Double-strand yarn comfortable and wear-resistant denim fabric and its preparation process

Abstract

The present invention relates to the field of fabrics, specifically to a double-yarn comfortable and wear-resistant denim fabric and its preparation process. A fabric base cloth is prepared by using a double-yarn process; a modified chitosan solution and composite silica are blended as a finishing solution; the base cloth is subjected to plasma treatment twice successively; using chitosan as a substrate, selective oxidation with sodium periodate is carried out to obtain dialdehyde chitosan, and then branched biguanide hydrochloride is grafted. By using the multi-amino groups on the branched chitosan, quaternary ammonium groups are partially introduced, thereby enhancing the broad-spectrum antibacterial property of the modified chitosan solution; the hollow nano-silica modified by γ-glycidoxypropyltrimethoxysilane, that is, epoxy hollow silica, is synthesized by the fine emulsion method. By using the ring-opening reaction of amino groups and epoxy groups, the branched biguanide hydrochloride is grafted onto the surface of the epoxy hollow silica to obtain composite silica with good antibacterial property, good dispersibility and good bonding strength with the fabric, improving the long-term antibacterial property of the fabric.

Description

Technical Field

[0001] The present invention relates to the field of fabrics, and specifically to a double - ply yarn comfortable and wear - resistant denim fabric and its preparation process. Background Art

[0002] With the progress of textile technology and the continuous improvement of people's material living standards, the demand for the diversification and functionality of clothing fabrics is on the rise. For young people pursuing fashion, personalized and color - differentiated clothing fabrics are highly attractive. Jeans are an essential item in the daily outfits of most young people. Compared with ordinary denim fabrics, double - ply yarn denim has better breathability and comfort, winning the attention of more and more consumers.

[0003] At the same time, the antibacterial and wear - resistant properties of fabrics are closely related to the lifespan of fabrics. How to prepare a denim fabric that combines comfort, wear resistance, and antibacterial properties is a hot issue in current industry research. Summary of the Invention

[0004] The purpose of the present invention is to provide a double - ply yarn comfortable and wear - resistant denim fabric and its preparation process to solve the problems in the prior art.

[0005] To solve the above - mentioned technical problems, the present invention provides the following technical solutions:

[0006] The preparation process of the double - ply yarn comfortable and wear - resistant denim fabric includes the following steps:

[0007] S1: Twisting, sizing and dyeing, threading the heddles, and weaving two single - ply yarns to form a base fabric;

[0008] S2: Performing a primary plasma treatment on the base fabric to obtain an activated base fabric;

[0009] S3: Preparing a finishing solution with a modified chitosan solution and composite silica;

[0010] S4: Placing the activated base fabric into the finishing solution for impregnation treatment to obtain a pretreated base fabric;

[0011] S5: Performing a secondary plasma treatment on the pretreated base fabric and drying to obtain the double - ply yarn comfortable and wear - resistant denim fabric.

[0012] Furthermore, the single - ply yarn is one of bamboo charcoal yarn, wool yarn, polyester yarn, spandex yarn, nylon yarn, and cotton yarn; the twist of the twisting is 2.5%.

[0013] Furthermore, the working conditions of the sizing and dyeing are: the sizing and dyeing vehicle speed is 20 m / min; the composition of the dye used for sizing and dyeing is: using 1 L of deionized water as the solvent, which contains 25 - 35 g of environmentally friendly dye and 0.7 - 0.8 g of penetrant.

[0014] Further, the working conditions for the first plasma treatment are as follows: the working gas is argon, the power is 88 W, the discharge pressure is 220 Pa, and the treatment time is 25 s; the working conditions for the second plasma treatment are as follows: the working gas is argon, the power is 100 W, the discharge pressure is 220 Pa, and the treatment time is 50 s.

[0015] Further, the mass ratio of the modified chitosan solution to the composite silica in the finishing liquid is 23:(1 - 3).

[0016] Further, the preparation of the modified chitosan solution includes the following steps:

[0017] 1) Mix chitosan and glacial acetic acid solution, add sodium periodate, stir in the dark for 2 - 3 h, add ethylene glycol solution, pour into a dialysis bag and dialyze in deionized water for 3 d, freeze at -80 °C for 12 h, and dry to obtain dialdehyde chitosan;

[0018] 2) Mix dialdehyde chitosan and deionized water, add a mixed solution of branched biguanide hydrochloride and deionized water, and keep warm at 18 - 25 °C for 7 - 8 h to obtain a branched chitosan solution;

[0019] 3) Heat the branched chitosan solution to 78 - 82 °C, adjust its pH to 9.9 - 10.1, add a mixed solution of 2,3 - epoxypropyltrimethylammonium chloride and deionized water, keep warm at 78 - 82 °C for 5 - 6 h, adjust the pH to 3, cool, rotary evaporate, and dialyze to obtain the modified chitosan solution.

