JPS58109609A - Production of fiber - Google Patents

Abstract

PURPOSE:A mesh-like spinneret with a specific void volume is heated and a powdery polymer is fed thereto and extruded out to produce fiber aggregates by melt-spinning a polymer of very high melt viscosity or readily decomposable or crosslinkable, when melted. CONSTITUTION:A mesh-like spinneret having more than 10% void volume alpha, which is defined with the equation (Va is the apparent whole volume in a unit area of the mesh part, Vf is the total volume of the sectioning material surrounding the fine gaps in the unit area of the mesh part), and having a number of fine pores closely arranged one another is used a powdery polymer is fed from the opposite side to the extruding surface, under feeding heat through the sectioning material surrounding the fine pores to melt the polymer, extruded out of the fine pores and cooled to give the objective fiber aggregate.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fibers by melt spinning by feeding a solid powder into a die having a polymeric spinneret. More details.

Polymers with extremely high melt viscosity or polymers that rapidly decompose or crosslink when melted are heated to a high temperature for a short period of time to make them opaque, and within a period of time during which the pattern coalesce does not lose its stringiness. This is a novel method that has not been seen before.

Conventionally, there are three types of molding methods for polymers, especially fiberization: melt molding, dry molding, and wet molding. Ta. All of these methods make polymer molecules more mobile
L (plasticizes) to form a desired molded product, solidifies (suppresses movement of polymer molecules) and arranges polymer molecules in a desired arrangement II#c. Two types of plasticizing means can be considered. One is called the melting method, in which the polymer is heated above its glass transition point or above its melting point.
It generates thermal motion that overcomes intermolecular interactions and plasticizes it. The other method is called the solution method, in which one polymer is dissolved in a submersible solvent, and the intermolecular interactions between the two polymers are weakened by the intermolecular interactions between the polymer and the S medium. It activates and plasticizes.

These three plasticization methods have also been combined. For example, there is a method in which the polymer and solvent phase separate or solidify at low temperatures, and dissolve when the temperature rises. This method is useful when it is desired to plasticize a polymer, which decomposes rapidly when heated above the melting point, at a temperature below the melting point.

The melting method is superior to the solution method in terms of manufacturing cost and flexibility in the shape of the molded product (particularly when obtaining a thick and uniform molded product). Therefore, polyethylene terephthalate can be used by melting method.

Polybutylene terephthalate, polyhexamethylene adipamide, poly-1-kabu platatam.

Polypropylene, polyethylene, etc. are industrially molded into various shapes by melt molding.

In the melting method, basic K&! , a heating device and a cooling device are all that is required.

on the other hand,! Polyacrylic acid that rapidly decomposes and crosslinks when melted 2) Zil. A solution method is used for polyvinyl chloride, polyvinyl alcohol, polymetaphenylene inphthalate, cellulose, etc. #The liquid method requires equipment to extract the solvent thermally or in phase equilibrium and equipment to recover or treat the solvent, and requires more complicated equipment and operations than the ilIFm method. do.

For these reasons, attempts are being made to apply methods as close to melting methods as possible to polymers to which ordinary melting methods cannot be applied.For example, as mentioned above, there are two plasticizing methods. Attempts are being made to combine the two. Specific examples include a method of high-temperature plasticization of polyacrylic 9ty-di)lyl with water, and a method of high-temperature plasticization of polymetaphenylene inphthalate 71 with a complex-forming solvent.

Examples include a method of phase separation molding using a solvent that dissolves the copolymerized fluororesin at high temperatures and causes phase separation at low temperatures.

However, these methods use a considerable amount of solvent, and do not fundamentally solve the above-mentioned drawbacks of the S* method.

The present inventors believe that there are conditions under which a polymer with a melting point can undergo II melting even if its molten state is unstable, and this is the result of extensive research.

Decomposition during melting JR bridges suddenly change #IC has discovered a method for melt-molding a polymer that has a very high viscosity and is difficult to mold even when melted.

That is, the present invention provides a method for producing a fiber aggregate by extruding a fiber-forming polymer through a spinneret having a large number of pores, the method comprising: A mesh-like spinneret having a large number of ams is used, and a solid powder polymer is supplied to the surface opposite to the discharge surface of the spinneret, while being heated from the partition member of the mesh-like spinneret. , the integral powder polymer is melted, and the melt is extruded through a number of slits surrounded by the partition member.

At this time, a cooling fluid is supplied to the discharge surface of the S melt of the spinneret and its vicinity, and the melt extruded through the wrinkles is cooled by four times, so that the #IIm polymer is substantially This method is characterized by converting the melt into a large number of separated fine streams and converting it into TM within a time without losing the molding layer.

