters and height of the feed hole 7: 1 mm; the diameters and height of the hole for punching are 1.1 mm and 1 mm, respectively. Angle.' deviation of the flow of the mixture 75.
    In addition, the metal mesh 12 has square cells of 0.4 mm in size.
    At the moment of penetration into the feed chamber 8, the mixture of polymer and solvent is subjected to preliminary bursting of 3 kg / cm 2 in order to turn it into two-phase.
    The biphasic mixture is passed through burst openings to 10.3 kg / h. polymer.
    Short fibrils with an average length of 1.7 mm are directly obtained. The specific surface area of these short fibrils is 3 m 2 / g.
    Example. 10. The mixture prepared in accordance with Example 10 is pressed by passing through a die with a perturbation chamber having the following geometric characteristics. The perturbation chamber 5 has a height of 2 mm and a diameter of 4 mm. The punch die has a height and a diameter of 1 mm.
    The connection between the feed chamber 8 and the perturbation chamber 5 is provided by two holes with a diameter of 0.8 and a length of 1.43 mm, the axes of the two holes forming each angle of 45 ° with the longitudinal axis of the die. The deviation angle of the mixture flow is 90 °.
    At the moment of penetration into the feed chamber 8, the mixture of polymer and solvent is preliminarily pressed at 3 kg / cm 2 in order to turn it into a two-phase one. The biphasic mixture is consumed through the opening for 65 punching 2 of 13.9 kg / h of the polymer.
    Short fibrils with an average length of 1.9 mm are obtained directly. The specific surface area of these short fibrils is 3 mg / g.
    Example 11. A mixture prepared. according to example 10, push through by passing through a die with: a perturbation chamber (Fig. 11).
    This die has characteristics identical to those of the die shown in FIG. 9 and 10, and used in example 11, taking into account that the die 2 for punching is limited (zero height) and is equipped with a deflector 11, the expansion angle of which is 150 °. The deviation angle of the mixture flow is 90 °.
    At the time of penetration into the feed chamber 8, the mixture of the molten polymer and the solvent is preliminarily pressed into 3 kg / cm 2 in order to turn it into a two-phase one. The two-phase mixture is consumed through the hole. For bursting 2 at 14.3 kg / h of polymer.
    Short fibrils with an average length of 1.2 mm are obtained directly. The specific surface of these short fibrils reaches 3 m 2 / g.
    Example 12. Prepare a mixture consisting of 85 wt.% Technical hexane and 15 wt.% Polyethylene according to example 1, containing 0.5 wt.%. calcium stearate, and bring this mixture to 194 ° C and to a pressure of 66 kg / cm 2 .
    This mixture is forced through a die with a perturbation chamber, as shown in FIG. 12, and having the following geometric characteristics: the ratio between the diameter of the perturbation chamber 5 and the diameter of the feed hole 7 is 16; the ratio between the height of the perturbation chamber 5 and the diameter of the feed hole 7 is 3; the ratio between the height of the perturbation ’chamber and the diameter of this chamber is 0.187; diameter and height of the feed hole 8 and the hole for punching 1 mm The deviation angle of the mixture flow is 46 °.
    At the time of penetration into the feed chamber 8, the mixture of polymer and solvent is subjected to preliminary bursting of 3 kg / cm 2 in order to turn it into two-phase.
    During punching, water is injected through the opening 16 at 195 ° C and under a pressure of 4–4 kg / cm · 2 with a flow rate of 95 l / h. The two-phase mixture is consumed at 14.4 kg of polymer per hour.
    We get directly short fibrils with an average length of 2.3 mm.
    These fibrils are particle free.
    When water injection is stopped, the flow rate of the mixture reaches 16.5 kg of polymer per hour. Fabricated Fibril60
    The mixture is consumed in an amount based on a flow rate of 30 kg / h of polymer. Short fibrils are obtained with an average length of 2.5 to 3.5 mm and a specific surface area of 4 m 2 / g.
