Textile printing and dyeing color fixing agent for improving color fastness and preparation method thereof

Abstract

The invention relates to the field of color fixing agents, in particular to a textile printing and dyeing color fixing agent capable of improving color fastness and a preparation method thereof, which are used for solving the problems that the existing textile printing and dyeing color fixing agent is not ideal in color fixing effect, influences the dyeing quality, has relatively large influence on the hand feeling of a fabric, and leads to a limited application range. The textile printing and dyeing color fixing agent can chemically react with fibers and dyes to form firm chemical bonds and form a highly diversified cross-linking system, so that the dyes and the fibers are tightly and firmly linked together, the dyes are prevented from falling off from the fibers, the color fastness of textile printed and dyed fabrics is further improved, the color fixing effect is remarkably improved, and the textile printing and dyeing color fixing agent is suitable for industrial production. A soft, elastic and wear-resistant protective film can be formed on the surface of the fiber, so that the fabric feels softer and smoother, the wearing comfort of the fabric is improved, the protective film is prevented from being damaged, the possibility that the dye falls off due to friction is reduced, and the color fastness of the fabric is further improved.

Description

Technical Field

[0001] The invention relates to the field of color fixing agents, and in particular to a textile printing and dyeing color fixing agent for improving color fastness and a preparation method thereof. Background Art

[0002] Cellulose fibers are made from natural cellulose (such as cotton, linen, bamboo, and wood pulp). Common examples include cotton, viscose, modal, and lyocell. Because cellulose fibers contain a large number of hydrophilic hydroxyl groups in their molecular structure, they can absorb and retain large amounts of water, making cellulose fiber products comfortable to wear and suitable for making undergarments. Cellulose fiber products are primarily dyed with reactive dyes, which are water-soluble dyes containing reactive groups. These dyes form covalent bonds with the cellulose fibers, but they are also susceptible to hydrolysis, dissolving and falling off the fibers, resulting in poor color fastness. Currently, while commonly used textile printing and dyeing fixing agents can improve color fastness to a certain extent, the fixing effect is less than ideal, affecting dyeing quality. They also significantly affect the feel of the fabric, making it rough and stiff, limiting their applicability.

[0003] Therefore, developing a textile printing and dyeing fixing agent that improves color fastness and a preparation method thereof has important practical significance. Summary of the Invention

[0004] In order to overcome the above technical problems, the purpose of the present invention is to provide a textile printing and dyeing fixing agent with improved color fastness and a preparation method thereof, which solves the problem that the existing textile printing and dyeing fixing agents have unsatisfactory color fixing effects, affect the dyeing quality, and have a significant impact on the feel of the fabric, resulting in a limited scope of application.

[0005] The purpose of the present invention can be achieved through the following technical solutions: A textile printing and dyeing fixing agent for improving color fastness, comprising the following components in parts by weight: 40-50 parts of modified cationic polymer, 18-32 parts of epoxy alkenyl polysiloxane, 5-13 parts of modified nano-alumina, 1-3 parts of triethylamine, 3-6 parts of penetrant, 1-2 parts of photoinitiator and 300-320 parts of deionized water; Wherein, the modified cationic polymer is prepared by the following steps: Dimethyldiallylammonium chloride, diallylamine, acrylamide, N-vinylimidazole, glacial acetic acid and deionized water are added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen protection is introduced. The mixture is stirred and reacted for 20-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min. Then, the temperature is raised to 70-75° C. and sodium persulfate solution and sodium metabisulfite solution are added dropwise while stirring. The dropping rate is controlled to 1-2 drops / s. After the addition is completed, the stirring reaction is continued for 3-4 hours. After the reaction is completed, the reaction product is cooled to room temperature and then added to anhydrous ethanol. The precipitate is then allowed to stand and then vacuum filtered. The filter cake is washed with anhydrous ether 2-3 times and then placed in a vacuum drying oven and dried at a temperature of 40-45° C. for 5-6 hours to obtain a modified cationic polymer.

[0006] As a further embodiment of the present invention, the usage ratio of the dimethyldiallylammonium chloride, diallylamine, acrylamide, N-vinylimidazole, glacial acetic acid, deionized water, sodium persulfate solution and sodium metabisulfite solution is 40-45 g: 12-24 g: 5-11 g: 4-8 g: 1.5-3.5 mL: 50-60 mL: 10-15 mL: 10-15 mL.

[0007] As a further solution of the present invention: the mass fraction of the sodium persulfate solution is 10-12%.