The fiber-forming polymer as used in the present invention means a polymer that can be converted into II11mIK in bulk form by some molding means. A linear polymer having a low chain length of 1,000 ohms or more is fiber-forming, but may have some branched chains.

According to the present invention, it is possible to produce a fiber collection body not only from fiber-forming polymers with good spinnability, but also from fiber-forming polymers with poor spinnability as shown below.

(1) Polyolefin or polyvinyl polymer:
For example, polyethylene, polybupylene, polybutylene,
Polyethylene, polyvinyl chloride.

Polyvinyl, polyacrylic trilyl, poly7talyl ester, or their mutual copolymers/polymers.

1 layer) polyamides; for example, aliphatic polyamides such as polyC-cabrolactan, polyhexamethylene adihamide, polyhexame + lance hakamide, and the following formula % (where R is a divalent aliphatic group or an aromatic group) dicarboxylic acid residues represented by the following formula % (where R' is a divalent aliphatic group or aromatic group); 81 is an aliphatic group or an aromatic group)
A fully aromatic boria ξ consisting of a constituent unit selected from one in five so that the carbonyl group (-CO-) and the 7Z group (-NH-) are equal in number (however, at least one of the total constituent units is 70
mole%.

Preferably at least 80 mol% consists of constitutional units containing aromatic residues).

The divalent aliphatic residue in the above formula is a group used in the field of aliphatic polyamides, such as tetramethylene, pentamethylene, and hexymethylene, and the octavalent aromatic group is a group such as para-phenylene group or meta-phenylene group -Ls-naphthylene group, tome 6-naphthylene group, tome 3'-@4 a'- or tome 4'-diphenylene group, tome $'-#44'- or tome 4'- diphenyl ether groups, etc.Specific examples of such aromatic polyamides include polyparaphenylene isophthalamide, polymethacrylate resin, polymethaphenylenetereathalamide, poly-1, Examples include 1-naphthylene isophthalate, poly-&4'-diphenylene terephthalate, and copolymers thereof.

(Polyester: For example, aromatic dicarboxylic acids such as phthalic acid, isophthalic acid, terephthalic acid, diphenyl dicarboxylic acid, naphthalene dicarboxylic acid; aliphatic dicarboxylic acids such as adipic acid, cepatic acid, decanedicarboxylic acid, etc.; or hexahydro-terephthalic acid; The dibasic acid component is aliphatic dicarboxylic acid such as acid, ethylene glycol, propylene glycol, trimethysine glycol, tetramethylene glycol, decamethylene glycol, diethylene glycol.

The glyconyl component is an aliphatic glycol such as 2-dimethylpropanediol, a tn cyclic glycol such as hexahydroxylylene glycol, an aromatic aliphatic glycol such as xylylene glycol, an aromatic dihydroxy compound such as hisorcinol, or hyde p-quinone. Polyesters or wholly aromatic polyesters, these polyesters or wholly aromatic polyesters may also contain components of oxydicarboxylic acids, such as p-1 xybenzoic acid.

Any of the above dibasic acid components or glycol components may be contained in the above polyester or wholly aromatic polyester.

Particularly preferred examples include polyethylene terephthalate, polytesiramethylene terephthalate, polytrimethylene terephthalate, and US Pat. l & 10 issue, same a
, os&ies issue, os&@ II issue 1,014 and os&? Polyester elastom "qj++" listed in @a14@1cle, or fully aromatic as described in U.S. Patent No. There are family polyesters.

According to the present invention, it is possible to stably procure a fiber-electrolyte without decomposing the wholly aromatic polyester K*h whose molding temperature is extremely high.

Other polymers Polycarbonate using various bisphenols in addition to the polymers listed (1) to (-): Poly 7 cetal:
Various polyurethanes: PoV fluoroethylene, polytrifluoride
Durable ethylene.

Polyvinylidene difluoride, polyflJ7) ethylene-propylene hexafluoride copolymer, ethylene fluoride-perfluoro-fluorinyl vinyl ether copolymer, polytetrafluorinated ethylene-ethylene copolymer, polytetrafluoride Ethylene-propylene copolymer, polyvinyl fluoride.

Polymers include fluorinated chlorinated ethylene-ethylene copolymer.

According to the present invention, polymers with chain lengths far exceeding 1000 ohms and rigid polymers with high molecular weight (
These fibers can be easily spun even though they are generally difficult to discharge and spin due to their ultra-high viscosity, and the fibers formed have high strength as befits fibers made of long chain polymers.
It has sufficient elongation. Examples of such ultra-high molecular weight polymers include polyethylene having a molecular weight of 1 million or more, fully aromatic polyester having an intrinsic viscosity of 4 or more and exhibiting melt anisotropy, and the like.