    Example 16. Get a mixture containing 15 weight. % high density polyethylene and 85 wt.% hexane, which is maintained at 195 ° C and a pressure of 65 kg / cm 2 .
    The mixture is throttled by passing the mixing chamber of FIG. 2, having a deflection angle of 120 ° and characterized by the following indicators: the ratio of the diameter of the mixing chamber to the diameter of the die of the mixing chamber 16; the ratio of the height of the mixing chamber to the diameter of the die of the mixing chamber 5; the ratio of the height of the mixing chamber to the diameter of this chamber is 0.312, the diameter of the mixing chamber die and the die for throttling is 1 mm, the height of the mixing chamber die and the die for throttling is 1 mm. . ’
    The mixture is consumed in an amount determined by a flow rate of 30 kg / h. polymer. Split fibrils are obtained with an average length of 1 cm and a maximum specific surface area of 1 m 2 / g.
    Thus, the invention allows to obtain high-quality fibrils in a simpler and more economical way without the use of expensive equipment.
    Then, they have an average length of ί 1.9 mm, and their production is accompanied by the formation of undesirable particles. Synthetic paper made from these last Fibrils has an incomplete clearance, since there is an average presence of 9 large particles per dm *.
    Example 13. Get a mixture containing 15 wt.% Polyethylene vysok! • pressure and 85% by weight of pentane, which is maintained at 140 ° C and a pressure of 100 kg / cm 2 .
    This mixture is throttled by passing through a die plate a perturbation chamber (Fig. 5) having the following geometric indicators: ratio of the diameter of the perturbation chamber to the diameter of the perturbation hole 11; the ratio of the height of the chamber for perturbation to the diameter of the holes for perturbation of 4.54; the ratio of the height of the perturbation chamber to the diameter of this chamber is 0.516; the diameters of the perturbation holes and the throttling holes are 1.1 mm; the height of the perturbation hole and the throttle hole is 1.3 mm.
    The consumption of the mixture is approximately 37.5 kg / h, calculated on the polymer. Short fibrils are obtained, the length of which is 1-1.5, the surface of which is 14 m 2 / g.
    Example 14. containing 1.3 wt.% Juice density and 87 wt.% Hexane, which is maintained at 210 ° C and a pressure of 87 kg / cm 2 .
    This mixture is throttled by passing a displacement chamber through the die (Fig. 5) having the following geometrical characteristics, which differs in that: the measurement of the ameter of the mixing chamber die and the die for 1 mm throttling; You are a cell of a die of a mixing chamber and a die for throttling 1 mm ..
    The mixture is consumed in an amount calculated from the consumption of 35 kg / h of polymer. Short fibrils are obtained, the average length of which is from 1 to 2 mm, and the specific surface of which increases to 29 m 2. · Example. 15. Get a mixture containing 10 weight. % polypropylene and 90 wt.% hexane, which is maintained at 220 ° C and a pressure of 96 kg / cm 2. This mixture is throttled through a mixing chamber similar to that described in the previous example.
