Softening agent for acrylic finishing and preparation method thereof
Through the combination of the modified amino silicone oil and the specific emulsifier, the problem of commercially available amino silicone oil poor effect in acrylic finishing is solved, significantly improving the clarity and feel of acrylic finishing, and achieving better adhesion of softener and chemical stability.
Patent Information
- Application Number
- CN202411444789.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-16
- Publication Date
- 2025-01-07
AI Technical Summary
Commercially available amino silicone oil is not effective in acrylic finishing and cannot meet market demand, especially in improving the clarity and feel.
Using the preparation method of modified amino silicone oil, a highly active silane coupling agent is formed through the reaction of silane coupling agent, modified monomer and hydrolyzing agent, and combined with basic raw materials and catalysts to form strong polarity and hydrophilicity. The amino silicone oil enhances its binding and adhesion with acrylic fibers, while using a specific emulsifier combination to reduce the surface tension of water and oil, forming a stable emulsion to improve uniform dispersion and penetration of the softener.
It significantly improves the clarity and feel of acrylic finish, enhances the adhesion and chemical stability of the softener, and makes the fabric softer and lasting.
Smart Images

Figure SMS_1
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of softeners, and in particular relates to a softener for acrylic fiber finishing and a preparation method thereof. Background Art
[0002] Acrylic (PAN) is a synthetic fiber commonly used in textiles, carpets, industrial products and many other applications. The production process of acrylic mainly includes polymerization, spinning, stretching, heat setting and other steps. First, a polyacrylonitrile solution is obtained through free radical polymerization, and then extruded through a spinneret to form a filament, which is then stretched to increase strength and heat-set to give the fiber the required physical properties. Acrylic has a wide range of applications in many fields due to its unique combination of properties, especially in those occasions where the material needs to have high strength, chemical resistance and easy dyeing.
[0003] Finishing softeners are a class of chemicals used to improve the feel and softness of fabrics during the textile production process. These softeners can be applied to a variety of fabrics, including natural fibers (such as cotton and wool) and synthetic fibers (such as polyester and acrylic). The main purpose of softeners is to make fabrics softer and more comfortable, and sometimes they can also give fabrics other properties such as antistatic and wrinkle resistance. There are several types of softeners: Cationic softeners: These softeners are usually quaternary ammonium salt compounds. They have a positive charge and can adsorb to negatively charged fibers to make the fabric soft. Cationic softeners have a good effect on cotton, man-made fibers, etc. Nonionic softeners: These softeners do not contain an electric charge. They achieve the softening effect by reducing the friction between fibers. Nonionic softeners are usually used for synthetic fibers such as polyester. Silicone oil-based softeners: Polysiloxane, or silicone oil, is a widely used softener. They can form a smooth film on the surface of the fabric, which not only increases softness, but also may bring additional functions such as waterproofing and stain resistance. Wax-based softeners: These softeners are based on natural or synthetic waxes and can form a protective layer on the surface of fabrics, making them feel softer. Fatty acid ester softeners: These softeners contain long-chain fatty acid esters, which can improve the feel of fabrics. Bio-based softeners: In recent years, with the improvement of environmental awareness, some biodegradable softeners have also been developed, which are usually derived from renewable resources such as vegetable oils.
[0004] Softeners are usually applied to fabrics in the finishing stage after dyeing or printing by dipping, padding, spraying, etc. The specific application method will vary depending on the type of fabric, the type of softener, and the desired effect. Summary of the invention
[0005] The purpose of the present invention is to provide a softener for acrylic fiber finishing and a preparation method thereof.
[0006] In order to achieve the above object, the present invention provides the following technical solutions: A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 to 15 parts of modified amino silicone oil, 8 to 10 parts of emulsifier, 1 to 3 parts of glacial acetic acid, 12 to 16 parts of polyvinyl alcohol, 5 to 7 parts of ternary copolymer silicone oil, 12 to 15 parts of polyethylene glycol fatty acid ester, 2 to 3 parts of stabilizer, 2 to 4 parts of stiffening agent and 50 to 60 parts of water.