Opinion The polymer used in tliK melts, albeit temporarily. The melting point is determined by differential thermal analysis (D?m) and differential calorimetry (D8C) $ 7a-tester etc. R''''C! It can be determined from Tsuru analysis. Some do not show a clear first-order thermodynamic transition point (not detected by D, DIICK), but begin to flow (detected by a flow tester).

The molded article forming section referred to in Opinion IR is the following (1) to (3).
This refers to the performance when all the requirements are satisfied.

(1) The polymer can be discharged from the discharge port according to the present invention (the combined viscosity of the pattern can be reduced to the viscosity necessary for passing through the discharge port) (!> The polymer is aligned in the discharge direction. It must be possible to continuously discharge from the discharge port.

131 The mechanical strength of the discharged continuous body of molded metal bodies after cooling is within a practical range.

The specific physical property values IIm of the requirements (1) and (2) above are 11)K5 viscosity of 1.0000 poise or less in the case of fibers, and the mechanical strength of (3) is α'& I/d.・A tensile strength higher than that is desirable.

These polymers can be prepared by polymerization in solution, in the S-molten state or in phase, and can be obtained in bulk or powder form, preferably in powder form. It may be fed into the mesh-like nozzle in this state, or it may be further ground into a fine powder, or formed into a rod shape, and then fed to the mesh-like nozzle, preferably in the case of powder. is 30 mesh to 100
Mesh viscosity is preferred.

Also, various types of these polymer powders may be mixed.

The polymer powder may be mixed with a low-molecular solid powder or impregnated with a low-molecular liquid to improve moldability or impart new functions to the molded product.

For example, the polymer may contain a light stabilizer, a #i material, a heat stabilizer, a fuel agent, a lubricant, a matting agent, etc. which are usually used as additives for fibers.

According to the method of the present invention, the various fiber-forming polymers described above have a porosity expressed by the following formula of about 10% or more. The 111-liquid is extruded from a mesh-like spinneret with many closely spaced slits and converted into a trickle.

The spinneret used in the present invention has a void ratio < a as described above.
> has a large number of near M defined by the value of
! 2! In the above formula that defines the porosity, *the mesh-like portion of the thread cap is the mesh-like portion t of the thread cap.

The spinneret used in the present invention has a large number of closely spaced holes defined by the above-mentioned porosity, and the shape of the partition member defining the shape or the shape of the hole may be any shape. good.

The mesh-shaped spinneret used in the present invention is as follows.

Therefore, for example, a circle, a circle, a triangle, a triangle.

It may be any other polygonal shape, or the partition member defining 1AIl may or may not have unevenness.

1-8 of the accompanying drawings 1-8 illustrate a typical example of a mesh-like spinneret used in the present invention. The illustrated mesh-like spinneret is a plain woven wire mesh. 3rd-b [
K is an illustration of a cutaway view of the wire mesh □ in Figures 1-8.

In the plain weave wire mesh shown in the figure, am has a rectangular shape.
Five concave portions are provided in the partition member between the adjacent slits 1IAIII so that the 1II1 melt extruded from the adjacent slits can come and go.

4-8 of the accompanying drawings illustrate another example of the mesh spinneret used in the present invention. The illustrated mesh spinneret is an etched perforated plate with a greater number of slits than the thin metal 11iK precision etching technique 1IIK. In this etched perforated paddle, Jllll forms a tri-oval, and as is clear from the cross-sectional view illustrated in FIG. 4-b, the adjacent partitioning members existing llAl111'&Ik do not cover the recessed portions.

The mesh-like spinneret used in the present invention is as follows.

In addition, it may be an island or a woven wire mesh, or it may be a thin sintered body in which many minute metal spheres are sintered to form many miosis, or a partition member where adjacent ml1MK exists. may be an etched porous spinneret having concave portions 1 Part of these mesh-like spinnerets used in the present invention
No. 140116) The newsletter specification Kll is shown.

In opinion q4, these mesh-like spinnerets can not only be used alone, but also in a combination [laminated].

According to one of these spinnerets according to the invention.

Preferably, the discharge mK of the spinneret has a large number of slits partitioned by narrow partition members having uneven parts, and the J
A mesh-like or squirrel cap is used, which is structured so that the molten liquid extruded from a certain slit in IIIl can come and go through the recess of the partition member.

Define the mesh-like spinning nozzle used in the present invention! 2
! In the above formula expressing porosity.

vl is the total apparent volume occupied by a unit area of the mesh-like part of the spinneret.

Vf is the total volume occupied by the partition member surrounding the slit under a unit area of the mesh-like portion of the spinneret.

From Figure 3-8 of the attached drawings and the ms-bllIK diagram, it is clear that the bottle stand is assumed to have a virtual surface that contacts the front and back surfaces of the cap, and the unit area (1- The total apparent volume (Va) is defined as the volume formed by the virtual laW of ).

