CN114775090A - Preparation method of graphene modified anti-static fabric - Google Patents
Preparation method of graphene modified anti-static fabric Download PDFInfo
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- CN114775090A CN114775090A CN202210533521.8A CN202210533521A CN114775090A CN 114775090 A CN114775090 A CN 114775090A CN 202210533521 A CN202210533521 A CN 202210533521A CN 114775090 A CN114775090 A CN 114775090A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
Abstract
The invention discloses a preparation method of a graphene modified anti-static fabric, which comprises the following steps: (1) preparing functional modified three-dimensional graphene powder; (2) preparing functional modified three-dimensional structure graphene powder doped with polyaniline; (3) and preparing the graphene modified anti-static fabric. According to the invention, the three-dimensional graphene powder material is adopted for silane functional modification, the three-dimensional graphene powder material has high specific surface area, high conductivity and low cost, good hydrophobicity and mechanical property are realized after the silane functional modification, and then the silane functional modification and the polyaniline are doped, so that the polyaniline has the excellent characteristics of conductivity and microelectrode, the integral antistatic capability is greatly improved, and finally the graphene modified antistatic fabric is subjected to fiberization, so that the graphene modified antistatic fabric is finally obtained, the manufacturing cost is lower, the adaptability is very strong, and the preparation of the fabric can be realized by various mixed weaving or interweaving methods.
Description
Technical Field
The invention relates to the technical field of fiber modification, and particularly relates to a preparation method of a graphene modified anti-static fabric.
Background
The clothes refer to various clothes worn on the body, and the clothes are the medium for cold protection, warm keeping and body protection. Far in the original society, our ancestors have made simple clothes using natural kudzu, hemp, silk or hide, hairiness to keep out the body from cold. In modern society, along with the development of science and technology and the improvement of the living standard of people, clothes are gradually evolved into decorative articles of human bodies, and the clothes represent the living standard and the social status of a person in more time; meanwhile, on the basis of unchanged basic functions of the clothes, people have higher requirements on the functionality, comfort, health, environmental protection and health care of the garment fabric.
Because the textile fibers in the textile fabric of the clothes are easy to accumulate static electricity to generate discharge behavior, the fire and personal accidents caused by the textile are increased year by year, especially in the industries of chemical engineering, mines and the like. Meanwhile, special industries such as fire fighting, military and the like need to have antistatic property to textile fabrics to ensure personal safety of users due to the particularity of operation objects and environment.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene modified anti-static fabric, so that an excellent anti-static effect is realized.
The technical purpose of the invention is realized by the following technical scheme:
the preparation method of the graphene modified anti-static fabric is characterized by comprising the following steps:
(1) preparing functional modified three-dimensional graphene powder: adding the three-dimensional structure graphene powder into an N, N-dimethylformamide solvent, uniformly dispersing for 3-5 hours under the action of ultrasound, adding triethylamine and a silane coupling agent after the three-dimensional structure graphene powder is completely dispersed, stirring for 30-60 min, transferring into a reaction kettle, introducing nitrogen to discharge residual air in the reaction kettle, heating for reaction, and collecting the functionalized modified three-dimensional structure graphene powder through centrifugation after the reaction is completed;
(2) preparing functionalized modified three-dimensional structure graphene powder doped polyaniline: dissolving redistilled aniline in a sulfuric acid aqueous solution, stirring for 10-20 min at room temperature, then continuously adding the functionalized modified three-dimensional graphene powder prepared in the step (1), stirring for 2-4 h, slowly dropwise adding ammonium persulfate, refrigerating and placing after stirring, then precipitating, filtering and washing, and then drying in a vacuum drying oven to obtain the functionalized modified three-dimensional graphene powder doped polyaniline;
(3) preparing the graphene modified antistatic fabric: the functionalized modified solid prepared in the step (2) is injected into a syringeDoping polyaniline into CaCl through graphene powder with bulk structure2Soaking an ethanol solution in a coagulating bath, sequentially washing away residual salts through ethanol and deionized water, finally collecting the washed residual salts through a polytetrafluoroethylene rod, drying the collected residual salts at room temperature, reducing the dried residual salts in 45% hydriodic acid, sequentially soaking and washing the washed residual salts through ethanol and deionized water, drying the washed residual salts, placing the dried residual salts in a carboxymethyl cellulose solution with the mass fraction of 5% for soaking at room temperature for 24 hours, performing vacuum drying to obtain graphene modified anti-static fibers, and blending or interweaving the graphene modified anti-static fibers with other fabrics to obtain the graphene modified anti-static fabric.
