Color fixing agent and finishing agent for real silk fabric as well as preparation method and application of color fixing agent and finishing agent

Abstract

The invention relates to a color fixing agent for a real silk fabric, a finishing agent and a preparation method and application of the color fixing agent for the real silk fabric. The color fixing agent for the real silk fabric is a hydroformylated chitosan-TiO2 chelate, and active groups and film-forming property of hydroformylated chitosan are utilized; according to the acid dye provided by the invention, the water washing color fastness and the soaping-resistant color fastness of a real silk fabric dyed by the acid dye are remarkably improved, the anti-ultraviolet performance of the chelated titanium dioxide is utilized, the sun-proof and light-resistant color fastness of a product is improved, and the hydroformylated chitosan part also provides an antibacterial effect, so that the real silk fabric has antibacterial property, and the color fastness of the real silk fabric to the soaping-resistant color fastness is improved. Meanwhile, certain help is also provided for the wrinkle resistance of the real silk fabric.

Description

Technical Field

[0001] The invention belongs to the technical field of textile fabric finishing, and particularly relates to a color fixing agent and a finishing agent for silk fabrics, as well as a preparation method and application thereof. Background Art

[0002] Silk, one of humanity's earliest textiles, consists primarily of protein filaments. Pure silk, crafted from silk, is a premium fabric renowned for its softness, lustre, and comfort. Its unparalleled comfort and luxurious appearance make it a treasure among textiles.

[0003] In recent years, traditional clothing has gradually taken over the Chinese apparel market, and demand for silk fabrics has been growing. However, the difficulty of caring for silk fabrics in daily life still deters many consumers. Dyed silk products require extreme care during use, washing, drying, and storage, and require high maintenance requirements. Even with careful care, silk products are prone to fading, graying, and aging after washing and sun exposure. This reduces the practicality of the products consumers have paid high prices for, hindering the promotion and application of silk products.

[0004] Silk fabrics easily fade and wrinkle after washing, affecting their appearance. This is primarily due to poor color fastness, particularly wash fastness and light fastness, as well as poor wet elasticity. The silk dyeing process is a complex one. Textile fibers and dyes are combined physically, chemically, and chemically, completing the dyeing process through three stages: adsorption, diffusion, and fixation. As a protein fabric, silk is commonly dyed with either acid or reactive dyes. While acid dyes produce vibrant colors, they exhibit lower wash fastness. Reactive dyes produce colors that are not as vibrant as acid dyes, and while their color fastness is slightly higher, they are still unsatisfactory. Color fastness is a comprehensive indicator encompassing multiple factors, including wash fastness, soap fastness, and light fastness. Some researchers have used polyurethane compounds to finish silk fabrics, but this has had limited effects on color fastness and has negatively impacted the fabric's feel.

[0005] Silk products are coveted by consumers for their bright colors, soft skin-friendly feel, and gorgeous and noble temperament. However, shortcomings such as easy fading, easy wrinkling, short wear time, and low cost-effectiveness have reduced the consumer market for silk products. Due to the small consumer market, few scientific research institutions have conducted research on modifying the properties of silk fabrics. For many years, there have been no reports on technical research to improve the performance of silk, especially the color fastness, and to keep silk fabrics long-lasting and bright.

[0006] Therefore, developing color fixing agents and finishing agents for silk fabrics to improve the durability of the performance of silk fabrics through post-finishing, especially improving the various color fastness levels of silk fabrics, will greatly increase the scope of use of silk fabrics and lay the foundation for the market promotion of silk fabrics. Summary of the Invention

[0007] The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a color fixing agent for silk fabrics and a preparation method thereof. The present invention also provides a finishing agent containing the color fixing agent. The quality of silk products treated with the finishing agent is significantly improved, especially the color fastness grades of various products are significantly improved.

[0008] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows:

[0009] A first aspect of the present invention provides a color-fixing agent for silk fabrics, wherein the color-fixing agent is a chelate of hydroformylated chitosan and nano-titanium dioxide.

[0010] According to some specific embodiments, the relative molecular mass of the hydroformylated chitosan is 20,000 to 30,000, and the nano-titanium dioxide is rutile.

