DE1619010B - Sizing or finishing agent for textile fibers - Google Patents

Description

1 2

The invention relates to sizing or finishing with only partially saponified polyvinyl finishing agent for all types of textile fibers 'one'. acetate is only unsatisfactory,
Finally, the hydrophilic and especially the other hand, the acrylic ester size or hydrophobic fibers, such as polyester and polyamide finish, have a greater adhesive power than partial fibers. The resulting warp yarns have to be made of 5-way saponified polyvinyl acetate. In addition, it is generally sized or appended prior to weaving, but has the disadvantage of strong moisture content, whereupon it absorbs the weft threads crosswise. Therefore, currently the use must go through. of partially saponified polyvinyl acetate and acrylic

Until now, depending on the type of acid ester, the warp size had to be used in combination as a size or

the threads or yarns to be sizing are chosen io wise finish spreads,

will. - As a result of studies on sizing for

In the case of hydrophobic fibers, such as polyester and poly warp yarns, it was found that the invention

amide fibers, can with the single use of appropriate sizing or finishing agents for textile

partially saponified Γ polyvinyl acetate or partially fibers not only for hydrophilic fibers, but also

saponified polyvinyl alcohol by 15 for the hydrophobic fibers mentioned without additives

finishing cannot be improved sufficiently. can be used as its excellent

On the other hand, although acrylic sizes have a high level of adhesion, its softness and moisture-stronger adhesion than partially saponified polyabsorption can be correctly adjusted depending on the type of vinyl acetate or alcohol sizes to be sized and a superior fiber.
Property of elasticity, but they show a stronger 20. In addition, the size of the present invention has moisture absorption. Apretur a better cohesive force than that at the moment

Therefore, at present, the combined use is common combinations of partially saponified

of the two sizing agents are widely used. Polyvinyl acetate or polyvinyl alcohol and acrylic

The invention relates to a warp size and the weaving method can therefore be used in

or finish for fibers of the above-described use of this size or finish for friction

Art. For these fibers one used as sizing to be carried out.

or finishes in general partially saponified Through numerous experiments it has been found that

Polyvinyl acetate and acrylic acid ester in combination. the sizing or finishing agent according to the invention

However, this size has the disadvantage of improving the quality of fabrics for textile fibers,

strong moisture absorption, which is too difficult. In addition, the size according to the invention can

in weaving. or finishing agent can be obtained as a powder. It

There are also sizing for synthetic fibers has a very high purity and is easy to handle,

known to be transported and weighed by complete or partial transport,

Soap the vinyl acetate units in copolymers from The sizing or finishing according to the invention

Vinyl acetate and dialkyl esters of unsaturated agents are easily soluble in water, which means that the additional

Dicarboxylic acids, alkyl esters of acrylic acids and borrowed use of another chemical agent

Vinyl alkyl ethers are obtained. This well-known becomes superfluous.

Sizing agents also have the disadvantage of having an extremely high moisture absorption, which is of superior quality, can therefore be used as a sizing or finishing liquid,
especially when processing hydrophobic fibers in 40. The size or finish appearance according to the invention occurs. When interweaving such fibers, medium by copolymerization of vinyl acetate, for example polyester fibers, the weaving takes place in and acrylamide and the subsequent partial combination atmosphere with very high relative humidity, soaps of this copolymer can be obtained. For example, 75 to 85% relative humidity is here. It is important that the sizing or finishing agent has a suitable acrylamide content and degree of saponification, sizing agents which are fully or partially saponified because they improve the adhesiveness, the adhesiveness, residues of the esters of unsaturated aliphatic dicarbon elasticity, moisture absorption and superior properties contain acids, such a strong stickiness of the chain, cohesive force in the powdery state adjusted that the weaving process is sensitively disturbed. . can be.

