DE1669505A1 - Process for the production of fibers from, in particular, high-melting polymers - Google Patents

Description

. AMTHOH

. WOLF

D β I ¹ BANKFUBT AM MAHi

Note: Hederlandse Organization voor η-β ϊηανκγιγβτα.μ.,

Toegepast-Iiatuurwetenschappelijk ^ UHJT » ^} " * ^ IQ 3 Onderzoek ten behoeve van !! IZiZIJL. Im «Nijverheid, Handel en Verkeer 8847 / I

Juliana von Stolberglaan 18

The Hague / Holland

Process for dividing fibers from, in particular, high-melting polymers.

The invention relates to a method of making fibers or other shaped articles from heat sensitive Polymers. Another object of the invention is a method of making fibers with a high filler content.

Under heat-sensitive polymers within the meaning of the present According to the invention, linear or branched, but not crosslinked polymers are to be understood, that is, not after the melt spinning process can be formed into fibers since they will undergo substantial discoloration or disintegration even before melting when they are exposed to higher temperatures. Such polymers can however, by means of suitable low molecular weight compounds which the polymers are plasticized or dissolved in this way, defl they can be processed at temperatures below their decomposition temperature, formed into fibers *

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BATH ORIGINAL

Thermosensitive polymers according to this definition can be: Polymers such as polyvinyl alcohol or polyacrylonitrile, which are essentially pure polymers never from the melt They can also be spun but also polyethylene or polypropylenes of such high molecular weight 'Be that these can be spun from the molten salt without any substantial decomposition.

Such heat-sensitive polymers can after a series known methods in which solvents are used to lower the softening point of the polymer, be formed into cords. However, each of these methods has various disadvantages that the method according to the invention has does not own.

Thus, when hate-spinning process, the polymers in a suitable Lösungemittel in a concentration range of 5 - 2596 dissolved and the solution is extruded into a suitable non-solvent coagulation bath by means of spinning nozzles, such that the polymer precipitates in the form of fibers. Since such a process is essentially based on the interdiffusion of liquids »the speed of fiber production after the wet spinning process is low (50 to 100 m / min)» compared to the spinning speeds that can be achieved during melt spinning of thermostable polymers (1000 m / min and more).

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BATH ORIGINAL

The dry spinning process (also known as solution evaporation spinning called) uses polymer solutions in the concentration range roughly between $ 20 and $ 35 and the solution will be perpendicular in extruded a hot duct, with the largest part

z '

of the solvent evaporated before winding the fibers will.

This method has the disadvantage that it requires costly solvent recovery equipment attached to the spinning shaft requires. The higher the boiling point and the heat of evaporation of the solvent, the longer or hotter the must Be spinning chute. This means serious disadvantages with regard to the cost and quality of the fiber product. This problem becomes particularly serious when dry spinning Polyacrylonitrile, where relatively expensive high-boiling solvents are used and also have to be recovered. The spinning speeds that can be achieved using this process are approximately between 300 and 500 m / min.

In the gel spinning process, polymer concentrations between 40 and "ö5 ^c / ° are used. The polymer gel is essentially spun in facilities similar to those used in melt spinning processes. The polymer gel is melted, through spinnerets extruded and wound up, still containing solvent. With a polymer content. · Above 45? ό, the extruded loads are usually dry enough to

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so that they do not stick together when they lie against one another on the spool. According to this process, spinning speeds exceeding 500 m / min can be achieved. One the great difficulty with this process lies in the production of the required highly concentrated and homogeneous gels. This must be done through common weddings and The polymer and the solvent are kneaded at temperatures close to the decomposition temperature of the polymer and yet molecular dispersion of the polymer in the solvent cannot be entirely achieved. The remaining, not separated, lumps of molecules have an unfavorable influence on the spinning process and the Quality of the end product produced.

Finally, it is already known to dissolve or swell polymers in high concentrations, above $ 33, in water let to spin the polymer solutions thus obtained and then evaporate the water from the spun polymer threads · Such a process is for example in the German Auslegeschrift 1 172 398 described. As in this process the evaporation of the water from the spun Threads must be carried out before they are wound, so they are also not high winding speeds achievable.

