Modified soybean fiber and preparation method thereof
By cross-linking the combination of modified soy protein and soy isoflavones and regenerated cellulose, combined with silane-modified and covalent bond networks, the problem of poor washing resistance of soy fibers is solved, and the high stability and antibacterial properties of the fiber are achieved.
Patent Information
- Application Number
- CN202510557857.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-29
- Publication Date
- 2025-08-05
AI Technical Summary
Soybean fiber has poor washing resistance during the washing process, resulting in a decline in fiber performance, which seriously limits its application in actual products.
The combination of cross-linked modified soy protein, regenerated cellulose and soy isoflavones is used to enhance binding stability through chemical bonds and physical entanglement. The addition of 3-aminopropyltriethoxysilane is modified to modify regenerated cellulose to form a siloxane network structure, and a covalent bond network is formed by combining tea polyphenols and genipine to form a covalent bond network to enhance the stability and antibacterial properties of the fiber.
The water-resistant washing performance, fracture strength and antibacterial properties of modified soybean fiber are improved, ensuring structural stability and functional components of the fiber during the washing process.
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Abstract
Description
Technical Field
[0001] The present application relates to the field of fiber technology, and in particular to a modified soybean fiber and a preparation method thereof. Background Art
[0002] Soy protein, a widely available, low-cost plant protein, has a rich amino acid composition, which gives it good biocompatibility and degradability. In the field of materials, soy protein has been tried in the preparation of various bio-based materials due to its film-forming and adhesive properties. Soy isoflavones have various physiological activities, such as anti-oxidation and endocrine regulation. Introducing them into material systems is expected to give the materials unique functionality. Regenerated cellulose is known for its excellent mechanical properties and moisture absorption and breathability, making it an ideal raw material for the preparation of high-performance fiber materials. The combination of the two can complement each other's strengths and provide new ideas and approaches for the development of new fiber materials.
[0003] Soy fiber, made from soy protein, soy isoflavones, and regenerated cellulose, shows promising application prospects in fields such as textiles and biomedicine. However, soy fiber suffers from poor wash fastness. The molecular structure within the fiber is easily damaged during washing, leading to a decrease in fiber performance, such as reduced strength and loss of functional components. This severely limits the application and promotion of soy fiber in practical products, and there is room for improvement. Summary of the Invention
[0004] In order to improve the wash resistance of soybean fiber, the present application provides a modified soybean fiber and a preparation method thereof.
[0005] The modified soybean fiber and its preparation method provided in this application adopt the following technical solutions: In the first aspect, the present application provides a modified soybean fiber, which adopts the following technical solution: A modified soybean fiber comprises the following components in parts by weight: 1-2 servings of soy isoflavones 6-8 parts cross-linked modified soy protein 40-50 parts of regenerated cellulose; The raw materials for preparing the cross-linked modified soybean protein include soybean protein body and butane tetracarboxylic acid.
[0006] Butanetetracarboxylic acid in cross-linked modified soy protein promotes the formation of a covalent cross-linked network in soy protein, which not only enhances its own structural stability, but also can be closely connected with soy isoflavones and regenerated cellulose through chemical bonds and physical entanglement, further improving the binding stability and breaking strength, and reducing the structural damage of the fiber caused by water absorption and swelling; soy isoflavones can produce intermolecular interactions with other components, such as hydrogen bonds and van der Waals forces, etc., which strengthen the binding stability between the components and lay the foundation for the stability of the entire fiber system; soy isoflavones have natural antibacterial activity, which can inhibit the growth and reproduction of bacteria, and after combining with other components, they create an antibacterial environment inside and on the surface of the fiber, making it difficult for bacteria to survive, giving the modified soybean fiber good antibacterial properties.
[0007] Preferably, the mass ratio of the soybean protein bulk to butanetetracarboxylic acid is 1:(0.3-0.4).
[0008] In the cross-linked modified soy protein prepared according to the above ratio, the carboxyl groups in butane tetracarboxylic acid fully react with the active groups such as amino and hydroxyl groups in the soy protein to form a rich and stable covalent cross-linking network, which enhances the interaction between the components and effectively fixes the soy isoflavones, so that their antibacterial activity can be fully and lastingly exerted, providing good antibacterial protection for the modified soy fiber and improving the stability, breaking strength and antibacterial properties of the modified soy fiber.
