Preparation process of textile auxiliary agent

Abstract

The invention belongs to the technical field of textile assistants, and particularly relates to a preparation process of a textile assistant.The preparation process comprises the following steps that organic silicon monomers and epoxy modified polyether are added into a four-opening flask and mixed and stirred, and a preliminary mixed solution is obtained; heating, adding a catalyst, and stirring for reaction to obtain a prepolymer; mixing the prepolymer with amino silicon oil, stirring and reacting, and adding an antioxidant to obtain a grafting solution; and mixing the grafting solution, nano silicon dioxide, an emulsifier and deionized water, and defoaming to obtain the textile auxiliary agent. And the nano silicon dioxide can fill tiny unevenness on the fiber surface, so that a smoother fiber surface is formed, and the local friction strength is reduced. The core reason of fiber pilling is that short fibers are pulled out and entangled into balls, the weaving auxiliary agent can form a stable lubricating film on the surfaces of the fibers, and pilling is inhibited from the source.

Description

Technical Field

[0001] This invention belongs to the field of textile auxiliary technology, and specifically relates to a preparation process for a textile auxiliary. Background Technology

[0002] Textile auxiliaries are indispensable chemicals in the production and processing of textiles. By imparting special functions to the fiber surface (such as softness, antistatic properties, and water resistance) or improving the fabric style (such as drape and elasticity), they significantly enhance the product quality and added value of textiles.

[0003] Pilling in textiles occurs when, during wear or washing, the fiber ends slip onto the fabric surface due to mechanical friction, becoming entangled and forming fuzzy balls. Traditional anti-pilling finishing methods often employ resin finishing or singeing. Resin finishing uses formaldehyde-releasing resins (such as melamine-formaldehyde resin) to form a cross-linked film on the fiber surface, inhibiting fiber slippage. However, these resins may release free formaldehyde, which is harmful to human health, and can easily lead to a stiffer fabric feel and reduced breathability. Singeing removes the surface fuzz with a high-temperature flame, but this can damage the main fiber structure, reduce fabric strength, and result in a rougher surface and decreased gloss.

[0004] Therefore, traditional anti-pilling finishing methods have significant limitations. Summary of the Invention

[0005] To address the problems existing in the prior art, the present invention provides a preparation process for textile auxiliaries that can reduce friction between fibers, thereby improving the anti-pilling and anti-fuzzing properties of fabrics.

[0006] To address the above problems, the present invention provides a preparation process for a textile auxiliary agent, comprising the following steps: S1. By weight, add 80-120 parts of organosilicon monomer and 10-30 parts of epoxy-modified polyether to a four-necked flask, mix and stir to obtain a preliminary mixture; S2. Heat the preliminary mixture to 80°C, add 0.1-0.5 parts of catalyst, stir and react for 6-8 hours to obtain the prepolymer; S3. Mix the prepolymer and amino silicone oil at a volume ratio of 1:0.8 to 1.5, stir and react at 70°C for 4 to 5 hours, add 0.5 to 1.5 parts of antioxidant, sieve, and obtain the grafting solution. S4. Mix the grafting solution, nano silica, emulsifier and deionized water at a volume ratio of 1:0.05-0.1:0.02-0.05:2-3, emulsify in a high-speed emulsifier for 30 minutes, defoam, and obtain the textile auxiliary agent.

[0007] Preferably, the median diameter of the nano-silica is 10–25 nm.

[0008] Preferably, the nano-silica is pre-modified with a silane coupling agent.

[0009] Preferably, the emulsifier is a composite emulsifier composed of a nonionic emulsifier and anionic emulsifier, and the HLB value of the composite emulsifier is 12 to 16.

[0010] Preferably, the nonionic emulsifier is OP-10.

[0011] Preferably, the anionic emulsifier is sodium dodecylbenzenesulfonate.

[0012] Preferably, the antioxidant is 2,6-di-tert-butyl-4-methylphenol.

[0013] Preferably, the organosilicon monomer is octamethylcyclotetrasiloxane.

[0014] Preferably, the catalyst is tetramethylammonium hydroxide.

[0015] Preferably, the epoxy value of the epoxy-modified polyether is 0.05 to 0.15 mol / 100g.