In order to determine Va for a mesh-like spinneret of 1111iK, vl can be easily determined from k by measuring the thickness of the mesh-like spinneret with a mechanical gauge having 17 contact surfaces.

In addition, in order to determine Vf for a certain mesh-like spinneret, it is sufficient to cut the mesh-like spinneret into a predetermined area, 1, for example, submerge it in a liquid, and determine the increased volume vIl at that time. Mesh-like spinneret 1
The value converted per d becomes Vf.

According to the present invention, the porosity α is expressed by the following formula as described above: * Va * vf & KII to be determined
Based on 1- of the L-mesh-shaped IIjA cap, V
It can be seen that the numerical value representing a is a numerical value representing the thickness of the mesh-like spinneret, as illustrated in Sections 5-bsia and 4-b-.

Opinion II! According to 1, the mesh-like spinneret used in the present invention has a void ratio of 10% or more, preferably about 20% to @S.%. If the porosity is small, SSt sites of one heavy metal body are generated, which makes it easy for one polymer to deteriorate or crosslink, resulting in clogging of pores, deterioration of molded product performance, etc. If the 4m ratio is too large, the strength of the spinneret will decrease and the spinneret will be easily torn (
Become.

According to the present invention, the mesh-like spinneret used in the present invention preferably has about 5 or more slits, more preferably about 10 to about 10,000 slits. Particularly preferably, it has 100 to 1000 slits.

Further, according to the present invention, the mesh-like spinneret used in the present invention has a diameter of about 10 cm or less, more preferably about a1 m
It has a thickness t of about 5 m. Special ka2~! ■ is preferred.

In the present invention, a solid polymer is supplied to the surface of the mesh spinneret opposite to the discharge surface.

By supplying it in solid form, deterioration and crosslinking of the #polymer can be prevented. For the feeding element RK, a moving/pressurizing method using a plunger, screw, pump, etc. is useful.
astlcm, ao, tso(1@@s)
K-plunger continuous extruders have been introduced and these are useful for continuous production IIK. It is also preferred to use a set of screws designed for transporting powder.

In the present invention, it is preferable that the TMK solid polymer on the opposite side of the discharge surface of the wrinkled mesh spinneret is supplied under pressure at a pressure of 1 oy/-1 degree or more. The wrinkled polymer powder (or agglomerate) is deposited in each fine 1lV of the spinneret.
In addition to being supplied evenly, it is possible to melt and discharge uniformly by supplying uniform heat. Moreover, the filling of the polymer powder (or lump) is progressed by pressurization, defoaming is performed (so-called pressure defoaming), and voids in the fibers to be molded can be reduced.

According to the present invention, the solid polymer supplied to the opposite side of the mesh spinneret from the discharge surface is heated at 1 wI given by the partition member of the mesh spinneret which is generating heat.
IK allows it to be melted and molded in an extremely short time. This makes it possible to prevent deterioration and crosslinking of the heavy metal body as much as possible.

In order to generate heat from the partition member itself and supply peaks to the polymer, there is a method of heating the partition member by passing an electric current through it (
Current heating method), heating by induction heating by applying a high-frequency electric field, heating by dielectric heating by applying a high-frequency electric field, constructing the partition member with a thin tube and heating it by flowing a heating medium into the tube. (thermal fluid heating method) etc. are advantageously employed.

Materials that can be conveniently used in the current heating method and the induction heating method include platinum, gold #*# copper, titanium, vanadium, tungsten, iridium, molybdenum-palladium e, iron a, nickel, lime, cobalt, and lead-zinc.・Metals such as screws, tin, and full miniram, stainless steel,
Nicomu.

Alloys such as tantalum, brass, phosphor copper, duralumin, lead rope, silicone, germanium.

Cele/, tin oxide, indium oxide, iron oxide.

Inorganic compounds that mainly exhibit semiconductor properties, such as nickel oxide, and organic compounds that do not exhibit semiconductor properties, such as polyacetylene and polyphenylene.

It is advantageous to use a material in which the spinneret is formed with a material having a specific resistance of 10-7 to 1-degrees.

The spinnerets described in FIGS. 1, 2, and 3 are all electrically conductive and suitable for the purpose of the present invention. The fake structure has a conductive structure by coating the surface of glass beads with silver and pressing them into contact, a conductive cap structure made by vapor-depositing aluminum metals on ceramic fibers such as alumina and zirconia, and press-molding them, and porous Examples include a conductive mesh-like spinneret structure in which a high-quality ceramic plate is immersed and deposited in a graphite dispersion, and various other possible structures have been improved to create 1i! The conductive mesh-like spinneret thus obtained is usually heated under an electric field of a1 to several hundred V/3 in the case of the current heating method.
A current of several hundred A is applied and a watt density of Ll to several thousand W/- is used.

