Blended wool fabric containing soybean fibers and production process thereof

Abstract

The invention discloses a soybean fiber-containing blended wool fabric and a production process thereof, and the production process specifically comprises the following steps: blending modified soybean fibers and modified wool fibers to prepare blended yarns, and carrying out plain weaving on the blended yarns to obtain a modified soybean fiber blended wool fabric, the modified soybean fiber blended wool fabric is subjected to two-dipping and two-rolling process finishing with a modified titanium oxide antibacterial agent, and the antibacterial modified soybean fiber blended wool fabric is obtained; according to the invention, soybean fibers are modified by adding a reinforcing modification solution, wool fibers are finished by using a protease base solution prepared by a co-bath cross-linking method, and a modified nano titanium oxide antibacterial agent is added into soybean and wool blended fibers, so that the shrink resistance, tensile wear resistance and antibacterial performance of the blended fabric are further improved; the service life of the blend fiber fabric is prolonged.

Description

Technical Field

[0001] The present invention relates to the technical field of blended fabrics, and particularly relates to a blended wool fabric containing soybean fiber and its production process. Background Art

[0002] A blended wool fabric containing soybean fiber is a composite fabric made by combining soybean fiber and wool fiber through textile processes. As a natural and environmentally friendly material, soybean fiber has excellent comfort, moisture absorption and breathability, and biodegradability, and is widely used in daily clothing, household fabrics, and functional textiles. Wool fiber itself has good warmth retention and softness. Blending soybean fiber with wool fiber can make the fabric maintain excellent warmth retention performance of wool while increasing breathability, moisture absorption and sweat discharge performance, and higher comfort, making it an ideal functional fabric, which is widely used in high-end clothing, underwear, sportswear, and household products and other fields.

[0003] However, soybean fiber itself has low strength, is more prone to stretching and damage especially in a humid environment, has poor abrasion resistance, is easy to pill or wear, resulting in a decline in the stability of antibacterial performance. In addition, wool fiber is prone to shrinkage during use. Due to its oriented structure, it will entangle with each other when subjected to external forces, forming an irreversible felting phenomenon, making the stability of soybean-wool blended fabrics poor, especially prone to changes in size and shape. The unique scale layer structure on the surface of wool makes its functionalization treatment difficult, which limits the performance of soybean-wool blended fibers in some high-performance applications. Therefore, soybean-wool blended fibers face certain challenges in terms of shrinkage resistance, tensile resistance, abrasion resistance, and antibacterial performance of the fabric. Summary of the Invention

[0004] The purpose of the present invention is to provide a blended wool fabric containing soybean fiber and its production process, which is used to solve the technical problems that the anti-felting, tensile strength, and antibacterial performance of the existing soybean-wool blended fabric need to be improved.

[0005] The purpose of the present invention can be achieved by the following technical solutions: A production process of a blended wool fabric containing soybean fiber, comprising the following steps:

[0006] S1. Add pretreated wool fiber and 2 g / L dopamine protease-based solution to a reaction kettle and stir for 4 - 5 h, and then perform post-treatment to obtain modified wool fiber;

[0007] The reaction mechanism of the modified wool fiber is:

[0008] Dopamine molecules have an amino group (-NH2) and a phenolic hydroxyl group (-OH). Under alkaline conditions, a self-polymerization reaction occurs first to form a polydopamine film. These polydopamine molecules have an affinity interaction with the amino group or other active groups on the surface of wool fibers through the phenolic hydroxyl group, forming a strong chemical bond. Serine protease can carry out a specific hydrolysis reaction with the protein molecules in wool fibers, acting on the keratin in wool. During the protein hydrolysis process, protease forms more amino or carboxyl groups by breaking peptide chains, providing more reaction sites for subsequent reactions. Through the dopamine polymer and the more active groups generated under the action of serine protease, a cross-linking reaction occurs. After dopamine binds to the wool surface, the formed polydopamine film forms a protective film on the wool surface.

[0009] S2. Add the pretreated soybean fiber, reinforcing and modifying liquid, and ammonium persulfate into the reaction kettle and stir for 2 - 3 h, then perform post-treatment to obtain the modified soybean fiber;

[0010] The reaction mechanism of the modified soybean fiber is as follows:

[0011] The surface of soybean fiber usually has active groups such as hydroxyl groups (-OH) and amino groups (-NH2). These groups can react with the silanol groups generated by the hydrolyzed tetraethoxysilane. The silane molecules form Si - O - C bonds or Si - O - Si bonds through reaction with the functional groups on the fiber surface. The epoxy groups in epoxidized soybean oil react with the silanol groups (Si - OH) to form Si - O - C bonds, connecting the silane molecules and soybean oil molecules, enabling tetraethoxysilane to effectively enhance the binding force between soybean oil and soybean fiber. At the same time, the silanol groups further undergo a condensation reaction to form Si - O - Si bonds, forming a cross-linked network of silicon oxygen silicon. This cross-linking reaction increases the cross-linking density of soybean fiber, making the silane molecules firmly adhere to the surface of soybean fiber.