[0011] According to some specific embodiments, the color fixing agent is obtained by reacting hydroformylation chitosan powder and nano-titanium dioxide in an acidic aqueous solution.

[0012] Furthermore, the mass ratio of the hydroformylated chitosan powder to the nano-titanium dioxide is 1:0.3-0.6, for example, 1:0.3, 1:0.35, 1:0.4, 1:0.45, 1:0.5, 1:0.55, 1:0.6.

[0013] Furthermore, the particle size of the hydroformylated chitosan powder is 80-100 mesh, such as 80 mesh, 90 mesh, or 100 mesh.

[0014] Furthermore, the reaction temperature is 40-60°C, for example, 40°C, 41°C, 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C, 49°C, 50°C, 51°C, 52°C, 53°C, 54°C, 55°C, 56°C, 57°C, 58°C, 59°C, and 60°C.

[0015] The second aspect of the present invention provides a method for preparing the above-mentioned color fixing agent, which comprises reacting hydroformylation chitosan powder and nano-titanium dioxide in the presence of acetic acid and water at 40-60°C. After the reaction is completed, the color fixing agent is obtained by neutralization, filtration, alcohol washing and drying.

[0016] According to some specific embodiments, the mass ratio of the hydroformylated chitosan powder, nano-titanium dioxide, acetic acid and water is 1:0.5-0.6:0.4-0.5:5-6.

[0017] Furthermore, the mass ratio of the hydroformylated chitosan powder, nano-titanium dioxide, acetic acid and water is 1:0.5-0.55:0.4-0.5:5-5.5.

[0018] Furthermore, the reaction time is 20 to 30 hours, for example, 20 hours, 21 hours, 22 hours, 23 hours, 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, or 30 hours.

[0019] Furthermore, the neutralization adopts a sodium hydroxide solution. The mass concentration of the sodium hydroxide solution is 10% to 30%, for example, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%.

[0020] Furthermore, the alcohol washing adopts ethanol.

[0021] Furthermore, the alcohol washing is performed 2 to 4 times.

[0022] Furthermore, the drying is performed by vacuum drying at 50-70°C, more preferably by vacuum drying at 50-60°C.

[0023] According to some specific embodiments, the preparation method of the color fixing agent is specifically as follows: hydroformylation chitosan powder, acetic acid, and nano-titanium dioxide are mixed in proportion, stirred evenly, and reacted at 40-60°C while stirring for 20-30 hours, then heating is stopped, and after cooling to room temperature, sodium hydroxide solution is added dropwise to the reaction solution until the solution is neutral, the solution is added dropwise while stirring, filtered, and the precipitate is collected, washed with ethanol 2-4 times, and vacuum dried to obtain hydroformylation chitosan-TiO2 chelate, which is the color fixing agent.

[0024] According to some specific embodiments, the preparation method of the hydroformylation chitosan powder is as follows: chitosan, dichromate, sulfuric acid and water are mixed and reacted at 70-80°C, for example, at 70°C, 71°C, 72°C, 73°C, 74°C, 75°C, 76°C, 77°C, 78°C, 79°C or 80°C. After the reaction is completed, the fraction is collected by distillation, and the fraction is dried and ground to obtain the hydroformylation chitosan powder. The mass ratio of the chitosan, dichromate, sulfuric acid and water is 1:2-2.5:0.3-0.4:4-6.

[0025] Furthermore, the mass ratio of the chitosan, dichromate, sulfuric acid and water is 1:2-2.2:0.3-0.35:4-5.

[0026] Furthermore, the chitosan has a deacetylation degree greater than 95%, a relative molecular mass of 20,000 to 30,000, and a particle size of 80 meshes.

[0027] Furthermore, the dichromate includes but is not limited to potassium dichromate and sodium dichromate.

[0028] According to some specific embodiments, the preparation method of the hydroformylation chitosan powder is specifically as follows: chitosan, potassium dichromate, sulfuric acid, and water are mixed in proportion, stirred evenly, and reacted at 70-80°C while stirring for 3-5 hours, heated and distilled, and the fractions are collected to obtain hydroformylation chitosan, and the hydroformylation chitosan is dried in an oven at 70-80°C for 1-2 hours and then ground into 80-100 mesh.

