SU38960A1 - A method of making artificial yarn from viscose - Google Patents

Description

This invention relates to the manufacture of rayon rayon. The dryness of a good extra-silk silk is about 1.5 grams per denier, and wet at -0.5 grams, while the extensibility is 16–18% (Hottenroth. Die Kunstseide, 1930). The proposed method is imget, made of yarn, dry strength of which is higher than 2 g per denier, which is achieved by using a precipitation bath, containing at least 5% sulfuric acid at a temperature between + 10 ° and -10 ° C and immersion length of the filaments in the bath more than 50 cm, and the viscose is prepared without pre-conditioned alkaline cellulose , when the content of cellulose in viscose is not less than 8%, carbon disulfide also takes more e 40% of the cellulose weight. The action of strong sulfuric acid is stopped by the occurrence of threads in the collecting device before. It is possible to expose the threads in the bath or outside it to an additional EXTENSION. Since the extensibility of the yarn made of viscose made by the proposed method ranges from 4-10%, i.e., lower than that of ordinary extra-silk silk TB. In order to increase the extensibility, the filaments are treated with caustic alkali at a concentration not lower than 18% and sodium sodium with the possible addition of alkaline nln neutral salts, or a solution of sodium sulphide at concentration ng below 30%. The treatment with anti-stiffening agents is carried out without tension or with slight tension.

The process of obtaining artificial liquor consists in forming filaments of viscose and coagulating them with a sulfuric acid concentration of at least 55%. Sturdy sulfuric acid can be taken in a mixture with one or more Neor blends (155)

gannic substances, for example, another strong mineral acid (hydrochloric, nitric acid or phosphoric acid), or in a mixture with neutral or acidic acid salt, sulfate, bisulfate, sodium sulfate, magnate sulphate, ammonium sulphate, ammonium sulfide, zinc sulfate, nitric acid, sodium sulfate, nitric acid with boric acid. To strong sulfuric acid or in mixtures of it with another strong acid, nln with one iln several inorganic substances from the above mentioned ones}, an appropriate amount of one or several organic substances (glucose, alcohol, aniline, etc., or acetic acid can be added , formic, milky nln sorrel knsloty). If you enter salt into the bath, which can react with HsSO, the amount of sulfuric acid should be chosen as follows. so that in addition to the acidic acid sulfate required, the precipitation bath contains free cross-acid of the desired cream; but less than 65 1, the dry parts of the acid per 100 parts by weight of the precipitation bath. In addition, the strength of sulfuric acid depends on the time of pre-ripening. and partly from the time of viscose ripening and from the age and amount of cellulose contained in the viscose. In general, viscose, which has been matured for several days or made from alkaline cellulose that has been created for two to three days, as well as viscose of low viscosity and poor cellulose, cannot withstand such strong sulfuric acid as an outgrowth, which it ripened from 3 to 48 hours, nln which was prepared using alkaline cellulose bases, either consoled or with prematurity from 3 to 36 hours, and finally, as risks of high viscosity n rich in cellulose. Therefore, the best viscose for consumption, according to the proposed invention.

ow uys are those whose koefsh avyt in zkosgk raken 2 or more. Production, the results are obtained in those, the slides, when the production of viscose is used: greol e1C alkaline cellulose 6j3 n untouched. or with creation; no more. H.-M for 36 hours, for example, from 1 to 24 hours. Good rezljaty give viscose, which at. Ogoyleny by non-mediocre, about mixing system parts. Viscose can be mixed with one or more suitable substances, well-known s viscose silk, for example, glycerin, glucose, sodium sulfate, sodium sulphite, acid sodium sulphate, ammonium sulphate, liquid glass, alkaline aluminum, etc. d. In some cases, it is advantageous to use viscose, in the manufacture of which the sulfurous carbon is collected in a quantity exceeding 40% of the weight of the cellulose.

The strength of sulfuric acid also depends on the lengthy and submerging of the thread in the precipitation bath and on the tension given. and not in it or her. The volume of the precipitator bath is .tw; room or somewhat i higher than it, but it is better to use only a temperature from -flO to -10 ° C.