[0020] Further, the preparation of the composite silica includes the following steps:

[0021] A. Mix cetyltrimethylammonium bromide and deionized water as the aqueous phase, mix tetraethyl orthosilicate, γ - glycidoxypropyltrimethoxysilane, and methyl silicone oil as the oil phase, add the oil phase to the aqueous phase under stirring conditions, stir for 15 - 20 min, use a homogenizing emulsifier to homogenize and emulsify in an ice - water bath for 5 min, add triethanolamine, and keep warm at 18 - 25 °C for 22 - 24 h to obtain epoxidized hollow silica;

[0022] B. Mix epoxidized hollow silica and deionized water, stir ultrasonically for 10 - 20 min, add a mixed solution of branched biguanide hydrochloride and deionized water, keep warm at 18 - 25 °C for 22 - 24 h, centrifuge, wash, and dry to obtain the composite silica.

[0023] Further, the mass ratio of epoxidized hollow silica to branched biguanide hydrochloride is 1:3.

[0024] Further, the preparation of the branched biguanide hydrochloride includes the following steps:

[0025] (1) Mix 1-(o-tolyl)biguanide with absolute ethanol, adjust to neutral with dilute hydrochloric acid, rotary evaporate and dry to obtain 1-(o-tolyl)biguanide hydrochloride;

[0026] (2) Under a nitrogen atmosphere, mix ethylenediamine and methanol, transfer to an ice-water bath, add methyl acrylate, raise the temperature to 28 - 32 °C and hold for 22 - 24 h, then rotary evaporate to obtain intermediate preparation A; mix intermediate preparation A, ethylenediamine and methanol, raise the temperature to 23 - 27 °C and hold for 22 - 24 h to obtain intermediate preparation B; mix intermediate preparation B, methyl acrylate and methanol, raise the temperature to 28 - 32 °C and hold for 22 - 24 h to obtain intermediate preparation C; mix intermediate preparation C, ethylenediamine and methanol, raise the temperature to 23 - 27 °C and hold for 22 - 24 h to obtain branched polyamide-amine;

[0027] (3) Under a nitrogen atmosphere, mix 1-(o-tolyl)biguanide hydrochloride and branched polyamide-amine, raise the temperature to melting, add polyethylene glycol, raise the temperature to 158 - 162 °C and hold for 3 - 5 h, absorb the tail gas with dilute hydrochloric acid solution, cool down, and separate the liquid to obtain branched biguanide hydrochloride.

[0028] The beneficial effects of the present invention:

[0029] The present invention provides a double-yarn comfortable and wear-resistant denim fabric and its preparation process. By adjusting the process and composition, a denim fabric with green environmental protection, good wear resistance, good antibacterial property, and high comfort is prepared.

[0030] In the present invention, a double-yarn process is used to prepare the fabric base cloth. Through process parameter control, a base cloth with high strength, good wear resistance, and being stiff and shaped is obtained. Compared with ordinary fabrics, it has better air permeability and moisture retention effect, thus enhancing the usability of the denim fabric.

[0031] In order to further improve the antibacterial property and wear resistance of the fabric, a modified chitosan solution prepared from the green bio-based raw material chitosan and composite silica are blended as the finishing solution. In order to improve the bonding strength between the finishing solution and the base cloth, the base cloth is first activated by primary plasma treatment. After the finishing solution impregnation treatment, secondary plasma treatment is used to enhance the crosslinking between the finishing solution and the fabric. At the same time, a complex crosslinking network is constructed in the finishing protective layer formed on the fabric surface, thereby improving the durability of the fabric's antibacterial and wear resistance.

[0032] In order to solve problems such as the poor solubility of chitosan, chitosan is modified. Using chitosan as the substrate, it is selectively oxidized with sodium periodate to obtain dialdehyde chitosan. Utilizing the Schiff base reaction of aldehyde group - amino group, it crosslinks branched biguanide hydrochloride with good antibacterial properties, thereby greatly improving the water solubility of chitosan. Among them, the branched biguanide hydrochloride is obtained by the thermal polycondensation reaction of 1-(o-tolyl)biguanide hydrochloride and branched polyamide - amine, resulting in a structure with multiple active groups, thereby greatly enhancing the binding strength between the finishing liquid and the fabric. The branched polyamide - amine is a multi-branched polyamide - amine prepared from ethylenediamine and methyl acrylate as raw materials; using the multiple amino groups on the branched chitosan, quaternary ammonium groups are partially introduced, thereby enhancing the broad-spectrum antibacterial property of the modified chitosan solution and improving the bactericidal effect of the fabric.

