DE2101823C3 - Process for the production of a fiber or a filament from vinyl chloride polymer by a dispersion spinning process - Google Patents

Description

2 10i 823

and for contact pages of even 5 minutes, the tearing NaUi of a process variant for the introduction of the

long the resulting fibers or threads even after Koalesziermitiels in the spun structure that will

Stretching generally in the range from 0.2 to 0.6 g / the web through a medium with or from the Koaies-

and the value for ornaments led. The coalescing agent can e.g. B,

5 be present in a bath through which the web

Length at break x elongation at break ⁰ x ⁸ is performed. Optionally, the coalescing agent can be mixed with the coagulating agent, if

generally: m ranges from 1.5 to 4.5. Others - these are miscible with each other. If the introduction, on the other hand, shows the coalescing agent, which is heated according to the invention, through contact between the structures with the coalescing agent and improved intrinsic web and the coalescing agent in a bath, the degree of improvement from the degree that the coalescing agent is to be achieved, then the coalescence must take place of the polymer particles is dependent. The contact time in the bath must be long enough to allow for an out-So it has been possible to produce webs with a tear length in the range of absorption of the coalescing agent to the Er range of 2 to 4 g / den and a value for tear targeting a coalescence of the vinyl chloride polymer length · elongation at break ⁰ x ⁵ in the range of 12 to 15 15 particles to accommodate in the post-heating, virken. To achieve a high throughput of the web

In order to achieve the desired improvement in spinning, it can e.g. B. necessary

the spun structure with coalescing agent e.g. B. be, the web by a long bath with the com

be heated by passing the web through an alesziermittel. Should the coalescing agent be used in

Heating chamber is guided, the temperature of the ao mixing with the coagulant in a single

Chamber and the dwell time appropriately selected bath are available, the bath must be even longer

will. In the following, the process is based on hand and the coalescing agent is developed in high concentration.

a heating chamber described; hold of course.

however, other heating methods such as B. di- According to another variant of the method that can

electric heater, can be used. The web coalesces thereby into the spun structure

can e.g. B. be introduced during and / or after the passage that the web is in contact with

be stretched through the heating chamber. is brought to the steam of the coalescing agent.

To achieve coalescence of the vinyl chloride it was surprisingly found that the Koales: derpulymerisat particles necessary heating depends on average in the dispersion of vinyl chloride polymer, to a certain extent on the type of coalescing agent. 30 from which the web is to be spun is available In general, the coalescence of the can be increased, with the spinning of this dispersion to Coalescing agent with temperature. Is the Koales- introducing the coalescing shaker into the woven Means a solid at room temperature, so structure results. In this case you can go to the bathroom The spun structure will preferably dispense with one with coalescing agent altogether, thereby reducing cost-temperature heated, which arise at least above the 35 savings. However, it can be advantageous »a, The melting point of the coalescing agent is; will continue to use as the bath with coalescing agent, Coalescing agent ε-caprolactam is used, although it can be shorter than if no

ne temperature of more than 62 ° C preferred. There is coalescing agent contained in the spinning dispersion.

vurd generally preferred that the spun According to a further embodiment of the invention

Structure is heated to a temperature above 8O ⁰ C. 40 the inventive method is a dispersion of

Significant degradation of vinyl chloride polymer-vinyl chloride polymer in solution of at least

! utt particles can be avoided by spinning a matrix that also contains at least one

the temperature in the heating chamber to a value coalescing agent for the vinyl chloride polymer

c is set, which is below the temperature, holds.

where degradation takes place. However, it is possible 45 Since the coalescing agent is a solvent or swelling agent

to work at a temperature that is above and medium for the vinyl chloride polymer, it is above-

even far above the decomposition temperature for the surprising that even a small amount of the coalescence.

