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CN-117166240-B - Graphene nylon spinning fiber and preparation process thereof

CN117166240BCN 117166240 BCN117166240 BCN 117166240BCN-117166240-B

Abstract

The invention relates to the technical field of spinning fibers and discloses a graphene nylon spinning fiber and a preparation process thereof, wherein raw materials of the modified graphene A comprise carboxyl activated graphene and tetra-polylysine, the modified graphene A, glutaraldehyde, ethanol, propanol and sodium carbonate are used for preparing an impregnating solution together for surface modification of the modified nylon fiber prepared in a subsequent step, raw materials of the modified graphene B comprise carboxyl activated graphene and polyamide polyether block copolymers, the modified graphene B, caprolactam and 6-aminocaproic acid are used for preparing modified nylon 6 together, and then the modified nylon fiber is obtained through melt spinning and post-drawing, the modified nylon fiber is placed into the impregnating solution, the graphene nylon spinning fiber is obtained through impregnating at 50-60 ℃ for 0.5-1 h, the bath ratio is 1:50-1:60, and the graphene nylon spinning fiber is taken out and dried.

Inventors

  • CAO JIANPENG
  • MA HONGMING
  • HUANG RONGQING
  • NI ZHANGGEN

Assignees

  • 江苏江山红化纤有限责任公司

Dates

Publication Date
20260508
Application Date
20230925

Claims (7)

  1. 1. The preparation process of the graphene nylon spinning fiber is characterized by comprising the following steps of: S1, preparing carboxyl activated graphene and tetra-polylysine to obtain modified graphene A; S2, taking carboxyl activated graphene, polyamide polyether block copolymer and water, uniformly stirring, heating to 120-140 ℃, stirring for 10-14 h, and drying to obtain modified graphene B; taking caprolactam, 6-aminocaproic acid and modified graphene B, opening reflux condensed water, introducing nitrogen, heating to 250-260 ℃, stirring for 6-7 h to obtain modified nylon 6, and carrying out melt spinning and post-drawing to obtain modified nylon fibers; S3, taking modified graphene A, glutaraldehyde, ethanol, propanol and sodium carbonate, uniformly stirring to obtain an impregnating solution, putting modified nylon fibers into the impregnating solution, impregnating, taking out and drying to obtain graphene nylon spinning fibers; The modified graphene B comprises, by mass, 10-15 parts of carboxyl activated graphene, 3-6 parts of polyamide polyether block copolymer and 8-15 parts of water; the modified nylon 6 comprises, by mass, 15-25 parts of caprolactam, 0.5-1.5 parts of 6-aminocaproic acid and 0.05-0.15 part of modified graphene B; The preparation method of the polyamide polyether block copolymer comprises the following steps of heating polyether amine to 200-210 ℃ under the protection of nitrogen, adding phosphorous acid, carrying out heat preservation and stirring for 0.5-1 h, slowly adding nylon 66 salt, heating to 220-230 ℃ and carrying out heat preservation and reaction for 2-4 h to obtain the polyether amine end-capped polyamide prepolymer, adding adipic acid and phosphorous acid, heating to 230-240 ℃ and reacting for 3-4 h, cooling to 210-220 ℃, vacuumizing, heating to 230-240 ℃ and carrying out heat preservation and reaction for 1-2 h, and cooling to obtain the polyamide polyether block copolymer.
  2. 2. The preparation process of the graphene nylon spinning fiber according to claim 1 is characterized in that the impregnating solution comprises the following raw materials of 5-15 parts of modified graphene A, 1-2 parts of glutaraldehyde, 600-700 parts of ethanol, 50-100 parts of propanol and 1-2 parts of sodium carbonate.
  3. 3. The preparation process of the graphene nylon spinning fiber is characterized by comprising the steps of taking carboxylated graphene and water, performing ultrasonic dispersion for 1-2 hours, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride into a dispersion liquid, stirring for 1-2 hours to obtain carboxyl activated graphene, adding tetra-polylysine, heating to 120-140 ℃, stirring for 10-14 hours, washing and drying to obtain the modified graphene A.
  4. 4. The preparation process of the graphene nylon spinning fiber according to claim 3 is characterized in that the modified graphene A comprises, by mass, 3-6 parts of carboxylated graphene, 1-2 parts of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 2-4 parts of tetra-lysine, and the concentration of the dispersion liquid is 1mg/mL.
  5. 5. The preparation process of the graphene nylon spinning fiber according to claim 1 is characterized in that the polyamide polyether block copolymer comprises, by mole, 1-2 mol of polyether amine, 0.8-1.5 mol of nylon 66 salt and 1-2 mol of adipic acid, 0.8-1.5 wt% of phosphorous acid is added to a polyether amine end-capped polyamide prepolymer, and 0.3-0.8 wt% of phosphorous acid is added to the polyamide polyether block copolymer.
  6. 6. The preparation process of the graphene nylon spinning fiber according to claim 1 is characterized in that the dipping process is that the graphene nylon spinning fiber is dipped for 0.5-1 h at 50-60 ℃ and the bath ratio is 1:50-1:60.
  7. 7. The graphene nylon spinning fiber obtained by the preparation process of the graphene nylon spinning fiber according to any one of claims 1-6.

