CN103966844B - A kind of preparation method of graphene conductive composite fibre - Google Patents
A kind of preparation method of graphene conductive composite fibre Download PDFInfo
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- CN103966844B CN103966844B CN201410220720.9A CN201410220720A CN103966844B CN 103966844 B CN103966844 B CN 103966844B CN 201410220720 A CN201410220720 A CN 201410220720A CN 103966844 B CN103966844 B CN 103966844B
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Abstract
The invention provides a kind of preparation method of graphene conductive composite fibre, be characterized in: textile fabric surface-modification processes: textile fabric being soaked in concentration is 2-3 hour in the silane coupler KH560 solution of 1%-30%, be placed in the dry rear obtained surfactant-modified textile fabric of 50-65 DEG C of baking oven; Graphene dispersion system preparation section: the standby graphene oxide water solution of Hummer ' s legal system by chemical preparation Graphene, and prepares uniform and stable graphene dispersion system under the effect of dispersant, and its concentration is 0.1%-5%; Graphene composite fibre preparation section is: modified textile fabric is immersed in 2-3 hour in graphene dispersion system, is placed in 50-65 DEG C of baking oven and dries, obtain graphene conductive composite fibre.Technique is simple, rationally, easy to operate, output is high, and Graphene consumption is few, and dispersion is uniform and stable, and reducing degree is good, and conduction, shielding property are good.
Description
Technical field
The invention belongs to textile product manufacturing technology field, be specifically related to functional fibre process technology, is a kind of preparation method of graphene conductive composite fibre specifically.
Background technology
Conductive fiber is the study hotspot of functional fiber always, generally refers to that resistivity is less than 10
8the fiber of Ω cm, has the functions such as conduction, electric heating and anti-electromagnetic radiation, the fields such as the antistatic clothes that usual pooled applications uses in special occasions or anti-electromalgnetic radiation clothes.
The main method of conductive fiber manufacture comprises, and one is conventional fibre surface coated with conductive composition, and another kind is that conductive material mixes with fibrous raw material, makes conductive fiber by spinning technique.Fiber surface conductive coating method is by the conductive material containing metal, carbon black or metallic compound, be coated on fiber surface and make conductive fiber, also the conduction high polymers such as polyaniline can be adsorbed in fiber surface by situ aggregation method and obtain conductive fiber, filamentary conductive prepared by said method can be given prominence to, but water-wash resistance and durability not ideal enough.Conducting particles (being mainly carbon black or metallic compound) and the main polymer of non-conductive composition carry out blended by co-blended spinning, composite conducting fiber is prepared by melting or wet spinning technology, in spinning process, conducting particles very easily produces reunion, affects the conductive effect of composite fibre.
Graphene be a kind of by carbon atom with sp
2hybridized orbit composition hexangle type is the two-dimension nano materials of honeycomb lattice, has the structure of perfect large pi-conjugated system and the thinnest individual layer atomic thickness (0.34nm).The physical and chemical performance (high-strength, high heat conduction, high connductivity, Ultralight) of the nanostructured special due to it and excellence and show huge application potential at numerous areas such as biomedicine, energy storage, sensor and composites.By Graphene and textile fabric compound, the research preparing electrically conductive composite fibre still rarely has report.
How to study a kind of preparation method of graphene conductive composite fibre, technique is simple, reasonable, is easy to operation, and output is higher, Graphene consumption is less, and graphene dispersion system is uniform and stable, reducing degree is good, and conduction, shielding property are good, and this is technical task urgently to be resolved hurrily at present.
Summary of the invention
The present invention, for solving prior art Problems existing, provides a kind of preparation method of graphene conductive composite fibre, and technique is simple, reasonable, be easy to operation, and output is higher, Graphene consumption is less, graphene dispersion system is uniform and stable, and reducing degree is good, and conduction, shielding property are good.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for graphene conductive composite fibre, is characterized in that, comprise carry out successively textile fabric surface modification, graphene dispersion system preparation, Graphene composite fibre preparation section; Described textile fabric surface-modification processes is: textile fabric being soaked in concentration is 2-3 hour in the silane coupler KH560 solution of 1%-30%, is placed in the dry rear obtained surfactant-modified textile fabric of 50-65 DEG C of baking oven; Described graphene dispersion system preparation section is: the standby graphene oxide water solution of Hummer ' s legal system by chemical preparation Graphene, and prepares uniform and stable graphene dispersion system under the effect of dispersant, and its concentration is 0.1%-5%; Described Graphene composite fibre preparation section is: modified textile fabric is immersed in 2-3 hour in graphene dispersion system, is placed in 50-65 DEG C of baking oven and dries, obtain graphene conductive composite fibre.