These values can change depending on the situation, and 1
Desired performance can be obtained by selecting the cap material and designing the cap structure.

The electrically conductive mesh spinneret of the current heating method is attached to the extruder outlet, and should be mounted in such a way that the desired current flows through the electrically conductive mesh spinneret. The conductive mesh spinneret and the extruder may be insulated, or the extruder and the conductive die may be electrically connected to suitably distribute the current flowing through the extruder and the conductive die to achieve the desired performance. It is also possible to obtain

The insulating material used to connect the conductive mesh spinneret to the extruder is determined depending on whether the temperature of the spinneret is raised to the temperature of one spinneret or the like. When used at temperatures below 200°C, silicone resins, phenolic resins, etc. are sufficient; when used at temperatures below SOO°C, fluororesins, aromatic polyimides, aromatic polyamides, polyphenylene sulfides, polyarylates, etc. may be used. A combination of a general ceramic plate and an inorganic adhesive such as silica, alumina, zirconia, etc.-1IIIJ can be used up to around 100°C.

On the other hand, when heating a conductive mesh-like spinneret as described above by induction heating, a coil is generally placed almost parallel to the spinneret, and a magnetic field is applied almost directly to the spinneret. Eddy currents are generated on the surface and Joule heating is generated.

If the heating frequency is selected to be high, the penetration of eddy current becomes shallow due to the one-skin effect, and local heating of only one surface can be performed. Depending on the thermal characteristics of the polymer to be molded and the material and shape of the apparatus, the optimum state can be obtained by appropriately combining the coil arrangement, magnetic field strength, and frequency.

The surface material of the mesh-like spinneret used in the dielectric heating method is generally a material that causes KII electric loss, and depending on the frequency of the applied electric field and the properties of the polymer to be molded, ceramics with Ti groups can be used. For use at relatively low temperatures, hard plastics such as phenol resin, preferably with hydroxyl groups, are used.The cap surface is made of materials with different dielectric properties, and an electric field of an appropriate frequency is applied to locally It is possible to create a temperature distribution.

When the surface of such a dielectric mesh spinneret is heated by a dielectric heating method, electrodes are usually arranged parallel or perpendicular to the surface of the spinneret, and an alternating electric field parallel or perpendicular to the surface of the spinneret is applied.

Dielectric loss occurs and heat is generated.

The capillary used in the thermal fluid heating process is preferably of high thermal conductivity, such as aluminum, stainless steel, iron, copper, brass, silica, nickel.

Insnel. Materials such as tungsten, tantalum, molybdenum, rhenium, titanium, and niobium are used. The heat medium is selected to be compatible with the operating temperature and the thin tube.1 For example, water, ammonia, methanol, 7 setone, freon11
．． Freon 21, Freon y x 1s e C6F@
e a-butane an-pentane, a-hebutane, benzene, toluene, Tausa A, Tausa AB, DCzoo,
DC209, baraculoethylene. Sulfurized.

Monsanto CP-S, Pyridine, Monsanto 7) CP-34
, lithium, sodium, potassium, cesium, mercury,
Lead, indium, tin, etc. are used in fluid or gas form.

According to the research of the present invention, the method of the present invention in which heat is generated from the partition member defining the l1llI of the spinneret can be applied to the side opposite to the discharge surface of the mesh-like part of the mesh-like spinneret having the above-mentioned large number of slits. Nearby 1. While supplying Joule heat from the messier-like partition member so that the temperature of the fiber-forming polymer reaches the maximum temperature, and cooling by supplying cooling a1m between and in the vicinity of the discharge of the spinneret,
It has been found that extruding the melt of the wrinkle-forming polymer through a wrinkle spinneret is more advantageously carried out.

No. 111 of the attached drawings shows, as will be detailed in later Examples, when po-v-tetra-1-ethylene is spun by the method of the present invention using a mesh-like spinneret, the flow rate between the discharge and the opposite direction of the mesh-like spinneret is shown. This diagram illustrates what kind of temperature change a single polymer powder exhibits until the side IIIC polymer powder turns out to be incorrect. mw indicating temperature change is shown.

In the ms diagram, the vertical axis (y) is the distance 1111 (m ) that travels from the discharge surface into the melt in the direction of the surface opposite to the discharge surface, with the discharge surface of the spinneret being zero.

In FIG. 5, the distance is in the opposite direction to the direction in which the polymer advances, so it is marked with a minus number 1), and the horizontal axis is the temperature (T'C) of the polymer.

In addition, the hatched portion in FIG. 1 indicates the substantial thickness of the mesh-like spinneret.