[0008] As a further solution of the present invention: the mass fraction of the sodium metabisulfite solution is 10-12%.

[0009] As a further embodiment of the present invention: the epoxy alkenyl polysiloxane is prepared by the following steps: Step a1: octamethylcyclotetrasiloxane, D4H cyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and tetramethyldisiloxane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced. The mixture is stirred at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 minutes, and then the mixture is heated to 90-95° C. and stirred for 20-30 minutes. After that, a tetramethylammonium hydroxide solution is added and the mixture is heated to 110-115° C. and stirred for 3-5 hours. After that, the mixture is heated to 150-160° C. and stirred for 2-3 hours. After the reaction is completed, the reaction product is cooled to room temperature and then placed in a vacuum drying oven and dried at 80-85° C. for 5-6 hours to obtain a hydroalkenyl polysiloxane; Step a2: Add hydrogenated alkenyl polysiloxane, allyl glycidyl ether and isopropanol to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, introduce nitrogen protection, and stir the reaction at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes. Then, add chloroplatinic acid solution and continue stirring the reaction at 80-85°C for 20-30 minutes, then continue stirring the reaction at 90-95°C for 3-5 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane.

[0010] As a further embodiment of the present invention: the usage ratio of the octamethylcyclotetrasiloxane, D4Hcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylammonium hydroxide solution in step a1 is 40-50 mmol: 11-23 mmol: 5-11 mmol: 3-5 mmol: 0.3-0.5 g.

[0011] As a further solution of the present invention: the mass fraction of the tetramethylammonium hydroxide solution in step a1 is 20-25%.

[0012] As a further embodiment of the present invention, the usage ratio of the hydrogenated alkenyl polysiloxane, allyl glycidyl ether, isopropyl alcohol and chloroplatinic acid solution in step a2 is 10 g: 1.1-3.7 g: 40-45 mL: 3-5 mL.

[0013] As a further solution of the present invention: the chloroplatinic acid solution in step a2 is a solution formed by dissolving chloroplatinic acid in isopropanol at a ratio of 1 g:49 g.

[0014] As a further solution of the present invention: the modified nano-alumina is prepared by the following steps: The silane coupling agent KH-560, anhydrous ethanol and hydrochloric acid solution are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The reaction is stirred for 30-40 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min. Then, nano-alumina is added and the temperature is raised to 90-95°C and the stirring reaction is continued for 5-6 hours. After the reaction is completed, the reaction product is cooled to room temperature and then vacuum filtered. The filter cake is washed with ethanol solution for 2-3 times, and then placed in a vacuum drying oven and dried at a temperature of 60-65°C for 3-4 hours to obtain modified nano-alumina.

[0015] As a further solution of the present invention: the usage ratio of the silane coupling agent KH-560, anhydrous ethanol, hydrochloric acid solution and nano-alumina is 0.8-2.4g:50-60mL:10-15mL:3g.

[0016] As a further solution of the present invention: the mass fraction of the hydrochloric acid solution is 20-22%.

[0017] As a further solution of the present invention: the average particle size of the nano-alumina is 30 nm.

[0018] As a further solution of the present invention: the volume fraction of the ethanol solution is 60-70%.

[0019] As a further embodiment of the present invention: a method for preparing a textile printing and dyeing fixing agent for improving color fastness comprises the following steps: Step 1: Weigh 40-50 parts of modified cationic polymer, 18-32 parts of epoxy alkenyl polysiloxane, 5-13 parts of modified nano-alumina, 1-3 parts of triethylamine, 3-6 parts of penetrant, 1-2 parts of photoinitiator and 300-320 parts of deionized water according to weight parts and set aside; Step 2: Add the modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stir and mix for 2-3 hours at a temperature of 40-50° C. and a stirring rate of 800-1000 r / min to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0020] As a further solution of the present invention: the penetrant is AEO-9 surfactant.

[0021] As a further solution of the present invention: the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal mass ratios.