The length of iti or fibers loaded into a precipitation bath with strong sulfuric acid can vary in very wide ranges, for example, from 3 s, m to 2 m, and isit mainly. from 1 color of the bubble, temperature and concentration of the bath with which the spinning is performed. the thread - “- should be stretched or not directly after it about asoi ai and, i.e., in a special bath, or waiting for i ann and a collecting device, or in both places of one branch. In order to start the deist and sulfuric acid, the thread is washed before or during loading onto the reel of the collecting mouth jofiCTs a. After washing and the thread can be Haipeia or steamed before or after drying. Example I. 100 wt. parts of sulfate pulp 9-10% moisture or 100 out. parts of the linter 7% of the moisture content is narrowed down to yours. consisting of 2000 weight. parts. 18% caustic soda solution. In this bath, the temperature of which should be around 15 ° O, the sulphite pulp is kept for 3 hours, after which it is pressed until the total weight reaches 300 weight. parts or, in the case of the linter-340 c. parts. But the mass is ground in machines; for 2.5 - 3 hours and the tempo:; a temperature of 11 ° 0 and, not allowing the alkaline pulp to ripen even., add from 40 to 60 parts and sulfurous carbon hydrogen and xytogenate for a period of 5 hours at a temperature of 15–18 ° 0. After this, remove the superfluous carbon and asth for 10–5 minutes. o-) cellulose is thus treated in such a quantity; st1. yoda and caustic soda, so that the final solution is about 6.5% cellulose and 8% NaOH. After that, the filv-g rub the viscose three times through cotton paper, with two filtration processes being made shortly after the production of viscose, and the last - immediately before the production of viscose; The second fi lter of the biscuit is kept at a distance of 90–96 h. At a temperature of 13–15 ° C and then filtered for a third time. To obtain yarn, viscose is extruded: ayut at a speed of 3 m to the inside of a platinum filter, having:; shu «24 open, with a diameter of 0.12 .Jii; each, in a bath containing 70% of the seawater: acid 0 W «p 11 ° C, give the length of the dipping into the gray 1 ICON Q cm and then; Wiring the thread through the air, approximately, iia prist ukenii. 120 cm and winding it on the spool, which gives the thread / translational speed, 30 m per minute. Thus obtained 06 JaafoM bovgo thread of fibers of 3-4 denier each. And above this, in three npvHeSi.yxKt, three article stitches are distributed .. sticks, the passage of which the thread receives is my Extra tension and stretching. The lower part of the coil is rotated in water, so that cepiiaH kis, is washed off to that point, the nig falls on the coil. Ate: this. The threads are washed, cleaned, twisted and trimmed, as usual. The yarns produced by this process have a strength in the CjXoM state of more than 2 grams per denier, and in some cases the strength reaches 5 grams per denier. Fortress, filament raw form is approximately 1.5-2.5 g per denier

Example P. 100 weight. parts of sulphite pulp or lichter are drunk with 900 to 2000 weight, parts of 18% caustic soda solution at a temperature of 15-18 ° o and this mixture is allowed to stand for 3 to 24 hours. After this, the mass 01 is pressed to 200–400 wt. parts and crushed. Size Here, lulose is kept for 60-72 hours at room temperature, after which from 30 to 75 weight is added to it. parts of carbon disulfide and the mixture is mixed, for example, in a closed month / liner machine in a sul: feed drum from 4 to 8 hours and a temperature of 16 ° -20 ° C. After that, the excess Cipple angle is removed and the mass of the solution; ; WATER or in a dilute solution of caustic sul l, thus, intake, contained from 8 to 12% cellulose. If the caustic soda solution is used as a solvent, it can be made so that the soda soda, which is in cellulose, is taken into account, and in 1-fold viscose contains from 5 to 8% caustic soda. The viscose sprit obtained in this way is filtered through, cotton or through a tight cotton mat: rial, or cheoez, both together and. released from gas bubbles. It is not a part of this i after maturation p) and a temperature of 16-1b ° C for a short (from 12 hours to 2 days; nd; or longer (or 4 to 7 days) interiors in the course of viscose will melt consisting of solution) and 133 wt .. with ammonium hydroxide in 120 i.ec. hours x sulfuric acid 50-55 ° Veu, which is from 7., 0 9 i her. parts of sulfuric acid in 66% Vyo or from a solution from ten parts of glucoJH in 10 -, - 185 Becoibix parts of sulfuric acid in 47-55 ° Vyo. Precipitation temperature 1-, under: rye:; is set to a limit from O - 16 ° G. The length of the filaments immersed in the bath may be equal to K) cm or 30-100 cm or more. Threads are wound on a bobbin or fed into the center | Ofogoo, which can be disassembled, rolls of the precipitator. iy i pnny and, w at a distance of 20-120 fM from it. Following this, the NIIHs are washed and dried.