FIG. 5 shows that the polymer, which did not show a large temperature change up to a distance of about 10 cm from the discharge surface, then increased in temperature as it moved closer to the opposite surface between the discharges of the spinneret; The figure shows that the temperature rises rapidly near the surface, and the temperature is maximum on the opposite surface (the surface of the partition member). The polymer leaves the discharge surface.

Thereafter, it is rapidly cooled by the cooling fluid supplied to or near the discharge surface, as described in detail, resulting in a rapid temperature drop and fibrous fine I/LK conversion.

The width in ms of the mesh-like spinneret depends on its material and the heat transfer efficiency between the polymers, but is preferably! l Oj
~N■spreferably 1110 j-1 simple lll1!
It is l. It is difficult for a high viscosity polymer to pass through a narrow slit between islands (a slit that is too wide is undesirable because it causes insufficient heating of the polymer and uneven heating).

The polymer can be used within the above-mentioned period of time without losing the molded article forming part.
It is necessary to pass through the narrow I1 group of the mesh-like spinneret. If the time for passing through the a + * sp is too long, the molded part will be lost, and if it is too short, the polymer cannot be heated to the appropriate temperature, so there is an optimal passing time @-.
The range S depends on the composition of the wrinkled polymer and the temperature, thickness, etc. of the wrinkled mesh spinneret, so it cannot be specified exactly, but the corrugated polymer is polytetra-ethylene, and the wrinkled mesh-like spinneret. 11140411 is 4 of 30 meshes
If it is a P wire mesh and the temperature when air-fired is see°C, the temperature is am seconds to II seconds.

An apparatus for producing a fiber aggregate according to the method K11 of the present invention will be explained using FIGS. 1 and 2.

In order to simplify aq, other devices that do not significantly impact the manufacturing plant or devices known to those skilled in the art have been omitted.

FIG. 1 is a schematic cross-sectional view of a plunger extruder for producing fiber aggregates according to the method of the present invention. A solid polymer 3 in the form of a powder or a lump is put into a barrel 1 equipped with a preheating heater 5, and is preheated at a temperature below which the mesh pattern does not melt. The spinneret 6 is supplied with a shaped spinneret. The cap is Squimec 9. [Low voltage and large current electricity is passed through the transformer. In addition, the base is touched by copper [7,! The base 6 and the barrel l are insulated with an inorganic adhesive to reduce the voltage drop at the joint. The solid polymer supplied to the nozzle is melted by the heat from the partition member of the nozzle at a point between the hand and the 10th line of the nozzle, and is passed through the nozzle in a molten state until the maximum temperature is reached. Then, it is discharged from the crest mouthpiece. Then, it is cooled by the cooling air blown from the cooling air nozzle 10 and turned into a rivulet-like stream, which is then collected.

FIG. 3 is a schematic cross-sectional view of a Sufuso two-piece extruder for producing fine aggregates according to the method of the present invention. According to this device, a solid polymer powder is continuously transferred to a mesh-like spinneret 1 by a changing star knee 12 designed for powder transportation.
1. The device may be an upward-pointing syringe as shown in this figure, or it may be downward-facing.

According to the opinion, the spun fibers may be stretched or subjected to heating to increase the crystallization of the porcelain. Alternatively, use heat II & seed to advance the orientation of the fibers, and then increase the glass transition point of the Monoriyari (depending on the type of polymer! zO℃~:I・℃
A method of dry heat stretching at a temperature above (near), heat I & Ru to advance the orientation and crystallization of the pattern: above the glass transition point of the filament without stretching in a warm layer or above. In this case, methods such as stretching with dry heat, heat treatment, etc. are applied.

According to the present invention, a fiber aggregate consisting of a large number of fibers is obtained, but the fiber aggregate of the present invention has a constant cross-sectional shape, size, distribution, and fluctuation of the fiber cross-section along the fine axis direction. HK1h, this 5-sized fiber collector is the conventionally known 41! It is something that cannot be obtained from the manufacturing method of embroidery, and its structural characteristics as a collection are also unique. Various interesting things that could not be obtained from conventionally known products are revealed.

The cross-sectional shape, size, distribution thereof, and range of variation of the fiber cross-section along the fiber axis direction are partially similar to those of natural silk or wool, so the fiber collector of the present invention Texture, such a natural product! It can be said that it is possible to provide synthetic fibers with similar properties.

Hidden χ1 The fiber aggregate of the present invention can be used as a material for all types of textile products, including woven fabrics and knitted fabrics, as well as other nonwoven fabrics.

The 4111 fiber aggregate of the present invention exhibits a high degree of crimp due to heat escape in many cases due to moderate irregularities in the fiber cross section and outermost direction and an anisotropic cooling effect provided during fiber molding. This property can be applied to increase the degree of entanglement between fibers.