[0009] Preferably, the regenerated cellulose is modified with 3-aminopropyltriethoxysilane to obtain modified regenerated cellulose.
[0010] Preferably, the mass ratio of the 3-aminopropyltriethoxysilane to the regenerated cellulose is (0.5-1.5):10.
[0011] Preferably, the mass ratio of the 3-aminopropyltriethoxysilane to the regenerated cellulose is 1:10.
[0012] The ethoxysilane group of 3-aminopropyltriethoxysilane can undergo a hydrolysis-condensation reaction with the hydroxyl groups on the surface of regenerated cellulose to form a siloxane network structure on the surface of the regenerated cellulose, thereby enhancing the stability of the regenerated cellulose structure itself. The aminopropyl group of 3-aminopropyltriethoxysilane reacts chemically with the active groups in soy isoflavones and cross-linked modified soy protein, such as carboxyl groups and amino groups, or forms hydrogen bonds and other interactions, thereby making the connection between the components tighter and improving the overall bonding stability and breaking strength of the fiber. The siloxane network structure is hydrophobic and can effectively block the invasion of water molecules, reduce the swelling and structural damage of regenerated cellulose caused by water absorption, and thus improve the wash resistance of the modified soybean fiber. The amino groups on the surface of the modified regenerated cellulose act synergistically with soy isoflavones to change the microenvironment for bacterial survival, inhibit the growth and reproduction of bacteria by interacting with the biological molecules on the bacterial surface, and enhance the antibacterial properties of the fiber.
[0013] Preferably, the modified regenerated cellulose is prepared by the following steps: Adding 3-aminopropyltriethoxysilane solution to bamboo pulp dispersion, heating and stirring to react, washing to neutrality after cooling, and drying to obtain modified bamboo pulp; The modified bamboo pulp is subjected to the steps of impregnation, pressing, crushing, aging, xantholysis, dissolution, degassing and ripening to obtain a dispersion of modified regenerated cellulose.
[0014] Preferably, the solvent of the 3-aminopropyltriethoxysilane solution includes anhydrous ethanol.
[0015] The modified regenerated cellulose prepared according to the above steps has good compatibility and can form a good connection with the cross-linked modified soy protein and soy isoflavones, effectively improving the stability, water washing resistance, breaking strength and antibacterial properties of the modified soybean fiber.
[0016] Preferably, the modified soybean fiber further comprises tannic acid.
[0017] Tannic acid contains multiple phenolic hydroxyl groups in its molecular structure, which can form hydrogen bonds with soy isoflavones, cross-linked modified soy protein and active groups in regenerated cellulose. At the same time, they are anchored to soy isoflavones through π-π stacking and combined with the hydrophobic region of soy protein, thereby strengthening the interaction between the components and improving the overall binding stability, water washing resistance and breaking strength of the fiber. Tannic acid has good antibacterial activity and can destroy the bacterial cell membrane structure and interfere with the bacterial metabolic process by reacting with proteins or enzymes on the bacterial cell membrane. It can also synergize with soy isoflavones to enhance the antibacterial effect. Tannic acid has good antioxidant properties. After anchoring with soy isoflavones, it can protect soy isoflavones and reduce the damage to the activity of soy isoflavones by adverse factors in the environment, thereby improving the stability and antibacterial properties of modified soybean fiber.
[0018] In a second aspect, the present application provides a method for preparing modified soybean fiber, which adopts the following technical solution: A method for preparing modified soybean fiber comprises the following steps: (1) dissolving soybean isoflavones and tannic acid in a solvent and stirring to obtain a flavonoid mixed solution; mixing the cross-linked modified soybean protein with the prepared flavonoid mixed solution and stirring to obtain a mixed solution; adding a stabilizer, a defoaming agent and the mixed solution to a modified regenerated cellulose dispersion, heating and stirring to react, and obtaining a composite spinning solution; (2) filtering the composite spinning solution, and forming the filtered composite spinning solution by wet spinning to obtain filaments, wherein the coagulation bath comprises sulfuric acid, sodium sulfate and zinc sulfate; (3) The modified soybean fiber is obtained by subjecting the filaments to post-processing steps such as drawing, cutting, water washing, acid washing, and desulfurization.