[0033] Silica is introduced into the finishing liquid as a filler to further improve the wear resistance of the fabric. In order to improve the uniformity of the dispersion of silica in the finishing liquid, fine emulsion method is used to synthesize hollow nano-silica modified by γ-glycidoxypropyltrimethoxysilane, that is, epoxy hollow silica. Utilizing the ring-opening reaction of amino group and epoxy group, the branched biguanide hydrochloride is grafted onto the surface of the epoxy hollow silica to obtain composite silica with long-lasting antibacterial property, good dispersibility and good binding strength with the fabric, thereby improving the long-term antibacterial property of the fabric. Specific embodiments

[0034] The following will combine the embodiments of the present invention to clearly and completely describe the technical solutions in the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0035] In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of those of ordinary skill in the art to implement. When the combination of technical solutions appears contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0036] The following further details the technical solutions of the present invention in combination with specific embodiments. It should be understood that the following embodiments are only used to explain the present invention and are not used to limit the present invention.

[0037] Example 1: The preparation process of double-strand comfortable and wear-resistant denim fabric includes the following steps:

[0038] S1: Two single-strand yarns are combined, sized and dyed, heddled and woven to form a base fabric;

[0039] The single-strand yarn is cotton yarn; the twist of the combined twist is 2.5%;

[0040] The working conditions for sizing and dyeing are as follows: the sizing and dyeing vehicle speed is 20 m / min; the composition of the dye used for sizing and dyeing is: using 1 L of deionized water as the solvent, which contains 25 g of environmentally friendly dye and 0.7 g of penetrant;

[0041] S2: Perform primary plasma treatment on the base fabric to obtain an activated base fabric;

[0042] The working conditions for the primary plasma treatment are as follows: the working gas is argon, the power is 88 W, the discharge pressure is 220 Pa, and the treatment time is 25 s;

[0043] S3: Prepare a finishing solution with modified chitosan solution and composite silica;

[0044] The mass ratio of the modified chitosan solution to the composite silica in the finishing solution is 23:1;

[0045] The preparation of the modified chitosan solution includes the following steps:

[0046] 1) Mix 5 g of chitosan and 100 mL of glacial acetic acid solution with a mass fraction of 2%, add 3.2 g of sodium periodate, stir in the dark for 2 h, add 20 mL of 0.1 mol / L ethylene glycol solution, pour it into a dialysis bag and dialyze in deionized water for 3 d, freeze at -80 °C for 12 h, and dry to obtain dialdehyde chitosan;

[0047] 2) Mix 0.6 g of dialdehyde chitosan and 100 mL of deionized water, add a mixture of 3.6 g of branched biguanide hydrochloride and 100 mL of deionized water, and keep it warm at 18 °C for 8 h to obtain a branched chitosan solution;

[0048] 3) Heat 100 mL of the branched chitosan solution to 78 °C, adjust its pH to 9.9, add a mixture of 2 g of 2,3-epoxypropyltrimethylammonium chloride and 10 mL of deionized water, keep it warm at 78 °C for 6 h, adjust the pH to 3, cool, rotary evaporate, and dialyze to obtain a modified chitosan solution;

[0049] The preparation of the composite silica includes the following steps:

[0050] A. Mix 0.6 g of cetyltrimethylammonium bromide and 200 mL of deionized water as the aqueous phase, mix 26.2 g of tetraethyl orthosilicate, 2.62 g of γ-glycidoxypropyltrimethoxysilane, and 2.92 g of methyl silicone oil as the oil phase, add the oil phase to the aqueous phase under stirring conditions, stir for 15 min, use a homogenizing emulsifier to homogenize and emulsify in an ice-water bath for 5 min, add 0.7 g of triethanolamine, and keep it warm at 18 °C for 24 h to obtain epoxidized hollow silica;

[0051] B. Mix 0.4 g of epoxidized hollow silica and 140 mL of deionized water, stir ultrasonically for 10 min, add a mixture of 1.2 g of branched biguanide hydrochloride and 20 mL of deionized water, keep at 18 °C for 24 h, centrifuge, wash, and dry to obtain composite silica;