    , average mm, and specific increased by
    Get a mixture of polyethylene
    权利要求:
    Claims (2)
    [1]
    The invention relates to a method of making fibrils of short length, as well as to a device intended for its implementation. A known method of producing fibrils is throttling a mixture of a melt of polylefin with a solvent at 140-220.CII. However, this method requires an increased consumption of solvent to achieve sufficient loosening. , long time thorough mixing of the mixture, to which water is added, at very high temperatures (230280s) and a pressure of more than 100 kg / cm, in addition, before the expansion of the mixture volume is necessary Neta it additional amount of water also at high temperatures and pressures.  It is also necessary to use expensive equipment that requires the use of a special extruder and includes a die plate, a chamber with coaxially arranged inlet and throttling holes with a ratio of the distance between these holes to the chamber diameter more than 8,. The purpose of the invention is to simplify the process, reduce economic costs.  The goal is achieved by the fact that in the process of producing fibrils by throttling the mixture of a melt of polyolefie with a solvent at 140–220 ° C, the mixture is fed to the throttling in the form of separate vortex jet streams at an angle of 46–120 to the axis of the choking hole.  In order to realize the production of fibrils, a device is used which contains the die plate, a chamber with inlet and coaxially arranged inlet and throttling holes, the ratio of the distance between these holes to the diameter of the chamber is selected within 0.187-2.5.  FIG.  1 shows an apparatus for carrying out the method; Figs 2-6 are embodiments of the end portion of the device; in fig.  7 shows an embodiment with several perturbation chambers arranged in series; in fig. 8 -. metal mesh device; in fig.  9 and 10 are versions of the device with two feeding holes; in fig.  11 shows section A-A in FIG.  9; in fig.  12 shows an embodiment of a die allowing the formation of a continuous film of lubricant, substances at the level of the wall of the punching hole; Filler 1 (Fig. 1-6) contains a punching hole 2 and a device for pre-punching.  This pre-bursting device, containing the reversal 3, having a central hole 4, is not necessary. Its purpose is to provide a pressure drop in the mixture of molten polymer and solvent, which is in a liquid single-phase form that intersects the die plate in order to cause the formation of a two-phase mixture.  In addition, the die contains a perturbation chamber 5, bounded by a wall, having punching holes 2 and an upper flat wall 6, containing a feeding hole 7 in the center.  The punching and feeding holes are opposite and coaxial.  The perturbation chamber is cylindrical with a circular cross section.  The holes are located in the centers of the bases.  The distance between the holes (height) is usually less than 10 cm and preferably 7.5 cm.  The inlet and outlet of the bore hole 2 (Fig.  2-6) may have different profiles.   When the spinneret chamber 8 is supplied with a two-phase mixture of molten polymer and solvent, this mixture, due to its alignment along the straight line. Does the research institute have openings 7 of wall 6 and openings 2 for pushing through the turbulent permeation chamber through the central g fluid jet 9 and lateral jets 10, which are located near the impulse 2 for bursting, are perturbative across the central jet; cameras.  Angle n.  These side jets can be altered by changing the profile of a stack containing a 2 dp burst hole, as shown in FIG.  2-6.  The angle formed by the axis of the piercing hole and the wall of the chamber in which this hole is made determines the angle of incidence of the lateral of the most eccentric jets, which are the most deflected.  In the die (FIG.  7) provide with several perturbation chambers 5 arranged in series.  In addition, it is desirable that the percussion chamber meets various criteria for maximum efficiency.  It is necessary for the perturbation chamber to have a sufficient dimension of transverse to allow the formation of side jets capable of disrupting the central jet at the level of the inlet, the orifice 2 for pressing.  The distance between the holes of the perturbation chamber (chamber height) must be greater than the diameter of the feed hole.  When the height of the perturbation chamber is small, the lateral deflected jets cannot effectively be directed across the central jet.  On the contrary, when the height of the perturbation chamber becomes very large, the transverse deflected streams tend to connect with the central stream and become parallel with them before they reach the piercing hole.  The height that the perturbation chamber can have is related to the diameter of this 1 meter.  The die 1 for abrupt pushing (FIG.  8) is equipped with a metal grid 12 located in the perturbation chamber 5.  