[0007] Furthermore, the preparation method of the modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4-3.7 parts; modified monomer: glycidyl methacrylate, 2.6-2.9 parts; hydrolyzing agent: deionized water, 0.55-0.6 parts; basic raw material: octamethylcyclotetrasiloxane, 80-82 parts; solvent: dimethylformamide, 14-15 parts; catalyst: potassium hydroxide, 0.01-0.03 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70-75°C, the modified monomer is added dropwise under heat preservation conditions for 3-4 hours. After the addition is completed, the mixture is stirred for 4-5 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90-95°C, keep the temperature for reaction for 1-2 hours, then lower the temperature to 50-53°C, vacuum and remove the low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature rises to 90-95°C, react for 20-30 minutes, maintain the temperature at 95-97°C, continue to heat and stir the reaction for 4-6 hours, cool to room temperature, and obtain modified amino silicone oil.
[0008] Furthermore, the silane coupling agent is selected from one or more of KH550, KH570, and KH590.
[0009] Furthermore, the silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2-1.5:0.6-0.8.
[0010] At present, the effect of finishing with commercially available amino silicone oil still cannot meet the market demand. The modified amino silicone oil prepared by the present invention can improve the stiffness and feel of acrylic fiber finishing with softener, because of its special chemical structure and the advantages brought by the functional groups introduced in the modification process. The amino group in the amino silicone oil of the present invention has strong polarity and hydrophilicity, and can form hydrogen bonds or other chemical bonds with the polar groups (such as cyano) on the surface of acrylic fiber, thereby enhancing the bonding force between the softener and the fiber. The amino group in the amino silicone oil can react with the fiber surface to form a thin film covering the fiber surface, reducing the friction between the fibers, thereby making the fabric softer. Glycidyl methacrylate (GMA): As a modified monomer, GMA can react with the amino group in the amino silicone oil to form a more stable cross-linked structure, thereby enhancing the stiffness of the fabric. At the same time, GMA can also increase the adhesion of the softener, making its distribution on the fabric more uniform. The silane coupling agent can be used as a bridge to connect the amino silicone oil and the acrylic fiber, enhance the interfacial bonding force between the two, and improve the durability and stability of the softener. The silane coupling agent reacts with the hydroxyl group on the fiber surface to enhance the chemical stability of the softener, making it difficult to decompose during processing. Through hydrolysis and polymerization, a stable network structure is formed, which not only enhances the adhesion of the softener, but also forms a uniform protective film on the fabric surface, further improving the feel of the fabric. The modified amino silicone oil of the present invention can not only form a firm combination with the acrylic fiber, but also form a uniform film on the fabric surface, reduce the friction between the fibers, and increase the softness of the fabric. At the same time, the functional groups introduced in the modification process make the softener have better adhesion and chemical stability, further improving the stiffness and feel of the fabric.
[0011] Furthermore, the stabilizer is sodium tridecanol polyoxyethylene ether carboxylate.
[0012] Furthermore, the stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0013] Furthermore, the emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3-0.5:1.4-1.7.
[0014] In textile finishing, emulsifiers are essential for the effective application of softeners. The main function of emulsifiers is to form a stable emulsion between modified amino silicone oil and aqueous medium, so that oily softeners can be evenly dispersed in water and more easily absorbed by fibers. Conventional emulsifiers cannot meet the requirements of forming a stable emulsion between amino silicone oil and water in the present invention. The addition of a specific emulsifier combination (isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate) in the present invention can improve the softener finishing effect on acrylic fibers, significantly reduce the surface tension between water and oil, and enable oily softeners to be better dispersed in water to form a stable emulsion, forming a protective film on the oil-water interface to prevent oil droplets from agglomerating and keep the emulsion stable. It helps the softener to be more evenly distributed on the fabric surface and more easily penetrate into the fiber, thereby improving its coverage and adhesion efficiency.
[0015] Furthermore, the polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0016] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60-80° C., stirring evenly, to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0017] Compared with the prior art, the advantages and beneficial effects of the present invention are: 1. The modified amino silicone oil of the present invention can not only form a firm bond with acrylic fiber, but also form a uniform film on the surface of the fabric, reduce the friction between fibers, and increase the softness of the fabric. At the same time, the functional groups introduced during the modification process make the softener have better adhesion and chemical stability, further improving the stiffness and feel of the fabric.
[0018] 2. The addition of a specific emulsifier combination (isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate) in the present invention can improve the finishing effect of the softener on acrylic fiber, significantly reduce the surface tension between water and oil, and enable the oily softener to be better dispersed in water to form a stable emulsion, and form a protective film on the oil-water interface to prevent oil droplets from agglomerating and keep the emulsion stable. It helps the softener to be more evenly distributed on the fabric surface and more easily penetrate into the fiber, thereby improving its coverage and adhesion efficiency. DETAILED DESCRIPTION
[0019] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0020] Example 1 The present embodiment provides a softener for acrylic fiber finishing, comprising the following components in parts by weight: 12 parts of modified amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffness agent, and 50 parts of water.