Vinyl chloride polymer is if the dwell time can be introduced into the spinning dispersion medium,

of the web in the heating chamber is so short that without agglomeration of the polymer particles

no undesired degradation of the particles of vinyl 50 follows and the spinning is prevented as a result,

chloride polymer takes place. It has been found that the coalescing agent can have a tendency to agglomerate

Kammertempcraturenjenach residence time of up to 250 ⁰ C, the polymer particles have meration. So there! ' the

and higher can be used. The concentration of the coalescing agent in the dispersion should also be

Dwell time not be so long that the web on preferably not be so high that such

a temperature above the melting point of the agglomeration of the polymer particles takes place and the

Matrix is heated. As a result, the web of dispersion is preferably not spun properly

heated to a temperature which can be at least 2O ⁰ C. If the coalescing agent is used in the

is below the melting point of the matrix. structure, however, only through its presence

In general it is introduced to determine the optimum in the spinning dispersion, so should the Kon-heating the concentration of the coalescing agent must be sufficiently high to achieve optimal properties, woven structure expediently, the web through to too. ensure the woven structure to run a heating chamber of a certain length contains enough coalescing agent to and to gradually increase the temperature, while heating the web lent a coalescence of the the speed of the web of unaltered polymer particles in the structure. the remains. The properties of the heating chamber are 65 Concentration of the coalescing agent in the dispersion letting product can be measured and so- has an upper limit that depends on the storage time of the with the temperature for optimal: physical and dispersion before spinning as well as from the spinning time mechanical properties set. is dependent. In general, the permissible concentration

Ration of the K, aalesziermUtels in the dispersion is higher, in order to avoid such «low-temperature polymerizations e shorter the storage time and the shorter the spinning time to obtain dispersions that are suitable for spinning into threads In general, the coalescing agent can be sufficiently stable and still have a high solids concentration from 4 to 25 percent by weight, based on the material, the polymerization is preferred the vinyl chloride polymer in the dispersion is present in the presence of a soluble salt of a suI be, fonsäurederivats of an alkylphenoxypolyether alcohol

Solvent or swelling agent for vinyl chloride poly carried out as a dispersion stabilizer. One such

merisat, which are suitable as coalescing agents, are derivative has the formula
z. B, N-methylpyreneUdon, tetrahydrofuran, cyclo-

hexanone, sulfolane, hexamethylphosphoric acid amide, io 9

Nitrobenzene, ethylene carbonate, propylene carbonate, '"

ε-caprolactam, 2,2'-dimethylvalerolactam, dimethyl- ^R - K / —O - (- CH, —CH ₃ -O -) "- S — OH—

acetamide and dimethylformamide. > - == ■ | i

The vinyl chloride polymer can be in any suitable O
th dispersion medium to be dispersed. From Wirt- 15 (I)
For critical reasons, however, it is particularly expedient if the vinyl chloride polymer is dispersed in an aqueous medium in which R eirae alkyl group has 5 to 20 carbon atoms, which means a particularly atoms and η an integer from 2 to 12, which is easy to represent. In the following, that in the laid-open specification 2,019,832 is described.
Invention based on dispersions of vinyl chloride 20 The particle size of the vinyl chloride polymer in an aqueous medium is described. Particles in the dispersion are subject to the requirement

Preferably the coalescing agent is soluble in that the dispersion is easily permeable. the spin dispersion medium used. However, if the coalescing agent does not flow, it must. The upper limit of the particle size insoluble or only partially soluble in the dispersion: - is expediently about 2 μ. Particles with a medium, so it can in general be in the form of an emulsion with a diameter of 0.05 to 0.2 μ, or a dispersion. In this case know a? stable dispersion, w easily be by the normal ^{advantageous:} hen the spin dispersion also can flow a spinneret. Such a range of partial emulsifier contains around the coalescing medium in fine size is also useful.,
to maintain a distributed state. The process is suitable for the production of a medium as a dispersant than in the aqueous 30 egg-filament as well as multi-filament webs.
Medium-soluble coalescing agents such as ε-caprolactarn. The concentration of the vinyl chloride polymer in dimethylacetamide and 2,2'-dimethylvalerolactam in the dispersion is as high as possible. The concentration of vinyl chloride polymer is preferably suitable

The dispersion of the vinyl chloride polymer can be at least 15 percent by weight, in particular 30 Gez. B. can be produced in that a finished, fine 35 percent by weight or more. One: upper limit is distributed. Vinyl chloride polymer in an aqueous sets by the need for maintenance Medium is dispersed. However, it is particularly a stable dispersion during spinning and by the Useful when a dispersion is made directly by poly- Demand that the viscosity of the mixture is below the merization of vinyl chloride in an aqueous me- shear conditions at the spinneret can not be so high dium is produced. It may be desirable that the mixture is no longer easy to handle The spinning dispersion phase is a dispersion phase.