The perturbation chamber 5 is bounded by a wall containing an extrusion hole 2, and an upper flat wall b, having in its center a feed hole 7, a 2 dp extrusion hole and a feed hole 7 are opposite and coaxial.  The side wall of the perturbation chamber 5, having a cylindrical shape, is bounded by a ring 13.  The perturbation chamber may be of another shape, in particular, a parallelepiped.  The function of ring 13 is double; on the one hand, this ring defines height.  perturbation chamber 5 and, on the other hand, it supports the grid with small cells 12, located in the perturbation chamber against the wall 6 containing the feed hole.  The dies shown in FIG.  9, 10 and 11, of the same type as the die, shown in FIG.  8, except that it does not contain a metal grid, located in the perturbation chamber.  In addition, the communication between the supply chamber 8 and the perturbation chamber 5 is provided by two supply openings 7, the axes of which are inclined with respect to each other and which are connected in one opening of the side of the perturbation chamber.  In these spinnerets, the ring 13, bounding the cylindrical side wall of the perturbation chamber, serves only to adjust the height of this chamber.  Dies, (FIG.  9, 10, and 11) are provided with a metal grid located in the perturbation chamber, and / or may have two or more openings, the axes of which are para-, parallel.   As shown in FIG.  1,2,3,4,7 and 11, it is possible to provide an expansion chamber 11 at the exit, a burst hole, the expansion angle preferably being more than 150.  The die 1 (FIG.  12), containing a pre-punching chamber 8, a powering hole 7 of the perturbation chamber 5 and a punching hole 2 equipped with a bet, a perforated chamber 15 which surrounds the perturbation chamber 5, and the partition 14 separating these chambers is interrupted at the level of the inlet opening pushing 2 like that. In order to create a slit round H-7, coaxial with a hole for. pushing through.  The peripheral chambers 15 are further provided with an opening 16 for connection to a source of liquid lubricant.  Example 1 A biphasic mixture is prepared by bringing to a temperature of 195 ° C and a pressure of 63 kg / cm2, containing 15 wt. % polyethylene of high density and with a melting index of 5 and 85 wt. % technical hexane. These conditions correspond to the onset of two liquid phases.  This mixture is forced through a spinneret with a perturbation chamber having the following geometrical characteristics: the ratio between the diameter of the perturbation chamber and the diameter of the perturbation hole 7 is 16; the ratio between the heights of the perturbation chamber and the diameter of the supply hole 7 is 5; the ratio between the height of the perturbation chamber and the diameter of this chamber is 0.313; diameters and heights of the supply hole 7 and pressure openings of 1 mm.  The expansive device, the continuation of the hole for a sharp push, has 150 °.  The angle of deflection flow of the mixture subjected to throttling is 90.  The biphasic mixture is dispensed at 21.4 kg / h of polymer.  Short fibrils are obtained with an average length of 1.7 mm.  The surface area of these fibrils has risen to 35 m / g.  Example 2  The process of Example 1 is carried out, except that it is pre-pressed at. pressure of 12 kg / cm.  Short fibrils are also obtained with an average length of 1.9 mm.  The specific surface of the product has risen to 23 m2 / g.  Example 3  The process of Example 2 is carried out, but using a spinneret with a perturbation chamber (Fig.  3), the geometric characteristics of which are identical to those specified in example 1.  Short fibrils are obtained with an average length of 1.8 mm.  Their specific surface is 21.  Example 4 - Carry out the process of Example 4, taking into  note that the die has the following altered geometrical characteristics: the ratio between the height of the perturbation chamber and the diameter of the perturbation hole 7 is 40; the ratio between the height of the perturbation chamber and its diameter is 2.5 -.  Angle of flow of the EO blend.  Again, short fibrils are obtained with an average length of 2.3 mm, whose specific surface is 26.  Example 5  The process of Example 2 is carried out, but using (dies (Fig.  6), the geometrical characteristics of which are as follows: the ratio of the diameter of the perturbation chamber and the diameter of the perturbation hole 7 is 6; the ratio between the height of the perturbation chamber and the diameter of the perturbation hole 7 is 3; the ratio between the height of the perturbation chamber and its diameter is 0.5; the diameters and heights of the feed hole 7 and the puncture hole 1 mm.  The angle of flow of the mixture is 60 °.  Short fibrils are obtained with an average length of 2.1 mm.  and with a curved surface 30.  Example 6  The process of Example 2 is carried out using a die equipped with an expansion chamber with an opening of 150 °.  