[0012] S3. Blended-spin the modified soybean fiber and the modified wool fiber to prepare a blended yarn, and then perform plain weaving on it to obtain a modified soybean fiber blended wool fabric;

[0013] S4. Use the modified titanium oxide antibacterial agent to finish the modified soybean fiber blended wool fabric by the two-bath two-roll process to obtain an antibacterial modified soybean fiber blended wool fabric.

[0014] Furthermore, the dosage ratio of the pretreated wool fiber to the 2 g / L dopamine protease-based solution is 1-2 g: 30-50 mL. The dopamine protease-based solution consists of serine protease, 1.0 g / L hydrochloric acid dopamine, and phosphate buffer solution. The volume ratio of 1.0 g / L hydrochloric acid dopamine to the phosphate buffer solution is 1:1:8. The content of serine protease is 2.5 U / mL. The phosphate buffer solution is composed of disodium hydrogen phosphate and sodium dihydrogen phosphate at 0.2 M in a volume ratio of 6:1, and the pH value of the system is 8. In step S2, the dosage ratio of the pretreated soybean fiber, the strengthening and modifying solution, and ammonium persulfate is 100 g: 30-50 mL: 1-5 g, the temperature is 70-80 °C, and the washing solution is composed of 5 g / L sodium sulfite and 2 g / L AEO-9 surfactant mixed in a volume ratio of 5:2.

[0015] Furthermore, the preparation method of the pretreated wool fiber is as follows: Add the wool fiber and 0.2 g / L AEO-9 surfactant to the reaction kettle according to the dosage ratio of 1-5 g: 0.001-0.005 g, stir at a temperature of 50-60 °C for 20-30 min. The post-treatment includes: suction filtration, washing with deionized water until neutral, and drying in a vacuum drying oven at a temperature of 70-80 °C until constant weight to obtain the pretreated wool fiber.

[0016] Furthermore, the preparation method of the strengthening and modifying solution is as follows: Add epoxy soybean oil, tetraethoxysilane, emulsifier, and glacial acetic acid to the reaction kettle according to the volume ratio of 40-60: 5-15: 1-5: 0.5-3, stir, keep the temperature at 60-80 °C, and react for 2-4 h. The post-treatment includes: suction filtration, washing with absolute ethanol 3-5 times, and suction filtration to obtain the strengthening and modifying solution.

[0017] Furthermore, the preparation method of the pretreated soybean fiber is as follows: Add the soybean fiber and 5 wt% poly(ethylene oxide) trialkylammonium chloride aqueous solution to the reaction kettle according to the dosage ratio of 1 g: 10-15 mL, stir at a temperature of 30-50 °C for 40-60 min. The post-treatment includes: suction filtration, washing with deionized water until neutral, and drying in a vacuum drying oven at a temperature of 70-80 °C until constant weight to obtain the pretreated soybean fiber.

[0018] Furthermore, the modified titanium dioxide antibacterial agent is obtained by the following steps:

[0019] A1. Add titanium tetraisopropoxide, ammonia water, and ethylene glycol amine sol to an ultrasonic disperser, disperse for 2-3 h, age for 24 h, and perform post-treatment to obtain nano-titanium dioxide powder;

[0020] A2. Add the nano-titanium dioxide powder, waterborne polyurethane, and deionized water to an ultrasonic disperser, disperse for 30-40 min, add sodium hydroxide aqueous solution to adjust the pH value of the system to 9, and perform post-treatment to obtain the modified titanium dioxide antibacterial agent.

[0021] The reaction mechanism of the modified titanium oxide antibacterial agent is as follows:

[0022] In the presence of ammonia water and ethylene glycol amine, tetra-isopropyl titanate undergoes a hydrolysis reaction to form titanium hydroxide Ti(OH)4 or TiO(OH)2. Subsequently, Ti(OH)4 further polymerizes to form larger particles or colloidal nano-titanium oxide particles. Ammonia molecules in the ammonia water react with titanium hydroxide to form an ammonia-coordinated titanium complex. N doping can reduce the band gap of TiO2, thereby stabilizing the reaction intermediate. As the reaction proceeds, titanium hydroxide is converted into nano-titanium oxide (TiO2) particles through a dehydration reaction. The amino and hydroxyl groups in ethylene glycol amine interact with the surface of the nano-titanium oxide particles through coordination, controlling the particle size and enhancing the dispersibility of the particles. Finally, the generated nano-titanium oxide particles have good dispersibility and particle size control. Waterborne polyurethane can undergo a coordination reaction with the surface of nano-titanium oxide, further enhancing its dispersibility and stability. Through this reaction mechanism, the finally prepared antibacterial liquid has excellent durability, stability, and antibacterial properties.