medium to add to the stability of the dispersion. The matrices include polyvinyl alcohol and

raise. Of course, such a dispersant may be sodium alginate. A preferred matrix

used in the polymerization of vinyl chloride. consists of a mixture of polyvinyl alcohol and

45 sodium alginate, for example with dnsm content

be at hand. Sodium alginate from 2 to 35 percent by weight, based on

According to the method according to the invention, the polyvinyl alcohol. Oe matrix is inserted into the

Fibers and filaments with very useful properties dispersion preferably incorporated in that a

be obtained, w ^ nn the vinyl chloride polymer aqueous dispersion of polymer particles with a

It is mixed by polymerization of vinyl chloride in an aqueous 50 aqueous solution of the matrix

However, it is also possible, for example, to convert the matrix in an aqueous medium at a low temperature

wisely below O ⁰ C, preferably below -15 ° C, z. B. be ^: to dissolve dispersion of the polymer or the polymer part

about -20 ° C. With such a polychene to be dispersed in an aqueous solution of the matrix

merization it may be necessary to use an anti-freeze.

medium such as B. ethylene glycol or methanol in the aqueous 55 In the mixture, the concentration of the matrix is present in the medium in which the polymerization is carried out, preferably between 5 and 20 percent by weight, to use the freezing point of the medium on the vinyl chloride polymerizate. In particular, to reduce it. If such an antifreeze agent can be used in a concentration of 10 to 15% by weight, then its concentration should be used in the zcnt. The spun structure or aqueous medium before the addition of the coagulant, the web, is produced in that the dispertels are preferably reduced to less than 5 percent by volume, since they are spon into the water in a coagulant for the matrix, since otherwise there will be water , so that a fibrous or thread-like structure, undesired agglomeration of the vinyl chloride door from the coagulated matrix and into this polymer particles formed by the addition of the coalesced particles formed from vinyl chloride polymer, can take place. A suitable method 6 _; ; will.

to reduce the concentration of the freezer The coagulation agent is of course n.; ch of the type

Protective agent, just..K! i'.r.-h dialysis, is chosen in the open matrix. Used as a matrix polyvinyl alcohol

Lebiincsschrift 2 01 ¹ J ίο ¹ iH .'- chriebcn. and / or sodium alginate is used, so ha'ncti

ζ 2 ΙΟΙ 823

7 8

as a coagulant 7. T). Acetone and methanol and held. Di <: dispersion taken from the container. Solutions of metal salts such as calcium chloride contained less than 2 percent by volume of ethylencnglycol and in methanol has been tried and tested. If the coalescing medium had a polyvinyl chloride content of '35 G in the spin dispersion, then it is preferred percentages: intrinsic viscosity = 2.12 dl / g to use a coagulant for the matrix, 5 (measured in cyclohexanone at 25 C). which is at the same time a non-solvent for the coalescing agent. Then aqueous solutions of is added to the dispersion so that the polyvinyl alcohol and sodium alginate present in the precipitated matrix are slowly added to the coagulant while stirring, so that an emulsion of 12.8 G is dissolved. On the other hand, the coagulant can be percent by weight polyvinyl alcohol and 3.5 percent by weight solvent for the coalescing agent, so percent sodium alginate, based on the length of the polyvinyl; Web only for the time in contact with the ohlorid. originated.

Coagulant remains in a self-supporting structure. The mixture was passed through a spinneret with a

door arises, but not yet a single hole (diameter 100 μ) in a bath of acce-

desired quantity takes place at Koalesziennittel and so-ton with 30 volume percent dimethylacetamide at 2O ⁰ C

with insufficient coalescence of vinyl chloride 15 pressed. After going through the bathroom over

polymer particles at the subsequent heat - a distance of about 120 cm was the result:

mation is achieved. In order to reduce the loss of KoalcKziermittel Gespinst with a speed of about 5.6m / min

Keeping it small can be useful. d; is Ge taken from the bath and immediately thereafter through

spinst in contact with some coalescing agent, a tubular heating chamber with a length of

by z. B. up to about 5 percent by weight Koaleszier- ao 0.31 m and a temperature of 250 ° C. then

agent is introduced into the coagulant bath. the thread was stretched 3 times, over