Geometric characteristics are changed as follows: the ratio between the diameter of the perturbation chamber and the diameter of the supply hole 7 is equal to 13.3; the ratio between the height of the perimeter chamber and the diameter of the supply hole 7 is 4.16; the ratio between the height of the perturbation chamber and its diameter is 0.313; diameters of the supply hole 7 and the hole for forcing 1.2mm of the height of the supply hole 7 and the hole for forcing 1 mm.  Mix flow angle 90.  Polymer weight consumption reaches ZOkg / h, and, additionally, fibrils with an average length of 2.2 mm are obtained.  Specific surface 30.  Example 7  The process is as in the previous example, but. change the geometric characteristics of the film as follows: the ratio between the diameter of the perturbation cavity and the diameter of the supply hole is 10.7; The ratio between the high perturbation chamber and the diameter of the perturbation hole 7 is equal to 3.34; diameters of the perturbation layer 8 and holes for pushing 1.5 mm; the height of the perturbation hole 7 and the hole for pressing 1 mm.  The angle of deflection of the mixture is 90.  The weight consumption of the polymer reaches 49 kg / h.  Kotkie fibrils with an average length of 6 mm pop. Specific surface 23.  Example 8  The software is carried out using the previous example, but using a spinneret (t; IG.  7), having three perturbation chambers arranged in series.  The diameters of the holes following in the direction of flow of the mixture are 2 mm, 1.5 mm, 1.2 mm and 1 mm, respectively.  The expansion chamber has an opening of 150.  Short fibrils are obtained with an average length of 1.9 mm.  whose specific surface is 10 m / g.  PRI me R 9.  A mixture containing 10 wt. % prolipropylene with a melting index of 2.9 6501 and 90 weight. % technical penta. on, adjusted to 195 ° C and to a pressure of 83 kg / cm.  This mixture is forced by passing through a die with a perturbation chamber equipped with a metal grid having the following geometrical characteristics: the ratio between the diameter of the perturbation chamber and the diameter of the supply hole 7 is 6; the ratio between the height of the perturbation chamber and the diameter of the supply hole 7 is 2; -The ratio between the height of the perturbation chamber and the diameter of this chamber is 0.333; diameters and height of the supply hole 7: 1 mm; the diameters and height of the hole for forgings are 1.1 mm and 1 mm, respectively.  Angle.  reject the flow of the mixture 75.  In addition, the metal mesh 12 has square cells of about 4 mm in size.  At the moment of penetration of the feed chamber, chamber 8, the mixture of polymer and solvent is subjected to preliminary pressing at 3 kg / cm in order to transform it into a two-phase one.  The two-phase mixture is passed through holes for squeezing up to 10.3 kg / h.  polymer  Short fibrils are obtained directly with an average length of 1.7 mm.  The specific surface of these short Try on.  The mixture prepared according to Example 10 is sold by passing through a die with a perturbation chamber having the following geometric characteristics. The perturbation chamber 5 has a height of 2 mm and a diameter of 4 mm.  The die for pressing has a height and diameter of 1 mm.  The connection between the feed chamber 8 and the perturbation chamber 5 is provided by two openings with a diameter of 0.8 and a length of 1.43 mm, with the axes of the two openings forming each angle of 45 with a longitudinal axis, dies.  The angle of the mixture flow is 90 °.  At the moment of penetration of the polymer mixture into the feed chamber 8, the solvent is subjected to preliminary prolongation of 3 kg / cm in order to convert it into a two-phase one.  The biphasic mixture is consumed through a bore 2 for 13.9 kg / h of polymea.  Short ibrills are obtained directly with an average milk yield of 1.9 mm.  Single surface of these short ibrill 3 MVr.  Example 11, A mixture prepared as in example 10 is forced through the passage through a spinneret with: a turbulence chamber (FIG.  eleven).  This die has characteristics similar to those of the spinneret depicted in FIG.  9 and 10, and used in Example 11, taking into account that the spinning nozzle 2 is limited (zero zero) and provided with a deflector 11, the expansion angle of which is 150 ° k. The deviation angle of the mixture flow is 90 °.  At the moment of penetration into the supply chamber 8, the mixture of molten polymer and solvent is subjected to preliminary punching of 3kg / cm in order to turn it into a two-phase one.  The biphasic mixture is consumed through the opening. for squeezing 2 to 14.3 kg / h of polymer.  Short fibrils with an average length of 1.2 mm are obtained directly.  The surface area of these short fibrils reaches 3, Example 12.  Prepare a mixture consisting of 85 wt. % technical hexane and 15 wt.% polyethylene in example 1, containing 0.5 wt. %  calcium stearate, and bring this mixture to 194 ° C and to a pressure of 66 kg / cm 2.  