[0023] Furthermore, in step A1, the volume ratio of tetra-isopropyl titanate, ammonia water, and ethylene glycol amine sol is 10 - 12:2 - 5:0.5 - 1. The ethylene glycol amine sol is composed of diethanolamine, ethanol, and water mixed in a volume ratio of 1:10:1. The post-treatment includes: aging, then drying in a vacuum drying oven at 100 °C until constant weight, passing through a 200-mesh sieve, washing, suction filtration, putting the filter cake into a muffle furnace at 600 °C for roasting for 2 - 3 h to obtain nano-titanium oxide powder; in step A2, the dosage ratio of nano-titanium oxide powder, waterborne polyurethane, and deionized water is 1 - 3 g:1 - 3 g:6 - 10 mL, and the temperature is 50 - 70 °C. The post-treatment includes: removing ethanol under reduced pressure, suction filtration, washing with deionized water until neutral, and drying in a vacuum drying oven at a temperature of 80 - 90 °C until constant weight to obtain the modified titanium oxide antibacterial agent.

[0024] Furthermore, the preparation method of the waterborne polyurethane is as follows: Add polyethylene glycol, polycarbonate diol, isophorone diisocyanate, diphenylmethane diisocyanate, and toluene to the reaction kettle according to a dosage ratio of 20 - 30 g:10 - 20 g:30 - 50 mL:5 - 10 g:200 - 300 mL and stir. The temperature of the reaction kettle is 100 - 120 °C, keep the temperature for reaction for 2 - 4 h, reduce the temperature of the reaction kettle to 50 - 80 °C, keep the temperature for reaction for 1 - 2 h, add triethylamine to adjust the system to neutral. The post-treatment includes: after the reaction is completed, raise the temperature of the reaction kettle to 80 - 90 °C, and distill off low-boiling molecules under reduced pressure to obtain waterborne polyurethane.

[0025] Furthermore, the blending ratio of the modified soybean fiber to the modified wool fiber is 4:6, the linear density of the blended yarn is 77 - 82 dtex, the warp density of the modified soybean fiber blended wool fabric is 140 - 170 threads per inch, and the weft density is 90 - 130 threads per inch.

[0026] Furthermore, the two-bath padding process is obtained by the following steps:

[0027] B1. Immerse the modified soybean fiber blended wool fabric and the modified titanium dioxide antibacterial agent in the padding machine tank according to the dosage ratio of 100 - 200 g:800 - 1000 mL, with an impregnation time of 10 - 20 min. Squeeze and roll through a two-roll calender. The rolling pressure is 400 - 600 KN, the rolling speed is 100 - 150 m / min, and the coiling speed is 100 - 280 m / min. Then put it into a heat setting machine for pre-drying. The pre-drying temperature is 90 - 110 °C, and the pre-drying time is 5 - 10 min. The curing temperature is 140 - 160 °C, and the curing time is 5 - 10 min to obtain pre-impregnated modified soybean fiber blended wool.

[0028] B2. Immerse the pre-impregnated modified soybean fiber blended wool and the modified antibacterial agent in the padding machine tank according to the dosage ratio of 100 - 200 g:800 - 1000 mL, with an impregnation time of 20 - 40 min. Squeeze and roll through a two-roll calender. The rolling pressure is 600 - 800 KN, the rolling speed is 150 - 200 m / min, and the coiling speed is 200 - 380 m / min. Then put it into a heat setting machine for pre-drying. The pre-drying temperature is 90 - 110 °C, and the pre-drying time is 5 - 10 min. The curing temperature is 170 - 190 °C, and the curing time is 5 - 10 min to obtain antibacterial modified soybean fiber blended wool.

[0029] Among them, a blended wool fabric containing soybean fiber is prepared by using a production process of a blended wool fabric containing soybean fiber.

[0030] The present invention has the following beneficial effects:

[0031] 1. The inner layer of the scales at the bottom of the wool fiber contains more polar amino acids. In traditional finishing techniques, the enzyme reagents used are prone to react with these amino acids, resulting in fiber swelling, damaging the cell membrane complex layer below, and causing excessive fiber damage. However, when the protease-based solution is prepared by the co-bath crosslinking method to finish the wool fiber in the present invention, the reaction is successfully controlled on the scale surface, avoiding damage to the inside of the fiber. In addition, this method also has the ability to reduce the disulfide bonds in keratin, which can not only enhance the shrinkage force of the fabric but also not damage the mechanical properties of the fiber. Through this method, hydrolysis reaction and surface polymerization reaction occur simultaneously in the same reaction system to achieve hydrolysis and coating repair of wool scales. This multi-step reaction characteristic balances the mechanical properties and felting properties of the fiber and enhances the anti-felting performance.

[0032] 2. Epoxidized soybean oil and silane coupling agent react through the epoxy group with the silanol group in the silane coupling agent to form covalent bonds (such as siloxane bonds), enhancing the interfacial bonding force between soybean fibers and the modified matrix, and further enhancing the mechanical properties such as the tensile strength and flexural strength of soybean fibers. Between the silane coupling agent and the fibers, the friction resistance of soybean fibers is improved by forming stable chemical bonds (such as Si-O-C bonds), preventing fiber degradation caused by water penetration. This enhanced interfacial bonding force also makes the modified material more corrosion-resistant and less prone to deformation in harsh environments.