[0016] After adopting the above technical solution, the beneficial effects of the present invention are: Nano-silica fills the tiny unevenness on the fiber surface, thus forming a smoother fiber surface and reducing local friction. The core cause of fiber pilling is that short fibers are pulled out and become entangled into balls. Fabric auxiliaries can form a stable lubricating film on the fiber surface, inhibiting pilling at its source. Detailed Implementation

[0017] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and not intended to limit it. Those skilled in the art will recognize that the invention can be practiced without some of these specific details. The following description of the embodiments is merely intended to provide a better understanding of the invention by illustrating examples of it.

[0018] Example 1 The preparation process of the textile auxiliary agent provided in this embodiment includes the following preparation steps: S1. Weigh 80 parts by weight of organosilicon monomer D4 (octamethylcyclotetrasiloxane) and 10 parts by weight of epoxy modified polyether. Place the raw materials in a four-necked flask and stir at a stirring speed of 300 rpm for 20 min to obtain a preliminary mixture. S2. The initial mixture was heated to 80°C by water bath heating, 0.1 parts of tetramethylammonium hydroxide were added, the speed was adjusted to 400 rpm, and the reaction was stirred for 6 hours. The prepolymer was obtained by base-catalyzed ring-opening polymerization and nucleophilic ring-opening grafting of epoxy groups. S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 5:4, adjust the stirring speed to 350 rpm, stir and react for 4 hours, add 0.5 parts of antioxidant BHT (2,6-di-tert-butyl-4-methylphenol), stir for 10 minutes, filter through a 100-mesh nylon screen to obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with nano-silica, composite emulsifier and deionized water in a volume ratio of 100:5:2:200, emulsified in a high-speed emulsifier for 30 min, and then defoamed under a pressure of -0.1 MPa for 15 min to obtain the textile auxiliary agent.

[0019] The epoxy value of the epoxy-modified polyether is controlled at 0.05 mol / 100g. The epoxy-modified polyether is synthesized by modifying polyether F-6 with epichlorohydrin. The specific steps are conventional technical methods and will not be elaborated here.

[0020] The catalyst tetramethylammonium hydroxide can be replaced with potassium hydroxide to increase the reaction rate.

[0021] The median diameter of the nano-silica is 10 nm. It is pre-modified with conventional techniques (such as silane coupling agent KH-550) to enhance its compatibility with organic phases.

[0022] The emulsifier is a composite emulsifier made by compounding nonionic emulsifier OP-10 and anionic emulsifier sodium dodecylbenzenesulfonate. The HLB value of the compounded emulsifier is controlled at 12.

[0023] Example 2 Based on Example 1, the preparation process of the textile auxiliary agent provided in this example includes the following preparation steps: S1. Weigh 80 parts of organosilicon monomer D4 and 30 parts of epoxy-modified polyether and place them in a four-necked flask. The epoxy value of the epoxy-modified polyether is controlled at 0.1 mol / 100g. Stir and mix to obtain a preliminary mixture. S2. Heat the initial mixture to 80°C, add 0.1 parts of tetramethylammonium hydroxide, adjust the speed to 400 rpm, and stir for 6 hours to obtain the prepolymer; S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 5:4, adjust the stirring speed to 350 rpm, stir for 4 hours, add 0.5 parts of BHT, stir for 10 minutes, filter, and obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with nano-silica, composite emulsifier and deionized water in a volume ratio of 100:5:2:200, emulsified in a high-speed emulsifier for 30 min, and then defoamed under a pressure of -0.1 MPa for 15 min to obtain the textile auxiliary agent.

[0024] Example 3 Based on Example 1, the preparation process of the textile auxiliary agent provided in this example includes the following preparation steps: S1. Weigh 80 parts of organosilicon monomer D4 and 30 parts of epoxy-modified polyether and place them in a four-necked flask. The epoxy value of the epoxy-modified polyether is controlled at 0.1 mol / 100g. Stir and mix to obtain a preliminary mixture. S2. Heat the initial mixture to 80°C, add 0.1 parts of tetramethylammonium hydroxide, adjust the speed to 400 rpm, and stir for 6 hours to obtain the prepolymer; S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 5:4, adjust the stirring speed to 350 rpm, stir for 4 hours, add 0.5 parts of BHT, stir for 10 minutes, filter, and obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with nano-silica, composite emulsifier and deionized water in a volume ratio of 100:5:2:200. The HLB value of the composite emulsifier is controlled at 16. The mixture is emulsified in a high-speed emulsifier for 30 min, and then defoamed for 15 min under a pressure of -0.1 MPa to obtain the textile auxiliary agent.