[0022] Beneficial effects of the present invention: The invention discloses a textile printing and dyeing color-fixing agent for improving color fastness and a preparation method thereof. The invention comprises the following steps: a modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-aluminum oxide, triethylamine, a penetrant, a photoinitiator and deionized water are stirred and mixed to obtain the textile printing and dyeing color-fixing agent for improving color fastness. The textile printing and dyeing color-fixing agent can react chemically with fibers and dyes to form strong chemical bonds, thereby forming a highly diversified cross-linking system, so that the dyes and fibers are tightly and firmly linked together, thereby preventing the dyes from falling off the fibers, thereby improving the color fastness of the textile printed and dyed fabrics and significantly improving the color-fixing effect. The invention also forms a soft, elastic and wear-resistant protective film on the fiber surface, making the fabric feel softer and smoother, improving the wearing comfort of the fabric, and simultaneously avoiding damage to the protective film, reducing the possibility of the dyes falling off due to friction, and further improving the color fastness of the fabrics. The preparation method is simple in process and easy to operate, is suitable for industrial production, can maintain good stability under different conditions, and has a wide range of applications.

[0023] In the process of preparing a textile printing and dyeing fixing agent, a modified cationic polymer is first prepared. Dimethyldiallylammonium chloride, diallylamine, acrylamide, and N-vinylimidazole are copolymerized to form a polymer to obtain a modified cationic polymer. The modified cationic polymer contains a large amount of quaternary ammonium cations in its molecular structure, which can form ionic bonds with the anionic groups of the dye, block the water-soluble groups of the dye, and generate insoluble lakes on the fabric, making the dye on the fabric difficult to dissolve and fall off when exposed to water, thereby achieving the purpose of improving wet processing fastness. It can also introduce multiple amino groups, imino groups, and imidazole rings as active groups, which can chemically react with specific groups in the dye (such as chlorine atoms) to further enhance the stability of the dye. At the same time, it can also chemically react with other components in the fixing agent to make the bond between the dye and the fiber more firmly, thereby improving the color fastness of the fabric.

[0024] In the process of preparing the textile printing and dyeing fixing agent, an epoxy alkenyl polysiloxane is also prepared. Octamethylcyclotetrasiloxane, D4H cyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and tetramethyldisiloxane are used as raw materials for polymerization to form a polymer to obtain hydrogen alkenyl polysiloxane. Then, the hydrogen alkenyl polysiloxane and allyl glycidyl ether react, and the Si-H on the hydrogen alkenyl polysiloxane reacts with the alkenyl group on the allyl glycidyl ether to undergo a silylation reaction, while introducing a large number of epoxy groups to obtain epoxy alkenyl polysiloxane. The epoxy alkenyl polysiloxane The molecular structure of alkenyl polysiloxane contains a large number of epoxy groups, which can form a soft and elastic protective film on the fiber surface in the form of chemical bonds, thereby preventing external factors (such as water, detergents, friction, etc.) from eroding and destroying the dye molecules, reducing dye shedding, and improving the feel of the fabric, making the fabric softer and smoother. At the same time, the large number of alkenyl groups introduced can undergo photosensitive polymerization under the action of photoinitiators, thereby increasing the density of the protective film, further improving the stability of the protective film, and significantly improving the color fastness of the fabric.

[0025] In the process of preparing a textile printing and dyeing fixing agent, a modified nano-alumina is also prepared. The nano-alumina is treated with a silane coupling agent KH-560. The siloxane on the silane coupling agent KH-560 is hydrolyzed to form silanols that are grafted onto the surface of the nano-alumina particles. At the same time, a large number of epoxy groups are introduced to obtain modified nano-alumina. The modified nano-alumina can be evenly dispersed in the textile printing and dyeing fixing agent, and the epoxy groups are used to enable it to chemically react with modified cationic polymers, epoxy alkenyl polysiloxanes and fibers, so that the nano-alumina is tightly attached to the fibers or evenly distributed in the protective film. On the one hand, the nano-particle size of the nano-alumina is used to achieve a filling effect, thereby reducing the activity space of the dye molecules on the fibers, restricting the movement of the dye molecules, and thus reducing the shedding of the dye. On the other hand, the high strength and high hardness of the nano-alumina particles can strengthen the protective film, improve the wear resistance and washing resistance of the protective film, and indirectly improve the color fastness of the fabric. DETAILED DESCRIPTION