[0033] 3. Nano-titanium oxide excites antibacterial free radicals such as superoxide ions and hydroxyl ions through light irradiation, which is easy to oxidize, unstable, and not long-lasting. After modification, the photo-cathode protection effect of doped N TiO2 under white light conditions is significantly enhanced, and the antibacterial agent does not fail for a long time; the carboxyl and hydroxyl bonds contained in the modified soybean fiber blended wool undergo a ring-opening reaction with the epoxy group in the modified titanium oxide antibacterial agent to form covalent bonds, enhancing the interfacial bonding ability between the modified blended fiber and the antibacterial agent and improving the stability of the composite material. After being modified by the modified antibacterial agent, a continuous, compact, and relatively dense film is formed on the fabric surface. Antibacterial tests show that when the addition amount of the modified antibacterial agent reaches 13.0%, good antibacterial performance is obtained; the results of the durability test show that the antibacterial performance of the obtained modified fabric has certain friction resistance and washing resistance; after finishing wool with dopamine-modified protease, the shrinkage area of the fabric reaches 2.15%. Specific embodiments

[0034] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present invention.

[0035] The polycarbonate diol used in the present invention refers to Wuhan Huaxiang Kejie Biotechnology Co., Ltd., with an active ingredient content of 99%, a molecular weight of 1000, and a CAS number of 24937-06-2;

[0036] The polyethylene glycol used in the present invention refers to Guangzhou Bolun Chemical Technology Co., Ltd., with a molecular weight of 400;

[0037] Example 1

[0038] This example provides a production process for a blended wool fabric containing soybean fibers, including the following steps:

[0039] S1. Prepare pretreated wool fibers

[0040] Weigh: Add 100 g of wool fibers and 0.1 g of 0.2 g / L AEO-9 surfactant into the reaction kettle, stir, the temperature is 50 °C, react for 20 min, filter by suction, wash with deionized water until neutral, place in a vacuum drying oven at 70 °C and dry to constant weight to obtain pretreated wool fibers.

[0041] S2. Prepare modified wool fibers

[0042] The dopamine protease-based solution consists of serine protease, 1.0 g / L hydrochloric acid dopamine, and phosphate buffer solution. The volume ratio of 1.0 g / L hydrochloric acid dopamine to phosphate buffer solution is 1:1:8, the content of serine protease is 2.5 U / mL, the phosphate buffer solution is composed of 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a volume ratio of 6:1, and the pH value of the system is 8;

[0043] Weigh: Add 100 g of pretreated wool fibers and 3000 mL of 2 g / L dopamine protease-based solution into the reaction kettle, stir for 4 h, the reaction temperature is 40 °C. After the reaction is completed, filter by suction, wash with deionized water until neutral, place in a vacuum drying oven at 70 °C and dry to constant weight to obtain modified wool fibers.

[0044] S3. Prepare pretreated soybean fibers

[0045] Weigh: Add 100 g of soybean fibers and 1000 mL of 5 wt% poly(ethylene oxide) trialkylammonium chloride aqueous solution into the reaction kettle, stir at 30 °C for 40 min, filter by suction, wash with deionized water until neutral, place in a vacuum drying oven at 70 °C and dry to constant weight to obtain pretreated soybean fibers.

[0046] S4. Prepare the enhanced modification liquid

[0047] Weigh: Add 400 mL of epoxidized soybean oil, 50 mL of tetraethoxysilane, 10 mL of emulsifier, and 5 mL of glacial acetic acid into the reaction kettle, stir, keep the temperature at 60 °C, react for 2 h, filter by suction, wash with absolute ethanol 3 - 5 times, and filter by suction to obtain the enhanced modification liquid.

[0048] S5. Prepare modified soybean fibers

[0049] The washing liquid is composed of 5 g / L sodium sulfite and 2 g / L AEO-9 surfactant mixed in a volume ratio of 5:2;

[0050] Weigh: Add 100 g of pretreated soybean fibers, 30 mL of enhanced modification liquid, and 1 g of ammonium persulfate into the reaction kettle at 70 °C, stir for 2 h. After the reaction is completed, filter by suction, wash with the washing liquid at 70 °C for 40 min to remove the unreacted enhanced modification liquid, and place in a drying oven at 100 °C and dry to constant weight.

[0051] S6. Nano-titanium oxide powder

[0052] The ethylene glycol amine sol is composed of diethanolamine, ethanol, and water in a volume ratio of 1:10:1;

[0053] Weigh: 100 mL of titanium tetraisopropoxide, 20 mL of ammonia water, and 5 mL of ethylene glycol amine sol, add them to an ultrasonic disperser, disperse for 2 - 3 h, age for 24 h, after aging, place them in a vacuum drying oven at 100 °C and dry to constant weight, pass through a 200 - mesh sieve, wash, filter by suction, put the filter cake into a muffle furnace at 600 °C and calcine for 2 h to obtain nano - titanium oxide powder.