[0052] The preparation of the branched biguanide hydrochloride includes the following steps:

[0053] (1) Mix 6 g of 1-(o-tolyl)biguanide and 50 mL of absolute ethanol, adjust to neutral with dilute hydrochloric acid, rotary evaporate and dry to obtain 1-(o-tolyl)biguanide hydrochloride;

[0054] (2) Under a nitrogen atmosphere, mix 1.35 g of ethylenediamine and 50 mL of methanol, transfer to an ice-water bath, add 18.34 g of methyl acrylate, raise the temperature to 28 °C and keep for 24 h, rotary evaporate to obtain intermediate preparation A; Mix 0.51 g of intermediate preparation A, 1.35 g of ethylenediamine, and 25 mL of methanol, raise the temperature to 23 °C and keep for 24 h to obtain intermediate preparation B; Mix 0.51 g of intermediate preparation B, 18.34 g of methyl acrylate, and 25 mL of methanol, raise the temperature to 28 °C and keep for 24 h to obtain intermediate preparation C; Mix 0.51 g of intermediate preparation C, 1.35 g of ethylenediamine, and 50 mL of methanol, raise the temperature to 23 °C and keep for 24 h to obtain branched polyamide-amine;

[0055] (3) Under a nitrogen atmosphere, mix 5 g of 1-(o-tolyl)biguanide hydrochloride and 1 g of branched polyamide-amine, raise the temperature to melting, add 0.3 g of polyethylene glycol 400, raise the temperature to 158 °C and keep for 5 h, absorb the tail gas with 100 mL of dilute hydrochloric acid solution, cool down, and separate the liquid to obtain branched biguanide hydrochloride;

[0056] S4: Put the activated base fabric into the finishing solution and impregnate it to obtain a pretreated base fabric;

[0057] S5: Perform secondary plasma treatment on the pretreated base fabric and dry it to obtain a double-yarn comfortable and wear-resistant denim fabric;

[0058] The working conditions of the secondary plasma treatment are: the working gas is argon, the power is 100 W, the discharge pressure is 220 Pa, and the treatment time is 50 s.

[0059] Example 2: The preparation process of a double-yarn comfortable and wear-resistant denim fabric includes the following steps:

[0060] S1: Twist, size-dye, thread, and weave two single yarns to form a base fabric;

[0061] The single yarn is cotton yarn; the twist of the twisting is 2.5%;

[0062] The working conditions for sizing and dyeing are as follows: the sizing and dyeing vehicle speed is 20 m / min; the composition of the dyes used for sizing and dyeing is: using 1 L of deionized water as the solvent, which contains 29 g of environmentally friendly dyes and 0.75 g of penetrant;

[0063] S2: Perform a primary plasma treatment on the base fabric to obtain an activated base fabric;

[0064] The working conditions for the primary plasma treatment are: the working gas is argon, the power is 88 W, the discharge pressure is 220 Pa, and the treatment time is 25 s;

[0065] S3: Prepare a finishing solution with a modified chitosan solution and composite silica;

[0066] The mass ratio of the modified chitosan solution to composite silica in the finishing solution is 23:2;

[0067] The preparation of the modified chitosan solution includes the following steps:

[0068] 1) Mix 5 g of chitosan and 100 mL of an ice acetic acid solution with a mass fraction of 2%, add 3.2 g of sodium periodate, stir in the dark for 2.5 h, add 20 mL of 0.1 mol / L ethylene glycol solution, pour it into a dialysis bag and dialyze in deionized water for 3 d, freeze at -80 °C for 12 h, and dry to obtain dialdehyde chitosan;

[0069] 2) Mix 0.6 g of dialdehyde chitosan and 100 mL of deionized water, add a mixture of 3.6 g of branched biguanide hydrochloride and 100 mL of deionized water, and keep it at 20 °C for 7.5 h to obtain a branched chitosan solution;

[0070] 3) Heat 100 mL of the branched chitosan solution to 80 °C, adjust its pH to 10, add a mixture of 2 g of 2,3-epoxypropyltrimethylammonium chloride and 10 mL of deionized water, keep it at 80 °C for 5.5 h, adjust the pH to 3, cool, rotary evaporate, and dialyze to obtain a modified chitosan solution;

[0071] The preparation of the composite silica includes the following steps:

[0072] A. Mix 0.6 g of cetyltrimethylammonium bromide and 200 mL of deionized water as the aqueous phase, and mix 26.2 g of tetraethyl orthosilicate, 2.62 g of γ-glycidoxypropyltrimethoxysilane, and 2.92 g of methyl silicone oil as the oil phase. Add the oil phase to the aqueous phase under stirring conditions, stir for 18 min, use a homogenizing emulsifier to homogenize and emulsify in an ice water bath for 5 min, add 0.7 g of triethanolamine, and keep it at 20 °C for 23 h to obtain epoxy-modified hollow silica;

[0073] B. Mix 0.4 g of epoxy hollow silica and 140 mL of deionized water, stir ultrasonically for 15 min, add a mixture of 1.2 g of branched biguanide hydrochloride and 20 mL of deionized water, keep warm at 20 °C for 23 h, centrifuge, wash, and dry to obtain composite silica;

[0074] The preparation of the branched biguanide hydrochloride includes the following steps:

[0075] (1) Mix 6 g of 1-(o-tolyl)biguanide and 50 mL of absolute ethanol, adjust to neutral with dilute hydrochloric acid, rotary evaporate and dry to obtain 1-(o-tolyl)biguanide hydrochloride;

[0076] (2) Under a nitrogen atmosphere, mix 1.35 g of ethylenediamine and 50 mL of methanol, transfer to an ice-water bath, add 18.34 g of methyl acrylate, raise the temperature to 30 °C and keep warm for 23 h, rotary evaporate to obtain intermediate preparation A; Mix 0.51 g of intermediate preparation A, 1.35 g of ethylenediamine, and 25 mL of methanol, raise the temperature to 25 °C and keep warm for 23 h to obtain intermediate preparation B; Mix 0.51 g of intermediate preparation B, 18.34 g of methyl acrylate, and 25 mL of methanol, raise the temperature to 30 °C and keep warm for 23 h to obtain intermediate preparation C; Mix 0.51 g of intermediate preparation C, 1.35 g of ethylenediamine, and 50 mL of methanol, raise the temperature to 25 °C and keep warm for 23 h to obtain branched polyamide-amine;

[0077] (3) Under a nitrogen atmosphere, mix 5 g of 1-(o-tolyl)biguanide hydrochloride and 1 g of branched polyamide-amine, heat to melting, add 0.3 g of polyethylene glycol 400, raise the temperature to 160 °C and keep warm for 4 h, absorb the tail gas with 100 mL of dilute hydrochloric acid solution, cool down, and separate the liquid to obtain branched biguanide hydrochloride;

[0078] S4: Put the activated base fabric into the finishing solution, impregnate it to obtain a pretreated base fabric;

[0079] S5: Perform secondary plasma treatment on the pretreated base fabric, and dry it to obtain a double-yarn comfortable and wear-resistant denim fabric;

[0080] The working conditions of the secondary plasma treatment are: the working gas is argon, the power is 100 W, the discharge pressure is 220 Pa, and the treatment time is 50 s.

[0081] Example 3: The preparation process of a double-yarn comfortable and wear-resistant denim fabric includes the following steps:

[0082] S1: Twist, size and dye, thread through the heddles, and weave two single yarns to form a base fabric;

[0083] The single yarn is cotton yarn; the twist of the twisting is 2.5%;

[0084] The working conditions for sizing and dyeing are as follows: the sizing and dyeing vehicle speed is 20 m / min; the composition of the dyes used for sizing and dyeing is: using 1 L of deionized water as the solvent, which contains 35 g of environmentally friendly dyes and 0.8 g of penetrant;

[0085] S2: Perform a primary plasma treatment on the base fabric to obtain an activated base fabric;

[0086] The working conditions for the primary plasma treatment are: the working gas is argon, the power is 88 W, the discharge pressure is 220 Pa, and the treatment time is 25 s;

[0087] S3: Prepare a finishing solution with a modified chitosan solution and composite silica;

[0088] The mass ratio of the modified chitosan solution to composite silica in the finishing solution is 23:3;

[0089] The preparation of the modified chitosan solution includes the following steps:

[0090] 1) Mix 5 g of chitosan with 100 mL of an ice acetic acid solution with a mass fraction of 2%, add 3.2 g of sodium periodate, stir in the dark for 3 h, add 20 mL of 0.1 mol / L ethylene glycol solution, pour it into a dialysis bag and dialyze in deionized water for 3 d, freeze at -80 °C for 12 h, and dry to obtain dialdehyde chitosan;

[0091] 2) Mix 0.6 g of dialdehyde chitosan with 100 mL of deionized water, add a mixture of 3.6 g of branched biguanide hydrochloride and 100 mL of deionized water, and keep it warm at 25 °C for 7 h to obtain a branched chitosan solution;