It has been found that at a molecular weight of an electrically heated plate with a temperature

of the vinyl chloride polymer of the Polymertdlchcn at 100 ° C. The thread had the following properties

the webs coalesced according to the invention result from:
This corresponds to a basal molar viscosity of 3.0 dl / g 35

or larger the fibers or threads according to the Thermo-Demu ¹ 8.2

lix a low shrinkage in the dry tear length 2.0 g / den

warmth as well as a low shrinkage in the elongation at break 36 9 ° /

Dry cleaning solvents used, such as breaking length · elongation at break '' · » 120 '°

/ .. B. perchlorethylene and trichlorethylene. haoen. Before 30 ' Zugsweisc one uses a vinyl chloride polymer

with an intrinsic molar viscosity (as defined below). For comparison, an aqueous dispersion of

in the range 3.0 to 5.0 dl / g. Polyvinyl chloride by polymerizing vinyl chloride

For some purposes the invention genius is produced at -20 ° C, with a concentration of

produced fibers or threads, it can advantageously 35 ethylene glycol in the dispersion in the above-described

being. if the matrix is removed from the web, it has been reduced in some way. The dispersion that

by this z. B. is washed with an agent, 30 percent by weight polyvinyl chloride with a basic

which contained a solvent for the matrix and a molar viscosity of 2.8 dl / g for the vinyl was with

Chloride polymer is a non-release agent. aqueous solutions of polyvinyl alcohol and sodium

The invention is mixed in the following on the basis of Aus 4 «alginate, so that the dispersion obtained

examples of management explained in more detail. 10.4 percent by weight of polyvinyl alcohol and 2.3 percent by weight

Below the intrinsic molar viscosity, the value for weight percent sodium alginate, based on the polyvinyl chloride, should be contained. The mixture was through a

t -: _η spinneret with a single hole (diameter

~ t ^ c 45 100 μ) in a bath of acetone with 50 volume percent di-

methylacetamide pressed at 20 ° C. After passing through

when extrapolated to zero concentration, it is understood that the passage through the bath over a distance of about one inch

being, where / the flow time of a solution of the poly- the web was formed at a speed

mers at a concentration of »c« g / dl solvent of about 6.1 m / min taken from the bath and applied to the

tel means through a viscometer and I ₀ the liquid 50 air dried before it was wound up. the

time of the same volume of pure solvent thread was triple over an electrically charged

by the same viscometer at the same temperature heated plate at a temperature of 130 ° C

turized. stretches.

_. . _{,, ss} denier 12.5

Example 1 ³³ ".", _ "..,.

^v Tear length 0.45 g / den

Elongation at break 26 ° / ₀

An aqueous dispersion of Polyvmylcbnd was breaking length · elongation at break · - 2.3

by dispersion polymerization of vinyl chloride
-20 ⁰ C in a mixture of water and ethylene glycol

toi (volume ratio 50:50) in the presence of For further comparison and investigation of the: an emulsifier produced, the effect of longer contact times with a sodium salt of a sulfonic acid derivative of an alkyl coalescing agent being samples of the phenoxy polyether alcohol of structure I, in the n comparative experiment produced spun 5 minutes equal to 4 and R is a nonyl group, was used. 65 in several different coalescing mixturesep, · The dispersion was then immersed in a container from, removed and then transferred to the Lui ■. Clerated cellulose introduced. The container was dried. The threads had the following self-opened and sheathed under running water for 24 hours:

Coalescence means and temperature

Acetone / dimethylacetamide (50: 50 by volume) 60 "C acetone / tetrahydrofuran (50: 50 by volume) 60 ⁰ C .. acetone / cyclohexanone (50: 50 by volume) 60 ° C

13.0
13.0
13.0

Tear length

g / i! en

0.4

0.42

0.29

Elongation at break

"/O

110
70
40

Length at break · Elongation at break "' ⁶

4.2
3.5
1.8

Example 2

An aqueous dispersion containing 31 percent by weight of polyvinyl chloride with an intrinsic viscosity of 2.4 dl / g v / was produced, and the concentration of the ethylene glycol in the dispersion was reduced, namely by the method of Example 1. The dispersion was with an aqueous solution of sodium alginate mixed, so that a dispersion with 8.7 percent by weight sodium alginate, based on the polyvinyl chloride was created.

The mixture was forced through a spinneret with a single hole (diameter 100 μ) into a bath of methanol containing 0.5 percent by weight calcium chloride at 20 ° C. After passing through the bath over a distance of about 120 cm, the web obtained was guided via a guide into a bath made of dimethylacetamide at 20 ° C. After passing through this bath over a distance of about 91 cm, the web became at one speed taken from about 7.6 m / min the bath and immediately thereafter passed through an about 0.3 m-long heating chamber in the form of a tube having a temperature of 18O ⁰ C. When leaving the heating chamber, the thread was stretched four times in a steaming box.