[0054] S7. Preparation of water - borne polyurethane

[0055] Weigh: 200 g of polyethylene glycol, 100 g of polycarbonate diol, 300 mL of isophorone diisocyanate, 50 g of diphenylmethane diisocyanate, and 2000 mL of toluene, add them to a reaction kettle and stir. The temperature of the reaction kettle is 100 °C, keep the temperature for 2 h, reduce the temperature of the reaction kettle to 50 °C, keep the temperature for 1 h, add triethylamine to adjust the system to neutral. After the reaction is completed, raise the temperature of the reaction kettle to 80 °C and distill off low - boiling - point molecules under reduced pressure to obtain water - borne polyurethane.

[0056] S8. Preparation of modified titanium oxide antibacterial agent

[0057] Weigh: 100 g of nano - titanium oxide powder, 100 g of water - borne polyurethane, and 600 mL of deionized water, add them to an ultrasonic disperser at 50 °C, disperse for 30 min, add sodium hydroxide aqueous solution to adjust the pH value of the system to 9, remove ethanol under reduced pressure, filter by suction, wash with deionized water until neutral, and place in a vacuum drying oven at 80 °C and dry to constant weight to obtain the modified titanium oxide antibacterial agent.

[0058] Example 2

[0059] This example provides a production process for a blended wool fabric containing soybean fibers, including the following steps:

[0060] S1. Preparation of pretreated wool fibers

[0061] Weigh: 300 g of wool fibers and 0.3 g of 0.2 g / L AEO - 9 surfactant, add them to a reaction kettle and stir. The temperature is 55 °C, react for 25 min, filter by suction, wash with deionized water until neutral, and place in a vacuum drying oven at 75 °C and dry to constant weight to obtain pretreated wool fibers.

[0062] S2. Preparation of modified wool fibers

[0063] The dopamine protease-based solution is composed of serine protease, 1.0 g / L hydrochloric acid dopamine, and phosphate buffer solution. The volume ratio of 1.0 g / L hydrochloric acid dopamine to phosphate buffer solution is 1:1:8, the content of serine protease is 2.5 U / mL, the phosphate buffer solution is composed of disodium hydrogen phosphate and sodium dihydrogen phosphate at a volume ratio of 6:1, and the pH value of the system is 8;

[0064] Weigh: Add 150 g of pretreated wool fibers and 4000 mL of 2 g / L dopamine protease-based solution into the reaction kettle and stir for 4.5 h at a reaction temperature of 45 °C. After the reaction is completed, filter by suction, wash with deionized water until neutral, and place in a vacuum drying oven at 75 °C to dry to constant weight to obtain modified wool fibers.

[0065] S3. Prepare pretreated soybean fibers

[0066] Weigh: Add 100 g of soybean fibers and 1300 mL of 5 wt% poly(ethylene oxide) trialkylammonium chloride aqueous solution into the reaction kettle and stir at 40 °C for 50 min. Filter by suction, wash with deionized water until neutral, and place in a vacuum drying oven at 75 °C to dry to constant weight to obtain pretreated soybean fibers.

[0067] S4. Prepare the enhanced modification solution

[0068] Weigh: Add 500 mL of epoxidized soybean oil, 100 mL of tetraethoxysilane, 30 mL of emulsifier, and 2 mL of glacial acetic acid into the reaction kettle and stir. Keep the temperature at 70 °C and react for 3 h. Filter by suction, wash with absolute ethanol 3 - 5 times, and filter by suction to obtain the enhanced modification solution.

[0069] S5. Prepare modified soybean fibers

[0070] The washing solution is composed of 5 g / L sodium sulfite and 2 g / L AEO-9 surfactant mixed at a volume ratio of 5:2;

[0071] Weigh: Add 100 g of pretreated soybean fibers, 40 mL of enhanced modification solution, and 4 g of ammonium persulfate into the reaction kettle at 75 °C and stir for 2.5 h. After the reaction is completed, filter by suction, wash with the washing solution at 70 °C for 40 min to remove the unreacted enhanced modification solution, and place in a drying oven at 105 °C to dry to constant weight.

[0072] S6. Nano-titanium oxide powder

[0073] The ethylene glycol amine sol is composed of diethanolamine, ethanol, and water mixed at a volume ratio of 1:10:1;

[0074] Weigh: 110 mL of titanium tetraisopropoxide, 30 mL of ammonia water, and 8 mL of ethylene glycol amine sol are added to an ultrasonic disperser, dispersed for 2.5 h, aged for 24 h, and then placed in a vacuum drying oven at 100 °C and dried to a constant weight, passed through a 200-mesh sieve, washed, filtered by suction, and the filter cake is calcined in a muffle furnace at 600 °C for 2.5 h to obtain nano-titanium oxide powder.

[0075] S7. Preparation of waterborne polyurethane

[0076] Weigh: 250 g of polyethylene glycol, 150 g of polycarbonate diol, 400 mL of isophorone diisocyanate, 80 g of diphenylmethane diisocyanate, and 2500 mL of toluene are added to a reaction kettle and stirred. The temperature of the reaction kettle is 110 °C, and the reaction is carried out under insulation for 3 h. Then the temperature of the reaction kettle is reduced to 60 °C, and the reaction is carried out under insulation for 1.5 h. Triethylamine is added to adjust the system to neutrality. After the reaction is completed, the temperature of the reaction kettle is raised to 85 °C, and low-boiling molecules are removed by vacuum distillation to obtain waterborne polyurethane.