[0019] Preferably, the monofilament fineness of the modified soybean fiber is 1.0D-4.0D.
[0020] Preferably, the solvent comprises an ethanol aqueous solution with a volume fraction of 50%, and the alkaline solution comprises a 0.1 mol / L sodium hydroxide aqueous solution.
[0021] The modified soybean fiber prepared according to the above steps has good stability, water-washing resistance and antibacterial properties.
[0022] Preferably, the mass ratio of the tannic acid to the soy isoflavones is 1:(0.4-0.6).
[0023] Tannic acid and soy isoflavones are compounded according to the above ratio. Tannic acid can act as an antioxidant barrier, preferentially react with oxidants in the environment, consume oxidizing substances, effectively inhibit the oxidation process of soy isoflavones, ensure their structural integrity and biological activity, and prolong their effective action time in modified soybean fibers. The catechol structure of tannic acid can fix soy isoflavones in the fiber system through special interactions such as π-π stacking. Tannic acid in this ratio can also form a large number of hydrogen bonds with soy isoflavones by virtue of its rich phenolic hydroxyl groups, thereby enhancing the binding force between the two and making the soy isoflavones more evenly and stably distributed in the fiber, ensuring that when they exert their antibacterial, regulatory and other functions, they will not be easily lost or migrated due to interference from external factors, thereby better exerting the positive role of soy isoflavones in improving the performance of modified soybean fibers.
[0024] Preferably, the coagulation bath further comprises silver nitrate and polyol.
[0025] In the coagulation bath environment, the silver ions in silver nitrate can interact with the groups on the surface or inside the fiber, firmly adhere to the fiber, and synergize with tannic acid and soy isoflavones to give the modified soybean fiber excellent antibacterial properties and effectively inhibit the growth of microorganisms; polyols can optimize the physical structure and properties of the fiber. Polyol molecules can form a large number of hydrogen bonds with fiber molecules, enhance the intermolecular forces inside the fiber, and promote the fiber to form a denser and more uniform microstructure during the coagulation process, thereby improving the stability and breaking strength of the fiber. The hydrophilicity of the polyol helps to improve the interaction between the fiber and water molecules, thereby improving the water-washing resistance of the modified soybean fiber.
[0026] Preferably, the stabilizer comprises tea polyphenols and genipin.
[0027] Tea polyphenols are rich in phenolic hydroxyl groups and have excellent antioxidant properties. During the fiber preparation process, they can scavenge free radicals in the system, prevent the oxidation of soy isoflavones, soy protein and other ingredients, maintain their molecular structure and activity, and ensure that each component can effectively function; genipin has good cross-linking ability, and the active groups in its molecules can undergo cross-linking reactions with soy protein, modified regenerated cellulose and other ingredients containing amino and hydroxyl groups to form a stable covalent bond network, strengthen the internal structure of the fiber, limit the penetration of water molecules, and improve the fiber's water resistance; the cross-linking structure helps to fix the antibacterial components, synergize the antibacterial substances of tea polyphenols and the fiber itself, enhance the antibacterial properties, and improve the stability, water resistance, breaking strength and antibacterial properties of the modified soybean fiber.
[0028] Preferably, the defoaming agent comprises polyether-modified silicone.
[0029] The polyether-modified silicone molecule contains silicone segments and polyether segments. The silicone segments have good defoaming activity and long-lasting anti-foaming properties, which can effectively prevent the generation of new bubbles; the polyether segments enhance the solubility and dispersibility of the defoamer in the system, allowing it to be evenly distributed in the reaction liquid and fully exert its defoaming effect; by eliminating bubbles, the fiber structure can be made dense and uniform, thereby improving the stability of the fiber.