[0026] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention. Example 1

[0027] This embodiment is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 40 g of dimethyldiallylammonium chloride, 12 g of diallylamine, 5 g of acrylamide, 4 g of N-vinylimidazole, 1.5 mL of glacial acetic acid and 50 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 20 minutes at a temperature of 25° C. and a stirring rate of 300 r / min. Then, 10 mL of a 10% sodium persulfate solution and 10 mL of a 10% sodium metabisulfite solution were added dropwise while heating to 70° C. while stirring. The dropping rate was controlled to 1 drop / s. After the addition was completed, the stirring reaction was continued for 3 hours. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The precipitate was then allowed to stand and then vacuum filtered. The filter cake was washed twice with anhydrous ether and then placed in a vacuum drying oven and dried at 40° C. for 5 hours to obtain a modified cationic polymer. Step S2: 40 mmol octamethylcyclotetrasiloxane, 11 mmol D4H cyclotetrasiloxane, 5 mmol tetramethyltetravinylcyclotetrasiloxane and 3 mmol tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25 ° C and a stirring rate of 300 r / min for 20 minutes, and then the temperature was raised to 90 ° C and the stirring reaction was continued for 20 minutes. Then, 0.3 g of a 20% mass fraction of tetramethylammonium hydroxide solution was added and the temperature was raised to 110 ° C and the stirring reaction was continued for 3 hours. Then, the temperature was raised to 150 ° C and the stirring reaction was continued for 2 hours. After the reaction, the reaction product was cooled to room temperature and then placed in a vacuum drying oven and dried at a temperature of 80 ° C for 5 hours to obtain a hydrogenated alkenyl polysiloxane; Step S3: 10 g of hydrogenated alkenyl polysiloxane, 1.1 g of allyl glycidyl ether and 40 mL of isopropanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25° C. and a stirring rate of 300 r / min for 20 minutes. Then, 3 mL of chloroplatinic acid was dissolved in isopropanol at a ratio of 1 g:49 g and the mixture was heated to 80° C. The mixture was stirred for 20 minutes, and then heated to 90° C. The mixture was stirred for 3 hours. After the reaction, the reaction product was cooled to room temperature, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane; Step S4: 0.8 g of silane coupling agent KH-560, 50 mL of anhydrous ethanol, and 10 mL of a 20% mass fraction hydrochloric acid solution were added to a three-necked flask equipped with a stirrer, a thermometer, and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30 minutes at a temperature of 25° C. and a stirring rate of 300 r / min. Subsequently, 3 g of nano-alumina with an average particle size of 30 nm was added and the temperature was raised to 90° C. and the stirring reaction was continued for 5 hours. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed twice with a 60% volume fraction ethanol solution, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 3 hours to obtain modified nano-alumina. Step S5: Weigh 40 parts of a modified cationic polymer, 18 parts of epoxy alkenyl polysiloxane, 5 parts of modified nano-alumina, 1 part of triethylamine, 3 parts of a penetrant, 1 part of a photoinitiator, and 300 parts of deionized water in parts by weight and set aside; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal mass ratios; Step S6: adding the modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 40° C. and a stirring rate of 800 r / min for 2 h to obtain a textile printing and dyeing fixing agent with improved color fastness. Example 2

[0028] This embodiment is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 42 g of dimethyldiallylammonium chloride, 18 g of diallylamine, 8 g of acrylamide, 6 g of N-vinylimidazole, 2.5 mL of glacial acetic acid and 55 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The reaction was stirred at a temperature of 28 ° C and a stirring rate of 350 r / min for 25 min, and then 12 ml of acetic acid was added dropwise while stirring at 72 ° C. 1 mL of 11% sodium persulfate solution and 12 mL of 11% sodium metabisulfite solution were added at a dropping rate of 1 drop / s. After the addition was complete, stirring and reacting were continued for 3.5 hours. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The product was allowed to stand for precipitation and then vacuum filtered. The filter cake was washed twice with anhydrous ether and then placed in a vacuum drying oven and dried at 42°C for 5.5 hours to obtain a modified cationic polymer. Step S2: 45 mmol octamethylcyclotetrasiloxane, 17 mmol D4H cyclotetrasiloxane, 8 mmol tetramethyltetravinylcyclotetrasiloxane and 4 mmol tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 28 ° C and a stirring rate of 350 r / min for 25 minutes, and then the temperature was raised to 92 ° C and the stirring reaction was continued for 25 minutes. Then, 0.4 g of a 22% mass fraction of tetramethylammonium hydroxide solution was added and the temperature was raised to 112 ° C and the stirring reaction was continued for 4 hours. Then, the temperature was raised to 155 ° C and the stirring reaction was continued for 2.5 hours. After the reaction, the reaction product was cooled to room temperature and then placed in a vacuum drying oven and dried at a temperature of 82 ° C for 5.5 hours to obtain a hydroalkenyl polysiloxane; Step S3: 10 g of hydrogenated alkenyl polysiloxane, 2.4 g of allyl glycidyl ether and 42 mL of isopropanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 28° C. and a stirring rate of 350 r / min for 25 minutes. Then, 4 mL of chloroplatinic acid was dissolved in isopropanol at a ratio of 1 g:49 g and the mixture was heated to 82° C. The mixture was stirred for 25 minutes, and then heated to 92° C. The mixture was stirred for 4 hours. After the reaction, the reaction product was cooled to room temperature, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane; Step S4: 1.6 g of silane coupling agent KH-560, 55 mL of anhydrous ethanol, and 12 mL of a 21% mass fraction hydrochloric acid solution were added to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 35 minutes at a temperature of 28° C. and a stirring rate of 350 r / min. Subsequently, 3 g of nano-alumina with an average particle size of 30 nm was added and the temperature was raised to 92° C. and the stirring reaction was continued for 5.5 hours. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed twice with a 65% volume fraction ethanol solution, and then placed in a vacuum drying oven and dried at a temperature of 62° C. for 3.5 hours to obtain modified nano-alumina. Step S5: Weigh 45 parts of a modified cationic polymer, 25 parts of epoxy alkenyl polysiloxane, 8 parts of modified nano-alumina, 2 parts of triethylamine, 4.5 parts of a penetrant, 1.5 parts of a photoinitiator, and 310 parts of deionized water in parts by weight for later use; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal weight ratios; Step S6: adding the modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 45° C. and a stirring rate of 900 r / min for 2.5 hours to obtain a textile printing and dyeing fixing agent with improved color fastness. Example 3

