CN103966844A - Preparation method of graphene electroconductive composite fiber - Google Patents
Preparation method of graphene electroconductive composite fiber Download PDFInfo
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- CN103966844A CN103966844A CN201410220720.9A CN201410220720A CN103966844A CN 103966844 A CN103966844 A CN 103966844A CN 201410220720 A CN201410220720 A CN 201410220720A CN 103966844 A CN103966844 A CN 103966844A
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Abstract
The invention provides a preparation method of a graphene electroconductive composite fiber. The method is characterized by comprising the following procedures: in a textile fiber surface modification procedure, a textile fiber is soaked into a silane coupling agent KH560 solution with the concentration of 1-30 percent for 2-3 hours and then is put into an oven of 50-65 DEG C to be dried to prepare the surfactant modified textile fiber; in a graphene dispersion system preparation procedure, graphene is prepared from an oxidized graphene aqueous solution prepared by means of a Hummer's method in a chemical reduction method, and a uniform and stable graphene dispersion system with the concentration of 0.1-5 percent is prepared under the function of a dispersing agent; in a graphene composite fiber preparation procedure, the modified textile fiber is soaked in the graphene dispersion system for 2-3 hours and then put into the oven of 50-65 DEG C to be dried to obtain the graphene electroconductive composite fiber. The preparation method is simple and reasonable in process, easy to operate, high in yield, high in reduction degree and high in conductivity and anti-radiation performance; the using amount of graphene is less and the dispersion system is uniform and stable.
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 field such as antistatic clothes or anti-electromalgnetic radiation clothes that pooled applications is used in special occasions conventionally.
The main method of conductive fiber manufacture comprises, 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 coated with conductive layer method is to contain the conductive material of 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 to fiber surface by situ aggregation method and obtain conductive fiber, Conductivity of Fiber electrical property prepared by said method is outstanding, but water-wash resistance and durability are not ideal enough.Conducting particles (being mainly carbon black or metallic compound) and the main polymer of non-conductive composition are carried out blend by co-blended spinning, prepare composite conducting fiber 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-dimensional nano material of honeycomb lattice, has the structure of perfect large pi-conjugated system and the thinnest individual layer atomic thickness (0.34nm).Show huge application potential due to the physical and chemical performance (high-strength, high heat conduction, high conduction, Ultralight) of its special nanostructured and excellence at numerous areas such as biomedicine, energy storage, sensor and composites.By compound to Graphene and textile fabric, the research of 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, easy operating, and output is higher, Graphene consumption is less, and Graphene dispersion is uniform and stable, reducing degree is good, and conduction, shielding property is good, and this is technical task urgently to be resolved hurrily at present.
Summary of the invention
The present invention solves the problem that prior art exists, and a kind of preparation method of graphene conductive composite fibre is provided, and technique is simple, reasonable, easy operating, and output is higher, and Graphene consumption is less, Graphene dispersion is uniform and stable, and reducing degree is good, and conduction, shielding property is 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, comprises the textile fabric surface modification, the preparation of Graphene dispersion, the Graphene composite fibre preparation section that carry out successively; Described textile fabric surface modification operation is: textile fabric is soaked in to 2-3 hour in the silane coupler KH560 solution that concentration is 1%-30%, is placed in after 50-65 DEG C of baking oven is dried and makes surfactant-modified textile fabric; Described Graphene dispersion preparation section is: the standby graphite oxide aqueous solution of Hummer ' s legal system passes through chemical preparation Graphene, and under the effect of dispersant, prepares uniform and stable Graphene dispersion, and its concentration is 0.1%-5%; Described Graphene composite fibre preparation section is: the textile fabric after modification is immersed in to 2-3 hour in Graphene dispersion, 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 standby graphene oxide concentration of aqueous solution 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.
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:
Preparation method's of the present invention production technology is simple, easy operating, and 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) improves tens orders of magnitude, has reached conductive fiber scope, and 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.