[0030] In summary, this application includes at least one of the following beneficial technical effects: 1. Butanetetracarboxylic acid in cross-linked modified soy protein promotes the formation of a covalent cross-linked network in soy protein, which not only enhances its own structural stability, but also can be closely connected with soy isoflavones and regenerated cellulose through chemical bonds and physical entanglement, further improving the binding stability and breaking strength, and reducing the structural damage of the fiber caused by water absorption and swelling; soy isoflavones can produce intermolecular interactions with other components, such as hydrogen bonds and van der Waals forces, etc., which strengthen the binding stability between the components and lay the foundation for the stability of the entire fiber system; soy isoflavones have natural antibacterial activity, which can inhibit the growth and reproduction of bacteria. After combining with other components, they create an antibacterial environment inside and on the surface of the fiber, making it difficult for bacteria to survive, and giving the modified soybean fiber good antibacterial properties.
[0031] The ethoxysilane group of 2.3-aminopropyltriethoxysilane can undergo hydrolysis and condensation reaction with the hydroxyl groups on the surface of regenerated cellulose to form a layer of siloxane network structure on the surface of regenerated cellulose, thereby enhancing the stability of the regenerated cellulose structure itself; the aminopropyl group of 3-aminopropyltriethoxysilane reacts chemically with the active groups in soy isoflavones and cross-linked modified soy protein, such as carboxyl groups and amino groups, or forms hydrogen bonds and other interactions, thereby making the connection between the components tighter and improving the overall bonding stability and breaking strength of the fiber. The siloxane network structure is hydrophobic and can effectively block the invasion of water molecules, reduce the swelling and structural damage of regenerated cellulose caused by water absorption, thereby improving the wash resistance of the modified soybean fiber; the amino groups on the surface of the modified regenerated cellulose act synergistically with soy isoflavones to change the microenvironment for bacterial survival, inhibit the growth and reproduction of bacteria by interacting with the biological molecules on the bacterial surface, and enhance the antibacterial properties of the fiber.
[0032] 3. Tea polyphenols are rich in phenolic hydroxyl groups and have excellent antioxidant properties. During the fiber preparation process, they can scavenge free radicals in the system, prevent the oxidation of soy isoflavones, soy protein and other ingredients, maintain their molecular structure and activity, and ensure that each component can effectively function; Genipin has good cross-linking ability, and the active groups in its molecules can undergo cross-linking reactions with soy protein, modified regenerated cellulose and other ingredients containing amino and hydroxyl groups to form a stable covalent bond network, strengthen the internal structure of the fiber, limit the penetration of water molecules, and improve the fiber's water resistance; the cross-linking structure helps to fix the antibacterial components, synergize the antibacterial substances of tea polyphenols and the fiber itself, enhance the antibacterial properties, and improve the stability, water resistance, breaking strength and antibacterial properties of the modified soybean fiber. DETAILED DESCRIPTION
[0033] The present application discloses a modified soybean fiber and a preparation method thereof. Unless otherwise specified, the raw materials used in the present application can be obtained from commercially available raw materials. The present application is further described in detail below in conjunction with the examples: Ingredients: Soy protein (CAS No.: 9010-10-0), butanetetracarboxylic acid (CAS No.: 1703-58-8), 3-aminopropyltriethoxysilane (CAS No.: 919-30-2), soy isoflavones (CAS No.: 486-66-8), tannic acid (CAS No.: 1401-55-4), tea polyphenols (CAS No.: 84650-60-2), genipin (CAS No.: 6902-77-8), defoaming agent polyether modified silicone model is BYK-022, glycerol (CAS No.: 56-81-5), PEG-400 is polyethylene glycol-400 (CAS No.: 25322-68-3).
[0034] Example 1 Preparation of cross-linked modified soybean protein 11.54 g of soybean protein and 3.46 g of butanetetracarboxylic acid were mixed and dispersed in 250 mL of 0.1 mol / L sodium hydroxide solution, stirred at 500 rpm at 55° C. for 2 hours, and then dialyzed and freeze-dried at −20° C. to obtain cross-linked modified soybean protein.
[0035] Preparation of modified regenerated cellulose An ethanol solution of 5% by weight of 3-aminopropyltriethoxysilane was added to a bamboo pulp dispersion, with a mass ratio of 3-aminopropyltriethoxysilane to bamboo pulp being 1:10. The mixture was stirred at 60° C. and 200 rpm for 3 hours. After cooling to below 30° C., the mixture was washed with deionized water until neutral, and vacuum-dried at 60° C. to obtain a modified bamboo pulp. The modified bamboo pulp is subjected to the steps of impregnation, pressing, crushing, aging, xantholysis, dissolution, degassing and maturation to obtain a modified regenerated cellulose dispersion with a methyl cellulose content of 8.15-8.90%, an alkali content of 4.75-5.10%, a viscosity of 35-50s and a maturation degree of 10-14mL.
