RU2288984C1 - Acetylcellulose fiber dyeing process - Google Patents

Abstract

FIELD: fiber dyeing.

SUBSTANCE: invention is intended for coloristic design of articles manufactured from modified, in particular antimicrobial, acetylcellulose fibers and is directed to impart smooth, deep, and strong color to fibers, while simultaneously increasing their biological activity. To that end, 8-hydroxyquinoline is added to spinning solution of acetylcellulose in amount 0.5-5.0% of the weight of polymer before formation of fibers, after which fibers are continuously impregnated with aqueous solution of cupric sulfate pentahydrate, pH 4.0-6.5, at 1-2°C and liquor ratio 10 for 4-5 min and then subjected to expression to weight increment 110-120%, heat treatment at 175-200°C for 30-40 sec, washing, and drying. Weight ratio of 8-hydroxyquinoline to CuSO₄·H₂O in impregnating solution is (1÷1.5):(20÷30).

EFFECT: improved quality of coloration and increased biological activity of fibers.

2 cl, 2 tbl, 4 ex

Description

The invention relates to the field of dyeing and finishing production and can be used in the color design of products from modified, in particular antimicrobial, cellulose acetate (AC) fibers.

In modern production, methods are used to obtain dyes on textile materials and deepen their tone on the same textile materials by forming fibers from spinning solutions of polymers in the presence of modifying additives, followed by dyeing of freshly formed fibers or products made from them with known classes of dyes.

It is known to introduce cellulose acetate into a spinning solution before forming 8-hydroxyquinoline films in order to modify the films and give them antimicrobial properties (SU 317660 A1, 1971). However, in the text of this copyright certificate there is no indication of the subsequent processing of the obtained films with a coloring substance.

It is also known to obtain a colored antimicrobial cellulose-containing fiber by pre-impregnating it with an aqueous acetic acid solution of 8-hydroxyquinoline followed by treatment with a copper (II) salt to form a color from yellow to greenish-yellow and brown (RU 2050859 C1, 1995). However, this patent cannot be opposed either as an analogue or as a prototype of the claimed invention for the following reasons:

8-hydroxyquinoline, which is used in the claimed method as a modifying substance, is poorly soluble in water. So, at the isoelectric point (pJ 7.2 at 18 ° C), the solubility of 8-hydroxyquinoline in water is 0.53 g / l, but it is well soluble in chloroform, benzene, isoamyl acetate, diethyl ether, isoamyl alcohol. Therefore, with an aqueous solution of this compound it is not possible to deeply and evenly impregnate cellulose acetate fibers, which are chemical artificial hydrophobic fibers. Based on this, during further processing of the AC fibers modified in this way with a copper (II) salt, it is not possible to ensure the diffusion of 8-hydroxyquinoline molecules deep into the fibrous substrate, which leads to the formation of fragile and unsaturated colors.

The closest in technical essence to the claimed invention is a method consisting in dyeing cellulose diacetate (DAC) knitted fabrics, which were produced from fibers containing an antimicrobial preparation, β- (5-nitro-2-furyl) acrolein ( NFA), conventional dispersed dyes (Polishchuk B.O., Wolf L.A., Kotetsky V.V., Brazauskas V.V., Plotkin L.L. Study of the possibility of processing antimicrobial cellulose acetate fibers into various medical devices // Newin the organization, engineering and technology of textile and light industry: Collected scientific papers - L., 1975. - T.XVI. - P.101-103).

Its significant disadvantage is the relatively long duration of the process, which leads to the desorption of NFA from the composition of the fiber and, as a result, a decrease in the biological activity of the textile material.

The technical problem to which the claimed invention is directed is to give AC fibers containing 0.5-5% 8-hydroxyquinoline even, deep and strong to the physicochemical effects of the color, while increasing their antimicrobial activity, simplifying dyeing technology and expanding the range dyes for AC fibers.