[0092] 3) Heat 100 mL of the branched chitosan solution to 82 °C, adjust its pH to 10.1, add a mixture of 2 g of 2,3-epoxypropyltrimethylammonium chloride and 10 mL of deionized water, keep it warm at 82 °C for 5 h, adjust the pH to 3, cool, rotary evaporate, and dialyze to obtain a modified chitosan solution;

[0093] The preparation of the composite silica includes the following steps:

[0094] A. Mix 0.6 g of cetyltrimethylammonium bromide with 200 mL of deionized water as the aqueous phase, and mix 26.2 g of tetraethyl orthosilicate, 2.62 g of γ-glycidoxypropyltrimethoxysilane, and 2.92 g of methyl silicone oil as the oil phase. Under stirring conditions, add the oil phase to the aqueous phase, stir for 20 min, use a homogenizing emulsifier to homogenize and emulsify in an ice-water bath for 5 min, add 0.7 g of triethanolamine, and keep it warm at 25 °C for 22 h to obtain epoxidized hollow silica;

[0095] B. Mix 0.4 g of epoxidized hollow silica and 140 mL of deionized water, stir ultrasonically for 20 min, add a mixed solution of 1.2 g of branched biguanide hydrochloride and 20 mL of deionized water, keep warm at 25 °C for 22 h, centrifuge, wash, and dry to obtain composite silica;

[0096] The preparation of the branched biguanide hydrochloride includes the following steps:

[0097] (1) Mix 6 g of 1-(o-tolyl)biguanide and 50 mL of absolute ethanol, adjust to neutral with dilute hydrochloric acid, rotary evaporate and dry to obtain 1-(o-tolyl)biguanide hydrochloride;

[0098] (2) Under a nitrogen atmosphere, mix 1.35 g of ethylenediamine and 50 mL of methanol, transfer to an ice-water bath, add 18.34 g of methyl acrylate, raise the temperature to 32 °C and keep warm for 22 h, rotary evaporate to obtain intermediate preparation A; mix 0.51 g of intermediate preparation A, 1.35 g of ethylenediamine and 25 mL of methanol, raise the temperature to 27 °C and keep warm for 22 h to obtain intermediate preparation B; mix 0.51 g of intermediate preparation B, 18.34 g of methyl acrylate and 25 mL of methanol, raise the temperature to 32 °C and keep warm for 22 h to obtain intermediate preparation C; mix 0.51 g of intermediate preparation C, 1.35 g of ethylenediamine and 50 mL of methanol, raise the temperature to 27 °C and keep warm for 22 h to obtain branched polyamide-amine;

[0099] (3) Under a nitrogen atmosphere, mix 5 g of 1-(o-tolyl)biguanide hydrochloride and 1 g of branched polyamide-amine, raise the temperature to melting, add 0.3 g of polyethylene glycol 400, raise the temperature to 162 °C and keep warm for 3 h, absorb the tail gas with 100 mL of dilute hydrochloric acid solution, cool down, separate the liquid to obtain branched biguanide hydrochloride;

[0100] S4: Put the activated base fabric into the finishing solution, impregnate it to obtain a pretreated base fabric;

[0101] S5: Perform secondary plasma treatment on the pretreated base fabric, dry it to obtain a double-strand comfortable and wear-resistant denim fabric;

[0102] The working conditions of the secondary plasma treatment are: the working gas is argon, the power is 100 W, the discharge pressure is 220 Pa, and the treatment time is 50 s.

[0103] Comparative Example 1: Using Example 3 as a control group, replace the modified chitosan solution with a branched chitosan solution, and the other processes are normal.

[0104] Comparative Example 2: Using Example 3 as a control group, replace the composite silica with silica (S433678: Aladdin reagent), and the other processes are normal.

[0105] Comparative Example 3: Taking Example 3 as the control group, branched biguanide hydrochloride was not prepared, and other processes were normal.

[0106] In the examples and comparative examples, the thickness of the base fabric was 3 mm, and the thickness of the finishing protective layer formed by the finishing liquid on the base fabric was 15 μm.