[0029] A third aspect of the present invention provides a finishing agent for silk fabrics, the finishing agent comprising the above-mentioned color fixing agent, water, and one or more of a thickener, a penetrant, a bulking agent, and an anti-wrinkle softener.

[0030] According to some specific embodiments, the thickener is sodium alginate with a viscosity of 450 to 550 mPa·s.

[0031] According to some specific embodiments, the finishing agent includes the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softening agent and water, and the mass ratio of the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softening agent and water is 1:0.4~0.5:0.2~0.3:0.3~0.4:0.3~0.4:4~6.

[0032] Furthermore, the mass ratio of the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water is 1:0.4-0.5:0.2-0.25:0.3-0.35:0.3-0.4:4-6.

[0033] Furthermore, the mass ratio of the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water is 1:0.4-0.5:0.2-0.25:0.3-0.35:0.3-0.4:4-5.

[0034] A fourth aspect of the present invention provides a post-treatment method for silk fabrics, comprising padding the silk fabrics with the finishing agent.

[0035] Furthermore, the padding treatment is one-dipping-one-padding or two-dipping-two-padding.

[0036] According to some specific embodiments, the post-finishing method is specifically as follows: adding the finishing agent into the immersion pressing tank, adding the silk fabric into the immersion pressing tank and fully contacting and impregnating it with the finishing agent, then rolling it with a uniform pressing roller until the moisture content is 30% to 40%, and then drying it at 120 to 130°C.

[0037] Due to the adoption of the above technical solution, the present invention has the following advantages compared with the prior art:

[0038] The color fixing agent for silk fabrics of the present invention is a hydroformylated chitosan-TiO2 chelate. Utilizing the active groups and film-forming properties of the hydroformylated chitosan, the color fastness to washing and soaping of the silk fabric dyed with acid dyes is significantly improved. Simultaneously, the anti-ultraviolet properties of the chelated titanium dioxide are utilized to improve the product's sun protection and light fastness. Furthermore, the hydroformylated chitosan portion also provides an antibacterial effect, which also contributes to wrinkle resistance. Furthermore, the color fixing agent of the present invention is combined with a finishing agent consisting of a thickener, a penetrant, a bulking agent, an anti-wrinkle softener, and water. This can improve the color fastness and antibacterial properties of the silk fabric while also improving the wrinkle resistance and self-cleaning ability of the silk fabric. This significantly improves the quality and durability of the silk fabric, greatly expanding the scope of use and performance durability of the silk fabric, and laying a foundation for the market promotion of the silk fabric. DETAILED DESCRIPTION

[0039] In order to solve the problem of low color fastness of silk fabric dyeing, the applicant has developed a color fixing agent for silk fabric after extensive research and experimental design. The color fixing agent is obtained by reacting hydroformylation chitosan powder and nano-titanium dioxide in an acidic aqueous solution, namely, hydroformylation chitosan-TiO2 chelate.

[0040] Chitosan, whose structural formula is Chitosan's macromolecular chains are rich in hydroxyl, amino, and acetyl groups, which form various intramolecular and intermolecular hydrogen bonds. These hydrogen bonds firmly bond the dye to the fabric, improving the color fastness of the dyed fabric. Mixtures of macromolecular chitosan and enols possess strong film-forming properties, high biocompatibility, and excellent breathability. They do not adversely affect the fabric's feel or wearing quality, making them an excellent substrate for improving fabric properties, such as color fastness, elasticity, hot water shrinkage, and antistatic properties.

[0041] The hydroxyl group attached to C5 in chitosan is a primary alcohol group and is most susceptible to oxidation. By controlling the reaction conditions, the hydroxyl group attached to C5 can be oxidized to an aldehyde group. Under acidic conditions, the amino group in the aldehyde molecule can react with the hydroxyl groups in the dye and the hydroxyl groups on the surface of the silk fabric, forming crosslinks and improving the color fastness of the product after dyeing. Chitosan's antibacterial and wrinkle-resistant properties can also improve product quality.