Description

Graphene nylon spinning fiber and preparation process thereof Technical Field The invention relates to the technical field of spinning fibers, and discloses graphene nylon spinning fibers and a preparation process thereof. Background Polyamide is a polymer polymerized from monomers containing carboxyl and amino groups through amide bonds, and is called nylon when being used as synthetic fibers, wherein PA-6 and PA-66 are mainly used for spinning the synthetic fibers, and are called nylon 6 (nylon 6) and nylon 66 (nylon 66), and have good comprehensive properties. Along with the increasing demand of diversified markets for products, single nylon fiber cannot meet the actual demand, so graphene is often added for modification, and graphene has excellent hydrophilicity, infrared heating performance, antibacterial performance and ultraviolet resistance, can improve the strength of the nylon fiber, and has wide application prospect. However, the graphene surface does not contain functional groups, so that the dispersibility is poor, and the application of the graphene in the modified nylon material is severely limited. Therefore, the graphene nylon spinning fiber with good antibacterial property, hydrophilicity, strength and performance has important significance. Disclosure of Invention The invention aims to provide graphene nylon spinning fiber and a preparation process thereof, so as to solve the problems in the background technology. In order to solve the technical problems, the invention provides the following technical scheme: A preparation process of graphene nylon spinning fiber comprises the following steps: S1, preparing modified graphene A by taking carboxyl activated graphene and tetra-polylysine; s2, preparing modified graphene B by taking carboxyl activated graphene, polyamide polyether block copolymer and water, preparing modified nylon 6 by taking caprolactam, 6-aminocaproic acid and modified graphene B, and obtaining modified nylon 6 by melt spinning and post-drafting the modified nylon 6; And S3, taking the modified graphene A, glutaraldehyde, ethanol, propanol and sodium carbonate, uniformly stirring to obtain an impregnating solution, putting the modified nylon fiber into the impregnating solution, impregnating, taking out and drying to obtain the graphene nylon spinning fiber. More optimally, the impregnating solution comprises the following raw materials of 5-15 parts of modified graphene A, 1-2 parts of glutaraldehyde, 600-700 parts of ethanol, 50-100 parts of propanol and 1-2 parts of sodium carbonate. More optimally, the preparation method of the modified graphene A comprises the steps of taking carboxylated graphene and water, performing ultrasonic dispersion for 1-2 hours, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride into a dispersion liquid, stirring for 1-2 hours to obtain carboxyl activated graphene, adding tetra-polylysine, heating to 120-140 ℃, stirring for 10-14 hours, washing and drying to obtain the modified graphene A. More optimally, the modified graphene A comprises, by mass, 3-6 parts of carboxylated graphene, 1-2 parts of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 2-4 parts of tetra-polylysine, wherein the concentration of the dispersion liquid is 1mg/mL. More optimally, the preparation method of the modified nylon 6 comprises the following steps of taking carboxyl activated graphene, polyamide polyether segmented copolymer and water, uniformly stirring, heating to 120-140 ℃, stirring for 10-14 h, drying to obtain modified graphene B, taking caprolactam, 6-aminocaproic acid and modified graphene B, opening reflux condensed water, introducing nitrogen, heating to 250-260 ℃ to melt the substances, and stirring for 6-7 h to obtain the modified nylon 6. The modified graphene B comprises, by mass, 10-15 parts of carboxyl activated graphene, 3-6 parts of polyamide polyether block copolymer and 8-15 parts of water, and the modified nylon 6 comprises, by mass, 15-25 parts of caprolactam, 0.5-1.5 parts of 6-aminocaproic acid and 0.05-0.15 part of modified graphene B. More optimally, the preparation method of the polyamide-polyether block copolymer comprises the steps of adding polyether amine under the protection of nitrogen, increasing the temperature to 200-210 ℃, adding phosphorous acid, carrying out heat preservation and stirring for 0.5-1 h, slowly adding nylon 66 salt, carrying out heat preservation and reaction for 2-4 h at 220-230 ℃, obtaining the polyether amine end-capped polyamide prepolymer, adding adipic acid and phosphorous acid, carrying out heat preservation and reaction for 3-4 h at 230-240 ℃, cooling to 210-220 ℃, vacuumizing, carrying out heat preservation and reaction for 1-2 h at 230-240 ℃, and cooling to obtain the polyamide-polyether block copolymer. More optimally, the polyamide polyether block copolymer comprises the following raw materials, by mole, 1-2 mol of polyether amine, 0.8-1.5 mol of nylon 66 salt and