[0029] This embodiment is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 45g of dimethyldiallylammonium chloride, 24g of diallylamine, 11g of acrylamide, 8g of N-vinylimidazole, 3.5mL of glacial acetic acid and 60mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 400r / min. Then, 15mL of a 12% sodium persulfate solution and 15mL of a 12% sodium metabisulfite solution were added dropwise while heating to 75°C while stirring. The dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The precipitate was then allowed to stand and then vacuum filtered. The filter cake was washed 3 times with anhydrous ether and then placed in a vacuum drying oven and dried at 45°C for 6h to obtain a modified cationic polymer. Step S2: 50 mmol octamethylcyclotetrasiloxane, 23 mmol D4H cyclotetrasiloxane, 11 mmol tetramethyltetravinylcyclotetrasiloxane and 5 mmol tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 minutes, and then the temperature was raised to 95 ° C and the stirring reaction was continued for 30 minutes. Then, 0.5 g of a 25% mass fraction of tetramethylammonium hydroxide solution was added and the temperature was raised to 115 ° C and the stirring reaction was continued for 5 hours. Then, the temperature was raised to 160 ° C and the stirring reaction was continued for 3 hours. After the reaction, the reaction product was cooled to room temperature and then placed in a vacuum drying oven and dried at a temperature of 85 ° C for 6 hours to obtain a hydrogenated alkenyl polysiloxane; Step S3: 10 g of hydrogenated alkenyl polysiloxane, 3.7 g of allyl glycidyl ether and 45 mL of isopropanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. Then, 5 mL of chloroplatinic acid was dissolved in isopropanol at a ratio of 1 g:49 g and the mixture was heated to 85° C. The mixture was stirred for 30 minutes, and then heated to 95° C. The mixture was stirred for 5 hours. After the reaction, the reaction product was cooled to room temperature, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane; Step S4: 2.4 g of silane coupling agent KH-560, 60 mL of anhydrous ethanol, and 15 mL of a 22% mass fraction hydrochloric acid solution were added to a three-necked flask equipped with a stirrer, a thermometer, and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 40 minutes at a temperature of 30° C. and a stirring rate of 400 r / min. Subsequently, 3 g of nano-alumina with an average particle size of 30 nm was added and the temperature was raised to 95° C. and the stirring reaction was continued for 6 hours. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed three times with a 70% volume fraction ethanol solution, and then placed in a vacuum drying oven and dried at a temperature of 65° C. for 4 hours to obtain modified nano-alumina. Step S5: Weigh 50 parts of a modified cationic polymer, 32 parts of epoxy alkenyl polysiloxane, 13 parts of modified nano-alumina, 3 parts of triethylamine, 6 parts of a penetrant, 2 parts of a photoinitiator, and 320 parts of deionized water in parts by weight and set aside; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal mass ratios; Step S6: adding the modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 50° C. and a stirring rate of 1000 r / min for 3 hours to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0030] Comparative Example 1: This comparative example is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 45g of dimethyldiallylammonium chloride, 24g of diallylamine, 11g of acrylamide, 8g of N-vinylimidazole, 3.5mL of glacial acetic acid and 60mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 400r / min. Then, 15mL of a 12% sodium persulfate solution and 15mL of a 12% sodium metabisulfite solution were added dropwise while heating to 75°C while stirring. The dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The precipitate was then allowed to stand and then vacuum filtered. The filter cake was washed 3 times with anhydrous ether and then placed in a vacuum drying oven and dried at 45°C for 6h to obtain a modified cationic polymer. Step S2: Weigh 50 parts of a modified cationic polymer, 3 parts of triethylamine, 6 parts of a penetrant, 2 parts of a photoinitiator, and 320 parts of deionized water in parts by weight and set aside; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal weight ratios; Step S3: adding the modified cationic polymer, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 50° C. and a stirring rate of 1000 r / min for 3 hours to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0031] Comparative Example 2: This comparative example is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 50 mmol octamethylcyclotetrasiloxane, 23 mmol D4H cyclotetrasiloxane, 11 mmol tetramethyltetravinylcyclotetrasiloxane and 5 mmol tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 minutes, and then the temperature was raised to 95 ° C and the stirring reaction was continued for 30 minutes. Then, 0.5 g of a 25% mass fraction of tetramethylammonium hydroxide solution was added and the temperature was raised to 115 ° C and the stirring reaction was continued for 5 hours. Then, the temperature was raised to 160 ° C and the stirring reaction was continued for 3 hours. After the reaction, the reaction product was cooled to room temperature and then placed in a vacuum drying oven and dried at a temperature of 85 ° C for 6 hours to obtain a hydroalkenyl polysiloxane; Step S2: 10 g of hydrogenated alkenyl polysiloxane, 3.7 g of allyl glycidyl ether and 45 mL of isopropanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. Then, 5 mL of chloroplatinic acid was dissolved in isopropanol at