[0036] Preparation of modified soybean fiber (1) 1 g of soy isoflavones and 2.5 g of tannic acid were dissolved in 70 mL of 50% ethanol aqueous solution, and stirred at 200 rpm for 30 min to obtain a flavonoid mixed solution; 8 g of cross-linked modified soy protein and the above-prepared flavonoid mixed solution were mixed, and stirred at 200 rpm for 30 min to obtain a mixed solution; 0.5 g of stabilizer, 0.3 g of defoamer and the mixed solution were added to a modified regenerated cellulose dispersion containing 40 g of modified regenerated cellulose, wherein the mass ratio of tea polyphenols to genipin in the stabilizer was 1:0.5, and the mixture was stirred at 50°C at 200 rpm for 1 h to obtain a composite spinning solution; (2) filtering the composite spinning solution, and forming the filtered composite spinning solution into filaments by wet spinning, wherein the composition of the coagulation bath includes 120 g / L sulfuric acid, 300 g / L sodium sulfate, and 20 g / L zinc sulfate, and the coagulation bath temperature is 50° C.; (3) After the filaments are subjected to post-processing steps such as drawing, cutting, water washing, acid washing, and desulfurization, modified soybean fibers are obtained, and the single fiber fineness of the modified soybean fibers is 2.0D.
[0037] Example 2 Preparation of cross-linked modified soybean protein 10.71 g of soybean protein and 4.29 g of butanetetracarboxylic acid were mixed and dispersed in 250 mL of 0.1 mol / L sodium hydroxide solution, stirred at 500 rpm at 55° C. for 2 hours, and then freeze-dried at −20° C. after dialysis to obtain cross-linked modified soybean protein.
[0038] Preparation of modified regenerated cellulose An ethanol solution of 5% by weight of 3-aminopropyltriethoxysilane was added to a bamboo pulp dispersion, with a mass ratio of 3-aminopropyltriethoxysilane to bamboo pulp being 1:10. The mixture was stirred at 60° C. and 200 rpm for 3 hours. After cooling to below 30° C., the mixture was washed with deionized water until neutral, and vacuum-dried at 60° C. to obtain a modified bamboo pulp. The modified bamboo pulp is subjected to the steps of impregnation, pressing, crushing, aging, xantholysis, dissolution, degassing and maturation to obtain a modified regenerated cellulose dispersion with a methyl cellulose content of 8.15-8.90%, an alkali content of 4.75-5.10%, a viscosity of 35-50s and a maturation degree of 10-14mL.
[0039] Preparation of modified soybean fiber (1) 2 g of soy isoflavones and 3.33 g of tannic acid were dissolved in 70 mL of 50% ethanol aqueous solution, and stirred at 200 rpm for 30 min to obtain a flavonoid mixed solution; 6 g of cross-linked modified soy protein and the above-prepared flavonoid mixed solution were mixed, and stirred at 200 rpm for 30 min to obtain a mixed solution; 0.5 g of stabilizer, 0.3 g of defoamer and the mixed solution were added to a modified regenerated cellulose dispersion containing 50 g of modified regenerated cellulose, wherein the mass ratio of tea polyphenols to genipin in the stabilizer was 1:0.5, and the mixture was stirred at 50°C at 200 rpm for 1 h to obtain a composite spinning solution; (2) filtering the composite spinning solution, and forming the filtered composite spinning solution into filaments by wet spinning, wherein the composition of the coagulation bath includes 120 g / L sulfuric acid, 300 g / L sodium sulfate, and 20 g / L zinc sulfate, and the coagulation bath temperature is 50° C.; (3) After the filaments are subjected to post-processing steps such as drawing, cutting, water washing, acid washing, and desulfurization, modified soybean fibers are obtained, and the single fiber fineness of the modified soybean fibers is 2.0D.