Yarns may be subjected to HS. of ways as in an oscillatory bath, between the bath and between the bath and the collective use of the Sco. may vary within wide limits. The upper limit of the possible speed depends on the temperature of the precipitation bath, on the length of the dives, on the distance between the bathtub and the collecting device, on the degree of stretching reported during the spinning time, and on the amount of viscose supplied by the pump. So-napriyr D) the bath has a temperature below 0 °, for example - 5 ° C, the length of the submerged filament pai na.SO l ".. .. the distance between the coagulating acid-n-collect. Equal to 120 cMi stretch, obtained by the thread between the bathroom and sairat.mel.ym. device, comparatively, and the pump delivers from 2 to 3 cm of viscose per-yinu.tu. Under these conditions, blah: oprititnye reaudatyaty can be achieved at speed and sprint per minute or more, 2) all the conditions of the exercise remain the same. Since a non-pump will feed from 4 to 5fM viscose per minute, then. up to 40-60 meters per minute; 3) if the springs remain the same, but the temperature of the bath will be equal, for example, 8 ° C, then the speed of the springs may be increased to 50-60 m per minute.

Before the final one, a new pr; m (.; Which yarn can be processed by a known method in a solution of sodium sulphite, acid sulphate or in weak sulfuric acid, etc.) The washed ones can be heated (approximately at 100-11b ° C) I.IaI are steamed d. Or dry. In addition, 1and can be processed by any .. known in viscose production with edSEV. D.L.L.

Example ill. The conditions of example II with this. BHueJi,. 1) the sulphided mass is diluted — like or diluted with caustic soda, so that yutov viscose contains 5% of cellulose; 2) in the capacity of an enamel ane ;; s, a pasture of 13 parts of ammonium sulphate and 120 parts of sulfuric acid is used from 50 to 60 ° Vy to which is added 7 to 9 parts of sulfuric acid 66 ° Vyo or.-Solution 10 -15 parts of glucose in 185 - 190 parts of sulfuric acid in 55-60 ° Be.

Example IV. Condition conditions I or P1 with the difference that the viscose is either not allowed to mature or allowed to mature only for 12-48 hours, and that the precipitation bath consists of sulfuric acid from 60 di 64 Vy at a temperature of from 6 to (f C. For such a strong acid, should be produced at a higher rate, for example, from 40 to 60 meters into clay.

C.I.V.V. 100 wt., Parts of sulphite pulp or lin-ger are impregnated with 90P.- 000 wt. parts of lS% -ropo; eastwest; static soda at a temperature of 15 -18 ° C, and the mixture is allowed to stand for 3 - 24. The grain weight of this mass is compressed - up to 200-300 weight. parts, in the case of the use of sulphite pulp and up to 340 i. parts, in the case of a linter, and crushed manually or in floors) in a machine. Immediately or soon this, for example. one hour later, the weight was W-40; D 75. weight. parts of serluglero a - and sulfonate for several hours (from 4 to 14 hours), at a temperature of 16 - 20 ° C. After this, the carbon disulfide carbon biscuit is removed, and the sulfided mass is absorbed; 650 - 900 degrees. parts, and in the case of the linter, in 1050 weight. parts 3-10% of the soda of K.ycTH4ecKOfl. Viscose is filtered and freed from gas bubbles. After the ripening or after ripening, at a temperature of between 15 and 18 ° C, viscose is obtained in a known manner in the precipitating tauHC. containing ratior 13, wt. parts of ammonium sulphate I; 120 weight. parts of sulfuric acid 55-60 ° Be. to which came; is 9-10 weight. parts of the sulfuric 66 ° Bie i temperature of the coagulating bath is maintained from 0 to 16 ° G,

PRI m "p VI. The method of preparation of viscose differs from that described in example V in that alkadia cellulose ripens and sulfates after squeezing and grinding: for about 3 to 24 hours, the temperature is between 16 and 20 0. The amount of caustic soda used by plants is: Vorenshgksanto enata, may be the same; that in example V, or slightly lower, for example, so that it turned out. 10-12% -on viscose.

PRI me r VII. a) 80-100 weight. parts finely ground sulphate pulp or bleached cotton cm: shivayu1 with 900 - 920 weight. in parts

810 ° / per-but; -o caustic soda solution. To this

Smeek added 40 to 150 EEC. parts of carbon dioxide and incubated at room temperature for IV-72 hours, with stirring. The viscoa solution thus obtained is filtered through a thick cotton fabric and blown away gas bubbles. Immediately thereafter l.; And after ripening at a temperature of 16 18 ° C for a short, for example, from 12 o'clock .; up to 2 F-1) or longer (for example, from 4 to 7 days) period of time, viscose and children in one of the following yann:

1) a solution of 13.3 wt. parts of se-sho-is. Yugo ammonium in 120 weight. partly; - xeric acid 45-60 ° Veu, to which the prnba. l are 7--9 weight. parts of sulfuric acid, at 6 ° Ve or

2) races: thief 10-15cc. parts of GLKO in 190-1S5 weight. parts of sulfuric acid in 45-60 Be.