According to the invention, these disadvantages are now avoided. The invention is a process for the production of Fibers made from, in particular, high-melting polymers such as polyvinyl alcohol, polyacrylonitrile, copolymers of acrylonitrile with more than $ 85 acrylonitrile as well as polyolefins with a molecular weight of over 750,000 by spinning the melt mixed with a solvent into a neutral one

009833/1819

Medium which has a temperature below the melting point the melt, which consists in that as a solvent or plasticizer of the polymer in question low molecular weight compounds with the exception of pure water or mixtures of low molecular weight compounds which dissolve the polymer at a temperature below its decomposition temperature, the polymer however, insoluble in the compound or at least one component of the mixture at a lower temperature or is only partially soluble, and the mixture of polymer em and low molecular weight compounds or mixtures with a polymer concentration between $ 2.5 and $ 33 a spinneret is immediately pressed into non-preheated air, in which air the fiber formation takes place, after which the fiber is taken up directly on spools or the like.

According to the method according to the invention, the polymer solutions are thus extruded through spinnerets, as in dry and gel spinning processes, u.zw. perpendicular in air so that fibers which can be wound on the bobbins without removing the spinning solvent. In this In this way, winding speeds that sometimes exceed 1000 m / min can be achieved. Hence is in spite of Due to the relatively low polymer concentration in the solutions, there is no coagulation bath or solvent evaporation unit Required between the spinneret and the first transport roller or take-up reel.

The spinning shaft can be kept as short as in the gel spinning process and only has to be long enough so that the spun threads can give off a sufficient amount of heat to the environment . The inventive method

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\ BATH

is based on the correct choice of the nature of the solvent in relation to the specific polymers to be deformed.

In one embodiment, the invention is a single low molecular weight compound or mixture low molecular weight compounds are used as process auxiliaries for the polymer. This must be selected so that it the polymer only dissolves at an elevated temperature, but this temperature must be below the decomposition temperature of the Polymers lie. At another lower temperature, for example room temperature, the low molecular weight Compound or a mixture of such compounds may be a Uichtlöser for the polymer.

If a hot polymer solution of the correct concentration is obtained using a solvent of this type from a The spinneret is extruded vertically downwards into the cold air, the thin falling streams suffer as it cools phase separation into a polymer phase and a "solvent" phase. The polymer phase then forms one continuous fiber matrix in which the low molecular weight compound or compounds are excluded or along the Surface can be carried along. In such a way the polymer becomes simply by removing the heat from its solution Coagulated and concentrated in a fading phase.

009833/1819

BATH ORIGINAL

The fibers formed in this way at a distance of about 30-150 cm behind the spinneret can be used without the risk of breakage with a winding speed of several 100 m / min. This winding speed can be hundreds or thousands of times greater than the linear velocity of the polymer solution in the spinneret bores.

The low molecular weight compound or mixture of low molecular weight Compounds can themselves be a solid or a liquid at room temperature.

In a further embodiment of the invention, a mixture of low molecular weight compounds is used. the Components of the low molecular weight mixture should only be completely miscible at an elevated temperature. These However, the temperature must be below the decomposition temperature of the polymer. The components should also be included in the The proportions used must be immiscible or only partially miscible at lower temperatures, e.g. room temperature. The completely miscible mixture of the low molecular weight compounds should be below its decomposition temperature be a solvent for the polymer. The presence of the polymer in this system as a further component is said to be the Do not significantly increase the miscibility of the low molecular weight components at a lower temperature.

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When a hot polymer solution (in the correct concentration determined by experiments and appropriate repetitions) unter.Use a solvent mixture of this kind vertically downwards from a spinneret into cold air is extruded, the thin polymer streams experience a separation into two or more phases of different composition with regard to the low molecular weight compounds involved. In this separation, practically all of the polymer is concentrated in the phase that is necessary for the polymer is the better solvent, giving a continuous gel-like product.

The low molecular weight components of the polymer-poor phases can either remain dispersed in the fiber or for a long time the surface and can either be carried out at Represent room temperature liquid or solid polymers. The fibers formed in this way can be at a certain distance from the spinneret without the risk of breakage at several 100 m / min.