[0021] The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4 parts; modified monomer: glycidyl methacrylate, 2.6 parts; hydrolyzing agent: deionized water, 0.55 parts; basic raw material: octamethylcyclotetrasiloxane, 80 parts; solvent: dimethylformamide, 14 parts; catalyst: potassium hydroxide, 0.01 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70° C., the modified monomer is added dropwise under heat preservation conditions for 3 hours. After the addition is completed, the mixture is stirred for 4 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90° C., keep the temperature for reaction for 1 hour, then lower the temperature to 50° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature reaches 90°C, react for 20 minutes, maintain the temperature at 95°C, continue to heat and stir the reaction for 4 hours, cool to room temperature, and obtain modified amino silicone oil.
[0022] The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2:0.6.
[0023] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0024] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0025] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3:1.4.
[0026] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0027] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0028] Example 2 The present embodiment provides a softener for acrylic finishing, comprising the following components in parts by weight: 15 parts of modified amino silicone oil, 10 parts of emulsifier, 3 parts of glacial acetic acid, 16 parts of polyvinyl alcohol, 7 parts of ternary copolymer silicone oil, 15 parts of polyethylene glycol fatty acid ester, 3 parts of stabilizer, 4 parts of stiffening agent, and 60 parts of water.
[0029] The preparation method of modified amino silicone oil is: Step 1: The formula includes the following components in parts by weight: silane coupling agent, 3.7 parts; modified monomer: glycidyl methacrylate, 2.9 parts; hydrolyzing agent: deionized water, 0.6 parts; basic raw material: octamethylcyclotetrasiloxane, 82 parts; solvent: dimethylformamide, 15 parts; catalyst: potassium hydroxide, 0.03 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 75°C, the modified monomer is added dropwise under heat preservation conditions for 4 hours. After the addition is completed, the mixture is stirred for 5 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 95° C., keep the temperature for 2 hours, then lower the temperature to 53° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature rises to 95°C, react for 30 minutes, maintain the temperature at 97°C, continue to stir and react for 6 hours, cool to room temperature, and obtain modified amino silicone oil.
[0030] The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1: 1.5: 0.8.
[0031] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0032] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0033] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1: 0.5: 1.7.
[0034] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0035] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 80° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0036] Comparative Example 1 The difference between this comparative example and Example 1 is that the commercially available amino silicone oil is purchased from Maclean, item number: A909718.
[0037] A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 parts of amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffening agent and 50 parts of water.
[0038] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0039] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0040] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3:1.4.
[0041] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0042] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mix the amino silicone oil, emulsifier, part of the water and glacial acetic acid and stir them evenly to prepare a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0043] Comparative Example 2 The difference between this comparative example and Example 1 is that the silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1:1.
[0044] A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 parts of modified amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffening agent and 50 parts of water.
[0045] The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4 parts; modified monomer: glycidyl methacrylate, 2.6 parts; hydrolyzing agent: deionized water, 0.55 parts; basic raw material: octamethylcyclotetrasiloxane, 80 parts; solvent: dimethylformamide, 14 parts; catalyst: potassium hydroxide, 0.01 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70° C., the modified monomer is added dropwise under heat preservation conditions for 3 hours. After the addition is completed, the mixture is stirred for 4 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90° C., keep the temperature for reaction for 1 hour, then lower the temperature to 50° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature reaches 90°C, react for 20 minutes, maintain the temperature at 95°C, continue to heat and stir the reaction for 4 hours, cool to room temperature, and obtain modified amino silicone oil.
[0046] The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2:0.6.
[0047] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0048] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0049] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3:1.4.
[0050] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0051] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0052] Comparative Example 3 The difference between this comparative example and Example 1 is that the silane coupling agent is N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane.
[0053] A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 parts of modified amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffening agent and 50 parts of water.