Vacna temperature from -16 ° C.

b) The conditions are the same as in clause a, with the difference that before or after the increase of carbon disulfide a small amount of any catalyst is injected in a pastor with caustic alkali, j-a example. from 0.2 about 1, weight. part of the soluble XJJOMO salt "whether salts of nickel or salt jelly per.

c) The conditions are the same as in paragraphs a and b, with the difference that a small amount of soluble peroxide is injected before and after the increase in carbon disulfide. HajjnnMep. RSC. parts of sodium peroxide on 1PO her. parts of pulp

. N) and m te p viii. 100 weight. parts of ground sulphite-1y whole .1lose). mix into a hermetically sealed case cooled cooling and mixing for stirring; a and. and add 200 cc there. parts of a .12-20 VHOPO caustic soda solution, preferably in small portions. As soon as the mass becomes synodny, by 40–60 it will be consumed. parts of carbon carbon, after which the fixed fixture is closed. After 4-8 hours, the mass is poured and diluted.

in 930 weight. parts & -16% -hard p Yard, to% "t of ches soda. The sulfide concentration in the end of the Tej: bHnM solution is about 330 wt. parts. Teaching viscose contains S of the original pulp.

In the examples that have been used in the manufacture of viscose, ground sulphite pulp, you can use bazlenny cotton or cellulose treated with dilute acids, for example, hydrochloric or sulfuric acid.

An artificial skin can be obtained by one of the methods described for the previous examples, if part or all of the sulfuric acid is replaced with another with a mineral acid, for example, hydrochloric acid (25--40% strength), nitric acid (70-90 %), phosphoric (beats. weight from 1.5 to 1.86) or a mouse with a varicelle (from 60-90%).

In many cases, it is desirable to increase the stretchability of artificial yarns made by the described method without at the same time decreasing the strength or luster of the yarns, which can be achieved if the artificial yarn is found to be refined. ; Challenges of art.

As a quality, their merits proved to be particularly suitable mercer. Detergents and, above all, caustic alkali solutions, for example, NaOH at a concentration of not less than 18%. But with other mercerizing agents, good results can be achieved, for example, with a concentrated solution of alkaline sulphide (for example, solution of gray sodium at a concentration of from 30 to 58%) or strong and insulin acid (for example, sulfuric acid in 46- 60 VioIl ppsforn and acid beats V. 1.5-1.8, or nitric acid (50-60%, or hydrochloric acid (26-32%) or a solution of zinc chloride, or thiocyanate, for example, calcium thiocyanate, etc. .

The processing of artificial yarns by means of contraction may be by coeepiu in various ways, for example, by immersing or drawing through a solution of evacuating agents or by covering the yarns with a sprayed solution, or by pulling artificial artificial materials through rollers in contact with the solution that causes contraction. funds n. p.

The proposed method of processing is suitable both for the artificial yarn itself, like napimer, artificial silk in the form of yarn, in various BHiax, and in the form of fabrics.

The material in processing cannot be stretched during or after treatment, and if it is still stretched, then it is necessary to allow it to fully or partially shrink.

It should be noted that with the above processing of artificial threads, they do not need to be pre-impregnated or coated with a substance that protects them from alkali, since they, unlike the known artificial silk threads, resist the action of stiffening agents without significant harm to themselves.

The treatment can be combined in one operation with the removal of sulfur from the filaments. For this, it is possible, NEP, to add sufficient kolnchesti about tiivivogo funds, for example, caustic

"1" before, chi-c, vrnmek eya la sulfur removal. Prn in the application of a strong solution of sodium sulfide; the further addition of the shaving agent may be completely unnecessary.

A shrinking agent, for example, a caustic alkali solution, can be supplied with a true amount of a neutral sun or alkali-reactive salt, for example, sodium chloride, sodium sulphate, sodium silicate, sodium alyinate, sodium trictate, borax, sodium phosphate, sodium hydroxide, or alcohol, such as ethyl alcohol or glycerin.

The stretchability of artificial china can be increased by 0–200% or more (so that even low-stretch threads can be reduced to stretch in at least S%.

Example 1. Viscose silk in finished dry, but not bleached condition, in coils, is placed without stretching into an IS-26% solution of caustic soda 15-Ib C. After 1-5, the skein is removed and after removal of excess nacTi Pressing or centrifugally, and in appropriate cases and after a short hunt, 5–10% strength, which has a room temperature of about 5 minutes, is placed in sulfuric acid. Hot or cold 5-25% ammonium sulphate or 4% hydrochloric acid can also be taken as sulfuric acid. Thereafter, the click is washed, if desired, whitens and dried without stretching or with moderate stretching.