The thread had the following properties:

Denier 6.0

Initial modulus 53.2 g / den

Tear length 2.3 g / den

Elongation at break ll.6 ° / ₀

Length at break x elongation at break ⁰ x ⁶ 7.8

Example 3

An aqueous dispersion containing 33 percent by weight polyvinyl chloride with an intrinsic molar viscosity ίο of 2.58 dl / g was prepared, and the concentration of ethylene glycol in the dispersion was reduced, specifically according to the method of Example 1. The dispersion was made with aqueous solutions of polyvinyl alcohol and sodium alginate mixed, so that a dispersion with 19.3 percent by weight of polyvinyl alcohol and 2.5 percent by weight of sodium alginate, based on the polyvinyl chloride, was formed.

The mixture was pressed through a spinneret with three holes (diameter 100 μ) into a bath of acetone with 30 percent by volume dimethylacetamide at 20 ° C. After passing through the bath over a distance of about 120 cm, the web formed was removed from the bath at a speed of about 15.2 m / min and immediately passed through an about 1.5 m long tubular heating chamber with temperatures of 13C ¹ C on Output passed up to 254 ⁰ C at the input. The web was removed from the heating chamber at a speed of about 15.2 m / min and stretched four times over an electrically heated plate at 110 ° C.

The thread had the following properties:

Derver 14.1

lnual modulus 61.0 g / den

Tear length 3.4 g / den

Elongation at break 17.2 ° / ₀

Length at break x elongation at break ⁰ x ⁵ 14.1

In order to investigate the effects of different heating chamber temperatures, the described method was used Procedure repeated in three separate experiments, with the difference that the one removed from the bath Webs were passed through heating chambers at different temperatures. The influence the heating chamber temperature on the properties

of the threads can be found in the following table.

attempt

Temperature gradient in the hek chamber, ⁰ C

denier

Initial module, g / den Tear length, g / den Elongation at break, ° / _1} Length at break · Elongation at break ⁰ · ⁵ Example 4

According to the procedure of Example 3, an aqueous dispersion of polyvinyl chloride, polyvinyl alcohol and sodium alginate was prepared and pressed through a spinneret with three holes (diameter ΙΟΟμ) into a bath of acetone with 30 percent by volume dimethylacetamide. After passing through the bath over a distance of about 120 cm, the web was withdrawn at a rate of about 25.2 m / min and immediately tubular heating chamber m long by about 1.5 with a 242-132
14.7
63.5
3.2
16.0
12.8

230 to 130 16.8 63.6 2.7
15.7
10.6

220 to 130 16.4 57.7

2.4 14.0

9.0

Temperature gradient of 240 ° C at the inlet up to 130 ⁰ C at the outlet. The thread was removed from the chamber at a speed of about 1/2 m / min and stretched 4 times ^{over an electrically heated plate at 110 ° C.}

The thread had the following properties:

Denier 14.7

Initial modes 63.5 ■

Tear length 3.Ξ <■ ;. cen

Elongation at break 16 »/ ₀ Length at break x elongation at break ⁰ x ⁴ 12.8

To investigate the effect at different speeds of the withdrawal from the bathroom as well as the After passing through the heating chamber, the above procedure was repeated in 3 separate experiments, with the difference that the threads were moved at speeds of 12.2, 8.38 and 6.1 m / min. The influence of the different speeds on the properties of the threads is shown in the table below refer to:

attempt

Thread speed,
m / min

denier

Initial module, g / den ...

Tear length, g / den

Elongation at break, ° / "...

Length at break · Elongation at break ⁰ · ⁶

12.2
18.7
59.4
3.1
15.0

12.0

8.38
26.3
63.6

2.9
15.0

11.3

6.1
37.4
57.2

2.3
11.3

8.6

Example 5

According to the procedure of Example 1, »5 an aqueous dispersion of polyvinyl chloride by dispersion polymerization of vinyl chloride at -20 ° C in a mixture of water and ethylene glycol (50:50 volume ratio). The concentration the ethyl glycol in the dispersion was reduced to less than 2 percent by volume as in Example 1, so that a dispersion with 30 weight percent polyvinyl alcohol with an intrinsic molar viscosity of 3.4 dl / g resulted.