The fiber aggregate of the present invention can also be easily applied to the above-mentioned parallel array sheets, orthogonal nonwoven fabrics made by orthogonally bonding them, random structure nonwoven fabrics made random by applying electricity or air, etc. I can do it.

In addition, according to the opinion, polymers in which one molecular chain is rigid or ultra-high molecular weight polymers can be easily made into fibers.

Fiber aggregates with high strength and high Young's modulus can be obtained. 1. Loops with excellent mechanical properties, nonwoven structures (random nonwoven fabrics, orthogonal nonwoven fabrics, etc.), woven fabrics (stitch weave etc.), and the fiber collectors. It is possible to obtain short fibers (can be used for KM such as resin dispersion reinforcement) etc. by cutting.

Furthermore, according to the present invention, it is possible to obtain fibers with a thick texture, and these fibers are called tegus. Printing is also used effectively for materials such as Sotsunkrete reinforcing material and Netsipel F.

EXAMPLES The present invention will be explained below using specific examples, but these are not intended to limit the scope of the present invention.

Note that the intrinsic viscosity (1, V,) K is based on the following formula.

I, V, = jnlrel/as (However, Ir@l is the polymer al!, f/10011
4@ It is the value obtained by dividing the viscosity of a liquid in a capillary type viscosity needle by the viscosity of the solvent determined using the same viscosity needle. ) Example 1 Using the Yokai plunger set extruder shown in Fig. 1, Mitsui Flo 11
Teflon 1-J (melting point: 121°C) manufactured by Cal was made into fibers. The barrel inner diameter of this extruder is 10mm, and the length is 10mm.
The part that is not discharged from the mesh-like spinneret is sealed with an aluminum-based inorganic adhesive, and the part that is discharged is directly sealed.
@■ circular wire mesh (made of stainless steel - embroidery diameter a)
14 items, SO Metshu Hirasen! 2! 77g7? -J#) Powder! Ill! Pour #@l into a heated barrel, leave it for 5 minutes, then 1. Approximately 70k
7.0 Wa per unit area (1d) of discharged page of one nozzle by pressing the pattern combination with a plunger with a pressure of 1/-.
A current of tts is applied to the nozzle, which is heated with Joule heat, to melt and discharge.

Blowing cooling air from both sides of the cap in a direction parallel to the cap surface at a wind speed of aS嘗/sac,
It was cut off at a length of 117 m to obtain a fibrous material of the polymer having an average fineness of 110 d. The strength of the five randomly selected single fibers was (L!, F/d·, and the elongation was S%).

In addition, let's take a look at the temperature change in the barrel of the pattern combination! l1aK
show.

Example 2 Hydroquinone l in which the benzene ring was randomly substituted with an alkyl group was prepared using a Zutomi Tsumugi Sufu-san set extruder.
I, V in orthora C20 phenol exhibiting melting isotherm obtained by polymerizing Il/l/blephthal O part/paraoxybenzoic acid SO part.

is 7.0 and the fully aromatic polyester (does not show a clear melting point, but starts to flow at 65°C according to the Koka-style two-tester (30kllI:II load-1st-S■L)K). I did this. The screw diameter of this extruder is 20 mm, and the mesh-like spinneret has a shape as shown in Fig. 1 and an average hole diameter of αS to φ. , empty rate 4
te%) was used. The hole is drilled so that the discharge portion has a diameter of 1 s φ.

Powder of fully aromatic polyester is put into a hopper, preheated by xso'CK while being transferred by a screw, and supplied in a solid state to the nozzle through which a current is flowing at a current density of 4 l Watts /-, From the drawing of the cap, cooling air is melted at about S, passes through the cap, and is discharged from the cap surface in a direction parallel to the cap surface at S. Spray it and say it.■
/Made with 11 JII average fineness 106d・0 strength 1
0 l/da, elongation 3%, Young's modulus 400 I/d
・A fibrous material was obtained.

Example 3 Using the plunger type extruder shown in Figure 1, the average degree of polymerization tz
OO polyvinyl chloride (melting point: 16°C) was made into fibers. The barrel inner diameter of this extruder is 10cm, and the length is 1.
■As a mesh-like spinneret, the discharge part is 11
Wire mesh with a circle fi (manufactured by Gunns, wire diameter
o mesh (porosity: 60%) was used.

Heat the pattern-combined powder to 11°C and put it in a barrel about sy
After putting it in and leaving it for S minutes,? ! Push the polymer with a plunger at a pressure of 5ekI/d.