This mixture is forced through a spinneret with a perturbation chamber, as shown in FIG. 12, and having the following geometrical characteristics: the ratio between the diameter of the perturbation chamber 5 and the diameter of the supply hole 7 is 16; the ratio between the depth of the perturbation chamber 5 and the diameter of the supply hole 7 is 3; the ratio between the height of the perturbation chamber and the diameter of this chamber is 0.187; the diameter and height of the feed hole 8 and the holes for the punctures of 1 mm.  The angle of flow of the mixture is 46 °.  At the moment of penetration into the supply chamber 8, the mixture of polymer and solvent is subjected to preliminary punching at 3 kg / cm in order to turn it into a two-phase one.  During squeezing, water is injected through the opening 16 at 195 ° C and under a pressure of 44 kg / cm with a flow rate of 95 l / h.  The biphasic mixture is consumed at 14.4 kg of polymer per hour.  We obtain directly short fibrils with an average length of 2.3 mm.  These fibrils do not contain particles.  When water injection is stopped, the mixture consumption reaches 16.5 kg of polymer per hour.  The manufactured fibrils then have an average length of 1.9 mm, and their production is accompanied by the formation of undesirable particles.  Synthetic paper made from these latter fibrils has an incomplete clearance, since an average of 9 large particles per dm is noted.  Example 13  Get a mixture containing 15 wt. % high pressure polyethylene and 85 wt. % of pentane, which is kept at 140 s and a pressure of 100 kg / cm.  This mixture is throttled by passing through the chamber of a perturbation through the die plate (FIG.  5) having the following geometrical parameters: the ratio of the diameter of the chamber for perturbation to the diameter of the hole for perturbation 11; the ratio of the height of the chamber for perturbation to the diameter of the hole for perturbation is 4.54; the ratio of the height of the perturbation chamber to the diameter of this chamber is 0.516; perturbation orifice and throttling apertures 1.1 mm; the height of the perturbation opening and the throttling opening is 1.3 mm.  The mixture consumption is about 37.5 kg / h, based on the polymer.  Short fibrils are obtained, the average length of which is 1-1.5 mm, and their specific surface area is increased by 14.  Example 14  Get the mixture containing (TSU 1. 3 wt. % high density polyethylene and 87 wt. % hexane, which is maintained at 210 ° C and a pressure of 87 kg / cm.  This mixture is throttled when a displacement chamber is passed through the die, (Fig.  5) having the following geometrical characteristics: the ratio of the diameter of the displacement chamber to the diameter of the nozzle of the mixing chamber 10; the ratio of the height of the chamber is displaced to the diameter of the die plate of the mixing chamber 4; the ratio of the height of the chamber is no less than the diameter of this chamber 0.4; diameters of the spinneret of the mixing chamber and the spinneret for throttling 1 mm; You are using a cell of the spinneret of the chamber by mixing the spinneret to choke 1 mm. .  “. . .  The mixture is consumed in an amount from the flow rate of 35 kg / h of polymer. Short fibrils are obtained whose average length is from 1. to 2 mm, and whose specific surface increases to 29 m, Example.  15.  Get a mixture containing 10 weight.  % polypropylene and 90 wt. % hexane, which is kept at 220 ° C and a pressure of 96 kg / cm. This mixture is throttled through ka, a measure of mixing similar to that described in the previous example.  The mixture is consumed in an amount based on the consumption of 30 kg / h of polymer.  Short fibrils are obtained, with an average length of 2.5 to 3.5 mm and a specific surface area of 4.  Example 16  Get a mixture containing 15 wt.  % polyethylene, high density and 85 wt. % hexane, which is maintained at 195s and a pressure of 65 kg / cm 2.  The mixture is throttled by passing the mixing chamber shown in FIG.  2, having a deflection angle and characterized by the following indicators: the ratio of the diameter of the mixing chamber to the diameter of the nozzle of the mixing chamber 16; the ratio of the height of the mixing chamber to the diameter of the spinneret of the mixing chamber 5; the ratio of the height of the mixing chamber to the diameter of this chamber is 0.312; the diameter of the mixing chamber dies and dies for throttling 1 mm; the height of the dies of the mixing chamber and dies for throttling 1 mm.  .   The mixture is consumed in an amount determined by the consumption of 30 kg / h of polymer.  Split fibrils are obtained, with an average length of 1 cm, a. the largest surface area is 1.  Thus, the invention makes it possible to obtain high quality fibrils in a simpler and more economical way, without using expensive equipment.  Claim 1.  A method of producing fibrils by throttling a mixture of a polyolefin melt with a solvent at 140-220 ° C, characterized in that, in order to simplify the process and reduce economic costs, the mixture is fed to the throttling as separate twisted jet streams at an angle of 46-12. 0 to the axis of the throttling hole.  