When the concentration of the polymer in the fiber gel phase exceeds $ 45, the fibers can be allowed to stick together without sticking be wound on the guide roller or spool when they meet. At a slightly lower concentration of the polymers in the gel phase can per se, known textile auxiliaries can be used to prevent the fibers from sticking together *

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'BAD ORIGINAL

"The lasers still carrying spinning solvent can be freed from them by a subsequent washing process can be done either on the bobbins or by guiding over washing reels.

Careful selection of the composition of the washing liquid enables the final fine fiber structure to be influenced. For example, you can use a washing liquid Select so that they have a porous fiber structure after removal the spinning solvent leaves behind, or the selection can be made so that after the spinning solvent has been removed the washing liquid plasticizes the lasers sufficiently to cause shrinkage. Many intermediate fiber structures can also be achieved.

The pasers can then as with conventional spinning processes and completed in the usual way.

The optimal polymer concentration to be used for the inventive The process must be determined through trials and repetitions; it depends essentially on three parameters Reaction between polymers and solvents, of molecular weight dt * polymers and the spinning temperature.

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_BATH

- ίο -

. The better a solvent is for a particular polymer, the higher the concentration with regard to one optimal spinnability. The higher the molecular weight, the lower the concentration for optimal spinnability. The temperature changes in these procedures are usually upwards by the decomposition temperature of the polymer or the boiling points of the solvents and after below by the phase separation or gelation temperature the spinning solutions limited.

Virtually all spinning solutions that are based on the principles of Invention made do not lose their properties of continuous fiber formation if without a change In the polymer concentration, a certain amount of an inert filler is dispersed in the polymer solution. The maximum permissible amount of filler depends largely on the influence of the Filler on the fluidity of the spinning solution, but not on the absolute concentration of the polymer. When using of a very high molecular weight polymer in a poor solution, therefore, may have that required for spinnability Polymer concentration are kept low, so that when dispersing a filler in the spinning solution Weight ratio of filler to polymer, kept very high · Since the spinning solvent is later removed from the spun fiber, a fiber with a high Filler content can be obtained.

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BATH ORIGINAL

A further embodiment of the invention therefore provides a method for producing fibers or other shaped ones Objects that have a high percentage of pulp, often over Own 50 Gw. $ Of Paser

To explain the invention, a few examples are given below:

example 1

Polyvinyl alcohol having a polymerization degree of about 1800 was dissolved in caprolactam, the yf> of the known under the trade name Aerosol OS ^ liquefaction agent containing dissolved at 16O ⁰ C to form a solution having a polymer content $ 25. This solution was sprayed vertically downwards through a nozzle maintained at 165 ° C. with 6 holes each 1 mm in diameter in air at 6 cm / min. The threads were wound up at a speed of 600 m / min.

The fibers were then washed on the spool with methanol to remove the caprolactam and allowed to air dry. Thereafter, the parsers are were drawn in an air duct at 220 ⁰ C to 3 times their original length to a Paser having a tensile strength of 6.7 g / denier to obtain the at a breaking elongation of 5 # and a single thread of 1.68 .

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Example 2

Polyvinyl alcohol having a polymerization degree of about 1800 was dissolved in caprolactam at 143 ° C in a 20 $ aqueous solution and cm through a spinneret having 6 holes of each 0.2 mm in diameter at 170 ⁰ C in air through a spinneret having 2.5 / min extruded. The fibers were wound up at a speed of 1000 m / min.

Example 5

Polyvinyl alcohol of the above type was dissolved in a 22 $ aqueous solution at 160 ⁰ C in benzenesulfonamide and through a spinneret having an orifice of 0.3 mm diameter with 0.5 emv min extruded. In air. The formed JPaden was wound up at 1000 m / min.

Example 4

Polyvinyl alcohol, as above was dissolved in trimethylolpropane to form a # 22 solution, the solution is heated to 190 ⁰ C and at a rate of 1.5 ml / min through a spinning hole of 0.6 mm diameter in air and at a rate wound at 1000 m / min.