An aqueous solution of ε-caprolactam became slow added to the dispersion so that the dispersion has an ε-caprolactam content of 20.5 percent by weight, based on the polyvinyl chloride. An aqueous solution of sodium alginate and polyvinyl chloride was then slowly baked into the dispersion with stirring, so that the dispersion was 20 percent by weight Polyvinyl alcohol and 2.85 percent by weight sodium alginate, based on the polyvinyl chloride, had.

The mixture was pressed through a spinneret having 20 holes (diameter 100 μ) in a bath of methanol with 20 ⁰ C. After passing through the bath over a distance of about 120 cm, the thread was removed from the bath and guided into an acetone bath at 20 ° C. via a guide. After passing through this bath for a distance of about 61 cm, the thread was removed from the bath at a speed of about 7.16 m / min and immediately passed through a tubular heating chamber about 1.5 in length with a maximum temperature of 250 ° C. directs. The thread was removed from the heating chamber at a speed of about 9.1 m / min and stretched four times over an electrically heated plate at 125 ° C. The properties of the thread were as follows:

Denier 58.6

Initial modulus 59.5 g / den Tear length 12 g / den Elongation at break 19.8% Length at break · Elongation at break · ⁶ 14.3 ^s

The above procedure was repeated with the difference that both the acetone bath and the methanol bath contained 5 percent by weight of f-caprolactam.

The thread obtained had the following properties:

Dernier 52.6

Initial module 52 I g / den

Tear length 2.9 g / den

Elongation at break 22.5 ° / "

Length at break · Elongation at break ⁰ · "13.6

In another attempt, the above procedure was used repeated, with the difference that both the methanol bath and the acetone bath each Contained 10 percent by weight ε-caprolactam.

The thread thus obtained had the following properties:

Denier 75.8

Initial modulus 26.6 g / den

Tear length 1.7 g / den

Elongation at break 24.1 "/"

Length at break x elongation at break ⁰ x ⁵ 8.3

Example 6

An aqueous dispersion of polyvinyl chloride was prepared by dispersion ^{polymerization of vinyl chloride at -20 3} C in a mixture of water and ethylene glycol (50:50 volume ratio). As in Example I, the concentration of ethylene glycol was reduced to less than 2 percent by volume, so that the dispersion contained 28 percent by weight of polyvinyl chloride with an intrinsic viscosity of 3.14 dl / g.

An aqueous solution of ε-caprolactam and an aqueous solution of sodium alginate and polyvinyl alcohol were added to the dispersion of polyvinyl chloride as in Example 5, so that a dispersion with 13.7 percent by weight e-caprolactam, 2.7 percent by weight sodium alginate and 20.5 percent by weight Polyvinyl alcohol, based in each case on the polyvinyl chloride, was created.

The mixture was (100 μ diameter) ε-caprolactam through a spinneret having five holes in a bath of acetone with 10 weight percent at 20 ⁰ C is pressed. After passing through the bath over a distance of about 120 cm, the thread was removed from the bath at a speed of about 9.1 m / min and from there via a guide immediately through an about 1.5 m long tubular heating chamber with a maximum temperature of 24O ⁰ C passed. The Fadsn was taken out of the heating chamber at a speed of about 9.1 m / min and drawn on an electrically heated plate at 109 ⁰ C for 4 times. The thread had the following properties:

Denier 13.5

Initial modulus 60.2 g / den

Tear length 3.7 g / den

Elongation at break 15.3 ° / ₀ Length at break · Elongation at break ⁰ · ⁶ ..... 14.7

In another experiment, an aqueous Di was spersion of polyvinyl chloride with an aqueous solution of sodium alginate and polyvinyl alcohol Lö mixed as above, wherein the ε-caprolactam aas the spinning dispersion was omitted.

The mixture was spun as above ; the thread was heated and stretched accordingly.

Dec thread had the following properties:

Γ / egg 13.8

initial modulus 58.0 g / dcn

Tear length 2.3 g / den

Elongation 12.1 ⁿ "

Length at break x elongation at break ⁰ x ⁶ 8.0

Example 7

An aqueous dispersion of polyvinyl chloride was prepared and treated as in Example 6 to reduce the concentration of ethylene glycol.