[0042] The pre-modified chitosan is added to a strongly acidic sodium dichromate aqueous solution, heated at a certain temperature, and distilled to obtain a distillation product, namely, modified chitosan, i.e., hydroformyl chitosan. The reaction equation is as follows:

[0043]

[0044] In the field of textiles, nano-TiO2 has attracted much attention due to its advantages such as low price and non-toxicity, small particle size, large specific surface area, strong magnetism, high catalytic activity, good absorption performance, strong ability to absorb ultraviolet rays, large surface activity, good thermal conductivity, good dispersibility and good stability. It mainly has the main advantages of anti-ultraviolet, antibacterial, antistatic, matte, anti-aging, self-cleaning and heat insulation in textiles. The anti-ultraviolet performance of rutile nano-TiO2 is the best. However, nano-TiO2 is difficult to be firmly fixed on the fabric, and especially washing very easily causes the nano-TiO2 on the fabric to fall off. Among the present invention, hydroformylation chitosan is a branched structure. Rutile nano-titanium dioxide is added to hydroformylation chitosan. Most of the amino groups in the macromolecular chitosan are distributed, which are the amino groups connected on the C2 of each monomer. The amino groups on different monomers are intertwined, and under acidic conditions, these amino groups can chelate with nano-TiO2. Titanium dioxide has anti-UV and sun protection properties. After the hydroformylation chitosan chelates titanium dioxide, the presence of titanium dioxide produces anti-UV properties. The improvement of anti-UV properties can reduce the damage of sunlight to fibers and colors, and further improve the anti-sunlight color fastness of silk fabrics.

[0045] The hydroformylation chitosan-TiO2 chelate is mixed with other additives in a certain proportion to form a finishing agent, which is used for the finishing of silk fabrics. It can improve the color fastness of silk fabrics, prevent the color of textile silk fabrics from being damaged and aging after wearing and washing, and make the clothing lose its beauty. It can also improve the wrinkle resistance of silk fabrics. The bioaffinity of the curing agent also makes slight wrinkles easier to recover, making it more suitable for daily wear. It can also improve antibacterial and self-cleaning abilities, etc., greatly increasing the scope of use of silk fabrics and the durability of their performance.

[0046] The technical solution of the present invention is further illustrated below with reference to specific embodiments and comparative examples.

[0047] In the present invention, it should be noted that, unless otherwise specified or contradicted by the context, the terms or expressions used herein should be read in conjunction with the entire content of this document and as understood by those of ordinary skill in the art. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art.

[0048] The technical solutions of the present invention are further described below in conjunction with specific embodiments, but the present invention is not limited to the following embodiments.

[0049] The sources of some of the raw materials and special chemical additives involved in the following examples and comparative examples are as follows:

[0050] Chitosan: water-soluble chitosan with a deacetylation degree of >95%, a relative molecular mass of 20,000 to 30,000, and a particle size of 80 mesh, produced by Qingdao Hehai Bioengineering Co., Ltd.

[0051] Nano-titanium dioxide: rutile nano-titanium dioxide powder from Zhejiang Zhiti Nano Micro New Materials Co., Ltd., CAS number: 13463-67-7.

[0052] Thickener: 30-mesh sodium alginate with a viscosity of 500 mPa·s from Lianyungang Huanyu Seaweed Additive Co., Ltd.

[0053] Penetrant: TY-20A penetrant from Dongguan Taiyang New Material Technology Co., Ltd.

[0054] Bulking agent: T60 fluffy weak cationic film produced by Dongguan Huihu Textile Auxiliary Co., Ltd.

[0055] Anti-wrinkle softener: Dow Corning OFX-8417 softener.

[0056] Anti-ultraviolet finishing agent: Anti-ultraviolet finishing agent HTUV100 type produced by Shanghai Hutt Chemical Co., Ltd.

[0057] Antimicrobial agent: Beijing Chonggao Nanotechnology Co., Ltd. CAG-A1 type antibacterial agent.

[0058] Commercially available fixing agent: Acid dye fixing agent AFX-3 produced by Hangzhou Yizhou Textile Auxiliary Co., Ltd.