a ratio of 1 g:49 g and the mixture was heated to 85° C. The mixture was stirred for 30 minutes, and then heated to 95° C. The mixture was stirred for 5 hours. After the reaction, the reaction product was cooled to room temperature, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane; Step S3: 32 parts of epoxy alkenyl polysiloxane, 3 parts of triethylamine, 6 parts of penetrant, 2 parts of photoinitiator, and 320 parts of deionized water are weighed and set aside; the penetrant is AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal mass ratios; Step S4: adding epoxy alkenyl polysiloxane, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 50° C. and a stirring rate of 1000 r / min for 3 hours to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0032] Comparative Example 3: This comparative example is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 45g of dimethyldiallylammonium chloride, 24g of diallylamine, 11g of acrylamide, 8g of N-vinylimidazole, 3.5mL of glacial acetic acid and 60mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 400r / min. Then, 15mL of a 12% sodium persulfate solution and 15mL of a 12% sodium metabisulfite solution were added dropwise while heating to 75°C while stirring. The dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The precipitate was then allowed to stand and then vacuum filtered. The filter cake was washed 3 times with anhydrous ether and then placed in a vacuum drying oven and dried at 45°C for 6h to obtain a modified cationic polymer. Step S2: 50 mmol octamethylcyclotetrasiloxane, 23 mmol D4H cyclotetrasiloxane, 11 mmol tetramethyltetravinylcyclotetrasiloxane and 5 mmol tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 minutes, and then the temperature was raised to 95 ° C and the stirring reaction was continued for 30 minutes. Then, 0.5 g of a 25% mass fraction of tetramethylammonium hydroxide solution was added and the temperature was raised to 115 ° C and the stirring reaction was continued for 5 hours. Then, the temperature was raised to 160 ° C and the stirring reaction was continued for 3 hours. After the reaction, the reaction product was cooled to room temperature and then placed in a vacuum drying oven and dried at a temperature of 85 ° C for 6 hours to obtain a hydrogenated alkenyl polysiloxane; Step S3: 10 g of hydrogenated alkenyl polysiloxane, 3.7 g of allyl glycidyl ether and 45 mL of isopropanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. Then, 5 mL of chloroplatinic acid was dissolved in isopropanol at a ratio of 1 g:49 g and the mixture was heated to 85° C. The mixture was stirred for 30 minutes, and then heated to 95° C. The mixture was stirred for 5 hours. After the reaction, the reaction product was cooled to room temperature, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain epoxy alkenyl polysiloxane; Step S4: Weigh 50 parts of a modified cationic polymer, 32 parts of epoxy alkenyl polysiloxane, 3 parts of triethylamine, 6 parts of a penetrant, 2 parts of a photoinitiator, and 320 parts of deionized water in parts by weight and set aside; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal weight ratios; Step S5: adding the modified cationic polymer, epoxy alkenyl polysiloxane, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 50° C. and a stirring rate of 1000 r / min for 3 hours to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0033] Comparative Example 4: This comparative example is a method for preparing a textile printing and dyeing fixing agent for improving color fastness, comprising the following steps: Step S1: 45g of dimethyldiallylammonium chloride, 24g of diallylamine, 11g of acrylamide, 8g of N-vinylimidazole, 3.5mL of glacial acetic acid and 60mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 400r / min. Then, 15mL of a 12% sodium persulfate solution and 15mL of a 12% sodium metabisulfite solution were added dropwise while heating to 75°C while stirring. The dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then added to anhydrous ethanol. The precipitate was then allowed to stand and then vacuum filtered. The filter cake was washed 3 times with anhydrous ether and then placed in a vacuum drying oven and dried at 45°C for 6h to obtain a modified cationic polymer. Step S2: 2.4 g of silane coupling agent KH-560, 60 mL of anhydrous ethanol, and 15 mL of a 22% mass fraction hydrochloric acid solution were added to a three-necked flask equipped with a stirrer, a thermometer, and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 40 minutes at a temperature of 30° C. and a stirring rate of 400 r / min. Subsequently, 3 g of nano-alumina with an average particle size of 30 nm was added and the temperature was raised to 95° C. and the stirring reaction was continued for 6 hours. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed three times with a 70% volume fraction ethanol solution, and then placed in a vacuum drying oven and dried at a temperature of 65° C. for 4 hours to obtain modified nano-alumina. Step S3: Weigh 50 parts of a modified cationic polymer, 13 parts of modified nano-alumina, 3 parts of triethylamine, 6 parts of a penetrant, 2 parts of a photoinitiator, and 320 parts of deionized water in parts by weight and set aside; the penetrant is an AEO-9 surfactant; the photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal weight ratios; Step S4: adding the modified cationic polymer, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stirring and mixing at a temperature of 50° C. and a stirring rate of 1000 r / min for 3 hours to obtain a textile printing and dyeing fixing agent with improved color fastness.