The specified technical result is achieved in that the method for producing a dyed AC fiber includes introducing a modifying compound into the cellulose acetate dope, spinning the fiber from it and dyeing the freshly formed fiber with dye, where 8-hydroxyquinoline is used as the modifying compound, and processing the freshly formed fiber containing 0 , 5-5% by weight of the polymer of 8-hydroxyquinoline, carried out by impregnation according to a continuous method with an aqueous solution of copper sulfate at a pH of 4.0-6.5, a temperature of 1-2 ° C, the bath module 10 for 4-5 minutes, followed by an extraction to a weight gain of 110-120%, heat treatment at 175-200 ° C for 30-60 seconds (for DAC and cellulose triacetate (TAC) fibers, respectively) with washing to remove loose salt and drying.

In addition, the ratio of mass amounts of the modifying compound, 8-hydroxyquinoline, in AC fibers and copper sulfate CuSO ₄ · 5H ₂ O in an impregnating solution is 1-1.5: 20-30.

The invention is illustrated by the following examples and tables, which show the indicators of color stability (in accordance with GOST 9733-61) on modified AC fibers processed according to the proposed method, as well as the antimicrobial activity of colored modified AC fibers.

Example 1. The dyeing of freshly formed TAC fibers obtained by introducing a modifying compound — 1% by weight of 8-hydroxyquinoline polymer into the spinning solution of TAC — is carried out by continuous method impregnation with an aqueous solution of copper sulfate (ratio of the amounts of 8-hydroxyquinoline and CuSO ₄ · 5H ₂ O 1: 20) at pH 4.0, a temperature of 1-2 ° C and a bath module 10 for 4-5 minutes, followed by an extraction to a gain of 120%, heat treatment at 195-200 ° C for 30 seconds, washing for 20 minutes in a solution of fine detergent with a concentration of 2 g / l at 50-60 ° C, warm (40 ° C) and cold (20 ° C) with distilled water to remove loose salt. Before treatment with a solution of copper sulfate, TAC fibers are light yellow in color, and the modified fibers after washing and drying contain 0.17% Cu ²⁺ and have an intense yellow-green color.

Example 2. The dyeing of freshly formed TAC fibers obtained by introducing a modifying compound — 5% by weight of 8-hydroxyquinoline polymer into the spinning solution of TAC — is carried out by continuous method impregnation with an aqueous solution of copper sulfate (ratio of the amounts of 8-hydroxyquinoline and CuSO ₄ · 5H ₂ O 1, 5:20) at a pH of 6.5 according to example 1, heat treatment at 195-200 ° C for 60 seconds and washing according to example 1. After washing and drying, the fibers contain 0.92% Cu ²⁺ and are dyed in intense yellow-green color.

Example 3. Dyeing of freshly formed DAC fibers obtained by introducing a modifying compound — 0.5% by weight of 8-hydroxyquinoline polymer into the DAC spinning solution — is carried out by the continuous method of impregnation with an aqueous solution of copper sulfate (ratio of the amounts of 8-hydroxyquinoline and CuSO ₄ · 5H ₂ O 1:30) at pH 4.0 according to Example 1, heat treatment at 175-180 ° C for 60 sec and washing according to Example 1. After washing and drying, the fibers contain 0.08% Cu ²⁺ and are colored yellow-green .

Example 4. The dyeing of freshly formed DAC fibers obtained by introducing a modifying compound, 3.5% by weight of 8-hydroxyquinoline polymer into the DAC spinning solution, is carried out by continuous method impregnation with an aqueous solution of copper sulfate (ratio of the amounts of 8-hydroxyquinoline and CuSO ₄ · 5H ₂ O 1.5: 30) at a pH of 6.5 according to Example 1, heat treatment at 180 ° C for 60 seconds and washing according to Example 1. After washing and drying, the fibers contain 0.63% Cu ²⁺ and are dyed in intense yellow-green color.