[0059] Test sample fabric: width 1.4 meters, 120g / m 2 Heavy-spun, acid-dyed green silk.

[0060] The conditions used in the following examples and comparative examples can be further adjusted according to specific requirements. The conditions not specified are generally those used in routine experiments. Unless otherwise specified, the instruments, raw materials, and reagents can be obtained from commercial sources or prepared by existing methods.

[0061] The room temperature in the following examples and comparative examples refers to 25±5°C.

[0062] Example 1

[0063] Chitosan, potassium dichromate, sulfuric acid and water were mixed in a mass ratio of 1:2:0.3:4, stirred evenly, and reacted at 70-80°C with stirring for 3 hours, heated and distilled, and the fractions were collected to obtain hydroformylation chitosan. The hydroformylation chitosan was dried in an oven at 80°C for 1 hour and then ground into 100 mesh for later use.

[0064] The prepared hydroformylation chitosan powder, acetic acid, nano-titanium dioxide and water were mixed in a mass ratio of 1:0.5:0.4:5, stirred evenly, and reacted at 40-60°C with stirring for 25 hours. Then, heating was stopped, and after cooling to room temperature, sodium hydroxide solution was added dropwise to the reaction solution until the solution was neutral. The mixture was added dropwise with stirring, filtered, and the precipitate was collected. It was washed with ethanol three times and vacuum dried to obtain hydroformylation chitosan-TiO2 chelate, which was the color fixing agent.

[0065] The hydroformylation chitosan-TiO2 chelate color fixing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water are uniformly mixed in a mass ratio of 1:0.4:0.2:0.3:0.3:5 to obtain a finishing agent.

[0066] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller until the moisture content is 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 1#, and tested according to the test standards.

[0067] Example 2

[0068] Chitosan, potassium dichromate, sulfuric acid and water were mixed in a mass ratio of 1:2.1:0.33:4.5, stirred evenly, and reacted at 70-80°C with stirring for 5 hours. The mixture was heated for distillation and the fractions were collected to obtain hydroformylation chitosan. The hydroformylation chitosan was dried in an oven at 80°C for 1 hour and then ground into 100 mesh for later use.

[0069] The prepared hydroformylation chitosan powder, acetic acid, nano-titanium dioxide and water were mixed in a mass ratio of 1:0.52:0.45:5.2, stirred evenly, and reacted at 40-60°C with stirring for 20 hours. Then, heating was stopped, and after cooling to room temperature, sodium hydroxide solution was added dropwise to the reaction solution until the solution was neutral. The mixture was added dropwise with stirring, filtered, and the precipitate was collected. It was washed with ethanol three times and vacuum dried to obtain hydroformylation chitosan-TiO2 chelate, which was the color fixing agent.

[0070] The hydroformylation chitosan-TiO2 chelate color fixing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water are uniformly mixed in a mass ratio of 1:0.45:0.23:0.32:0.35:5.5 to obtain a finishing agent.

[0071] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller to a moisture content of 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 2#, and tested according to the test standards.

[0072] Example 3

[0073] Chitosan, potassium dichromate, sulfuric acid and water were mixed in a mass ratio of 1:2.2:0.35:5, stirred evenly, and reacted at 70-80°C with stirring for 4 hours. The mixture was heated for distillation and the fractions were collected to obtain hydroformylation chitosan. The hydroformylation chitosan was dried in an oven at 80°C for 1 hour and then ground into 80 mesh for later use.

[0074] The prepared hydroformylation chitosan powder, acetic acid, nano-titanium dioxide and water were mixed in a mass ratio of 1:0.55:0.5:5.5, stirred evenly, and reacted at 40-60°C with stirring for 30 hours. Then, heating was stopped, and after cooling to room temperature, sodium hydroxide solution was added dropwise to the reaction solution until the solution was neutral. The mixture was added dropwise with stirring, filtered, and the precipitate was collected. It was washed with ethanol three times and vacuum dried to obtain hydroformylation chitosan-TiO2 chelate, which was the color fixing agent.