An aqueous solution of ε-caprolactam and an aqueous solution of sodium alginate and polyvinyl alcohol were added to the dispersion of polyvinyl chloride as in Example 1, so that a dispersion with 22.5 percent by weight e-caprolactam, 2.8 percent by weight Sodium alginate and 20 percent by weight of polyvinyl alcohol, each based on the polyvinyl chloride, originated.

The mixture was pressed through a spinneret having five holes (diameter 100 μ) in a bath of acetone with 15 percent by weight of e-caprolactam with 20 C ^1. After passing through the bath over a distance of about 120 cm, the thread was removed from the bath at a speed of about> .l m.min and then immediately through a guide through an about 1.5 m long tubular heating chamber with a maximum temperature of 24O ° C routed the thread was of the heating chamber at a rate son about 6.1 m / min and then taken stretched out over an electrically heated plate at 108 ⁰ C to 4 times gc. The thread then had the following properties:

Denier 8.9

Initial modulus 54.5 g / den

Tear length 3.4 g / den

Elongation at break 15.2 ⁰ _{; 0}

Length at break x elongation at break ⁰ x ⁵ 13.3

Example 8

An aqueous dispersion of polyvinyl chloride was prepared and treated as in Example 5 in order to reduce the concentration of the ethylene glycol, so that a dispersion containing 33 percent by weight of polyvinyl chloride and an intrinsic viscosity of 2.58 dl / g resulted.

The dispersion was mixed with an aqueous solution of dimethylacetamide and an aqueous solution of sodium alginate and polyvinyl alcohol as in Example 5, so that a dispersion with 5.3 percent by weight of dimethylacetamide, 2.5 percent by weight of sodium alginate and 22.5 percent by weight of polyvinyl alcohol, each based on the polyvinyl chloride was created.

The mixture was pressed through a spinneret having five holes (diameter 100 μ) in a Lad from b acetone with 5 volume percent Oimethylacetamid 20 C ^c. After passing through the had over a distance of about 1.5 m, the thread was removed from the bath at a speed of about iM and then immediately guided through a guide through an about 1.5 m long tubular heating chamber with a maximum temperature of 240 ° C directed. The thread was removed from the heating chamber at a speed of about 9.1 m / min and then stretched four times ^{over an electrically heated plate at 110 ° C.} The properties of the thread were then as follows:

Denier 7/19

Tear length 3.0 g / dcn

Elongation at break 18. ⁷ °, "

Length at break · Elongation at break ⁰ · ⁵ 13.0

Example 9

An aqueous dispersion of polyvinyl chloride mil

A basic molar viscosity of 4.0 dl / g was prepared as in Example 1, and the concentration of Ac- Ethylcnghkols was set to less than 2 percent by volume as there.

Aqueous solutions of 2.2-Dimethyiva1erolaci.uv:

Polyvinyl alcohol and sodium alginate w irdon dci Dispersion slowly added with stirring, so that cmc dispersion with 10 percent by weight 2.2-Dimethy! - valerolactam, 2.5 percent by weight sodium, ileinat uik 11.0 percent by weight of polyvinyl alcohol, based in each case on the polyvinyl chloride, was formed. The Disper sion contained 30 percent by weight polyvinyl chloride. The dispersion was mixed through a spinneret

20 holes (E> diameter 100 μ) in a bath of Me ethanol with 2.5 percent by weight calcium nitrate pressed After passing through the bath over a; Distance of about 120 cm the thread was in a somewhat 0.6 m long Elad made of acetone out and this Bat at a speed of about 6.24 m / min ent nommcr. and immediately through a roughly 1.5 m long raw Ren-shaped heating chamber with a maximum temperature of 223 = C.

A thread was stretched 4 times over an electrically heated plate with HO ^{0 C.}

_so The thread had the following properties:

Denier 88.0

Initial module! 60.4 g / den Tear length 2.5 g / den Elongation at break 1.2.1 ° / ₀ Length at break · elongation at break ^{0 s} 8.7

Claims (4)

