RU2190052C1 - Method of joint cottonizing and dyeing of flax fiber - Google Patents

Abstract

FIELD: textile industry. SUBSTANCE: in a method comprising treatment of flax fiber with solution including alkali, dye, and reducing agent, after which dye is oxidized, fiber is subjected to acidification and washing to remove acid, is distinguished by that starting flax fiber is brown material preliminarily subjected to mechanical garneting to attain linear density 0.3-1.5 tex, treatment solution is completed by complexone based on ethylenediaminetetraacetic acid sodium salt or ethylenediphosphonic acid derivative, dye is of vat dye type, reducing agent is represented by hydrosulfite, rongalite, and nitrogen-containing reducer taken individually or in various combinations with each other, and oxidation of dye and acidification are conducted simultaneously by consecutively performing washing with cold water and treatment with acidic hydrogen peroxide solution. EFFECT: increased workability of cottonine in a variety of operations and improved coloration quality. 2 cl, 4 tbl, 11 ex

Description

Technical field
The invention relates to the textile industry, namely to the processing of flax fiber for further use in wool and cotton spinning for the production of blended melange and plain yarns and the manufacture of fabrics and knitted fabrics and products from them, as well as in the production of non-woven materials for medical purposes.

State of the art
When processing cotonin into blended yarn with cotton, viscose and synthetic fibers, significant difficulties arise in obtaining uniform and uniform dyes of yarn or fabrics, since the susceptibility of cotton, viscose and linen to dyes of even one class varies significantly. It is impossible to obtain monophonic dyes on a three-component flax-wool yarn or fabrics developed from it, since dyeing of protein, cellulose and synthetic fibers requires the use of dyes of various classes with dyeing parameters that are not compatible with a single technological process. Therefore, pre-dyed fibers are subjected to spinning.

 Known methods of chemical cotonization of bast fibers, which consist in sequential processing of flax fiber cooking and bleaching solutions / DI Rudakov, V.M. Fishermen. Cotonin technology. M., Gizlegprom, 1934, S. 60-63; THEM. Bukhtanov, D.A. Kobylyansky, N.P. Lepeshinsky. Cotonin technology. M., Gizlegprom ,. 1939, p. 42; US Pat. RI 2073753, IL, 6 D 01 C 1/02 /.

 Their disadvantages are multi-stage basic chemical operations (at least three), long duration, increased water consumption.

 It is also known the use of complexones in the alkaline treatment of flax fiber / GB 2186002 A, 02/05/1987 /. The purpose of their use is the removal of pectins and hemicelluloses from flax, which improves the process of scrubbing flax and facilitates the process of removing bonfires and short flax fiber.

 However, with such processing, the process of fiber cotonization does not pass.

 There is also known a method for dyeing vat dyes of cellulose-containing fibrous materials using a dye-containing composition, a reducing agent selected from the group consisting of hydrosulfite, rongalite, a nitrogen-containing reducing agent (for example, GB 1509450 A, 04.05.78).

 However, providing the necessary colors, the method does not allow to carry out the process of elementary fiber flax and get cotonin with the desired spinning properties.

 Since the process of chemical cotonization can be carried out in an alkaline medium at high temperature in the presence of sodium sulfide, combined technologies of cotonization and dyeing with sulfur dyes have been proposed according to continuous and periodic dyeing schemes / I.M. Bukhtanov, D.A. Kobylyansky, N.P. Lepeshinsky. Cotonin technology. M., Gizlegprom, 1939, p. 59-63 /.

The main disadvantages of the continuous technology is the rapid cooling of solutions, which requires a large flow of steam to heat them, and a high rate of evaporation due to the open surface of the barrels with technological solutions having a temperature of 85-95 ^o C.

 The closest technical solution is a periodic method of cotonization and dyeing with sulfur dyes / I.M. Bukhtanov, D.A. Kobylyansky, N.P. Lepeshinsky. Cotonin technology., M., Gizlegprom, 1939, p. 59-63 /. It consists of the following operations.

1. Cooking fiber in a composition containing,% by weight of fiber:
Paint - 11 - 16
Sodium Sulphide - 7 - 8
Caustic soda or - 1,0
Calcium hydroxide - 2.5
Soda - 3.0
Sodium Silicate - 3.0 - 5.0
Sodium Chloride - 15.0
Contact - 1.5 - 2.0
The cooking time is 2 hours, the temperature is 100 ^o C.

 2. Oxidation of the leuco compound of the dye. The operation is carried out by blowing air into the boiler after draining the solution or laying fiber in air for 15-20 minutes.

 3. Flushing with hot and cold water.

 4. Acidification with a solution of sulfuric acid (0.5% by weight of fiber).

 5. Rinsing with cold water.

The method has the following disadvantages:
- low processability of processing in various operations of spinning production. Thus, cotonin fibers are characterized by increased stiffness and fragility due to the deposition of insoluble calcium salts and silicate deposits on their surface. In addition, strength indicators are reduced in flax fiber due to degradation caused by exposure to sodium sulfide in an alkaline environment. The manufacturability of cotonin processing also reduces its lack of properties that determine its spinnability, in particular crimpiness, softness, necessary water absorption, and a high degree of fiber elementization;
- low quality of the paint, which is manifested in the low strength of the coatings to wet treatments, light weather and the inability to obtain bright and clean colors, as well as medium and light colors;
- low environmental purity due to the use of strong mineral acid, sodium sulfide, which releases hydrogen sulfide into the airspace of the working areas, and sulfide ions into wastewater.