Example 5 .

• Polyvinyl alcohol of the type mentioned above was mixed in from sulfuric urea and water in the ratio of

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BATH ORIGINAL

56 ι 44 (weight percent) solved. The 21% solution obtained was ^{extruded in air at 95 °} C. at 4.5 cm / min through a spinneret with 6 bores, each 0.2 mm in diameter. The nozzle was held at 115 ° 0. The fibers were wound onto spools at 400 m / min and then washed on these with methanol in order to remove the spinning solution. Air drying then took place. In a hot-air channel of 22O ⁰ C the Päden were then stretched to four times its original length to Päden having a tensile strength of 5.16 g / in to obtain the elongation at break of 3.8 $, wherein the single filament denier 0.8 degrees Has.

Example 6

Polyvinyl alcohol as above was dissolved in a mixture of 77 parts urea, 21 parts water and 2 parts of the liquefying agent known under the trade name Aerosol MA from the American Oyanamid Comp to form a 23 # solution which was heated under pressure of 2 atm and at 115 ° 0 was held. This solution was extruded at 4.5 cm / min through a spinning nozzle with 6 holes of each 0.2 mm in diameter in air · This die was maintained at 140 ⁰ O. The fibers were wound up in 150 cm distance from the nozzle at a speed of 250 m / min and washed with methanol on the bobbin, stretched and dried to 6.3 times at 230 ⁰ C. According to this, the fibers had a tensile strength of 8.4 g / denier, with an elongation at break of 4.3% for one

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-H- single thread denier of 1.36.

Example 7

• Polyvinyl alcohol dissolved as above in a mixture of 77 parts of urea, 21.5 parts of water and 1.5 parts of Aerosol MA gave a solution with a polymer concentration of 237 ». The solution was at 2 aiäf at 110 ⁰ C and held extruded at a rate of 18.6 ml / min through a spinneret having 15 holes of 0.2 mm diameter in air. The spinneret was kept at HO ⁰ O. The fibers were taken up 150 cm behind the spinneret at a speed of 1200 m / min. They were washed on the bobbins with methanol to remove the spinning solution and air dried. Then, they were stretched in hot air at 23O ⁰ C to 3 times their length. The fibers had a tensile strength of 4.6 g / den with an elongation at break of 4.6 $ with a single thread denier of 1.08.

Example 8

Polyvinyl alcohol of the type mentioned above was dissolved in a mixture of 6 »4 dimethyl sulfoxide and pentaerithritol. 1.5 $ Aerol MA was added to the solution. In this solution the polymer concentration was 26 _f 5 #. It was held at 15O ⁰ C and held 4.5 onr / ^min speed by means of a spinneret having 6 holes of each 0.6 mm in diameter, and 16O ⁰ O, extruded into air · The threads were 150 cm behind

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'■■■' ■ * ■ "' .: ·:;: BAD ORIGINAL

the nozzle wound at a speed of 500 m / min and washed on the bobbins to remove the spinning solution with alcohol and then air-dried. In a hot air duct 220 ⁰ C, the filaments were veretreckt to the 3 '25 times its original length, said chamfers having a tensile strength of 5 "32 g / d and a. Elongation at break of 4 »4 $ resulted.

Example 9

Polyvinyl alcohol of the type mentioned above was mixed in a mixture of dimethyl sulfide and pentaerythritol in a ratio of 6: 4 with the addition of 0.3 percent by weight boric acid. The polymer concentration in the solution mixture was $ 21.5. The mixture was held at 15O ⁰ G and extruded into air of 150 ⁰ O at a rate of 4 »5 cm / min through a nozzle with 6 holes of each 0.6 mm in diameter.

The fibers were wound up at 80 m / min. The dimethyl sulfoxide was extracted on the coil for one hour with acetone, then was air-drying and heat drying at 130 ⁰ O for one hour. This was followed by washing with cold water and drying on drying reels. Hot stretching to 7 »7 times its original length gave cases with a tensile strength '

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BATH

- 16 of 9.7 g / den and an elongation at break of 3.85ε.