4LIsWat per unit area (1-) of the discharge surface of the mouthpiece
A current of t- is applied to the nozzle heated by Joule heat, melted and discharged, and the wind speed measured in the direction parallel to the nozzle surface at two points below the nozzle surface is 1 m/ A cooling air with a temperature of 100 mm was blown onto the product, and the material was wound up with a 100 mm diameter shoe to obtain a fibrous material with an average fineness of 100 mm. This is about s, tlOd
The strength and elongation measured using the ant body are αs, respectively.
g7a・Elongation was 50%.

Example 4 Using a plunger set extruder as shown in Figure 1, ultra-high molecular weight polyethylene (Hoechst Homtal@nGUR41m) was
) was made into fibers. The dimensions of the extruder are the same as in Example 1, and the extruder is a mesh-like spinneret, and the discharge part is a circle with a diameter of 1 m. 1. Chrome It on the wire mesh, M diameter 0
3 sheets, 40 mesh plain weave! 2! - cars (67%) were used.

Heat the pattern-combined powder to 130'C and place it in a barrel for about 50 minutes.
JF was added, and after being left for 20 minutes, the solid polymer was pushed with a plunger at a pressure of about 106 #/-, and a current of 17 Watts was passed per unit area (17) of the discharge surface of one nozzle, and the joule was Supplied to the nozzle heated with heat, discharged with a 1W spoon, and blown cooling air at a wind speed of 10 m/min in a direction parallel to the nozzle surface 5lIl below the nozzle surface to 100 m1. Winding with /■, average fineness! A fibrous material of 1 Isd. was obtained. Then add this to 11
The yarn was stretched 18 times in an air bath at 0° C. to obtain high-strength yarns with a 1-strength elongation of tail/de and 11%, respectively.

Practical example S Using a plunger set extruder as shown in Fig. 1 and using the same equipment as practical example 1, I, V, and Ll in orthocou-phenol were
Polyethylene terephthalate chips (chip shape: 2 mm x 4.L) with a moisture content of 142% were turned into fibers.The chips were put into a barrel heated to 34°C (1°C Km) and immediately heated with a plunger. Extrusion was started after ensuring a good seal so that water would not scatter due to evaporation).Plunger pressure was sOk# sea, and 1 nozzle was used.
Neat port/sf current passed/11 from the cap surface
The extrudate was evaporated to 1 ml in the direction parallel to the mouth surface @ WC under 111 ml, and the extrudate was taken out at 60 ml/ml while cooling. Average single-system fineness 1 strength of the obtained fibrous material.

The elongation is tL L 5 d@/ L T 77/
do/110%. In addition, the fibrous materials I and V
, is 1.0! Yes.

The decrease in I and V is small, which is surprising considering that the moisture content of the original chip is as high as 0.s%.

Table A BA simple drawing Figure 1 is a diagram schematically showing a cross section of a plunger set extruder for carrying out the present invention. What is the name of each number?

l...Barrel, 2...Plunger, S...Solid polymer, 4...
・Base holding plate, S-... Preheating heater.

......Mesh-like spinneret, 7...
・Copper plate, t...-transformer, 9...
Slider, 10... It is a cooling air nozzle.

FIG. 8 is a diagram schematically showing a cross section of a screw extruder for carrying out the present invention. What is the name of each number?

11---Dice, 12...Screw for transporting powder.

1s... Preheating heater, 14...
...Powdered polymer.

1%...-mesh-like spinneret, 1@-tortoise, b
...--capture stopper, 11---wire cone assembly,
1B---Q cooling air nozzle.

19・Axis...p-ra It is.

Figures IIIE3-a and b are a top view and a sectional view of a plain-woven wire mesh used in the present invention.

Figures 4-a and 4-b are a top view and a cross section NWj of a mesh-like cap made by the font etching method used in the present invention.

The second figure shows the temperature relative to the distance from the mouth surface of the combined pattern when polytetrafluoroethylene is made into fibers by the method of the present invention.

'A twice 12 Dimension α diagram Dimensions - L times

Claims (1)

[Claims] A method for producing a fine aggregate by extruding a finely forming polymer through a spinneret having a large number of JIIlml, comprising:
9 expressed by the following formula % formula %! Knee rate is about 10% or more! Using a mesh-like spinneret having a number of closely spaced spinnerets, a WKIi experiential mold on the opposite side of the discharge surface of the spinneret is supplied, and heat is released from the partition member of the mesh-like spinneret. While supplying the liquid, the polymer in the form of a solid powder is melted and the molten liquid is extruded from a large number of IaIlI surrounded by the partition member, and at this time, the molten liquid discharge surface of the spinneret and its By supplying a cooling fluid to the vicinity and taking over the melt extruded through the all while cooling, the axillary melt is collected in large quantities within a time period in which the melted polymer does not substantially lose the molded article forming rod. A method characterized in that it is converted into a separated fibrous stream and solidified.