 Thus, an environmentally friendly combined method of cotonization and dyeing is unknown, which allows one to obtain cotonin, which is highly technological in spinning and has a good quality of coatings.

SUMMARY OF THE INVENTION
The inventive task was to find an environmentally friendly method of combined cotonization and dyeing, which would allow to obtain cotonin with high technological properties that determine its further processing, and high quality indicators of color.

 The problem is solved by the method of combined cotonization and dyeing of flax fiber, including processing it in a solution containing alkali, dye and a reducing agent, subsequent oxidation of the dye, acidification and washing to remove acid, characterized in that the treatment in this solution is subjected to severe flax fiber, previously mechanical dispersion to a linear density of 0.3-1.5 tex, complexon is additionally introduced into the solution on the basis of the sodium salt of ethylenediaminotetraacetic acid or based on of ethylidene diphosphonic acid, cubic dye is used as a dye, hydrosulfite, rongalite and a nitrogen-containing reducing agent taken separately or in combination with one another are used, the dye is oxidized and acidified simultaneously by successive washing with cold water and treatment with an acidic solution of hydrogen peroxide. Complex used in a concentration of 0.1-2.0 g / L.

The invention allows to obtain a number of advantages:
- get high-tech cotonin. So, the fiber has no rigidity and brittleness, since the complexon binds calcium ions, and sodium silicate is excluded from the solution. The use of certain complexones and reducing agents, taken in optimal concentrations and combinations among themselves, virtually eliminates fiber destruction and provides a high degree of elementization of the bast bundles having a linear density of up to 1.5 tex; the fiber as a result of such processing appears crimp, it becomes soft. The presence of crimp improves the adhesion of flax fiber to other fibers during spinning and helps to reduce its loss. The invention allows to provide a high degree of dedusting of the fiber during boiling and washing, which dramatically reduces dust emission at subsequent transitions of spinning, weaving and finishing;
- melange yarn developed using colored cotonin is suitable for use in the production of knitwear and fabrics of a wide assortment and purpose: from linen to dress and costume. A significant advantage of products made from such materials is the resistance of the dye to household washing using detergents with peroxide bleaches. Vat dyes do not change the shade and do not paint over the white background of the products when boiled. Therefore, colored cotonin can be invested in blended yarn for the manufacture of linen knitwear, bedding and table linen, towels;
- in woolen production, the use of colored cotonin allows you to produce plain wool yarn of a dyed tone to match the color of flax, wool and chemical fiber, or multi-colored melange, depending on the purpose of the fabric and customer requirements.

 The invention improves the environmental cleanliness of the process by eliminating sodium sulfide from the solution.

Information confirming the reproducibility of the invention
To implement the method, you can use the following reagents.

 As the nitrogen-containing reducing agent, for example, triethanolamine, hydrazine hydrate can be used.

Triethanolamine (OCHN ₂ CH ₂ ) ₃ N mol. M. 149, 19 - colorless viscous liquid, t _bales. 360 ^o C. It is well soluble in water, alcohol, acetone. Widely used in the production of surfactants and CMC.

Hydrazine hydrate N ₂ H ₄ • H ₂ O mol. m. 50 - colorless transparent liquid with a boiling point of 118.5 ^o With, soluble in water, alcohol, ammonia. It is used in organic synthesis, in the production of plastics, rubber, explosives, as a component of rocket fuel.

 As a sulfur-containing reducing agent, for example, rongalite, sodium hydrosulfite (dithionite) can be used.

Rongalit H ₂ OCH ₂ S (O) ONa • 2H ₂ O mol.m. 153.23. Colorless hygroscopic crystals, t _melt. 63-64 ^o C, soluble in water. It is widely used in the textile industry as a reducing agent for vat dyes and for bleaching wool and silk.

Hydrosulfite Na ₂ S ₂ O ₄ mol. m. 128. A white crystalline substance, soluble in water. It is widely used in the textile industry as a reducing agent for dyeing with vat dyes, for bleaching wool and silk, as an oxygen scavenger in gas analysis, and as a reagent for the photometric determination of selenium.

 As a complexone based on a derivative of ethylene diphosphonic acid, for example, its hydroxy derivatives - hydroxyethylidene diphosphonic acid or hydroxy derivatives - hydroxyethylidene diphosphonic acid in conc. 0.1-2.0 g / l.

Oxyethylidene diphosphonic acid C ₂ H ₈ O ₇ P ₂
[CH ₃ C (OH) (P (O) (OH) ₂ ) ₂ ]
pier m. 206.03 is a paste or powder of white color with a grayish or pink tint, it is soluble in water, worse in methyl and ethyl alcohols, hot acetic acid. Oxyethylidene diphosphonic acid is a combustible but not explosive substance, t _melt. 175 ^o C, t self-ignition 310 ^o C.