Preferably, the purity of the graphene powder with the three-dimensional structure in the step (1) is experimental grade, and the mass-to-volume ratio of the graphene powder with the three-dimensional structure to the N, N-dimethylformamide solvent is 1.5-2 mg: 1ml, wherein the molar ratio of the stereo-structure graphene powder to the triethylamine to the alkyl coupling agent is 1: (0.05-0.1): (0.2-0.5).
Preferably, the catalyst in (1) is selected from hexadecyl trimethoxy silane, vinyl triethoxy silane or vinyl trimethoxy silane.
Preferably, after the heating reaction in the step (1) is completed, the mixture is refluxed for 22-26 hours under the protection of nitrogen, and the functional modified three-dimensional graphene powder after centrifugal collection needs to be dried in vacuum at 60 ℃ for 30-45 min.
Preferably, the concentration of the sulfuric acid aqueous solution in the step (2) is 0.1mol/L, and the molar volume ratio of the redistilled aniline, the functionalized modified three-dimensional graphene powder and the sulfuric acid aqueous solution is (0.1-0.2) mol: 1 mol: (5-7) ml, wherein the molar ratio of the ammonium persulfate to the functionalized modified three-dimensional structure graphene powder is (0.05-0.09): 1.
preferably, the refrigerating temperature in the step (2) is 0 ℃, the set temperature in the vacuum drying oven is 60 ℃, and the drying time is 10-12 h.
Preferably, CaCl in the (3)2The mass fraction of the ethanol solution is 9% -11%, and the coagulating bath is a mixed solution of ethanol and water in a volume ratio of 1: 1.
Preferably, the graphene modified antistatic fiber interweaving in the step (3) is introduced into other fibers in a manner of interweaving with a conductive lattice by an inlaying method.
In conclusion, the beneficial effects of the invention are as follows: according to the invention, the three-dimensional graphene powder material is adopted for silane functional modification, the three-dimensional graphene powder material has high specific surface area, high conductivity and low cost, good hydrophobicity and mechanical property are realized after the silane functional modification, and then the silane functional modification and the polyaniline are doped, so that the polyaniline has the excellent characteristics of conductivity and microelectrode, the integral antistatic capability is greatly improved, and finally the graphene modified antistatic fabric is subjected to fiberization, so that the graphene modified antistatic fabric is finally obtained, the manufacturing cost is lower, the adaptability is very strong, and the preparation of the fabric can be realized by various mixed weaving or interweaving methods.
Detailed Description
The following is a further description of specific embodiments of the invention, which are not to be construed as limiting the invention.
Example 1
A preparation method of a graphene modified antistatic fabric comprises the following steps:
(1) preparing functional modified three-dimensional graphene powder: the purity of the three-dimensional structure graphene powder is experimental grade, the three-dimensional structure graphene powder is added into an N, N-dimethylformamide solvent, the three-dimensional structure graphene powder is uniformly dispersed for 3 hours under the ultrasonic action, triethylamine and hexadecyl trimethoxy silane are added after the three-dimensional structure graphene powder is completed, the three-dimensional structure graphene powder is stirred for 40 minutes, and the mass volume ratio of the three-dimensional structure graphene powder to the N, N-dimethylformamide solvent is 2 mg: 1ml, the molar ratio of the stereo-structure graphene powder, triethylamine and hexadecyl trimethoxy silane is 1: 0.1: 0.2, transferring the mixture into a reaction kettle, introducing nitrogen to discharge residual air in the reaction kettle, carrying out heating reaction, refluxing the mixture for 23 hours under the protection of the nitrogen, collecting functionalized modified three-dimensional graphene powder by centrifugation after the reaction is finished, and carrying out vacuum drying at 60 ℃ for 35 min.