[0040] Example 3 Preparation of cross-linked modified soybean protein 11.11 g of soybean protein and 3.89 g of butanetetracarboxylic acid were mixed and dispersed in 250 mL of 0.1 mol / L sodium hydroxide solution, stirred at 500 rpm at 55° C. for 2 hours, and then freeze-dried at −20° C. after dialysis to obtain cross-linked modified soybean protein.
[0041] Preparation of modified regenerated cellulose An ethanol solution of 5% by weight of 3-aminopropyltriethoxysilane was added to a bamboo pulp dispersion, with a mass ratio of 3-aminopropyltriethoxysilane to bamboo pulp being 1:10. The mixture was stirred at 60° C. and 200 rpm for 3 hours. After cooling to below 30° C., the mixture was washed with deionized water until neutral, and vacuum-dried at 60° C. to obtain a modified bamboo pulp. The modified bamboo pulp is subjected to the steps of impregnation, pressing, crushing, aging, xantholysis, dissolution, degassing and maturation to obtain a modified regenerated cellulose dispersion with a methyl cellulose content of 8.15-8.90%, an alkali content of 4.75-5.10%, a viscosity of 35-50s and a maturation degree of 10-14mL.
[0042] Preparation of modified soybean fiber (1) 1.5 g of soy isoflavones and 3 g of tannic acid were dissolved in 70 mL of 50% ethanol aqueous solution, and stirred at 200 rpm for 30 min to obtain a flavonoid mixed solution; 7 g of cross-linked modified soy protein was mixed with the above-prepared flavonoid mixed solution, and stirred at 200 rpm for 30 min to obtain a mixed solution, 0.5 g of stabilizer, 0.3 g of defoamer and the mixed solution were added to a modified regenerated cellulose dispersion containing 45 g of modified regenerated cellulose, wherein the mass ratio of tea polyphenols to genipin in the stabilizer was 1:0.5, and the mixture was stirred at 50°C at 200 rpm for 1 h to obtain a composite spinning solution; (2) filtering the composite spinning solution, and forming the filtered composite spinning solution into filaments by wet spinning, wherein the composition of the coagulation bath includes 120 g / L sulfuric acid, 300 g / L sodium sulfate, and 20 g / L zinc sulfate, and the coagulation bath temperature is 50° C.; (3) After the filaments are subjected to post-processing steps such as drawing, cutting, water washing, acid washing, and desulfurization, modified soybean fibers are obtained, and the single fiber fineness of the modified soybean fibers is 2.0D.
[0043] Example 4 Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in Example 4, the amount of soy protein used is 12.5 g, and the amount of butanetetracarboxylic acid used is 2.5 g.
[0044] Example 5 Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, the amount of soy protein used is 10 g and the amount of butanetetracarboxylic acid used is 5 g.
[0045] Example 6 Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that the mass ratio of tannic acid to soy isoflavones in Example 6 is 1:0.2.
[0046] Example 7 Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that the mass ratio of tannic acid to soy isoflavones in Example 7 is 1:0.8.
[0047] Example 8 Example 8 is based on Example 3. The only difference between Example 8 and Example 3 is that tannic acid is not added when preparing the modified soybean fiber in Example 8.
[0048] Example 9 Example 9 is based on Example 3. The only difference between Example 9 and Example 3 is that in Example 9, when preparing the modified soybean fiber, the regenerated cellulose is not modified, and the modified regenerated cellulose is replaced by regenerated cellulose.
[0049] Example 10 Example 10 is based on Example 3. The only difference between Example 10 and Example 3 is that the coagulation bath in Example 10 further includes 1 g / L silver nitrate, 6% by volume of glycerol, and 3% by volume of PEG-400.
[0050] Example 11 Example 11 is based on Example 3. The only difference between Example 11 and Example 3 is that in Example 11, no genipin is added to the stabilizer.
[0051] Example 12 Example 12 is based on Example 3. The only difference between Example 12 and Example 3 is that tea polyphenols are not added to the stabilizer in Example 12.
[0052] Comparative Example 1 Comparative Example 1 is based on Example 3. The only difference between Comparative Example 1 and Example 3 is that in Comparative Example 1, the cross-linked modified soy protein is replaced by soy protein.