The inventive warp size or finish 50 by increasing the acrylamide content and the has the advantage over the known sizes, partially saponified portion of the acrylamide copolymer that they do without the addition of any other chemical agent, the moisture absorption becomes stronger, and the can be used and that contain a unique .schlichteten or finished warp yarns Application is sufficient. In addition, it shows too much moisture. This is of course for the web Less moisture absorption than hitherto ”55 is disadvantageous, since the undesirable tackiness, known sizing agents based on polymers, increases with the speed of the yarn partially saponified ester groups, so that they have a particularly low acrylamide content The weaving of fibers in a humid atmosphere is more difficult to carry out and is equally suitable for animal processes. early on, the abrasion resistance and scuff resistance

The object of the invention is therefore a simplicity and softness of the with the simplicity or

or finishing agent for textile fibers, containing a finishing agent treated and processed warp

Copolymer of vinyl acetate and an acrylic mono-yarn reduced.

mers, which has partially saponified acetate residues and The preferred acrylamide content in the saponified

is characterized in that it is a copolymer copolymer is therefore 0.2 to 17 mole percent,

from vinyl acetate and acrylamide, whose acetate 65 It was also found that by conversion

remnants are partially saponified. from 75 to 95 mole percent of the acetate residues in hydroxy

For example, in the case of hydrophobic fibers, such as groups, the size or finish can be easily powdered

Polyester or polyamide fibers that can be obtained sizing or shaped.

However, if the saponified content is reduced below 75 mole percent, the sizing or Finishing agents are increasingly difficult to obtain in powder form.

If more than 95 mole percent of the acetate residues are converted into hydroxy residues, the desizing becomes almost impossible impossible

In the copolymerization of vinyl acetate (M ₁ ) and acrylamide (M ₂ ), the polymerization _{parameters T 1} : -0.07 and r ₂ : -7.5, respectively. In order to obtain a uniform copolymer, it is therefore preferred to copolymerize in accordance therewith by gradually adding acrylamide at a faster reaction rate in accordance with the degree of polymerization of vinyl acetate.

The invention is explained in more detail with reference to the following examples. Here, parts mean parts by weight and percentages percentages by weight, unless otherwise noted.

example 1

A total of 0.10 parts of acrylamide becomes a liquid mixture consisting of 0.0053 parts Azo-bis (isobutyronitrile) in 1 part of vinyl acetate and 1.13 parts of methanol are added continuously. the Polymerization is carried out at 65 ° C for about 12 hours. It becomes a vinyl acetate-acrylamide copolymer produced in a yield of more than 99%.

A solution of 30 parts of the copolymer and 70 parts of methanol is then admixed with V75 moles of sodium methylate per mole of vinyl acetate. The saponification reaction is carried out at 40 ⁰ C. Partially saponified vinyl acetate-acrylamide copolymer having a degree of polymerization of 500 and a degree of saponification of 85 mole percent of the acetic acid residues has been obtained (the product is shown in Table I as sample No. 1 according to the invention). The above procedure is repeated with 0.024 parts and 0.002 parts, respectively, of acrylamide (samples No. 2 and No. 3 according to the invention) in place of the 0.10 part of acrylamide.

After the three copolymers have been dissolved, polyester warp yarns are processed on a two-stage roller finishing machine, settled.

The finishing conditions and the test results are summarized in Table I. For comparison, yarns are also treated in the manner indicated with sizing agents which are partially saponified by the sole use of partially saponified polyvinyl acetate with a degree of saponification of 88 mol percent (comparative test No. 1 in Table T) and using 4.2 parts of the above-mentioned Polyvinyl acetate and 1.8 parts of acrylic chain sizing, an aqueous solution of a partially saponified methyl acrylate copolymer (Comparative Experiment No. 2 in Table I) have been obtained. The properties test of the yarns was carried out in the same way. The results are shown in Table I. As can be seen, Sample No. 2 of the invention is superior to Comparative Test Sample No. 2 in flexibility and cohesive strength.

Even if the size intake was kept lower than in the comparative test No. 2, the sample No. 2 according to the invention shows an even higher one Cohesive force. It can also be seen that the moisture absorption of Sample No. 1 after Invention is limited by the degree of increase in the acrylamide content, while also in the Sample no. 3 according to the invention, its frictional resistance by reducing the acrylamide content is limited.