[0107] Source of raw materials (only as a demonstration example):

[0108] Full cotton yarn (32 counts): Shantou Hongfa Color Yarn Textile Co., Ltd.; environmental protection dye (Lanasol Navy Blue 2R): Huntsman; penetrant SF (68131-39-5): Linyi Guoli Chemical Co., Ltd.; chitosan C434554, ethylene glycol E103319, cetyltrimethylammonium bromide H108983, tetraethyl orthosilicate T110593, γ-glycidoxypropyltrimethoxysilane G107576, methyl silicone oil S104750, triethanolamine T108151, 1-(o-tolyl)biguanide O159965, ethylenediamine E112132, methyl acrylate M100030, 2,3-epoxypropyltrimethylammonium chloride C120679, polyethylene glycol 400 P432449: Aladdin reagent; glacial acetic acid, NaOH solution, sodium periodate, absolute ethanol, hydrochloric acid, methanol, analytical pure: Sinopharm Group reagent.

[0109] Performance test: The fabrics in the examples and comparative examples were tested: Antibacterial persistence test: The test strains were Staphylococcus aureus ATCC6538 and Escherichia coli ATCC8739, and the oscillation method was used for testing, referring to GB / T20944.3-2008. The antibacterial property was tested after the test samples were washed 50 times in a household twin-tub washing machine; Abrasion resistance: The test was carried out referring to GB / T21196.2-2007. The size of the test sample was a circle with a diameter of 38 mm, the load was 9 KPa, and it was considered excellent if it did not break, deform, or twist after more than 25,000 times of friction (including 25,000 times); It was considered qualified if it did not break, deform, or twist after 20,000-25,000 times of friction; The obtained test results are shown in Table 1 below;

[0110] Table 1

[0111]

[0112]

[0113] The present invention provides a double-strand yarn comfortable and wear-resistant denim fabric and its preparation process. Through process and composition adjustment, a denim fabric with green environmental protection, good wear resistance, good antibacterial property, and high comfort is prepared.

[0114] Example 3 was compared with Comparative Example 1 and Comparative Example 3. To solve the water solubility problem of chitosan, chitosan was modified. Using chitosan as the substrate, it was selectively oxidized by sodium periodate to obtain dialdehyde chitosan. By using the Schiff base reaction of aldehyde group - amino group, a branched biguanide hydrochloride with good antibacterial property was grafted, thereby greatly improving the water solubility of chitosan. The branched biguanide hydrochloride was obtained by the thermal polycondensation reaction of 1-(o-tolyl)biguanide hydrochloride and branched polyamidoamine to obtain a structure with multiple active groups, thereby greatly improving the binding strength between the finishing solution and the fabric. The branched polyamidoamine was a multi-branched polyamidoamine prepared from ethylenediamine and methyl acrylate as raw materials; by using the multiple amino groups on the branched chitosan, quaternary ammonium groups were partially introduced, thereby enhancing the broad-spectrum antibacterial property of the modified chitosan solution and improving the bactericidal effect of the fabric.

[0115] Example 3 was compared with Comparative Example 2. Silicon dioxide was introduced as a filler in the finishing solution to improve the wear resistance of the fabric. To improve the uniformity of the dispersion of silicon dioxide in the finishing solution, epoxy hollow silica modified by γ-glycidoxypropyltrimethoxysilane was synthesized by the fine emulsion method, that is, epoxy hollow silica. By using the ring-opening reaction of amino group and epoxy group, branched biguanide hydrochloride was grafted onto the surface of epoxy hollow silica to obtain composite silica with good antibacterial property, good dispersibility and good binding strength with the fabric, improving the long-term antibacterial property of the fabric.