(2) Preparing functional modified three-dimensional structure graphene powder doped polyaniline: dissolving secondary distilled aniline in a sulfuric acid aqueous solution, wherein the concentration of the sulfuric acid aqueous solution is 0.1mol/L, stirring for 15min at room temperature, then continuously adding the functional modified three-dimensional structure graphene powder prepared in the step (1), stirring for 3h, then slowly dropwise adding ammonium persulfate, wherein the molar volume ratio of the secondary distilled aniline to the functional modified three-dimensional structure graphene powder to the sulfuric acid aqueous solution is 0.1 mol: 1 mol: 6ml, wherein the molar ratio of ammonium persulfate to the functionalized modified three-dimensional graphene powder is 0.06: 1, refrigerating and placing at 0 ℃ after stirring, filtering and washing the precipitate, and drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain the functionalized modified three-dimensional graphene powder doped polyaniline.
(3) Preparing the graphene modified antistatic fabric: injecting the functional modified three-dimensional graphene powder prepared in the step (2) doped with polyaniline into CaCl through an injector2Ethanol solution of CaCl2The mass fraction of an ethanol solution is 9%, the ethanol solution is soaked in a coagulating bath of a mixed solution of ethanol and water in a volume ratio of 1:1, residual salt is washed away through ethanol and deionized water in sequence, finally, a polytetrafluoroethylene rod is used for collection, the polytetrafluoroethylene rod is used for drying at room temperature, reduction treatment is carried out in 45% hydriodic acid, then, the ethanol and the deionized water are used for soaking and washing in sequence, the dried product is placed in a carboxymethyl cellulose solution with the mass fraction of 5% for soaking at room temperature for 24 hours, vacuum drying is carried out to obtain graphene modified anti-static fibers, then, the graphene modified anti-static fibers are blended or interwoven with other fabrics to obtain the graphene modified anti-static fabric, and the graphene modified anti-static fibers are introduced into other fibers in an embedding weaving method and a conductive grid interweaving mode.
Example 2
A preparation method of a graphene modified antistatic fabric comprises the following steps:
(1) preparing functional modified three-dimensional graphene powder: the purity of the three-dimensional structure graphene powder is experimental grade, the three-dimensional structure graphene powder is added into an N, N-dimethylformamide solvent, the graphene powder is uniformly dispersed for 4 hours under the ultrasonic action, triethylamine and vinyltriethoxysilane are added after the dispersion is completed, the stirring is carried out for 50 minutes, and the mass-to-volume ratio of the three-dimensional structure graphene powder to the N, N-dimethylformamide solvent is 1.8 mg: 1ml, the molar ratio of the stereo-structure graphene powder, triethylamine and vinyltriethoxysilane is 1: 0.06: 0.4, transferring the mixture into a reaction kettle, introducing nitrogen to discharge residual air in the reaction kettle, carrying out heating reaction, refluxing the mixture for 24 hours under the protection of the nitrogen, collecting functionalized modified three-dimensional graphene powder through centrifugation after the reaction is finished, and carrying out vacuum drying at 60 ℃ for 40 min.
(2) Preparing functionalized modified three-dimensional structure graphene powder doped polyaniline: dissolving redistilled aniline in a sulfuric acid aqueous solution, wherein the concentration of the sulfuric acid aqueous solution is 0.1mol/L, stirring for 18min at room temperature, then continuously adding the functional modified three-dimensional structure graphene powder prepared in the step (1), stirring for 4h, then slowly dropwise adding ammonium persulfate, wherein the molar volume ratio of the redistilled aniline, the functional modified three-dimensional structure graphene powder to the sulfuric acid aqueous solution is 0.2 mol: 1 mol: 5ml, wherein the molar ratio of ammonium persulfate to the functionalized modified three-dimensional graphene powder is 0.07: 1, refrigerating and placing at 0 ℃ after stirring, then precipitating, filtering and washing, and drying in a vacuum drying oven at 60 ℃ for 11 hours to obtain the functionalized modified three-dimensional graphene powder doped polyaniline.