Table I.

Samples according to the invention No. 2 No. 3 ■ Comparative
attempt Comparison
attempt No. 1 I 2 0.3 No. l No. 2 11th 5.1 5.0 5.5 28 23 4.9 5.7 32 138 165 15th 19th 108 ■ 180 175

Acrylamide content (in mol percent) ... Sizing agent absorption (in percent)

Cohesive force (in times)

flexibility

The values in Table I are obtained under the following conditions:

Arbitration Conditions:

Roller speed 4.5 / minute

Roller contact length 1-step roller

1.4 to 1.6 cm 2-step roller 1.2 to 1.4 cm

Sizing speed 118 m / minute

Temperature of the sizing liquid.

at 20 ± l ° C

Relative humidity 58 ± 1%

Warp thread, polyester 50 denier, ..

24 F twist - 300 times / m

Property test (temperature 2O ⁰ C relative humidity 65%).

55

60 Composition of the sizing bath:

Samples according to the invention or comparative test samples 6%

35% aqueous wax solution 0.4%

30 to 40% aqueous solution of
Polyoxyethylene 0.5%

Cohesive force:

Tested by using a TM-type friction tester.
After the sized yarns had been fixed at a bending angle of 130 ° using three steel mandrels, one end of the yarn was held in place and the other end was loaded with 10 g / piece.

After applying friction to the sized yarns by moving the three Thorns parallel to the threads are the times it takes to move the thorns until they separate of the threads necessary have been measured.

Flexibility:

Tested with a twist type slope tester.

One end of the sized threads with a length of 3 m was attached to a movable roller, while a magnet was attached to the other end in such a way that the substance could hang vertically and come to rest in a less strong magnetic field.
If the roller rotates at a speed of 1 revolution per minute and the angle of rotation of the roller required for the magnet to rotate a certain angle (φ) is set as Θ , the flexibility is given as follows:

Flexibility = - ^ - 100.
Θ

The smaller this value, the greater the softness.

The acrylamide content was determined by nitrogen analysis.

As can be seen from Table I, Sample No. 2 is according to the invention in terms of flexibility superior to comparative test sample No. 2.

It can also be seen that the moisture absorption property of sample no. 1 according to the invention is limited by the extent of the increase in the acrylamide content, while furthermore at of sample no. 3 according to the invention, its elasticity due to the extent of the reduction in the acrylamide content is limited.

Example 2

The following comparison was made: Between the use of sample No. 2 after Invention as a warp size and the use of a known size made of partially saponified polyvinyl acetate and acrylic acid esters (Comparative Experiment No. 2 in Table I).

Using a total of 4600 sized or finished warp yarns in an automatic Loom, on the right and left side of each 2300 with the sample no. 2 according to the invention The weaving test is carried out.

The test leads to the result that the number of warps sized with the sample according to the invention, which were separated or cut during weaving, averages 1 per 32.9 m of fabric, while the number of warp sides sized with the comparative test sample is the same of the separated or cut yarns is 1 yarn per 7.0 m of textile web. This means that the ratio of cut yarns during weaving between the two cases is 1: 5.
. The sizing conditions are identical to those of Example 1.

The web conditions are as follows:

Temperature 24 to 28 ° C

relative humidity 74 to 82%

Loom revolutions ... 150 revolutions

per minute
Warp yarn tension 50 to 55 g

Example 3

A solution of 0.1 part of acrylamide and 0.009 part of methanol becomes a copolymerization-5 liquid consisting of 1 part vinyl acetate, 0.155 part methanol, 0.0005 part azo-bis- (isobutyronitrile) and 0.0006 part of acetic acid was continuously added dropwise. The polymerization will last for about 5 hours at 62 bis 64 ° C carried out.