[0077] S8. Preparation of modified titanium oxide antibacterial agent

[0078] Weigh: 200 g of nano-titanium oxide powder, 200 g of waterborne polyurethane, and 800 mL of deionized water are added to an ultrasonic disperser at 60 °C, dispersed for 35 min, and the pH value of the system is adjusted to 9 by adding sodium hydroxide aqueous solution. Ethanol is removed by vacuum, filtered by suction, washed with deionized water to neutrality, and placed in a vacuum drying oven at 85 °C and dried to a constant weight to obtain a modified titanium oxide antibacterial agent.

[0079] Example 3

[0080] This example provides a production process of a blended wool fabric containing soybean fiber, including the following steps:

[0081] S1. Preparation of pretreated wool fiber

[0082] Weigh: 500 g of wool fiber and 0.5 g of 0.2 g / L AEO-9 surfactant are added to a reaction kettle and stirred at a temperature of 60 °C for 30 min, filtered by suction, washed with deionized water to neutrality, and placed in a vacuum drying oven at 80 °C and dried to a constant weight to obtain pretreated wool fiber.

[0083] S2. Preparation of modified wool fiber

[0084] The dopamine protease-based solution consists of serine protease, 1.0 g / L hydrochloric acid dopamine, and phosphate buffer solution. The volume ratio of 1.0 g / L hydrochloric acid dopamine to phosphate buffer solution is 1:1:8, the content of serine protease is 2.5 U / mL, the phosphate buffer solution is composed of 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate at a volume ratio of 6:1, and the pH value of the system is 8;

[0085] Weigh: Add 200 g of pretreated wool fibers and 5000 mL of 2 g / L dopamine protease-based solution into the reaction kettle, stir for 5 h at a reaction temperature of 50 °C. After the reaction is completed, perform suction filtration, wash with deionized water until neutral, and place in a vacuum drying oven at 80 °C to dry to a constant weight to obtain modified wool fibers.

[0086] S3. Prepare pretreated soybean fibers

[0087] Weigh: Add 100 g of soybean fibers and 1500 mL of 5 wt% poly(ethylene oxide) trialkylammonium chloride aqueous solution into the reaction kettle, stir at 50 °C for 60 min, perform suction filtration, wash with deionized water until neutral, and place in a vacuum drying oven at 80 °C to dry to a constant weight to obtain pretreated soybean fibers.

[0088] S4. Prepare the enhanced modification liquid

[0089] Weigh: Add 600 mL of epoxidized soybean oil, 150 mL of tetraethoxysilane, 50 mL of emulsifier, and 30 mL of glacial acetic acid into the reaction kettle, stir, keep the temperature at 80 °C, react for 4 h, perform suction filtration, wash with absolute ethanol 3 - 5 times, and perform suction filtration to obtain the enhanced modification liquid.

[0090] S5. Prepare modified soybean fibers

[0091] The washing liquid is composed of a 5:2 volume ratio mixture of 5 g / L sodium sulfite and 2 g / L AEO - 9 surfactant;

[0092] Weigh: Add 100 g of pretreated soybean fibers, 50 mL of enhanced modification liquid, and 5 g of ammonium persulfate into a reaction kettle at 80 °C, stir for 3 h. After the reaction is completed, perform suction filtration, wash with the washing liquid at 70 °C for 40 min to remove the unreacted enhanced modification liquid, and place in a drying oven at 110 °C to dry to a constant weight.

[0093] S6. Nano - titanium oxide powder

[0094] The ethylene glycolamine sol is composed of diethanolamine, ethanol, and water in a volume ratio of 1:10:1;

[0095] Weigh: Add 120 mL of tetra(isopropyl) titanate, 50 mL of ammonia water, and 10 mL of ethylene glycolamine sol into an ultrasonic disperser, disperse for 2 - 3 h, age for 24 h. After aging, place in a vacuum drying oven at 100 °C to dry to a constant weight, sieve through a 200 - mesh sieve, wash, perform suction filtration, and place the filter cake in a muffle furnace at 600 °C for roasting for 2 - 3 h to obtain nano - titanium oxide powder.

[0096] S7. Prepare water - borne polyurethane

[0097] Weigh: 300 g of polyethylene glycol, 200 g of polycarbonate diol, 500 mL of isophorone diisocyanate, 100 g of diphenylmethane diisocyanate, and 3000 mL of toluene and add them to a reaction kettle for stirring. The temperature of the reaction kettle is 120 °C, and keep the temperature for reaction for 4 h. Then lower the temperature of the reaction kettle to 80 °C and keep the temperature for reaction for 2 h. Add triethylamine to adjust the system to neutral. After the reaction is completed, raise the temperature of the reaction kettle to 90 °C, and distill off low-boiling molecules under reduced pressure to obtain waterborne polyurethane.