[0025] Example 4 Based on Example 1, the preparation process of the textile auxiliary agent provided in this example includes the following preparation steps: S1. Weigh 100 parts by weight of organosilicon monomer D4 (octamethylcyclotetrasiloxane) and 20 parts by weight of epoxy-modified polyether. The epoxy value of the epoxy-modified polyether is controlled at 0.1 mol / 100g. Place the raw materials in a four-necked flask and stir at a stirring speed of 300 rpm for 20 min to obtain a preliminary mixture. S2. The initial mixture was heated to 80°C by water bath heating, 0.35 parts of tetramethylammonium hydroxide were added, the speed was adjusted to 400 rpm, and the reaction was stirred for 7 hours. The prepolymer was obtained by base-catalyzed ring-opening polymerization and nucleophilic ring-opening grafting of epoxy groups. S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 1:1, adjust the stirring speed to 350 rpm, stir for 4.5 h, add 1 part of antioxidant BHT (2,6-di-tert-butyl-4-methylphenol), stir for 10 min, filter through a 100-mesh nylon screen to obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with nano-silica, composite emulsifier and deionized water in a volume ratio of 100:8:3:250. The median diameter of the nano-silica is 12nm and the HLB value of the composite emulsifier is controlled at 14. The mixture is emulsified in a high-speed emulsifier for 30min and then defoamed for 15min under a pressure of -0.1MPa to obtain the textile auxiliary agent.

[0026] Example 5 Based on Example 1, the preparation process of the textile auxiliary agent provided in this example includes the following preparation steps: S1. Weigh 120 parts by weight of organosilicon monomer D4 (octamethylcyclotetrasiloxane) and 30 parts by weight of epoxy-modified polyether. The epoxy value of the epoxy-modified polyether is controlled at 0.15 mol / 100g. Place the raw materials in a four-necked flask and stir at a stirring speed of 300 rpm for 20 min to obtain a preliminary mixture. S2. The initial mixture was heated to 80°C in a water bath. 0.5 parts of tetramethylammonium hydroxide were added, the speed was adjusted to 400 rpm, and the mixture was stirred for 8 hours. The prepolymer was obtained through base-catalyzed ring-opening polymerization and nucleophilic ring-opening grafting of epoxy groups. S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 2:3, adjust the stirring speed to 350 rpm, stir for 5 hours, add 1.5 parts of antioxidant BHT (2,6-di-tert-butyl-4-methylphenol), stir for 10 minutes, filter through a 100-mesh nylon screen to obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with nano-silica, composite emulsifier and deionized water in a volume ratio of 20:2:1:60. The median diameter of the nano-silica is 15nm and the HLB value of the composite emulsifier is controlled at 16. The mixture is emulsified in a high-speed emulsifier for 30min and then defoamed for 15min under a pressure of -0.1MPa to obtain the textile auxiliary agent.

[0027] Example 6 Based on Example 1, the preparation process of the textile auxiliary agent provided in this example includes the following preparation steps: S1. Weigh 120 parts by weight of organosilicon monomer D4 (octamethylcyclotetrasiloxane) and 30 parts by weight of epoxy-modified polyether. The epoxy value of the epoxy-modified polyether is controlled at 0.15 mol / 100g. Place the raw materials in a four-necked flask and stir at a stirring speed of 300 rpm for 20 min to obtain a preliminary mixture. S2. The initial mixture was heated to 80°C in a water bath. 0.5 parts of tetramethylammonium hydroxide were added, the speed was adjusted to 400 rpm, and the mixture was stirred for 8 hours. The prepolymer was obtained through base-catalyzed ring-opening polymerization and nucleophilic ring-opening grafting of epoxy groups. S3. Mix the prepolymer obtained in step 2 with amino silicone oil at a volume ratio of 2:3, adjust the stirring speed to 350 rpm, stir for 5 hours, add 1.5 parts of antioxidant BHT (2,6-di-tert-butyl-4-methylphenol), stir for 10 minutes, filter through a 100-mesh nylon screen to obtain the grafting solution. S4. The grafting solution obtained in step 3 is mixed with the composite emulsifier and deionized water at a volume ratio of 20:1:60. The median diameter of the nano silica is 25 nm, and the HLB value of the composite emulsifier is controlled at 16. The mixture is emulsified in a high-speed emulsifier for 30 min, and then defoamed for 15 min under a pressure of -0.1 MPa to obtain the textile auxiliary agent.