(3) Preparing the graphene modified antistatic fabric: injecting the functional modified three-dimensional graphene powder prepared in the step (2) doped with polyaniline into CaCl through an injector2Ethanol solution of CaCl2The mass fraction of an ethanol solution is 10%, the ethanol solution is soaked in a coagulating bath of a mixed solution of ethanol and water in a volume ratio of 1:1, residual salt is washed away by ethanol and deionized water in sequence, a polytetrafluoroethylene rod is finally used for collection, the product is dried at room temperature, is subjected to reduction treatment in 45% hydroiodic acid, is then soaked and washed by ethanol and deionized water in sequence, is finally dried, is placed in a carboxymethyl cellulose solution with the mass fraction of 5% for soaking at room temperature for 24 hours, and is subjected to vacuum drying to obtain graphene modified anti-static fibers, and the graphene modified anti-static fibers are blended or interwoven with other fabrics to obtain the graphene modified anti-static fabric, wherein the graphene modified anti-static fibers are introduced into other fibers in an embedding weaving method and a conductive grid interweaving method.
Example 3
A preparation method of a graphene modified anti-static fabric comprises the following steps:
(1) preparing functionalized modified three-dimensional structure graphene powder: the purity of the three-dimensional graphene powder is experimental grade, the three-dimensional graphene powder is added into N, N-dimethylformamide solvent, is uniformly dispersed for 5 hours under the ultrasonic action, triethylamine and vinyl trimethoxy silane are added after the three-dimensional graphene powder is completely dispersed for 60 minutes, and the mass volume ratio of the three-dimensional graphene powder to the N, N-dimethylformamide solvent is 1.5 mg: 1ml, the molar ratio of the stereo-structure graphene powder, triethylamine and vinyl trimethoxy silane is 1: 0.05: 0.5, transferring the mixture into a reaction kettle, introducing nitrogen to discharge residual air in the reaction kettle, carrying out heating reaction, refluxing the mixture for 26 hours under the protection of the nitrogen, collecting functionalized modified three-dimensional graphene powder through centrifugation after the reaction is finished, and carrying out vacuum drying for 45min at 60 ℃.
(2) Preparing functionalized modified three-dimensional structure graphene powder doped polyaniline: dissolving redistilled aniline in a sulfuric acid aqueous solution, wherein the concentration of the sulfuric acid aqueous solution is 0.1mol/L, stirring for 15min at room temperature, then continuously adding the functional modified three-dimensional structure graphene powder prepared in the step (1), stirring for 3h, then slowly dropwise adding ammonium persulfate, wherein the molar volume ratio of the redistilled aniline, the functional modified three-dimensional structure graphene powder to the sulfuric acid aqueous solution is 0.2 mol: 1 mol: 7ml, wherein the molar ratio of ammonium persulfate to the functionalized modified three-dimensional graphene powder is 0.05: 1, after stirring, refrigerating at 0 ℃, standing, filtering and washing precipitates, and then drying in a vacuum drying oven at 60 ℃ for 10 hours to obtain the functional modified three-dimensional structure graphene powder doped polyaniline.
(3) Preparing the graphene modified antistatic fabric: injecting the functional modified three-dimensional structured graphene powder doped with polyaniline prepared in the step (2) into CaCl through an injector2Ethanol solution of CaCl2The mass fraction of the ethanol solution is 11 percent, the ethanol solution is soaked in a coagulating bath of a mixed solution of ethanol and water with the volume ratio of 1:1, the residual salt is washed off by sequentially passing through ethanol and deionized water, and finally, a polytetrafluoroethylene rod is used for collectingThe preparation method comprises the steps of drying at room temperature, reducing in 45% hydroiodic acid, soaking and washing with ethanol and deionized water in sequence, drying, soaking in a carboxymethyl cellulose solution with the mass fraction of 5% for 24 hours at room temperature, drying in vacuum to obtain graphene modified anti-static fibers, blending or interweaving the graphene modified anti-static fibers with other fabrics to obtain the graphene modified anti-static fabric, and introducing the graphene modified anti-static fibers into other fibers in an interweaving mode of an inlaying method and a conductive grid.