[0054] The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4 parts; modified monomer: glycidyl methacrylate, 2.6 parts; hydrolyzing agent: deionized water, 0.55 parts; basic raw material: octamethylcyclotetrasiloxane, 80 parts; solvent: dimethylformamide, 14 parts; catalyst: potassium hydroxide, 0.01 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70° C., the modified monomer is added dropwise under heat preservation conditions for 3 hours. After the addition is completed, the mixture is stirred for 4 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90° C., keep the temperature for reaction for 1 hour, then lower the temperature to 50° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature reaches 90°C, react for 20 minutes, maintain the temperature at 95°C, continue to heat and stir the reaction for 4 hours, cool to room temperature, and obtain modified amino silicone oil.
[0055] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0056] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0057] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3:1.4.
[0058] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0059] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0060] Comparative Example 4 The difference between this comparative example and Example 1 is that the emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:1:1.
[0061] A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 parts of modified amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffening agent and 50 parts of water.
[0062] The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4 parts; modified monomer: glycidyl methacrylate, 2.6 parts; hydrolyzing agent: deionized water, 0.55 parts; basic raw material: octamethylcyclotetrasiloxane, 80 parts; solvent: dimethylformamide, 14 parts; catalyst: potassium hydroxide, 0.01 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70° C., the modified monomer is added dropwise under heat preservation conditions for 3 hours. After the addition is completed, the mixture is stirred for 4 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90° C., keep the temperature for reaction for 1 hour, then lower the temperature to 50° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature reaches 90°C, react for 20 minutes, maintain the temperature at 95°C, continue to heat and stir the reaction for 4 hours, cool to room temperature, and obtain modified amino silicone oil.
[0063] The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2:0.6.
[0064] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0065] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0066] The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:1:1.
[0067] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0068] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0069] Comparative Example 5 The difference between this comparative example and Example 1 is that the emulsifier is isomeric decanol polyoxyethylene ether.
[0070] A softener for acrylic fiber finishing comprises the following components in parts by weight: 12 parts of modified amino silicone oil, 8 parts of emulsifier, 1 part of glacial acetic acid, 12 parts of polyvinyl alcohol, 5 parts of ternary copolymer silicone oil, 12 parts of polyethylene glycol fatty acid ester, 2 parts of stabilizer, 2 parts of stiffening agent and 50 parts of water.
[0071] The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4 parts; modified monomer: glycidyl methacrylate, 2.6 parts; hydrolyzing agent: deionized water, 0.55 parts; basic raw material: octamethylcyclotetrasiloxane, 80 parts; solvent: dimethylformamide, 14 parts; catalyst: potassium hydroxide, 0.01 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70° C., the modified monomer is added dropwise under heat preservation conditions for 3 hours. After the addition is completed, the mixture is stirred for 4 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90° C., keep the temperature for reaction for 1 hour, then lower the temperature to 50° C., vacuumize and remove low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 3: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature reaches 90°C, react for 20 minutes, maintain the temperature at 95°C, continue to heat and stir the reaction for 4 hours, cool to room temperature, and obtain modified amino silicone oil.
[0072] The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2:0.6.
[0073] The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
[0074] The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
[0075] The emulsifier is isomeric decanol polyoxyethylene ether.
[0076] The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
[0077] A method for preparing a softener for acrylic fiber finishing, the method comprising the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating to 60° C., and stirring uniformly to prepare a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
[0078] Performance Testing The softeners prepared in Examples 1 to 2 and Comparative Examples 1-5 were used in the post-finishing process. The acrylic fabric to be treated (the specification of the acrylic fabric was 10 cm×20 cm) was dipped into the softener and then shaped at a high temperature of 120° C. to obtain acrylic fabric products. The stiffness and softness were tested. Ten pieces of the same fabric were treated each time, and the average of the test results was taken. The test results are shown in Table 1.
[0079] Hand feel test: Fluffiness and softness are assessed by touch. Specifically, 10 professionals are divided into groups to touch and score 10 samples in each group, and the average score is given. The score is 100 points. A high score indicates good fluffiness and softness. Stiffness: Using the right-angle test method, move the sample along the upper right-angle side of the test bench to a cantilever state with a suspended length of 10 cm. Test the angle between the suspended section of the sample and the vertical direction (i.e., the lower right-angle side perpendicular to the upper right-angle side of the test bench). The larger the angle, the better the stiffness.
[0080] Table 1 Performance test results
[0081] As can be seen from Table 1, the softener of the present invention has an excellent acrylic fiber finishing effect.
[0082] By comparing Example 1 with Comparative Examples 1-2, it can be seen that the modified amino silicone oil described in the present invention can significantly improve the finishing feel effect, and the modified amino silicone oil prepared by the preparation method of the present invention can significantly improve the crispness effect.