[0098] S8. Preparation of modified titanium oxide antibacterial agent

[0099] Weigh: 300 g of nano-titanium oxide powder, 300 g of waterborne polyurethane, and 1000 mL of deionized water and add them to an ultrasonic disperser at 70 °C, disperse for 40 min, add sodium hydroxide aqueous solution to adjust the pH value of the system to 9, remove ethanol under reduced pressure, filter by suction, wash with deionized water until neutral, and place in a vacuum drying oven at 90 °C to dry to constant weight to obtain the modified titanium oxide antibacterial agent.

[0100] Comparative Example 1

[0101] The difference between this comparative example and Example 3 is that in step S1, the strengthening and modification liquid was not added.

[0102] Comparative Example 2

[0103] The difference between this comparative example and Example 3 is that in step S2, the dopamine protease-based liquid was not added.

[0104] Comparative Example 3

[0105] The difference between this comparative example and Example 3 is that in step S6, the modified titanium oxide antibacterial agent was not added.

[0106] Performance test:

[0107] For the antibacterial performance, refer to Standard GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles - Part 3: Oscillation method" to determine the antibacterial rate of the test sample;

[0108] Refer to GB / T8628—2013 "Preparation, marking and measurement of fabric specimens and garments in the test for determining dimensional changes of textiles" to test the area shrinkage rate of wool fabrics. The area shrinkage rate is obtained from the change rate of the marked area before and after washing the specimen, and is calculated according to the following formula: Among them, S1 is the marked position before washing, S2 is the marked area after washing, the test is carried out in an infrared dyeing machine, using an aqueous solution of 1 g / L Na2CO3 and 1 g / L JFC penetrant, treating at 45 °C for 60 min, washing with clean water and then drying in an oven at 60 °C;

[0109] Under the test standard atmospheric pressure (temperature 20±2°C, relative humidity 65±2%), the fiber directional friction effect is measured. The sample is stored in the standard atmosphere for 48 hours before the test. The fiber pre-tension is 0.1 g, the test speed is 30 rpm, and the friction rod used in the measurement is a metal rod with a diameter of 8 mm. After testing 50 fibers, the average value is calculated according to the formula. Among them, δμ is the directional friction effect; μa is the friction factor against the scale; μs is the friction factor along the scale.

[0110] Referring to the first part of GB / T3923.1-2013 "Textiles - Tensile properties of fabrics", the breaking strength and breaking elongation of the fabric are tested. The size of the fabric to be tested is 100.0 mm × 25.0 mm, the tensile test speed is 100 mm / min, and the average value is taken after 6 - 8 tests in each group. The specific test results are shown in Table 1:

[0111] Table 1 - Data sheet for performance detection of samples

[0112]

[0113]

[0114] Data analysis:

[0115] From the relevant data in Table 1, it can be seen that compared with the comparative example, the modified soybean wool blended fiber provided by the present invention uses N / nano titanium oxide as an antibacterial agent. The modified soybean wool blended fiber adopts a two-dip two-roll finishing process, which can significantly improve the antibacterial property, tensile resistance, and shrinkage resistance of the fabric, while ensuring that the performance of the fabric remains stable under the action of washing or friction. This enables the fabric to maintain its good functionality and comfort during long-term use.

[0116] When comparing Comparative Example 1 with Examples 1 - 3, its friction resistance coefficient and breaking tensile performance decrease, indicating that adding the strengthening modification liquid, that is, epoxy soybean oil and silane coupling agent react through the epoxy group and the silanol group in the silane coupling agent to form a covalent bond (such as a siloxane bond), enhancing the interfacial bonding force between the soybean fiber and the modified matrix, so as to enhance the mechanical properties such as the tensile strength and friction resistance coefficient of the soybean fiber reinforced material.

[0117] When comparing Comparative Example 2 with Examples 1 - 3, the fabric area shrinkage rate decreases significantly and there is no difference in the anti-tensile and friction resistance coefficients, indicating that the modification of the blended fiber with dopamine protease-based liquid not only has the ability to reduce the disulfide bonds in keratin but also can enhance the shrinkage force of the fabric without damaging the mechanical properties of the fiber.

[0118] Comparing Comparative Example 3 with Examples 1-3, its antibacterial stability decreased, indicating that N doping can reduce the band gap of TiO2, the antibacterial agent has high stability, good visible light response and strong effect, can effectively resist external bacteria, and prolong the duration of the antibacterial effect.

[0119] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only the specific embodiments. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification to better explain the principles and practical applications of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A production process of a blended wool fabric containing soybean fiber, characterized in that, It includes the following steps: S1. Add the pretreated wool fibers and 2 g / L dopamine protease-based solution into a reaction kettle, stir for 4 - 5 h, and then perform post-treatment to obtain modified wool fibers; S2. Add the pretreated soybean fibers, reinforcing modification solution, and ammonium persulfate into a reaction kettle, stir for 2 - 3 h, and then perform post-treatment to obtain modified soybean fibers; S3. Blend the modified soybean fibers and modified wool fibers to prepare a blended yarn, and then perform plain weaving on it to obtain a blended fabric of modified soybean fibers and wool; S4. Use the modified titanium oxide antibacterial agent to finish the blended fabric of modified soybean fibers and wool by the two-bath two-roll process to obtain an antibacterial blended fabric of modified soybean fibers and wool.

2. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, In step S1, the dosage ratio of the pretreated wool fibers to the 2 g / L dopamine protease-based solution is 1 - 2 g:30 - 50 mL. The dopamine protease-based solution is composed of serine protease, 1.0 g / L hydrochloric acid dopamine, and phosphate buffer solution. The volume ratio of 1.0 g / L hydrochloric acid dopamine to the phosphate buffer solution is 1:1:8, the content of serine protease is 2.5 U / mL, the phosphate buffer solution is composed of 0.2 M disodium hydrogen phosphate and 0.2 M sodium dihydrogen phosphate in a volume ratio of 6:1, and the pH value of the system is 8. In step S2, the dosage ratio of the pretreated soybean fibers, the reinforcing modification solution, and ammonium persulfate is 100 g:30 - 50 mL:1 - 5 g, the temperature is 70 - 80 °C, and the washing solution is composed of 5 g / L sodium sulfite and 2 g / L AEO-9 surfactant mixed in a volume ratio of 5:

2.

3. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, The preparation method of the pretreated wool fibers is as follows: Add the wool fibers and 0.2 g / L AEO-9 surfactant into a reaction kettle according to the dosage ratio of 1 - 5 g:0.001 - 0.005 g, stir at a temperature of 50 - 60 °C for 20 - 30 min, and then perform post-treatment to obtain the pretreated wool fibers.

4. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, The preparation method of the reinforcing modification solution is as follows: Add epoxy soybean oil, tetraethoxysilane, emulsifier, and glacial acetic acid into a reaction kettle according to a volume ratio of 40 - 60:5 - 15:1 - 5:0.5 - 3, stir, keep the temperature at 60 - 80 °C, react for 2 - 4 h, and then perform post-treatment to obtain the reinforcing modification solution.

5. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, The preparation method of the pretreated soybean fibers is as follows: Add the soybean fibers and 5 wt% poly(ethylene oxide) trialkylammonium chloride aqueous solution into a reaction kettle according to the dosage ratio of 1 g:10 - 15 mL, stir at a temperature of 30 - 50 °C for 40 - 60 min, and then perform post-treatment to obtain the pretreated soybean fibers.

6. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, The modified titanium oxide antibacterial agent is obtained by the following steps: A1. Add tetra-isopropyl titanate, ammonia water, and ethylene glycol amine sol into an ultrasonic disperser, disperse for 2 - 3 h, age for 24 h, and then perform post-treatment to obtain nano-titanium oxide powder; A2. Add the nano-titanium oxide powder, waterborne polyurethane, and deionized water into an ultrasonic disperser, disperse for 30 - 40 min, add sodium hydroxide aqueous solution to adjust the pH value of the system to 9, and then perform post-treatment to obtain the modified titanium oxide antibacterial agent.

7. The production process of a blended wool fabric containing soybean fiber according to claim 6, characterized in that, In step A1, the volume ratio of tetra-isopropyl titanate, ammonia water, and ethylene glycol amine sol is 10 - 12:2 - 5:0.5 - 1. The ethylene glycol amine sol is composed of diethanolamine, ethanol, and water mixed in a volume ratio of 1:10:

1. In step A2, the dosage ratio of nano-titanium oxide powder, waterborne polyurethane, and deionized water is 1 - 3 g:1 - 3 g:6 - 10 mL, and the temperature is 50 - 70 °C.

8. The production process of a blended wool fabric containing soybean fiber according to claim 7, characterized in that, The preparation method of the waterborne polyurethane is as follows: Add polyethylene glycol, polycarbonate diol, isophorone diisocyanate, diphenylmethane diisocyanate, and toluene into a reaction kettle according to a dosage ratio of 20 - 30 g:10 - 20 g:30 - 50 mL:5 - 10 g:200 - 300 mL and stir. The temperature of the reaction kettle is 100 - 120 °C, and keep the temperature for reaction for 2 - 4 h. Then lower the temperature of the reaction kettle to 50 - 80 °C and keep the temperature for reaction for 1 - 2 h. Add triethylamine to adjust the system to neutral, and perform post-treatment to obtain the waterborne polyurethane.

9. The production process of a blended wool fabric containing soybean fiber according to claim 1, characterized in that, The blending ratio of the modified soybean fiber and the modified wool fiber is 4:

6. The linear density of the blended yarn is 77 - 82 dtex. The warp density of the blended wool fabric containing modified soybean fiber is 140 - 170 per inch, and the weft density is 90 - 130 per inch.

10. A blended wool fabric containing soybean fiber, characterized in that, The blended wool fabric containing soybean fiber is prepared by using the production process of a blended wool fabric containing soybean fiber according to any one of claims 1 - 9.

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