Example 10

Polyvinyl alcohol as above was dissolved in a mixture of dimethyl sulfoxide (6 parts) and pentaerythritol (4 parts) to which 0.4 percent by weight boric acid was added. The polymer concentration in the mixture 19 $ · The mixture was held at 15O ⁰ C and treated with 6 cm / min in air through a spinning nozzle of 6 mm hole with a diameter of 0.6 extruded "The DüBentemperatur was az.f 140 0 maintained. The threads were wound up 150 cm behind the nozzle at 120 m / min. The filaments were treated with acetone, dried and placed on the bobbins in an oven at 150 ° C for two hours. After a cold water wash, the bobbins were again placed in acetone. The fibers were drawn off directly from the bobbins and immediately drawn at 220 ° C., resulting in a tensile strength of 10.4 g / denier and an elongation at break of 3.6 $.

Example 11

A high molecular weight polyvinyl chloride with a K value of 65 + 2, known under the trade name Solvic 239 the Solvic company, Paris, was in a mixture of 81 parts of caprolactam, 18 parts of cyclohexane and 1 part of di-N-Ootyltin stabilizer, known under the trade name Advan-

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ORIGINAL INSPECTED

stab 17 M from the German "Advance Produktions GmbH" ^{dissolved 11} ·, the solution having a polymer concentration of $ 26. The solution was kept at 110 ⁰ O and at this temperature at a speed of 1.5 cm / min through a nozzle with 6 extruded hole, and 0.2 mm in diameter. the fibers were / wound up at 270 m min 150 cm behind the nozzle, washed on the coil with methanol and then dried _o this was followed by a stretching at 110 ⁰ O to 4 times its length, very white fibers were obtained with a tensile strength of 3.3 g / ^{denier, with an elongation at break of 7 | 2 c} / o and a single fiber denier of 0.59.

Example 12

Polyvinyl chloride as in Example 11 was dissolved in a mixture of 86 parts of caprolactam, 12 parts of cyclohexanone and 2 parts of Advanstab 17 M to give a 3Q polymer solution. The solution was kept at 110 ^° C. and extruded into air at 3 cm / min. The spinneret had 15 held hole of 0.2 mm diameter and was at 115 ⁰ C.

150 cm behind the nozzle, the threads were wound up at 250 m / min and washed on the bobbins first with water and then with methanol. After drying, hot stretching was carried out in an air shaft at 115 ^° C. to five times its length. The fiber bundle had a tensile strength of 3.5 g / den at an elongation at break of 12.5 and a denier of 0.5 for one of the individual fibers.

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\ ORIGINAL INSPECTED

Example 13

A fibrous polyacrylonitrile, known under the trade name Nyma-B (a product from UV Nyma Kunstseidenspinnerei, Nijmegen) was dissolved in a mixture of 68 parts of DMP, 30 parts of urea and 2 parts of dimethylaminopropionitrile. The solution has thereby a polymer concentration of 24 Io at 125 ⁰ C with 9 CMVmin was extruded solution in the air. The nozzle, with 15 holes, each 0.2 mm in diameter, was kept at 155.degree.

150 cm behind the nozzle, the threads were wound up at 100 m / min and washed on the bobbins with methanol and then air-dried. At 136 ⁰ O a Heißreckung took place on 7.6 times its original length. The fiber bundle had a tensile strength of 4 g / den., An elongation at break of 7f3 #, and each individual fiber had a denier of 0.97.

Example 14

A polyacrylonitrile as in Example 13 was in a mixture of 79 parts of dimethyl sulfoxide, 19 »5 parts of urea and 1.5 Parts of polyethylene glycol (DP 200) dissolved to a solution with a 24 | 5% polymer concentration. This solution was developed 105 ° 0 and also spun at this temperature, at a speed of 9 cm / min through a spinneret extruded with 15 holes of 0.2 mm diameter each, 150 cm

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'behind the nozzle, the lasers were wound up at .160 m / min «. The fibers were washed on reels in benzene, butanol and water at 5 times their original "length" bei.140 ⁰ C stretched and relaxed at 17O ⁰ O. The fibers had a tensile strength of 2.7 g / denier and an elongation at break of 15 »9 $ ·

Example 15

A polyacrylonitrile as in Example 13 was dissolved in a mixture of 85 parts of dimethyl sulfoxide, 14 parts of MgClp 6 HpO and 1 part of polyethylene glycol (DP 200). The polymer concentration of this solution was $ 24.5. The solution was maintained at 105 ° C and extruded at a spinneret temperature of 100 ⁰ C in air with 6 cm / min from a nozzle with 15 holes of 0.2 mm diameter.