[0034] The textile printing and dyeing fixing agents of Examples 1-3 and Comparative Examples 1-4 were diluted in clean water to prepare a 5% fixing solution, and the dyed pure cotton cloth (dyed with 2% Reactive Red 11 relative to the weight of the fabric) was immersed in the fixing solution at a bath ratio of 1:10 for 30 minutes, and then immersed and rolled at a rolling rate of 80%, and then baked at 120°C for 20 minutes, and taken out to obtain a control sample; wherein, the blank sample was fixed according to the above process using clean water without adding the fixing agent.

[0035] The control sample and blank sample were tested for color fastness to soaping according to GB / T 3921-2008, and for color fastness to rubbing according to GB / T 3920-2008. The test results are shown in the following table:

[0036] Referring to the data in the above table, based on the comparison between Examples 1-3, Comparative Examples 1-4 and the blank sample, it can be seen that the textile printing and dyeing fixing agent of the present application has excellent color fastness.

[0037] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0038] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in similar ways. As long as they do not deviate from the invention or exceed the scope defined in this application, they should all fall within the scope of protection of the present invention.

Claims

1. A textile printing and dyeing fixing agent for improving color fastness, characterized in that: It comprises the following components in parts by weight: 40-50 parts of modified cationic polymer, 18-32 parts of epoxy alkenyl polysiloxane, 5-13 parts of modified nano-alumina, 1-3 parts of triethylamine, 3-6 parts of penetrant, 1-2 parts of photoinitiator and 300-320 parts of deionized water; Wherein, the modified cationic polymer is prepared by the following steps: Dimethyldiallylammonium chloride, diallylamine, acrylamide, N-vinylimidazole, glacial acetic acid and deionized water are stirred for reaction, and then a sodium persulfate solution and a sodium metabisulfite solution are added dropwise while stirring. After the addition is completed, the stirring reaction is continued. After the reaction is completed, the reaction product is cooled, and then added to anhydrous ethanol and allowed to stand for precipitation. Then, vacuum filtration is performed, and the filter cake is washed and dried to obtain a modified cationic polymer.