[0116] The above are only the embodiments of the present invention, and do not limit the patent scope of the present invention. All equivalent structural transformations made using the specification of the present invention under the inventive concept of the present invention, or direct / indirect applications in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. Preparation process of double - ply yarn comfortable and wear - resistant denim fabric, characterized in that, It includes the following steps: S1: Twisting, sizing and dyeing, threading the heddles, and weaving two single strands of yarn to form a base fabric; S2: Conducting a primary plasma treatment on the base fabric to obtain an activated base fabric; S3: Preparing a finishing solution with a modified chitosan solution and composite silica; S4: Placing the activated base fabric into the finishing solution for impregnation treatment to obtain a pretreated base fabric; S5: Conducting a secondary plasma treatment on the pretreated base fabric and drying it to obtain a comfortable and wear-resistant denim fabric made of double-strand yarn; The preparation of the modified chitosan solution includes the following steps: 1) Mix chitosan and an acetic acid solution, add sodium periodate, stir in the dark for 2 - 3 h, add an ethylene glycol solution, pour it into a dialysis bag and dialyze in deionized water for 3 d, freeze at -80 °C for 12 h, and dry to obtain dialdehyde chitosan; 2) Mix dialdehyde chitosan and deionized water, add a mixed solution of branched biguanide hydrochloride and deionized water, and keep it warm at 18 - 25 °C for 7 - 8 h to obtain a branched chitosan solution; 3) Heat the branched chitosan solution to 78 - 82 °C, adjust its pH to 9.9 - 10.1, add a mixed solution of 2,3-epoxypropyltrimethylammonium chloride and deionized water, keep it warm at 78 - 82 °C for 5 - 6 h, adjust the pH to 3, cool, rotary evaporate, and dialyze to obtain a modified chitosan solution; The preparation of the composite silica includes the following steps: A. Mix cetyltrimethylammonium bromide and deionized water as the aqueous phase, and mix tetraethyl orthosilicate, γ-glycidoxypropyltrimethoxysilane, and methyl silicone oil as the oil phase. Under stirring conditions, add the oil phase to the aqueous phase, stir for 15 - 20 min, use a homogenizing emulsifier to homogenize and emulsify in an ice-water bath for 5 min, add triethanolamine, and keep it warm at 18 - 25 °C for 22 - 24 h to obtain epoxidized hollow silica; B. Mix epoxidized hollow silica and deionized water, stir ultrasonically for 10 - 20 min, add a mixed solution of branched biguanide hydrochloride and deionized water, keep it warm at 18 - 25 °C for 22 - 24 h, centrifuge, wash, and dry to obtain composite silica; The preparation of the branched biguanide hydrochloride includes the following steps: (1) Mix 1-(o-tolyl)biguanide and absolute ethanol, adjust it to neutral with dilute hydrochloric acid, rotary evaporate and dry to obtain 1-(o-tolyl)biguanide hydrochloride; (2) Under a nitrogen atmosphere, mix ethylenediamine and methanol, transfer it to an ice-water bath, add methyl acrylate, heat up to 28 - 32 °C and keep it warm for 22 - 24 h, rotary evaporate to obtain intermediate preparation A; Mix intermediate preparation A, ethylenediamine, and methanol, heat up to 23 - 27 °C and keep it warm for 22 - 24 h to obtain intermediate preparation B; Mix intermediate preparation B, methyl acrylate, and methanol, heat up to 28 - 32 °C and keep it warm for 22 - 24 h to obtain intermediate preparation C; Mix intermediate preparation C, ethylenediamine, and methanol, heat up to 23 - 27 °C and keep it warm for 22 - 24 h to obtain branched polyamide-amine; (3) Under a nitrogen atmosphere, 1-(o-tolyl)biguanide hydrochloride and branched polyamide-amine are mixed and heated to melting. Then polyethylene glycol is added, and the temperature is raised to 158 - 162 °C for heat preservation for 3 - 5 h. The tail gas is absorbed by a dilute hydrochloric acid solution, and after cooling, liquid separation is carried out to obtain branched biguanide hydrochloride.

2. The preparation process of the double-strand yarn comfortable and wear-resistant denim fabric according to claim 1, characterized in that, The single-strand yarn is one of bamboo charcoal yarn, wool yarn, polyester yarn, spandex yarn, nylon yarn, and cotton yarn; the twist of the ply yarn is 2.5%.

3. The preparation process of the double-strand yarn comfortable and wear-resistant denim fabric according to claim 1, characterized in that, The working conditions for sizing and dyeing are: the sizing and dyeing vehicle speed is 20 m / min; the composition of the dye used for sizing and dyeing is: using 1 L of deionized water as the solvent, which contains 25 - 35 g of environmentally friendly dye and 0.7 - 0.8 g of penetrant.

4. The preparation process of the double-strand yarn comfortable and wear-resistant denim fabric according to claim 1, characterized in that, The working conditions for the primary plasma treatment are: the working gas is argon, the power is 88 W, the discharge pressure is 220 Pa, and the treatment time is 25 s; the working conditions for the secondary plasma treatment are: the working gas is argon, the power is 100 W, the discharge pressure is 220 Pa, and the treatment time is 50 s.

5. The preparation process of the double-strand yarn comfortable and wear-resistant denim fabric according to claim 1, characterized in that, In the finishing solution, the mass ratio of the modified chitosan solution to the composite silica is 23:(1 - 3).

6. The preparation process of the double - strand yarn comfortable and wear - resistant denim fabric according to claim 1, characterized in that, In the preparation of the composite silica, the mass ratio of the epoxidized hollow silica to the branched biguanide hydrochloride is 1:

3.

7. Comfortable and wear-resistant denim fabric made of double-stranded yarn, characterized in that, Prepared by the preparation process of any one of claims 1 - 6.

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