CN102586922B - Preparation method for macroscopic fiber of polyacrylonitrile grafted graphene - Google Patents
Preparation method for macroscopic fiber of polyacrylonitrile grafted graphene Download PDFInfo
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- CN102586922B CN102586922B CN 201210014844 CN201210014844A CN102586922B CN 102586922 B CN102586922 B CN 102586922B CN 201210014844 CN201210014844 CN 201210014844 CN 201210014844 A CN201210014844 A CN 201210014844A CN 102586922 B CN102586922 B CN 102586922B
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Abstract
The invention discloses a preparation method for macroscopic fiber of polyacrylonitrile grafted graphene. The preparation method comprises the following steps: adding 1 part by weight of graphene or oxidized graphene, 10-1000 parts by weight of solvent and 10-1000 parts by weight of acrylonitrile monomer; adding 0.01-10 parts by weight of initiating agent under nitrogen protection; heating to 50-95DEG C; reacting for 1-60 hours; precipitating, carrying out centrifugation, washing and drying to obtain the polyacrylonitrile grafted graphene; dispersing the polyacrylonitrile grafted graphene into polar organic solvent to obtain spinning solution sol of which the mass concentration is 1-20%; continuously extruding the spinning solution from a spinning head capillary at a constant speed to enter solidification solution; collecting the solidified primary fiber under the tensile force; and drying to obtain the macroscopic fiber of the polyacrylonitrile grafted graphene. The preparation method disclosed by the invention is simple and convenient, has a simple technology and can be suitable for large-scale production, and the obtained graphene fiber has excellent intensity, toughness, modulus and electrical conductivity and can be applied in various industrial fields serving as high-strength fiber.
Description
Technical field
The present invention relates to the preparation method of graphene fiber, relate in particular to a kind of preparation method of macroscopic fiber of polyacrylonitrile grafted graphene.
Background technology
2010, two of Univ Manchester UK professor Andre Geim and Konstantin Novoselov obtained Nobel Prize in physics because successfully isolate first stable Graphene, have started the upsurge of the whole world to Graphene research.Graphene (Graphene) is a kind of monolayer two dimensional crystal, have the highest intensity of known materials (Science, 2008,
321, 385-388) and excellent electric conductivity and thermal conductivity, be present optimal two-dimensional nano material.Take native graphite as raw material, can produce the Graphene presoma of grapheme material and chemistry functional in batches.In up-to-date research, the Graphene by chemical oxidation has prepared macroscopical graphene fiber (Nature communication, 2011,2:571), but, improve the graphene film Interaction between layers, prepare more high performance graphene fiber and remain a challenge.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of macroscopic fiber of polyacrylonitrile grafted graphene is provided.
The preparation method's of macroscopic fiber of polyacrylonitrile grafted graphene step is as follows:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, the initator that adds 0.01 ~ 10 weight portion under the nitrogen protection, be heated to 50 ~ 95 ℃, reacted 1 ~ 60 hour, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene of 1 weight portion polyacrylonitrile grafting is added the solvent of 5 ~ 150 weight portions, in 30 ~ 80 ℃ with the ultrasonic processing of 5 ~ 50 KHz 0.1 ~ 10 hour, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 1 ~ 100 mL/h by the spinning capillary of diameter as 5 ~ 500 μ m, in 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk, the use wrapping head is collected, and obtains macroscopic fiber of polyacrylonitrile grafted graphene after the drying.
Described graphene oxide is that natural flake graphite makes by the chemical oxidation stripping method.
The solvent of described step 1) is methyl alcohol, ethanol, 1-METHYLPYRROLIDONE, acetone, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone second, glycol, diethylene glycol (DEG) or their mixed liquor.
Described step 2) solvent is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
Described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
The macroscopic fibres of described polyacrylonitrile graft grapheme is arranged vertically to pile up by Graphene and is formed, crosslinked by the crystalline polypropylene nitrile between graphene layer, the diameter of fiber is the 5-1000 micron, and TENSILE STRENGTH is 100 ~ 700MPa, elongation at break is 0.3-15%, and conductance is greater than 10000S/m.
The beneficial effect that the present invention compared with prior art has:
1) primary raw materials of Graphene or graphene oxide is graphite, raw material sources extensively, be easy to get, with low cost;
2) the Graphene presoma of polyacrylonitrile grafting of highly dissoluble and the Graphene colloidal sol of stable polyacrylonitrile grafting have been prepared simplely;
3) adopt the method for solution spinning to prepare graphene fiber, easy and simple to handle;
4) graphene fiber that makes has good intensity and toughness, and excellent electric conductivity is arranged simultaneously;
Description of drawings
Fig. 1: graphene fiber is wound on the digital camera photo on the glass roller bearing, and fibre length reaches several meters;
Fig. 2: the electron scanning micrograph of graphene fiber stretching section show that it has good stratiform orientation arrangement structure, and interlayer has obvious polyacrylonitrile crystallization crosslinked.
The specific embodiment
The preparation method's of macroscopic fiber of polyacrylonitrile grafted graphene step is as follows:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, the initator that adds 0.01 ~ 10 weight portion under the nitrogen protection, be heated to 50 ~ 95 ℃, reacted 1 ~ 60 hour, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene of 1 weight portion polyacrylonitrile grafting is added the organic solvent of 5 ~ 150 weight portions, in 30 ~ 80 ℃ with the ultrasonic processing of 5 ~ 50 KHz 0.1 ~ 10 hour, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 1 ~ 100 mL/h by the spinning capillary of diameter as 5 ~ 500 μ m, in 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk, the use wrapping head is collected, and obtains macroscopic fiber of polyacrylonitrile grafted graphene after the drying.
Described graphene oxide is that natural flake graphite makes by the chemical oxidation stripping method.