Brief description of the drawings
Fig. 1 is Graphene composite conducting fiber preparation 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 preparation method's of a kind of graphene conductive composite fibre of the present invention detailed description of the invention, comprises the textile fabric surface modification, the preparation of Graphene dispersion, the Graphene composite fibre preparation section that carry out successively;
Described textile fabric surface modification operation is: textile fabric is soaked in to 2-3 hour in the silane coupler KH560 solution that concentration is 1%-30%, is placed in after 50-65 DEG C of baking oven is dried and makes surfactant-modified textile fabric;
Described Graphene dispersion preparation section is: the standby graphite oxide aqueous solution of Hummer ' s legal system passes through chemical preparation Graphene, and under the effect of dispersant, prepares uniform and stable Graphene dispersion, and its concentration is 0.1%-5%;
Described Graphene composite fibre preparation section is: the textile fabric after modification is immersed in to 2-3 hour in Graphene dispersion, 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 preparation method, comprise the PET fiber surface modified process, Graphene dispersion preparation section and the Graphene terylene composite fibre preparation section that carry out successively, wherein:
Described PET fiber surface modified process is: it is in 30% silane coupler KH560 solution 3 hours that polyster fibre is soaked in to concentration, is placed in 65 DEG C of baking ovens and makes surfactant-modified polyster fibre after dry; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:5;
Described Graphene dispersion preparation section is: the standby graphene oxide concentration of aqueous solution 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, and dispersant accounts for 10% of Graphene weight, and graphene solution concentration is 0.5%.
After tested, be 10 without the polyster fibre resistivity of conductive processing
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 preparation method, comprise the cotton composite fibre preparation section of the cotton fiber surface modification operation, Graphene dispersion preparation section and the Graphene that carry out successively, wherein:
Described cotton fiber surface modification operation is: it is in 20% silane coupler KH560 solution 3 hours that cotton fiber is soaked in to concentration, is placed in 65 DEG C of baking ovens and makes surfactant-modified cotton fiber after dry; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:3;
Described Graphene dispersion preparation section is: the standby graphene oxide concentration of aqueous solution 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, and dispersant accounts for 15% of Graphene weight, and graphene solution concentration is 0.3%.
After tested, be 10 without the cotton fiber resistivity of conductive processing
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%.There is huge application prospect in fields such as anti-electromalgnetic radiation clothes.
Embodiment 3: the compound viscose acetal fibre preparation method of a kind of graphene conductive, comprise the viscose acetal fibre surface modification operation, Graphene dispersion preparation section and the Graphene viscose composite fibre preparation section that carry out successively, wherein:
Described viscose acetal fibre surface modification operation is: it is in 3% silane coupler KH560 solution 2.5 hours that viscose acetal fibre is soaked in to concentration, is placed in 60 DEG C of baking ovens and makes surfactant-modified viscose acetal fibre after dry; Silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:5;
Described Graphene dispersion preparation section is: the standby graphene oxide concentration of aqueous solution 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, and dispersant accounts for 20% of Graphene weight, and graphene solution concentration is 1%.
After tested, be 10 without the viscose acetal fibre resistivity of conductive processing
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%.There is huge application prospect in fields such as conduction and anti-electromalgnetic radiation clothes.
Above embodiment is only in order to technical scheme of the present invention to be described, but not is limited; Although the present invention is had been described in detail with reference to previous embodiment, for the person of ordinary skill of the art, the technical scheme that still can record previous embodiment is modified, or part technical characterictic is wherein equal to replacement; 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 (5)
1. a preparation method for graphene conductive composite fibre, is characterized in that, comprises the textile fabric surface modification, the preparation of Graphene dispersion, the Graphene composite fibre preparation section that carry out successively; Described textile fabric surface modification operation is: textile fabric is soaked in to 2-3 hour in the silane coupler KH560 solution that concentration is 1%-30%, is placed in after 50-65 DEG C of baking oven is dried and makes surfactant-modified textile fabric; Described Graphene dispersion preparation section is: the standby graphite oxide aqueous solution of Hummer ' s legal system passes through chemical preparation Graphene, and under the effect of dispersant, prepares uniform and stable Graphene dispersion, and its concentration is 0.1%-5%; Described Graphene composite fibre preparation section is: the textile fabric after modification is immersed in to 2-3 hour in Graphene dispersion, 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 claimed in claim 1, it is characterized in that, preferred, described silane coupler KH560 solution is water mixed alkoxide solution, and water alcohol is than being 1:1-5.
3. according to the preparation method of the graphene conductive composite fibre described in claim 1 or 2, it is characterized in that, the standby graphene oxide concentration of aqueous solution 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.
4. according to the preparation method of the graphene conductive composite fibre described in claim 1 or 2, 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.
5. according to the preparation method of graphene conductive composite fibre claimed in claim 3, 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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