2. A textile printing and dyeing fixing agent for improving color fastness according to claim 1, characterized in that: The usage ratio of the dimethyldiallylammonium chloride, diallylamine, acrylamide, N-vinylimidazole, glacial acetic acid, deionized water, sodium persulfate solution and sodium metabisulfite solution is 40-45 g: 12-24 g: 5-11 g: 4-8 g: 1.5-3.5 mL: 50-60 mL: 10-15 mL: 10-15 mL; the mass fraction of the sodium persulfate solution is 10-12%; the mass fraction of the sodium metabisulfite solution is 10-12%.

3. A textile printing and dyeing fixing agent for improving color fastness according to claim 1, characterized in that: The epoxy alkenyl polysiloxane is prepared by the following steps: Step a1: octamethylcyclotetrasiloxane, D4H cyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane and tetramethyldisiloxane are stirred and reacted, and then tetramethylammonium hydroxide solution is added and the stirring reaction is continued. After the reaction is completed, the reaction product is cooled and then dried to obtain a hydroalkenyl polysiloxane; Step a2: stirring the epoxy alkenyl polysiloxane, allyl glycidyl ether and isopropyl alcohol, then adding chloroplatinic acid solution and continuing to stir the reaction. After the reaction is completed, the reaction product is cooled, then vacuum filtered, and the filtrate is rotary evaporated to obtain epoxy alkenyl polysiloxane.

4. A textile printing and dyeing fixing agent for improving color fastness according to claim 3, characterized in that: The usage ratio of the octamethylcyclotetrasiloxane, D4Hcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane, tetramethyldisiloxane and tetramethylammonium hydroxide solution in step a1 is 40-50 mmol: 11-23 mmol: 5-11 mmol: 3-5 mmol: 0.3-0.5 g; the mass fraction of the tetramethylammonium hydroxide solution is 20-25%.

5. A textile printing and dyeing fixing agent for improving color fastness according to claim 3, characterized in that: The amount ratio of the hydroalkenyl polysiloxane, allyl glycidyl ether, isopropyl alcohol and chloroplatinic acid solution in step a2 is 10g:1.1-3.7g:40-45mL:3-5mL; the chloroplatinic acid solution is a solution formed by dissolving chloroplatinic acid in isopropyl alcohol at a ratio of 1g:49g.

6. A textile printing and dyeing fixing agent for improving color fastness according to claim 1, characterized in that: The modified nano-alumina is prepared by the following steps: The silane coupling agent KH-560, anhydrous ethanol and hydrochloric acid solution are stirred and reacted, and then nano-alumina is added and the stirring reaction is continued. After the reaction is completed, the reaction product is cooled and then vacuum filtered. The filter cake is washed and dried to obtain modified nano-alumina.

7. A textile printing and dyeing fixing agent for improving color fastness according to claim 6, characterized in that: The usage ratio of the silane coupling agent KH-560, anhydrous ethanol, hydrochloric acid solution and nano-alumina is 0.8-2.4g:50-60mL:10-15mL:3g; the mass fraction of the hydrochloric acid solution is 20-22%; and the average particle size of the nano-alumina is 30nm.

8. A method for preparing a textile printing and dyeing fixing agent for improving color fastness, characterized in that: The following steps are involved: Step 1: Weigh 40-50 parts of modified cationic polymer, 18-32 parts of epoxy alkenyl polysiloxane, 5-13 parts of modified nano-alumina, 1-3 parts of triethylamine, 3-6 parts of penetrant, 1-2 parts of photoinitiator and 300-320 parts of deionized water according to weight parts and set aside; Step 2: Add the modified cationic polymer, epoxy alkenyl polysiloxane, modified nano-alumina, triethylamine, penetrant, photoinitiator and deionized water into a mixer, stir and mix for 2-3 hours at a temperature of 40-50° C. and a stirring rate of 800-1000 r / min to obtain a textile printing and dyeing fixing agent with improved color fastness.

9. The method for preparing a textile printing and dyeing fixing agent for improving color fastness according to claim 8, characterized in that: The penetrant is AEO-9 surfactant; The photoinitiator is a mixture of hydroxycyclohexane phenone and benzoin isopropyl ether in equal mass ratio.

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