Preferably, described silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:1-5.
Preferably, the graphene oxide water solution concentration that described Hummer ' s legal system is standby is 0.05%-0.2%; Described reductant is one or more in hydrazine hydrate, hydroiodic acid, NaOH, potassium hydroxide; Described dispersant is at least one in sodium carboxymethylcellulose, neopelex, and described reductant concentration is 20%-50%, and reduction temperature is 60-90 DEG C, recovery time 2-4 hour; Described dispersant accounts for the 10%-20% of Graphene weight.
Further, described textile fiber material comprises natural fabric and chemical fibre, and described natural fabric comprises cotton, fiber crops, silk, hair, and described chemical fibre comprises viscose, terylene, polyamide fibre, aramid fiber.
The present invention compared with prior art has many advantages and good effect:
The production technology of preparation method of the present invention is simple, and be easy to operation, output is higher, and Graphene consumption is less; The resistivity of Graphene composite fibre prepared by the inventive method is 10 ~ 10
5Ω m, than conventional fibre resistivity (~ 10
14Ω m) improve tens orders of magnitude, reached conductive fiber scope, in composite fibre, Graphene content is 1% ~ 3%, has huge application prospect in fields such as conduction, radiation proof, thermoelectricity, smart fabric and flexible batteries.
Accompanying drawing explanation
Fig. 1 is graphene composite conductive fiber manufacturing process schematic diagram of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
The detailed description of the invention of the preparation method of a kind of graphene conductive composite fibre of the present invention, comprise carry out successively textile fabric surface modification, graphene dispersion system preparation, Graphene composite fibre preparation section;
Described textile fabric surface-modification processes is: textile fabric being soaked in concentration is 2-3 hour in the silane coupler KH560 solution of 1%-30%, is placed in the dry rear obtained surfactant-modified textile fabric of 50-65 DEG C of baking oven;
Described graphene dispersion system preparation section is: the standby graphene oxide water solution of Hummer ' s legal system by chemical preparation Graphene, and prepares uniform and stable graphene dispersion system under the effect of dispersant, and its concentration is 0.1%-5%;
Described Graphene composite fibre preparation section is: modified textile fabric is immersed in 2-3 hour in graphene dispersion system, is placed in 50-65 DEG C of baking oven and dries, obtain graphene conductive composite fibre.
Specific embodiments of the invention are as follows:
Embodiment 1: a kind of graphene conductive composite terylene fiber producing processes, comprises the PET fiber surface modified process, graphene dispersion system preparation section and the Graphene terylene composite fibre preparation section that carry out successively, wherein:
Described PET fiber surface modified process is: polyster fibre being soaked in concentration is in the silane coupler KH560 solution of 30% 3 hours, be placed in 65 DEG C of baking ovens dry after obtained surfactant-modified polyster fibres; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:5;
Described graphene dispersion system preparation section is: the standby graphene oxide water solution concentration of Hummer ' s legal system is 0.5%, by chemical preparation Graphene, reductant is hydrazine hydrate, reduction temperature is 90 DEG C, 2 hours recovery times, and under the effect of dispersant neopelex, prepare uniform and stable graphene dispersion system, dispersant accounts for 10% of Graphene weight, and graphene solution concentration is 0.5%.
After tested, the polyster fibre resistivity without conductive processing is 10
14Ω m, the resistivity of gained Graphene terylene composite fibre is 10
3Ω m, has reached conductive fiber scope, and in composite fibre, Graphene content is 3%, has huge application prospect in fields such as conduction, thermoelectricity and flexible batteries.