    [2]
    2. An apparatus for carrying out the method according to claim 1, comprising a spinneret, a chamber with inlet and throttling openings which are made therein and coaxially arranged, is about as long as the ratio of the distance between these openings to the dieter cameras selected in the range 0,187, 5. Sources of information taken into account during the examination 1. Belgium patent 787032, cl. D. 01 D pub. 1972 (prototype)
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    同族专利:
    公开号 | 公开日
    ZA748009B|1976-01-28|
    JPS56154511A|1981-11-30|
    US4010229A|1977-03-01|
    JPS5916001B2|1984-04-12|
    LU69196A1|1975-12-09|
    TR18455A|1977-02-16|
    BE824484A|1975-07-17|
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    US3386488A|1966-03-18|1968-06-04|Leuna Werke Veb|Process for producing powders from plastic and wax masses|
    US3461193A|1967-01-04|1969-08-12|Du Pont|Novel procedure for starting the flash-extrusion of expandable resin compositions|
    US3663668A|1968-02-28|1972-05-16|Fmc Corp|Sonic nucleation in foam extrusion|
    GB1262285A|1968-03-28|1972-02-02|Ici Ltd|Method and apparatus for flow rate control in continuous extrusion|
    JPS5116533B1|1971-06-01|1976-05-25|
    BE787890A|1971-09-09|1973-02-23|Solvay|
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    US3902957A|1973-04-05|1975-09-02|Crown Zellerbach Corp|Process of making fibers|US4107243A|1976-06-10|1978-08-15|Suntech, Inc.|Preparation of thermoplastic polymer fibrilla and fibril|
    US4387144A|1977-05-11|1983-06-07|Tullis Russell & Company Limited|Battery separator material|
    FR2426099B1|1978-05-05|1980-12-19|Solvay|
    US4376747A|1980-12-11|1983-03-15|Union Carbide Corporation|Process for controlling the cross-sectional structure of mesophase pitch derived fibers|
    US4480977A|1980-12-11|1984-11-06|Union Carbide Corporation|Apparatus for controlling the cross-sectional structure of mesophase pitch derived fibers|
    US4352650A|1981-03-24|1982-10-05|E. I. Du Pont De Nemours And Company|Nozzle for flash-extrusion apparatus|
    DE3809735C1|1988-03-23|1989-06-08|Werner & Pfleiderer Gmbh, 7000 Stuttgart, De|
    KR0168680B1|1989-06-01|1999-03-20|데이비드 마이클리스|Starch derived shaped articles|
    US5833900A|1995-07-28|1998-11-10|E. I. Du Pont De Nemours And Company|Process for modifying porosity in sheet made from flash spinning olefin polymer|
    WO1999023306A1|1997-10-31|1999-05-14|Dexter Corporation|Heat seal infusion web material and method of manufacture|
    EP1891256B1|2005-05-11|2012-08-01|Ahlstrom Corporation|Highly resilient, dimensionally recoverable nonwoven material|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    LU69196A|LU69196A1|1974-01-18|1974-01-18|
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