As can be seen from tables 1 and 2, the use of the proposed method for dyeing AC fibers containing 0.5-5.0% 8-hydroxyquinoline, in comparison with the existing technical and economic advantages:

a) gives the fibers a color that is highly resistant to various physico-chemical influences;

b) contributes to the simultaneous increase in their biological activity;

c) allows to carry out the process of dyeing these fibers by a continuous method with a sufficiently high speed;

g) expands the range of dyes for AC fibers.

The optimal concentration of the introduced modifying additive - 8-hydroxyquinoline - in the spinning solutions of cellulose acetates is in the range of 0.5-5.0% by weight of the polymer, and its further increase in spinning solutions, as well as varying the above parameters of the dyeing process of freshly formed fibers, are practically not affects the indicators of color stability and antibacterial activity of 8-hydroxyquinoline-containing AC fibers.

Table 1
Indicators of color stability on modified AC fibers obtained according to examples 1-4 to various physicochemical effects Physicochemical effects Non-examples and color fastness, points one 2 3 four Shine 6-7 7 6-7 7 Light and weather 6-7 7 6-7 7 Distilled water 5/5/5 5/5/5 5/5/5 5/5/5 "Sea water" 5/5/5 5/5/5 5/5/5 5/5/5 Soap solution at 40 ° C 5/5/4 5/5/5 5/5/4 5/5/5 Wash at 60 ° C 5/5/5 5/5/5 5/5/5 5/5/5 Flue gas 5 5 5 5 Sublimation: 120 ° C, 80 min 5/5/5 5/5/5 5/5/5 5/5/5 210 ° C, 30 sec 5/5/5 5/5/5 5/5/5 5/5/5 210 ° C, 60 sec 5 5 5 5 Ironing dry 5 5 5 5 wet 5/5 5/5 5/5 5/5 Friction dry 5 5 5 5 wet 5 5 5 5

table 2
Antibacterial activity of 8-hydroxyquinoline-containing AC fibers treated with aqueous solutions of copper sulfate CuSO ₄ · 5H ₂ O (with impregnation bath module 10) Fiber name The content of 8-hydroxyquinoline in the fiber,% (by weight of the polymer) pH of the impregnation bath Heat treatment Zone of growth inhibition of test cultures (including the diameter of the hole, equal to 10 mm), mm T, ° C τ min Staphylococcus aureus 209 P Salmonella typhimurium 362 b / o TAC one 6.5 200 one 26.4 / 15.3 30.6 / 27.4 TAC 5 6.5 200 0.5 29.9 / 22.8 18.1 / 17.0 TAC 5 6.5 200 one 28.9 / 22.8 23.6 / 17.0 DAC 0.5 6.5 180 one 22.8 / 17.4 24.3 / 22.9 DAC 3,5 6.5 180 one 30.2 / 26.2 22.7 / 17.0 Note. Numerator - antimicrobial effect after treatment with a copper salt;
denominator - antimicrobial effect before treatment with a copper salt.

Claims (2)

1. A method for dyeing cellulose acetate fibers, comprising introducing a modifying compound into a cellulose acetate dope, forming the fiber therefrom and treating the freshly formed fiber with a coloring material, characterized in that 8-hydroxyquinoline is used as the modifying compound, and the processing of the freshly formed fiber containing 0.5 -5.0% by weight of the polymer of 8-hydroxyquinoline, carried out by continuous impregnation with an aqueous solution of sulfuric acid copper at pH 4.0-6.5, temperature 1-2 ° C and bath module 10 for 4-5 minutes followed by squeezing to 110-120% weight gain, heat treatment at 175-200 ° C for 30-60 seconds, washing and drying. 2. The method according to claim 1, characterized in that the ratio of the mass amounts of the modifying compound 8-hydroxyquinoline in cellulose acetate fibers and sulfuric acid copper CuSO ₄ · 5H ₂ O in the impregnating solution is 1-1.5: 20-30.