ίο It will be a copolymer of vinyl acetate and acrylamide obtained in a yield of about 70%. Then unpolymerized vinyl acetate monomer is added to separated in a known manner and then from the copolymer a solution consisting of 3 parts of copolymer and 7 parts of methanol.

After addition of sodium V200M0I per mole of vinyl acetate in said copolymer, the saponification reaction is carried out at 3O ⁰ C. A vinyl acetate-acrylamide copolymer with a degree of saponification of 88 mol percent and a degree of polymerization of 1,800 is thus obtained (sample no. 4 according to the invention).

Then, after transferring these products into an aqueous solution, the following are specified Composition and subsequent sizing of polyester-cotton blend yarn using The property test on the yarns and the weaving test were carried out using a slot sizing machine.

Then, for comparison using the comparison is test sample Nos. 3, which partially saponified polyvinyl acetate having a polymerization degree of 1800 and a saponification degree of 88% and 0.24 parts of a 40 ° / ₀ aqueous solution containing 4.5 parts of a partially saponified Polyacrylsäuremethylesters, finishing is carried out in the same manner as indicated above.

The results are shown in Table II.

Table II

Acrylamide content

(in mole percent)

Sizing agent intake

Strength (in g)

Degree of stretching (in%)

Frictional resistance
(in times)

Number of yarns separated or cut during weaving per hour

Sample No. 4 according to the invention

1.1

10.7 186 10.1

2219 0.2 to 0

Comparative test sample No. 3

11.5 187 9.0

1870 0.5

Arbitration Conditions:
Composition of the sizing bath:

For sample no.4 according to the invention, 4.45%

For comparative test sample No. 3 ... 4.78%

Cellulose Glycolate (CMC) 0.42%

Corn starch .... 1.82%

Solid mixture of saponifiable oils, mineral oils and non-ionic activator from m.p. 45 to 50 ° C 0.42%

7 8

An appre sizing conditions are used for finishing or finishing:

Kawamoto 15 D animal machine used. Sample no. 4 according to the invention or the temperature of the sizing bath .... 80 ⁰ C same test sample no. 4 according to the

• Squeezing pressure 0.75kg / cm ² finding 3.80 ° / ₀

Sizing speed 25 m / minute " ⁵ Colloidal silicon dioxide 0.38%

Drying temperature 90 to 95 ° C corn starch 4.86%

Carbomethylcellulose 0.15 ° / ₀

Weaving conditions: '· "^; mixture of cleaned wax, yarn: mixed yarn of Polytster 65 hardened oil and non-ionic active-'

and BaumwoUe .. Λ ".... 35 45 / S * ° _{tor from} melting point 45 to 50 ⁰ C 0.23 ° / ₀

Total number of warp yarns 5054 silicone emulsion 0.04%

Fabric density .. '. · .... 126 · 72 / 2.54 cm

Number of revolutions des'.auto-; Finishing machine: Suzuki hot air machine

matic loom: ....: 185 / minute type.

Temperature 15 'temperature of the sizing

in the weaving process · 6 to 11 ° C. bath 94 ° C

relative humidity. - ·.; "■""". * "'", * ". * _Oril _., - _{/ ΛΛ} ·..

when weaving · ...., 55 to 73% layer speed .... 30 to 32m / minute

Firmness:. ',. Drying temperature 90 to 95 ^{0 C}

With the help of Shimazu Autograph Model 20 for regrowth, a solution is used

P-110 checked.-,. ·. the purified wax, hardened oil and one

Contains nonionic activator.

Abrasion resistance: "The regrowth is carried out at 85 ° C.
During the time, after its expiry, every 10 pieces of the _{yarn used} ...
the friction times have been obtained 65/35 34 / S. It is a tension of 400 g / 10 sized yarns at a bending angle of weaving conditions:

115 ° has been used. 30 automatic loom

loom

The acrylamide content is determined by nitrogen analysis

determined. T ο y ο d a

According to the test result (1), those with the total number of warp yarns are 3874 33 / S

Sample according to the invention sized yarns of the 35 fabric density 85-60 yarns /

with the comparative test sample sized yarns 2 54 _C m

superior in terms of abrasion resistance because the number _TT ,, ,,, " _r,. ,. - «" ,,.,. .

of the warp yarns cut away during the weaving operation, revolutions of the loom 170 / minute

is lower than that with the comparative test temperature during weaving 21 ° C

try sized yarns and they have a better 40 relative humidity during weaving ... 78%
show workability in weaving.