[0053] Comparative Example 2 Comparative Example 2 is based on Example 3, and the only difference between Comparative Example 2 and Example 3 is that no stabilizer is added in Comparative Example 2.
[0054] Performance testing (1) GB / T 20944.3-2008 Evaluation of antibacterial properties of textiles Part 3: Oscillation method was selected as the standard to test the antibacterial rate of the test samples against Escherichia coli (A), Staphylococcus aureus (B) and Candida albicans (C). Three samples were prepared for each sample, and the average value was taken after measurement. The results are recorded in Table 1.
[0055] (2) Selecting "FZ / T 50018-2013 Test method for protein content of protein viscose fiber" as the standard, the soy protein content of the samples before washing and after washing 30 times was tested, and the soy protein retention rate was calculated. Each sample was tested three times, and the average value was taken after measurement. The results are recorded in Table 1.
[0056] (3) GB / T 23788-2009 Determination of isoflavones in soy products - High performance liquid chromatography method was selected as the standard to test the isoflavone content of the samples before and after washing, and calculate the retention rate. Each sample was tested three times, and the average value was taken after measurement. The results are recorded in Table 1.
[0057] (4) Select "GB / T 3916-2013 Textiles - Determination of breaking strength and elongation of single yarn in packaged yarn" to test and calculate the dry and wet breaking strength of the sample. Prepare three samples for each sample, take the average value after measurement, and record the results in Table 1.
[0058] Table 1 Test results of antibacterial properties, stability and washability of modified soybean fiber As can be seen from Table 1, the antibacterial rate of Escherichia coli in Examples 1-3 is greater than 96.1%, the antibacterial rate of Staphylococcus aureus is greater than 98.3%, the antibacterial rate of Candida albicans is greater than 88.6%, the soy protein retention rate is greater than 81.4%, the soy isoflavone retention rate is greater than 78.7%, the dry breaking strength is greater than 3.0 cN / dtex, and the wet breaking strength is greater than 1.7 cN / dtex. It can be seen that the modified soybean fiber prepared in this application has good antibacterial properties, stability, water washability and high breaking strength.
[0059] As can be seen from Table 1, the only difference between Examples 4 and 5 and Example 3 is that the mass ratio of soy protein to butane tetracarboxylic acid in Example 4 is 1:0.2, and the mass ratio of soy protein to butane tetracarboxylic acid in Example 5 is 1:0.5. Compared with Example 3, the performance of Examples 4 and 5 is reduced. This is because too little butane tetracarboxylic acid will lead to insufficient crosslinking, and the binding force, stability and breaking strength between components will decrease, thereby reducing the antibacterial rate and retention rate; too much butane tetracarboxylic acid can maintain a good retention rate through high crosslinking degree, but the antibacterial effect is slightly affected.
[0060] As can be seen from Table 1, the only difference between Examples 6, 7, and 8 and Example 3 is that the mass ratio of tannic acid to soy isoflavones in Example 6 is 1:0.2, the mass ratio of tannic acid to soy isoflavones in Example 7 is 1:0.8, and no tannic acid is added when preparing the modified soybean fiber in Example 8. Compared with Example 3, the performance of Examples 6, 7, and 8 is reduced. This is because too little tannic acid weakens the anchoring and antioxidant effects, and too much tannic acid may self-aggregate and compete for active sites, thereby reducing the stability of the fiber, affecting the antibacterial rate and retention rate, and affecting the breaking strength. Failure to add tannic acid will further reduce the performance.
[0061] As can be seen from Table 1, the only difference between Example 9 and Example 3 is that the modified regenerated cellulose is replaced by regenerated cellulose in Example 9. Compared with Example 3, the performance of Example 9 is reduced. This is because the compatibility and stability are reduced due to the lack of modification treatment with aminosilane, and the bonding force between the components is weakened, thereby reducing the breaking strength, antibacterial properties and stability.
[0062] As can be seen from Table 1, the only difference between Example 10 and Example 3 is that silver nitrate, propylene glycol and PEG-400 are added to the coagulation bath in Example 10, and the performance of Example 10 is improved compared with Example 3; this is because the addition of silver nitrate and polyols can regulate the structure between fibers, enhance the bonding force and synergistic effect, thereby improving the antibacterial performance, stability and water washability.