[0083] By comparing Example 1 with Comparative Examples 3 to 5, it can be seen that the present invention significantly improves the stiffening effect by compounding the emulsifier, and the specific ratio and type of the present invention have a better finishing effect than other types of emulsifiers.
[0084] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A softener for acrylic fiber finishing, characterized in that: The invention comprises the following components in parts by weight: 12 to 15 parts of modified amino silicone oil, 8 to 10 parts of emulsifier, 1 to 3 parts of glacial acetic acid, 12 to 16 parts of polyvinyl alcohol, 5 to 7 parts of ternary copolymer silicone oil, 12 to 15 parts of polyethylene glycol fatty acid ester, 2 to 3 parts of stabilizer, 2 to 4 parts of stiffening agent and 50 to 60 parts of water.
2. The softener for acrylic fiber finishing according to claim 1, characterized in that: The preparation method of modified amino silicone oil is: Step 1, the formula includes the following components in parts by weight: silane coupling agent, 3.4-3.7 parts; modified monomer: glycidyl methacrylate, 2.6-2.9 parts; hydrolyzing agent: deionized water, 0.55-0.6 parts; basic raw material: octamethylcyclotetrasiloxane, 80-82 parts; solvent: dimethylformamide, 14-15 parts; Catalyst: potassium hydroxide, 0.01-0.03 parts; Step 2: In a nitrogen atmosphere, when the temperature of the silane coupling agent is raised to 70-75°C, the modified monomer is added dropwise under heat preservation conditions for 3-4 hours. After the addition is completed, the mixture is stirred for 4-5 hours to obtain a highly active silane coupling agent; Step 3: Mix the highly active silane coupling agent and the hydrolyzing agent, raise the temperature to 90-95°C, keep the temperature to react for 1-2 hours, then lower the temperature to 50-53°C, vacuum and remove the low-boiling substances, and obtain a highly active silane coupling agent hydrolyzate; Step 4: Mix the high-activity silane coupling agent hydrolyzate with the basic raw material and the solvent, stir and heat, add the catalyst when the temperature rises to 90-95°C, react for 20-30 minutes, maintain the temperature at 95-97°C, continue to heat and stir the reaction for 4-6 hours, cool to room temperature, and obtain modified amino silicone oil.
3. The softening agent for acrylic fiber finishing according to claim 2, characterized in that: The silane coupling agent is selected from one or more of KH550, KH570 and KH590.
4. The softening agent for acrylic fiber finishing according to claim 3, characterized in that: The silane coupling agent is a mixture of KH550, KH570 and KH590 in a mass ratio of 1:1.2-1.5:0.6-0.
8.
5. The softener for acrylic fiber finishing according to claim 1, characterized in that: The stabilizer is sodium tridecyl alcohol polyoxyethylene ether carboxylate.
6. The softener for acrylic fiber finishing according to claim 1, characterized in that: The stiffness agent is N,N-di(2-hydroxyethyl)dodecylamide.
7. The softener for acrylic fiber finishing according to claim 1, characterized in that: The emulsifier is a mixture of isomeric decanol polyoxyethylene ether, polyethylene glycol fatty acid ester and sodium lauryl sulfate in a mass ratio of 1:0.3-0.5:1.4-1.
7.
8. The softener for acrylic fiber finishing according to claim 1, characterized in that: The polyethylene glycol fatty acid ester is polyethylene glycol stearate.
9. A method for preparing a softening agent for acrylic fiber finishing according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: (1) adding polyvinyl alcohol, polyethylene glycol fatty acid ester, stiffness agent and fatty amide to a portion of water, heating and stirring to obtain a mixed solution A; (2) Mixing the modified amino silicone oil, the emulsifier, a portion of the water and the glacial acetic acid and stirring them evenly to obtain a mixed solution B; (3) Octadecaned tertiary amine, ternary copolymer silicone oil, stabilizer, remaining water, the A mixed solution and the B mixed solution are mixed and stirred uniformly to prepare a softener for acrylic fiber finishing.
10. The method for preparing a softener for acrylic fiber finishing according to claim 9, characterized in that: Heat to 60-80°C.
Citation Information
Cited By
Preparation method of multifunctional softening agent for fabric after-finishing
CN120647958A
Process for the preparation of a multifunctional softener for fabric after-treatment
CN120647958B