Example 2. The conditions, as in Example 1, are only the difference that a solution consisting of 200 parts of sodium chloride in 1500 parts of a 20% aqueous solution of sodium hydroxide with water serves as a shrinking medium.

Example 3. A method of treatment as in example 1. with the only difference being that solution is taken as a solution for dissolving out of 88 parts of sodium sulphate in 1500 parts of a 20% ONE caustic soda solution.

Example 4. A treatment method as in approx 1, with the same principle that a 20% aqueous solution of caustic soda containing 8-10% glycerol is used as a defiant shrinkage of the agent.

Example 5. Rayon silk on a bobbin and a zaghem, after more or less soaking, is twisted and wound into a skein, which is worn in a wet condition and a weak solution of sodium sulphide, and then in the case of the WTO-1 a-and without oast givani, placed in the growth, consisting of 200 weight. sodium chloride or 88 wt. parts of sodium sulfate and 1500 weight. partly and a 20% aqueous solution of sodium hydroxide, where 1 to 5 minutes remain. Further processing is carried out, KU in example 1.

Example 6. A treatment method as in Example 1 n 5 with the difference that a mixture of 1500 wt.% Is used as a tinting agent. parts of a 22.5% aqueous solution of caustic natp with 150 weight. parts of liquid glass in 39 ° &

Example 7. The method of processing, as in prnmer; 1 or 5, with the difference that the strand is not desulfurized, but only washed, so that the solution is used as a shrinking bath.

from 270 weight. parts of caustic soda and 450 parts of sodium sulphide in 1050 weight. portions of water, k); at the same time serves as a desulfurization agent.

Example 8. A method of treatment as in Example 7.0, with the difference that B as a tightening medium is used, bV or sodium sulfide solution, which also serves as a desulfurizing agent.

Example 9. Treatment with CnocoJ as in Example 1 or 7, with the difference that as a defiant shrinkage of the treatment with a 30-50% sodium sulphide solution containing 1-5% sodium hydroxide.

Example 10 A treatment method as in Example 1 or 7, with the difference that 18 to 22% sodium hydroxide solution containing 8 to 10% sodium sulfate is used as a shrink agent.

Prior to shrinking treatment, nts or tissues are lined or ground with a 2-3% solution of gelatin or protein or 3-4% pacTBopOjU starch.

Other methods can also be used. Iwayupshe means, in addition to those indicated in the examples, for example, instead of caustic soda solution can serve as a solution of another caustic alkali, for example, a solution of caustic potassium, equivalent to stanetrapine; instead of sodium sulphide, it can be used for another alkali alkali, for example, potassium sulphide or sulfuric acid 47-S0 ° Be, or hydrochloric acid at 27-30%, or nitric acid at 50-60%, or, finally, 40 -80% calcium cyanate solution.

The subject of the patent.

1. A method of making viscose yarns of high dry fortress exceeding 2 g per denier, characterized in that a precipitation bath containing at least 55% sulfuric acid is used to precipitate the yarns.

2. A method for making viscose yarns according to claim 1, characterized in that. that viscose is prepared from alkaline cellulose, without pre-ripening or with a small pre-ripening.

3. The method of manufacture and viscose nnty, according p.n. 1 and 2, characterized in that the action of sulfuric acid is terminated at the time the threads enter the collecting device or earlier.

4. Method of manufacture; artifical yarns, according to p. 1, characterized in that the tusk contains at least 8% cellulose.

5. Method of making viscose yarns according to p. 1-4, characterized in that the immersion length of the threads in the bath is 50 cm.

6. Method of making viscose yarns according to p. 1-5, characterized in that nt in the bath or outside of the bath is subjected to an additional stretch.

7. Method of making viscose yarns, according to p. 1-6, characterized in that the temperature of the precipitation bath is maintained between - (- 10 ° and - 10 ° C.

8. Method of making viscose yarns according to p. 1 to 7, characterized in that, in xanthogenesis, carbon disulfide is taken more than 40% of the weight of the pulp.

9. Method of making viscose yarns according to p. 1-5, characterized in that, with the purpose of increasing the stretch, the threads are treated with caustic alkali at a concentration not lower than 18% and sulphurous sodium, with addition of alkali or neutral salts d .yiHX or

10. Acceptance of the method indicated in paragraph 9, characterized in that the processing of the filaments is carried out with a solution of sodium sulphide in a concentration not lower than 30%.

11. Acceptance of the method indicated in paragraph 9, characterized in that the processing of the threads is carried out without tension or with a slight tension.