[0028] Nylon material that is prone to pilling was selected as the test material.

[0029] Record the initial weight. Completely immerse the 45D nylon fabric (after removing surface oil and impurities) in the textile auxiliary agent for 20 seconds. Adjust the roller pressure to 0.2 MPa, and use two rollers to remove excess auxiliary agent. Weigh the fabric to ensure a liquid content of 60%. Lay the nylon fabric flat on a hot press and hot press at 150℃ and 0.3 MPa for 60 seconds. Allow it to cool naturally to room temperature to obtain an anti-pilling nylon fabric.

[0030] Following the Martindale method (GB / T 4802.2—2008), the treated group (nylon fabric treated with textile auxiliaries from Examples 1-6) and the control group (untreated nylon fabric) were placed in a Martindale pilling tester under a load of 12 kPa and 2000 cycles. The pilling grade was recorded, and the specific evaluation criteria are shown in Table 1. The grade value is inversely correlated with the degree of pilling; the higher the pilling grade, the less pilling the fabric and the better its quality.

[0031] Table 1 Comparison of Test Indicators

[0032] Nano-silica fills the tiny unevenness on the fiber surface, thus forming a smoother fiber surface and reducing local friction. The core cause of fiber pilling is that short fibers are pulled out and become entangled into balls. Fabric auxiliaries can form a stable lubricating film on the fiber surface, inhibiting pilling at its source.

[0033] In Examples 4-5, due to the increased use of D4 and epoxy-modified polyether, the prepolymer molecular weight was higher, the film formation was more complete, and the pilling grade was significantly better than that of Example 1. Example 6 had a pilling grade of only 3.0, demonstrating that nano-silica particles are crucial for filling fiber surface defects and reducing friction.

[0034] The embodiments described above are not exhaustive and do not limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the above description. These embodiments are selected and specifically described in this specification to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to effectively utilize the invention and its modifications. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the invention should be included within the scope of protection of the invention.

Claims

1. A preparation process for a textile auxiliary agent, characterized in that, Includes the following steps: S1. By weight, add 80-120 parts of organosilicon monomer and 10-30 parts of epoxy-modified polyether to a four-necked flask, mix and stir to obtain a preliminary mixture; S2. Heat the preliminary mixture to 80°C, add 0.1-0.5 parts of catalyst, stir and react for 6-8 hours to obtain the prepolymer; S3. Mix the prepolymer and amino silicone oil at a volume ratio of 1:0.8 to 1.5, stir and react at 70°C for 4 to 5 hours, add 0.5 to 1.5 parts of antioxidant, sieve, and obtain the grafting solution. S4. Mix the grafting solution, nano silica, emulsifier and deionized water at a volume ratio of 1:0.05-0.1:0.02-0.05:2-3, emulsify in a high-speed emulsifier for 30 minutes, defoam, and obtain the textile auxiliary agent.

2. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The median diameter of the nano-silica is 10–25 nm.

3. The preparation process of the textile auxiliary agent according to claim 2, characterized in that: The nano-silica is pre-modified with a silane coupling agent.

4. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The emulsifier is a composite emulsifier composed of a nonionic emulsifier and anionic emulsifier, and the HLB value of the composite emulsifier is 12 to 16.

5. The preparation process of the textile auxiliary agent according to claim 4, characterized in that: The nonionic emulsifier is OP-10.

6. The preparation process of the textile auxiliary agent according to claim 4, characterized in that: The anionic emulsifier is sodium dodecylbenzenesulfonate.

7. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The antioxidant is 2,6-di-tert-butyl-4-methylphenol.

8. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The organosilicon monomer is octamethylcyclotetrasiloxane.

9. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The catalyst is tetramethylammonium hydroxide.

10. The preparation process of the textile auxiliary agent according to claim 1, characterized in that: The epoxy value of the epoxy-modified polyether is 0.05–0.15 mol / 100g.

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