мол. м. 206,03 представляет собой порошок белого цвета с сероватым оттенком, хорошо растворим в воде, хуже в метиловом и этиловом спиртах. Гидроксиэтилидендифосфоновая кислота - горючее вещество, t самовоспламенения 177±3^oС. Комплексоны на основе фосфоновой кислоты широко используют в текстильной промышленности как стабилизаторы перекисного беления.Hydroxyethylidene diphosphonic acid C ₂ H ₈ O ₇ P ₂

pier m. 206.03 is a white powder with a grayish tint, soluble in water, worse in methyl and ethyl alcohols. Hydroxyethylidene diphosphonic acid is a combustible substance, self-ignition t 177 ± 3 ^o С. Phosphonic acid-based complexones are widely used in the textile industry as peroxide bleaching stabilizers.

As a complexon, you can also use disodium salt of ethylenediaminetetroacetic acid EDTA) - Trilon B C ₁₀ H ₈ O ₁₀ N ₂ Na ₂ mol.m. 372.25. It is a white crystalline powder, highly soluble in water and alkalis. Trilon B is widely used in analytical chemistry for water softening, pharmaceutical and chemical industries.

 As a wetting agent, you can use any non-ionic preparation used for this purpose in textile finishing, for example, sulfoside-31, phenoxol 9/10 BV.

 As a fibrous raw material, severe flax fiber is used in the form of short flax fiber, tow, shake, which have undergone preliminary razvolennom and have a linear density of 0.3-1.5 tex.

 For dyeing, you can use various vat dyes in the form of powders or pastes to obtain colors of any color from light to dark tones. In the preparation of a dye suspension, an NF type dispersant is used. A dye suspension is prepared in a known manner. The dye can be taken in a concentration of 0.3-4.0 g / l, depending on the desired color intensity. Based on the concentration of the dye and taking into account the flow rate for the process of cotonization, the concentration of the reducing agent is selected in the range of 5-15 g / l, alkali 5-20 g / l, complexone 0.1-2.0 g / l and dispersant 0.5-1, 0 g / l

 The method is implemented by sequentially carrying out the following operations.

Processing is subjected to flax fiber, which has undergone mechanical razvolenenie to a linear density of 0.3-1.5 tex. Flax flax is treated in a solution containing the following components, g / l:
Caustic soda - 5 - 20
Restorer - 5 - 15
Complexon - 0.1 - 2.0
Dye - 0.3 - 4.0
Dispersant NF - 0.5 - 1.0
Wetting agent - 0.5 - 1.0
The fibers are treated for 100-120 minutes at 100 ^{° C.} , then the dye is oxidized by successively washing with cold water and treating with a solution containing the following components, g / l:
Hydrogen Peroxide 100% - 0.5 - 3.0
Acetic acid 32% - 2.0 - 3.0
at a temperature of 25-40 ^o C for 20-30 minutes

 The dye content on the fiber was determined by the method of sulfuric acid sols / Laboratory workshop on the chemical technology of fibrous materials. M., Gizlegprom, 1963, p. 318 /, color fastness to dry friction and wet wiping - according to standard methods. The quality indicators of cotonin were determined by known methods described in the book "Laboratory workshop on textile materials science" M., "Light Industry", 1974. Table 1-4 shows examples of obtaining colored cotonin according to the invention and the results of its tests in comparison with the prototype.

 The data of tables 1-4 show that the invention provides the production of colored cotonin, which in its main indicators is superior to the colored cotonin obtained by the prototype method. High hygiene indicators - wetting speed - 1 s, capillarity - not less than 60 mm, absorption capacity - not less than 12 g / g of fiber provide the possibility of its use for obtaining a variety of non-woven materials for medical use, linen knitwear, hosiery from light pastel to intense tones. The softness and the presence of a specific “curl” determine the good formability and the necessary strength indicators of non-woven canvases and yarn for the manufacture of knitted and weaving fabrics. By such indicators as the content of fibers of the down group (not higher than 6-10%), linear density (0.39-0.90 tex), the softness obtained by cotonin exceeds the prototype, and the tortuosity given to it during processing is a unique property inherent only this fiber. Curl of colored cotonin was determined as the number of curls per 1 cm of fiber length.

Claims (2)

 1. The method of combined cotonization and dyeing of flax fiber, including processing it in a solution including alkali, dye and reducing agent, oxidation of the dye and acidification, washing to remove acid, characterized in that the solution in the solution is subjected to severe flax fiber, previously subjected to linear mechanical razvolenie density of 0.3-1.5 tex, complexon is additionally added to the solution on the basis of the sodium salt of ethylenediaminotetraacetic acid or on the basis of the derivative of ethylidene diphosphonic acid, as ve use dye vat dye used as a reducing taken individually or in various combinations with one another hydrogen sulfite, rongalite, and a nitrogen-containing reductant and dye oxidation and acidification is performed simultaneously by sequentially carrying out washing with cold water and treatment with an acidic solution of hydrogen peroxide.  2. The method according to p. 1, characterized in that the complexone is used in a concentration of 0.1-2.0 g / L.

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