The threads were wound up 150 cm behind the nozzle at 600 m / min and washed successively in butanol and benzene. At 80 ^° C., the fibers were drawn 1.6 times their length, a tensile strength of 2 g / denier, an elongation at break of 26 μm and a single fiber denier of 1.67 being achieved.

Example 16 · ·,

A polypropylene sample with an original viscosity of (n) * 6 (resulting from the formula (n) = 1.1 χ 10- ⁴ M ⁰ * ⁷⁸ ) was set up so that an average molecular

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ORIGINAL INSPECTED

weight of over 1 million, and in naphthalene to one 11.5% solution dissolved at 165 ° C. This solution was made with 1 cm / min through a spinneret with a hole 0.6 mm in diameter while the nozzle was kept at 165 ° C. The thread was wound up at a winding speed of 1000 m / min.

Example 17

A polypropylene sample according to 16 was dissolved in naphthalene at 180 °, the solution having a polymer concentration of 11.5 $. This solution was extruded at 3> 6 cm / min through a ^{nozzle maintained at 170 °} C. and having 20 holes 0.2 mm in diameter.

The threads were wound onto bobbins at 250 m / min and washed on this in petroleum ether to remove the spinning solution.

Example 18

A polypropylene sample according to Example 16 was dissolved in p-dichlorobenzene at 130 ⁰ C to a 13 $ aqueous solution and extruded at 0.5 cm / min through a maintained at 130 ⁰ C nozzle. This nozzle had only one opening with a diameter of 2 mm. The fiber was wound up at 1500 m / min.

Example 19 A polypropylene sample according to Fig. 16 was in a 1il solution

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ORIGINAL INSPECTED

16695Θ5

dissolved in a solution with 17 $ of polymer concentration Uaphthalen and paraffin wax (melting point 7O ⁰ C) at 175 ⁰ C and extruded with 9 cm ^ / min by a maintained at 175 ⁰ O nozzle. The nozzle had 6 holes, each 0.8 mm in diameter. The fibers were wound onto bobbins at 400 m / min, washed in petroleum ether and then dried. At 125 ° 0, the fibers were stretched to 9 times their length. The tensile strength was 7 g / denier, the elongation at break of 17 $ Binzelfaserdenier 0.72.

Example 20

A polypropylene sample according to Example 16 was dissolved in a mixture of 88 parts of para-dichlorobenzene, 10 parts of paraffin wax and 2 parts of Aerosol MA to form a 16 # strength polymer solution at 170 ⁰ O and the solution was passed through at a spinning speed of 9 em / min extruded a spinneret held at 17O ⁰ O with 6 holes each with a 0.6 mm Durohmesser. The threads were taken up on bobbins at 200 m / min 150 cm below the nozzle and washed in petroleum ether to remove the spinning solution on the bobbins, dried and then scattered in a Y / arm air duct at 125 ° 0 to 8 times their original length. The pads then had a tensile strength of 7.4 g / den with an elongation at break of 20 $ and a single fiber denier of 2.14.

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0098 3 3/1819 _0RIG , _NAL , nspecIed

- 22. , Example 21

A Polyäthylenprobe (known under the trade name Polyethylene AC-X, as a product of the company. Allied Chemical Company, USA) whose specified by the manufacturer molecular weight 1-3 million, is, was stirred at 18O ⁰ C in naphthalene, to a solution with a 3 # strength polymer content, the solution at 0.5 cm / min spinning speed by means of a held at 18O ⁰ C spinneret with a 0.6 mm opening-extruded. The fiber was wound up at a winding speed of 800 m / min.