[0075] The hydroformylation chitosan-TiO2 chelate color fixing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water are uniformly mixed in a mass ratio of 1:0.5:0.25:0.35:0.4:6 to obtain a finishing agent.

[0076] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller until the moisture content is 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 3#, and tested according to the test standards.

[0077] Example 4

[0078] Chitosan, potassium dichromate, sulfuric acid and water were mixed in a mass ratio of 1:2.2:0.35:5, stirred evenly, and reacted at 70-80°C with stirring for 4 hours. The mixture was heated for distillation and the fractions were collected to obtain hydroformylation chitosan. The hydroformylation chitosan was dried in an oven at 80°C for 1 hour and then ground into 80 mesh for later use.

[0079] The prepared hydroformylation chitosan powder, acetic acid, nano-titanium dioxide and water were mixed in a mass ratio of 1:0.55:0.5:5.5, stirred evenly, and reacted at 40-60°C with stirring for 30 hours. Then, heating was stopped, and after cooling to room temperature, sodium hydroxide solution was added dropwise to the reaction solution until the solution was neutral. The mixture was added dropwise with stirring, filtered, and the precipitate was collected. It was washed with ethanol three times and vacuum dried to obtain hydroformylation chitosan-TiO2 chelate, which was the color fixing agent.

[0080] The hydroformylation chitosan-TiO2 chelate color fixing agent, thickener, penetrant, bulking agent, anti-wrinkle softener and water are uniformly mixed in a mass ratio of 1:0.5:0.25:0.35:0.4:5 to obtain a finishing agent.

[0081] Add the finishing agent into the dipping tank, add the sample cloth into the dipping tank and fully contact and immerse it with the finishing agent, then press it with a uniform pressing roller until the moisture content reaches 30%, and then dry it at 120-130℃ to obtain the finished product. Wash the finished product 3 times to obtain sample 4#, and test it according to the test standards.

[0082] Comparative Example 1

[0083] The untreated chitosan raw material, the untreated TiO2 raw material, the thickener, the penetrant, the bulking agent, the anti-wrinkle softener and water are uniformly mixed in a mass ratio of 1:0.5:0.5:0.25:0.35:0.4:6 to obtain a finishing agent.

[0084] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller to a moisture content of 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 5#, and tested according to the test standards.

[0085] Comparative Example 2

[0086] The commercially available color fixing agent, thickener, penetrant, bulking agent, anti-wrinkle softener, UV protection finishing agent, antibacterial agent and water are uniformly mixed in a mass ratio of 1:0.5:0.25:0.35:0.4:0.5:0.5:6 to obtain a finishing agent.

[0087] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller to a moisture content of 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 6#, and tested according to the test standards.

[0088] Comparative Example 3

[0089] The thickener, penetrant, bulking agent, anti-wrinkle softener, UV protection finishing agent, antibacterial agent and water are uniformly mixed in a mass ratio of 1:0.5:0.7:0.8:0.5:0.5:12 to obtain a finishing agent.

[0090] The finishing agent is added to the dipping tank, and the sample cloth is added to the dipping tank to fully contact and immerse with the finishing agent, and then pressed by a uniform pressing roller until the moisture content is 30%, and then dried at 120-130 ° C to obtain the finished product. The finished product is washed 3 times to obtain sample 7#, and tested according to the test standards.

[0091] The performance test results of the samples of the above embodiments and comparative examples are shown in Table 1.

[0092] Table 1

[0093] Sample number 1# 2# 3# 4# 5# 6# 7# Color fastness to washing (grade) 4.5 4.5 4.5 4.5 2 3 2 Color fastness to soap washing (grade) 4 4.5 4.5 4.5 2 3 2 Color fastness to light (grade) 4 4 4.5 4.5 2 2 2 Wrinkle resistance (grade) 3 3 4 5 2 3 3 Antibacterial effect have have have have none have have

[0094] The performance test methods in Table 1 are as follows:

[0095] The washing color fastness test is in accordance with the national standard GB / T 5713-2013-2014.

[0096] The color fastness to soaping test is in accordance with the national standard GB / T 3921-2008.