Example 4 Example 5

After mixing starch and additive 45 After preparing an aqueous solution of the with an aqueous solution of the following composition from that given in example 3 in example 3 Sample No. 4 of the invention according to the held sample No. 4 of the invention and the subsequent composition and subsequent subsequent sizing of wool yarn with sizing of polyester-cotton blended yarn becomes a twist of the mentioned sizing liquid and one the web attempt carried out. 5 ° roll sizing machine is used for the desizing

For comparison, as stated above, after trying the sized yarn as follows:

Mixing of starch and additive with one out: For comparison purposes, by using

aqueous solution, consisting of 3.47 parts partially manure of 5.5 parts partially saponified polyvinyl

saponified polyvinyl acetate (degree of polymerization: 1800, acetate (degree of polymerization: 1800, degree of saponification: Degree of saponification: 88 mol percent) and 0.35 parts of a 55 88 mol percent) and 0.5 part of vinyl acetate maleic acid

25% igeci aqueous solution of partially saponified anhydride copolymer (comparative test sample No. 5)

Polyacrylate copolymer (comparative test sample No. 4), an aqueous solution of the following composition

the weaving attempt made using sneaked and after sizing wool yarn

tetem yarn carried out. a desizing attempt with the yarns

The test results show that the results achieved.

according to the invention sample no. 4 sized or the composition of the sizing agents is like

finished yarns the number of the weaving process follows:
cut yarn a little under 0.2 yarn per

Hour and the operating performance or the loading sample no. 4 according to the invention or sales efficiency is almost 100% and in the case of the 65 identical test sample No. 5 6.0%

Comparative test sample No. 4 0.6 yarn per hour maize starch 3.0%

is cut away and the operating performance or the acetylated white potato starch l> 0%

Operating efficiency is 95%. Carboxymethyl cellulose 0.2%

Claims (1)

9 10 The finishing conditions are as follows: continuously desizing, 'while with the comparative Finishing machine 2-stage roller of the test sample No. 5 after sized yarn itself Kakimoto Tvds Carrying Out the Similar Discrimination Procedure Solution temperature " ^ns still show an approx. 3% sizing content, of the size 60 to 70 ⁰ C '^{"5 is} therefore the desizing in the latter Finishing speed ';;! ". 107m / minute Trap not completely. Roll revolutions Claims: ■ per minute. : ■ No. 4: 1; No. 5: 2.2 Contact angle in mm .... No. 4:15 ^L Sizing or finishing agent for textile Nr 5 * 14 ^lo fibers, containing a copolymer of vinyl acetate and an acrylic monomer that is partially Desizing conditions: has saponified acetate residues, thereby Ester of Caro's acid with a indicates that it is a copolymer higher alcohol 2 0 ° / vinyl acetate and acrylamide with partly saponified 30% aqueous solution "of a polyoxy- '° ^is contains acetate residues. ethylene alkyl ester 0.5% ² · Sizing or finishing agent according to An claim 1, characterized in that the co- After dipping the yarns to be desized, polymers of vinyl acetate and acrylamide 0.2 to in the said desizing bath at a tempe- 17 mole percent acrylamide and its acetate temperature of 60 to 80 ° C and for about 24 hours, 20 residues are saponified to 75 to 95 mol percent,
they are rinsed with lukewarm water and then 3. sizing or finishing agent according to claim washed with water. 1 or 2, characterized in that the co- As this experiment shows, those with the sample become polymeric from vinyl acetate and acrylamide No. 4 according to the invention sized yarns by such, which in an anhydrous methanol the above procedure has easily been saponified almost 100% completely.