Example 22

A Polyäthylenprobe according to Example 21 was dissolved in a 3: 1 mixture of naphthalene and sulfur at ·· 150 ⁰ C in a solution having a polymer content of 2.75 #> and transferred to a spin speed of 2 cm / min through a spinneret having a 0.6 mm opening. The nozzle was ^{kept at 170 0} G and the thread was wound up at a winding speed of 200 m / min. After removing the naphthalenes by washing with petroleum ether, the fiber had a sulfur content of 90 percent by weight.

Example 23

Three parts of the polyethylene according to Example 21 were dissolved at 15O ⁰ O * in 97 ropes of naphthalene, the 5.5 parts of carbon black.

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009833/1819

ORlGiNAL INSPECTED

were greed. This solution was spinning through a nozzle maintained at 158 0 at a spinning speed of 2.5 cm / min spun out, which had an opening with a diameter of 2 mm. The paser was wound at a winding speed of 200 m / min wound. After the naphthalene was removed with petroleum ether, the paser had a carbon filler content from $ 64 to, they v / ar electrically conductive.

Example 24

Polyvinyl alcohol according to Example 1 was dissolved in a 6: solved 4 mixture of dimethyl-Sulfftxyd and pentaerythritol at 150 ⁰ C to a 26.5 / o polymer solution and in the solution to an ion exchange resin, known under the name Dowex 50 Dow Chemical Co., with a particle size between 200 and 400 mesh dispersed. The weight of this ion exchanger was 289έ of the polymer. The solution was spun at 5.1 cm / min through a spinneret maintained at 15O ⁰ C with 6 holes of each 0.8 mm in diameter. The resulting fibers were washed on spools in a sodium sulfate solution and then air dried. Subsequently, a heat treatment was performed on the coils at 13O ⁰ C for one hour in an oven. The adhering sodium sulfate was then washed off with pure water and the fibers were dried again. At 18O ⁰ C then the parsers are were brought to twice their length. The stored ion exchanger made up $ 28 of the paser weight. '

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ORIGINAL INSPECTED

Claims (7)

Claims 1. A process for the production of fibers from, in particular, high-melting polymers such as polyvinyl alcohol, polyacrylonitrile, copolymers of acrylonitrile with more than 85% acrylonitrile and polyolefins with a molecular weight of over 750,000 by spinning the melt mixed with a solvent in a neutral medium which has a temperature below the melting point of the melt, characterized in that low molecular weight compounds with the exception of pure water or mixtures of low molecular weight compounds are used as solvents or plasticizers of the polymer in question, which dissolve the polymer at a temperature below its decomposition temperature, but the polymer at a lower temperature in the compound or at least one component of the mixture is insoluble or only partially soluble and the mixture of polymers and low molecular weight compounds or mixtures with a polymer concentration between 2.5 u nd 33% is immediately pressed through a spinneret into non-preheated air, the fiber formation taking place in this air, after which the Paser or the like directly on bobbins. is recorded. New documents ww. 7 51 w ». a no. ι Sou s * »*» change «, v. 4.9.:. ■; 009833/1819 BATH ORIGfNAl. 2. The method according to claim 1, characterized that the fiber-forming material is mixed with solid fillers in an amount that is 10% of the fiber weight exceeds. 3. The method according to claim 1 and / or 2, characterized that the fibers are wound up at a bobbin speed of over 50 m / min. 4. The method according to one or more of claims 1-3, characterized in that solutions with a polymer concentration between 2.5 to 33% are used and the fibers produced are wound up with solvents preferably still contained therein. 5. The method according to one or more of claims 1-3, characterized in that a solution of polyvinyl alcohol with a polymer concentration of 5-30X is used. 6. The method according to claim 1, characterized in that one uses polyacrylonitrile or a copolymer of acrylonitrile which is at least 85% Acrylonitrile contains a polymer solution with a concentration between 5-30%. . ./3 009833/1819 BATH ORIGINAL 7. The method according to one or more of claims 1-3, characterized in that one Polyolefins with a molecular weight of over 750,000 are used. 009833/1819 ^SAD