According to the invention, the three-dimensional structure graphene powder material is adopted to carry out silane functional modification, the three-dimensional structure graphene powder material has the advantages of high specific surface area, high conductivity and low cost, good hydrophobicity and mechanical property are realized after the silane functional modification, doping is realized with polyaniline, and the polyaniline has the excellent characteristics of conductivity and microelectrode, so that the integral anti-static capability is greatly improved, and finally, the fibrillation is carried out, so that the graphene modified anti-static fabric is finally obtained, the manufacturing cost is lower, the adaptability is very strong, and the preparation of the fabric can be realized through various mixed weaving or interweaving methods.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention.
Claims (8)
1. A preparation method of a graphene modified antistatic fabric is characterized by comprising the following steps:
preparing functionalized modified three-dimensional structure graphene powder: adding the three-dimensional graphene powder into an N, N-dimethylformamide solvent, uniformly dispersing for 3-5 h under the action of ultrasound, adding triethylamine and a silane coupling agent after the three-dimensional graphene powder is completely dispersed, stirring for 30-60 min, transferring the mixture into a reaction kettle, introducing nitrogen to discharge residual air in the reaction kettle, performing heating reaction, and collecting the functionalized modified three-dimensional graphene powder through centrifugation after the reaction is completed;
preparing functionalized modified three-dimensional structure graphene powder doped polyaniline: dissolving redistilled aniline in a sulfuric acid aqueous solution, stirring for 10-20 min at room temperature, continuously adding the functional modified three-dimensional graphene powder prepared in the step (1), stirring for 2-4 h, slowly dropwise adding ammonium persulfate, stirring, refrigerating, placing, precipitating, filtering, washing, and drying in a vacuum drying oven to obtain the functional modified three-dimensional graphene powder doped polyaniline;
preparing the graphene modified antistatic fabric: injecting the functional modified three-dimensional graphene powder prepared in the step (2) doped with polyaniline into CaCl through an injector2Soaking an ethanol solution in a coagulating bath, sequentially washing away residual salts through ethanol and deionized water, finally collecting the washed residual salts through a polytetrafluoroethylene rod, drying the collected residual salts at room temperature, reducing the dried residual salts in 45% hydriodic acid, sequentially soaking and washing the washed residual salts through ethanol and deionized water, drying the washed residual salts, placing the dried residual salts in a carboxymethyl cellulose solution with the mass fraction of 5% for soaking at room temperature for 24 hours, performing vacuum drying to obtain graphene modified anti-static fibers, and blending or interweaving the graphene modified anti-static fibers with other fabrics to obtain the graphene modified anti-static fabric.
2. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: the purity of the three-dimensional graphene powder in the step (1) is an experimental grade, and the mass-volume ratio of the three-dimensional graphene powder to the N, N-dimethylformamide solvent is 1.5-2 mg: 1ml, wherein the molar ratio of the stereo-structure graphene powder to the triethylamine to the alkyl coupling agent is 1: (0.05-0.1): (0.2-0.5).
3. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: the catalyst in the step (1) is one selected from hexadecyl trimethoxy silane, vinyl triethoxy silane or vinyl trimethoxy silane.
4. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: after the heating reaction in the step (1) is finished, the mixture is refluxed for 22-26 hours under the protection of nitrogen, and the functional modified three-dimensional graphene powder after centrifugal collection needs to be dried in vacuum for 30-45 minutes at 60 ℃.
5. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: the concentration of the sulfuric acid aqueous solution in the step (2) is 0.1mol/L, and the molar volume ratio of the redistilled aniline, the functionalized modified three-dimensional structure graphene powder and the sulfuric acid aqueous solution is (0.1-0.2) mol: 1 mol: (5-7) ml, wherein the molar ratio of the ammonium persulfate to the functionalized modified three-dimensional graphene powder is (0.05-0.09): 1.
6. the preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: the refrigerating temperature in the step (2) is 0 ℃, the set temperature in the vacuum drying oven is 60 ℃, and the drying time is 10-12 h.
7. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: CaCl in the (3)2The mass fraction of the ethanol solution is 9% -11%, and the coagulating bath is a mixed solution of ethanol and water in a volume ratio of 1: 1.
8. The preparation method of the graphene modified antistatic fabric according to claim 1, characterized by comprising the following steps: and (3) introducing the graphene modified anti-static fiber interweaving into other fibers in an interweaving mode of an inlaying method and a conductive lattice interweaving mode.
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