[0097] The color fastness to light test is in accordance with the national standard GB / T 8427-2008.

[0098] Wrinkle resistance testing is carried out in accordance with industry standard GB / T 29257-2012.

[0099] The antibacterial test was carried out according to the national standard GB / T 20944.3-2008 oscillation method.

[0100] Table 1 shows that compared with samples 5# to 7#, samples 1# to 4# have significantly improved performance in many aspects. The hydroformylated chitosan-TiO2 chelate color fixing agent used in Examples 1 to 4 can utilize the active groups and film-forming properties of hydroformylated chitosan to improve the color fastness to washing and soaping of silk fabrics dyed with acid dyes from level 2 to level 4 to 4.5. At the same time, the anti-ultraviolet properties of chelated titanium dioxide are utilized to improve the product's sun protection and sunlight fastness. At the same time, the hydroformylated chitosan portion also provides an antibacterial effect. In combination with the finishing agent composed of a thickener, penetrant, bulking agent, anti-wrinkle softener, and water, the wrinkle resistance and self-cleaning ability of the silk fabric are improved, thereby significantly improving the quality and durability of the silk fabric.

[0101] The above detailed description of the present invention is intended to enable those skilled in the art to understand the contents of the present invention and implement them, but it does not limit the scope of protection of the present invention. The present invention is not limited to the above embodiments. Any equivalent changes or modifications made based on the spirit of the present invention should be included in the scope of protection of the present invention.

Claims

1. A color fixing agent for silk fabrics, characterized in that: The color fixing agent is a chelate of hydroformylation chitosan and nano titanium dioxide.

2. The color fixing agent according to claim 1, characterized in that The relative molecular mass of the hydroformylation chitosan is 20,000-30,000, and the nano titanium dioxide is rutile.

3. The color fixing agent according to claim 2, characterized in that The color fixing agent is obtained by reacting hydroformylation chitosan powder and nano titanium dioxide in an acidic aqueous solution.

4. The color fixing agent according to claim 2, characterized in that The mass ratio of the hydroformylated chitosan powder to the nano-titanium dioxide is 1:0.3-0.6; and / or, the particle size of the hydroformylated chitosan powder is 80-100 mesh; And / or, the acidic aqueous solution is acetic acid solution.

5. The method for preparing a color fixing agent according to any one of claims 1 to 4, characterized in that: The hydroformylation chitosan powder and nano titanium dioxide are reacted in the presence of acetic acid and water at 40-60 DEG C. After the reaction is completed, the color fixing agent is obtained by neutralization, filtration, alcohol washing and drying.

6. The method for preparing a color fixing agent according to claim 5, characterized in that: The mass ratio of the hydroformylated chitosan powder, nano-titanium dioxide, acetic acid and water is 1:0.5-0.6:0.4-0.5:5-6; And / or, the reaction time is 20 to 30 hours; And / or, the neutralization adopts sodium hydroxide solution; And / or, the alcohol washing adopts ethanol.

7. The method for preparing a color fixing agent according to claim 5, characterized in that: The preparation method of the hydroformylation chitosan powder comprises the following steps: mixing chitosan, dichromate, sulfuric acid and water, reacting the mixture at 70-80°C, collecting the fraction by distillation after the reaction, drying and grinding the fraction to obtain the hydroformylation chitosan powder, wherein the mass ratio of the chitosan, dichromate, sulfuric acid and water is 1:2-2.5:0.3-0.4:4-6.

8. A finishing agent for silk fabrics, characterized in that: The finishing agent comprises the color fixing agent according to any one of claims 1 to 4 and water, and further comprises one or more of a thickener, a penetrant, a bulking agent, and an anti-wrinkle softener.

9. The finishing agent according to claim 8, characterized in that The finishing agent comprises the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softening agent and water, and the mass ratio of the curing agent, thickener, penetrant, bulking agent, anti-wrinkle softening agent and water is 1:0.4-0.5:0.2-0.3:0.3-0.4:0.3-0.4:4-6.

10. A finishing method for silk fabric, characterized in that: The silk fabric is subjected to padding treatment using the finishing agent according to claim 8 or 9.

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