Embodiment 2: a kind of graphene conductive composite cotton fabric fiber producing processes, comprises the cotton composite fibre preparation section of the cotton fiber surface-modification processes, graphene dispersion system preparation section and the Graphene that carry out successively, wherein:
Described cotton fiber surface-modification processes is: cotton fiber being soaked in concentration is in the silane coupler KH560 solution of 20% 3 hours, be placed in 65 DEG C of baking ovens dry after obtained surfactant-modified cotton fibers; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:3;
Described graphene dispersion system preparation section is: the standby graphene oxide water solution concentration of Hummer ' s legal system is 1%, by chemical preparation Graphene, reductant is hydroiodic acid, reduction temperature is 90 DEG C, 4 hours recovery times, and under the effect of dispersant neopelex, prepare uniform and stable graphene dispersion system, dispersant accounts for 15% of Graphene weight, and graphene solution concentration is 0.3%.
After tested, the cotton fiber resistivity without conductive processing is 10
8Ω m, the resistivity of the cotton composite fibre of gained Graphene is 10
2Ω m, has reached conductive fiber scope, and in composite fibre, Graphene content is 2.5%.Huge application prospect is had in fields such as anti-electromalgnetic radiation clothes.
Embodiment 3: a kind of graphene conductive compound viscose acetal fibre preparation method, comprises the viscose acetal fibre surface-modification processes, graphene dispersion system preparation section and the Graphene viscose composite fibre preparation section that carry out successively, wherein:
Described viscose acetal fibre surface-modification processes is: viscose acetal fibre being soaked in concentration is in the silane coupler KH560 solution of 3% 2.5 hours, be placed in 60 DEG C of baking ovens dry after obtained surfactant-modified viscose acetal fibres; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:5;
Described graphene dispersion system preparation section is: the standby graphene oxide water solution concentration of Hummer ' s legal system is 1%, by chemical preparation Graphene, reductant is hydroiodic acid, reduction temperature is 85 DEG C, 3.5 hours recovery times, and under the effect of dispersant neopelex, prepare uniform and stable graphene dispersion system, dispersant accounts for 20% of Graphene weight, and graphene solution concentration is 1%.
After tested, the viscose acetal fibre resistivity without conductive processing is 10
9Ω m, the resistivity of gained Graphene viscose composite fibre is 10
4Ω m, has reached conductive fiber scope, and in composite fibre, Graphene content is 2%.Huge application prospect is had in fields such as conduction and anti-electromalgnetic radiation clothes.
Above embodiment only in order to technical scheme of the present invention to be described, but not is limited; Although with reference to previous embodiment to invention has been detailed description, for the person of ordinary skill of the art, still can modify to the technical scheme described in previous embodiment, or equivalent replacement is carried out to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of the present invention's technical scheme required for protection.
Claims (2)
1. a preparation method for graphene conductive composite fibre, is characterized in that, comprise carry out successively textile fabric surface modification, graphene dispersion system preparation, Graphene composite fibre preparation section;
Described textile fabric surface-modification processes is: textile fabric being soaked in concentration is 2-3 hour in the silane coupler KH560 solution of 1%-30%, is placed in the dry rear obtained surfactant-modified textile fabric of 50-65 DEG C of baking oven; Described silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:1-5;
Described graphene dispersion system preparation section is: the standby graphene oxide water solution of Hummer ' s legal system by chemical preparation Graphene, and prepares uniform and stable graphene dispersion system under the effect of dispersant, and its concentration is 0.1%-5%; The standby graphene oxide water solution concentration of described Hummer ' s legal system is 0.05%-0.2%; Described reductant is one or more in hydrazine hydrate, hydroiodic acid, NaOH, potassium hydroxide; Described dispersant is at least one in sodium carboxymethylcellulose, neopelex, and described reductant concentration is 20%-50%, and reduction temperature is 60-90 DEG C, recovery time 2-4 hour; Described dispersant accounts for the 10%-20% of Graphene weight;
Described Graphene composite fibre preparation section is: modified textile fabric is immersed in 2-3 hour in graphene dispersion system, is placed in 50-65 DEG C of baking oven and dries, obtain graphene conductive composite fibre.
2. according to the preparation method of graphene conductive composite fibre according to claim 1, it is characterized in that, described textile fiber material comprises natural fabric and chemical fibre, and described natural fabric comprises cotton, fiber crops, silk, hair, and described chemical fibre comprises viscose, terylene, polyamide fibre, aramid fiber.
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Application publication date: 20140806 Assignee: Shengquan Group Co., Ltd., Ji'nan City Assignor: Qingdao University Contract record no.: 2016370000009 Denomination of invention: Preparation method of graphene electroconductive composite fiber License type: Exclusive License Record date: 20160310 |
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