1 2 Temperature close to or above the softening or patent claims: melting point experienced a significant reduction. From the British patent specification 767 015 isv a ver 1. A method for producing a fiber or drive known in which the polymer particles in the a filament by spinning a dispersion 5 spun structure thereby grow together Polymer particles in a solution are at least let that a medium (im steps a matrix material through at least one following coalescing agent called), which is a solution spinneret iit a coagulant for the matrix or swelling agent for the polymer is introduced, material and koala seeds of the polymer particles in If the spun structure is made of polyvinylder particles Spun structure shaped in such a way that it contains chloride, especially with a high molecular weight marked that one holds as, experience has shown that one also holds one Polymer Particles Particles of vinyl chloride poly-solvent for the coalescer which is the polymer If a decorative agent is used in the spun structure, there is no sufficient coalescence of the poly coalescing agent for the particles of vinyl chloride particles to provide fibers or threads with useful polymer introduces and the structure that give the 1.5 properties. In particular, it was used as a coalescing agent contains, heated to coalescing found that even with prolonged contact between of the vinyl chloride particles without sacrificing the spun structure and coalescing agent Vinyl chloride polymer particles essentially disintegrate the fibers or filaments thus obtained into small ones are set. Have tear length and a low initial modulus. 2. The method according to claim 1, characterized in that there has now been a method for coalescing into one indicates that the spun structure is made of particles of Vinyi-Vinylchloridpolymerisat particles embedded in the spun structure developed by a heating chloride polymer, in which the coherence chamber leads, whereby the temperature of the heating and strength of the structure are increased and fibers chamber and the dwell time of the thread in the or threads with improved tear length and increased Heating chamber can be chosen so that the desired initial module can be obtained. Warming takes place. The subject of the contract is a process for the production 3. The method according to claim 1 or 2, characterized by spinning a fiber or a filament characterized in that the coalescing agent is a dispersion of polymer particles in a solution by introducing that the spun structure of at least one matrix material through at least a medium from or with the coalescing agent> a spinneret leads into a coagulant for the tel or that a dispersion of vinyl matrix material and coalescing of the polymer particles Spun chloride polymer particles, in which a coalescing agent formed in this way, spun structure in a concentration of 4 to indicates that the polymer particles are particles 25 percent by weight is already included. Made from vinyl chloride polymer used in the spun 4. The method according to any one of claims 1 to 3, 35 structure of a coalescing agent for the particles, characterized in that a dispersion of vinyl chloride polymer is introduced and the structure used by vinyl chloride polymer, which is contained by the coalescing agent, heated to coalescing polymerization of vinyl chloride in an aqueous one of the vinyl chloride ^{particles without the medium being made substantially decomposed at a temperature below 0} ° C. vinyl chloride polymer particles. Turn 40. Under a vinyl chloride polymer. is in the sense of the invention from polyvinyl chloride and copolymers Vinyl chloride and small amounts (e.g. up to 15 percent by weight) to be understood in terms of monomers copolymerizable with vinyl chloride. The object of the invention is to improve the heating of the spun structure with the Coherence and strength of a spun structure Coalescing agent promotes coalescence of the particles with discrete particles of vinyl chloride polymer. made of vinyl chloride polymer and thus improves the It is known that threads and threads thereby produce mechanical properties. U.N.-. the extent of the Can be shared that a dispersion of a poly- 50 coalescence of the polymer particles in the spun mers in a solution νο · η a fiber-forming poly- structure can be determined, the structure can be physically kidney material (hereinafter referred to as matrix) can be examined in a, e.g. B. by electron micrograph Medium (hereinafter referred to as coagulant) since the degree of coalescence of the polymer particles is irr woven that is a nonsolvent for the matrix. spun structures, however, improve in the The spun structure thus formed consists of 55 mechanical and physical properties de; discrete particles of the polymer, which are expressed in the lower structure, can have such properties as Mal »Embedded matrix. These woven are used for the degree of coalescence. A good thing Structure is weak, and it is particularly important to increase the strength characteristics of the degree of coalescence ness and stretchability are necessary, which in the matrix include the measurement of the tear length and / or the reach embedded polymer particles grow together to yield the value sen or to coalesce. , .. ,, "_. . Breaking length · Elongation at break »·« From the British patent specification 767 015 a ⁶ Dispersion spinning process known in which the Koa for the finished fibers or threads, lescence by heating the structure to eirteTempe- If the coalescence z. B. by contact between temperature takes place at which the polymer particles soften or 65 of the spun structure, the discrete particles au melt and thereby melt together. This vinyl chloride polymer contains, and the Koalesziei However, method is not suitable for polymers, such as medium evoked, it has been found that auc z. B. polyvinyl chloride, which when heated to a real solvent for the polymerize