[0063] As can be seen from Table 1, the only difference between Examples 11 and 12 and Example 3 is that no genipin is added to the stabilizer in Example 11, and no tea polyphenols are added to the stabilizer in Example 12. Compared with Example 3, the performance of Examples 11 and 12 is reduced. This is because reducing the components in the stabilizer will affect the synergistic effect between the components, reduce the stability of the fiber structure, and thus reduce the performance.
[0064] As can be seen from Table 1, the only difference between Comparative Example 1 and Example 3 is that the cross-linked modified soy protein is replaced with soy protein in Comparative Example 1. Compared with Example 3, the performance of Comparative Example 1 is significantly reduced. This is because the lack of cross-linking modification reduces the binding force of soy protein to other components and weakens its own stability, thereby affecting the stability and antibacterial properties of the modified soy fiber.
[0065] As can be seen from Table 1, the only difference between Comparative Example 2 and Example 3 is that no stabilizer is added in Comparative Example 2. Compared with Example 3, the performance of Comparative Example 2 is significantly reduced. This is because the lack of stabilizer will affect the active components during the spinning process and be oxidized and destroyed, thereby affecting the stability of the modified soybean fiber, and further affecting its antibacterial properties and water washability.
[0066] This specific embodiment is merely an explanation of the present application and does not limit the present application. Based on the above description, relevant personnel can make various changes and modifications without departing from the technical scope of the present application. The technical scope of the present application is not limited to the contents of the specification and must be determined according to the scope of the claims.
Claims
1. A modified soybean fiber, characterized in that: The composition includes the following parts by weight: 1-2 servings of soy isoflavones 6-8 parts cross-linked modified soy protein 40-50 parts of regenerated cellulose; The raw materials for preparing the cross-linked modified soybean protein include soybean protein body and butane tetracarboxylic acid.
2. The modified soybean fiber according to claim 1, characterized in that: The mass ratio of the soybean protein body to butane tetracarboxylic acid is 1:(0.3-0.4).
3. The modified soybean fiber according to claim 1, characterized in that: The regenerated cellulose is modified by 3-aminopropyltriethoxysilane to obtain modified regenerated cellulose.
4. The modified soybean fiber according to claim 3, characterized in that: The modified regenerated cellulose is prepared by the following steps: Adding 3-aminopropyltriethoxysilane solution to bamboo pulp dispersion, heating and stirring to react, washing to neutrality after cooling, and drying to obtain modified bamboo pulp; The modified bamboo pulp is subjected to the steps of impregnation, pressing, crushing, aging, xantholysis, dissolution, degassing and ripening to obtain a dispersion of modified regenerated cellulose.
5. The modified soybean fiber according to claim 1, characterized in that: The modified soybean fiber also includes tannic acid as a component.
6. A method for preparing the modified soybean fiber according to any one of claims 1 to 5, characterized in that: The steps include: (1) dissolving soybean isoflavones and tannic acid in a solvent and stirring to obtain a flavonoid mixed solution; mixing the cross-linked modified soybean protein with the prepared flavonoid mixed solution and stirring to obtain a mixed solution; adding a stabilizer, a defoaming agent and the mixed solution to the modified regenerated cellulose dispersion, heating and stirring to react, and obtaining a composite spinning solution; (2) filtering the composite spinning solution, and forming the filtered composite spinning solution by wet spinning to obtain filaments, wherein the composition of the coagulation bath includes sulfuric acid, sodium sulfate and zinc sulfate; (3) The modified soybean fiber is obtained after the filaments are subjected to post-processing steps such as drawing, cutting, water washing, acid washing, and desulfurization.
7. The method for preparing modified soybean fiber according to claim 6, characterized in that: The mass ratio of the tannic acid to the soy isoflavones is 1:(0.4-0.6).
8. The method for preparing modified soybean fiber according to claim 6, wherein: The coagulation bath also includes silver nitrate and polyol.
9. The method for preparing modified soybean fiber according to claim 6, wherein: The stabilizer includes tea polyphenols and genipin.
10. The method for preparing modified soybean fiber according to claim 6, characterized in that: The defoaming agent includes polyether-modified silicone.