The solvent of described step 1) is methyl alcohol, ethanol, 1-METHYLPYRROLIDONE, acetone, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, ethylene glycol, diethylene glycol (DEG) or their mixed liquor.
Described step 2) solvent is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
Described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
The macroscopic fibres of described polyacrylonitrile graft grapheme is arranged vertically to pile up by Graphene and is formed, crosslinked by the crystalline polypropylene nitrile between graphene layer, the diameter of fiber is the 5-1000 micron, and TENSILE STRENGTH is 100 ~ 700MPa, elongation at break is 0.3-15%, and conductance is greater than 10000S/m.
Below in conjunction with embodiment the present invention is described specifically; the present embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; those skilled in the art makes some nonessential change and adjustment according to the content of foregoing invention, all belongs to protection scope of the present invention.
Embodiment 1:
1) graphene oxide of 20 mg, the DMF of 20 mL (DMF), the acrylonitrile monemer of 15 g, the initator that adds 0.01 g weight portion under the nitrogen protection, be heated to 60 ℃, reacted 48 hours, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene with the polyacrylonitrile grafting adds 10 mL methyl-sulfoxides (DMSO), in 30 ℃ with the ultrasonic processing of 0 ~ 50KHz 5 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 10 mL/h by the spinning capillary of diameter as 30 μ m, in 20 ℃ water and methyl-sulfoxide (DMSO) mixed liquor, stop 50 s and be frozen into silk, use wrapping head to collect, obtain graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in methyl-sulfoxide (DMSO), show equally good Shear Flow.The graphene fiber intensity of spinning is 400 ~ 750MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 2:
1) Graphene of 20 mg, the dioxane of 20 mL, the acrylonitrile monemer of 10 g adds the initator of 0.01 g weight portion under the nitrogen protection, be heated to 50 ℃, react 48 hours, and is centrifugal through precipitation, washs, and drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene with 50 mg polyacrylonitrile grafting adds 3 mL oxolanes, in 30 ℃ with the ultrasonic processing of 0 ~ 50KHz 5 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting,, in 20 ℃ water and DMF mixed liquor, stop 50 s and be frozen into silk by the spinning capillary of diameter as 30 μ m take the extruded velocity of 10 mL/h, the use wrapping head is collected, and obtains graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in oxolane, show equally good Shear Flow.The graphene fiber intensity of spinning is 300 ~ 350MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 3:
1) adopt the reactions steps identical with embodiment 1 to prepare the Graphene of polyacrylonitrile grafting;
2) Graphene with 50 mg polyacrylonitrile grafting adds 5 mL 1-METHYLPYRROLIDONEs, in 30 ℃ with the ultrasonic processing of 30 KHz 5 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting,, in 20 ℃ butanone, stop 50 s and be frozen into silk by the spinning capillary of diameter as 50 μ m take the extruded velocity of 10 mL/h, use wrapping head to collect, obtain graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in 1-METHYLPYRROLIDONE, show equally good Shear Flow.The graphene fiber intensity of spinning is 300 ~ 350MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 4:
1) graphene oxide of adding 20 mg, the DMA of 20 mL, the acrylonitrile monemer of 10 g, add the initator of 0.01 g weight portion under the nitrogen protection, be heated to 50 ℃, reacted 60 hours, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene with 50 mg polyacrylonitrile grafting adds 10 mL DMFs (DMF), in 50 ℃ with the ultrasonic processing of 30 KHz 10 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) adopt the step spinning identical with embodiment 1, prepare graphene fiber.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in DMF, show equally good Shear Flow.The graphene fiber intensity of spinning is 400 ~ 450MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 5:
1) adopt the reactions steps identical with embodiment 1 to prepare the Graphene of polyacrylonitrile grafting;
2) adopt the reactions steps identical with embodiment 1 to prepare the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 10 mL/h by the spinning capillary of diameter as 30 μ m, in 20 ℃ water and acetone mixed liquor, stop 80 s and be frozen into silk, use wrapping head to collect in the collection process and add certain pulling force, make fiber obtain stretch orientation, obtain graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in DMF, show equally good Shear Flow.The graphene fiber intensity of spinning is 300 ~ 350MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 6:
1) acrylonitrile monemer of the butanols of the Graphene of 1 weight portion or graphene oxide, 10 weight portions, 10 weight portions, the initator of adding 0.01 weight portion is heated to 50 ℃ under the nitrogen protection, reacted 1 hour, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene of 1 weight portion polyacrylonitrile grafting is added the acetone of 5 weight portions, in 30 ℃ with the ultrasonic processing of 5 KHz 0.1 hour, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5 μ m, in 10 ℃ solidification liquid, stop 1s and be frozen into silk, use wrapping head to collect, obtain macroscopic fiber of polyacrylonitrile grafted graphene after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in acetone, show equally good Shear Flow.The graphene fiber intensity of spinning is 300 ~ 350MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Embodiment 7:
1) acrylonitrile monemer of the oxolane of the Graphene of 1 weight portion or graphene oxide, 1000 weight portions, 1000 weight portions, the initator of adding 10 weight portions is heated to 95 ℃ under the nitrogen protection, reacted 60 hours, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene of 1 weight portion polyacrylonitrile grafting is added the dioxane of 150 weight portions, in 80 ℃ with the ultrasonic processing of 50 KHz 10 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 100 mL/h by the spinning capillary of diameter as 500 μ m, in 80 ℃ solidification liquid, stop 100s and be frozen into silk, use wrapping head to collect, obtain macroscopic fiber of polyacrylonitrile grafted graphene after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable colloidal sol in dioxane, show equally good Shear Flow.The graphene fiber intensity of spinning is 300 ~ 350MPa, and elongation at break is 5% ~ 10%, and conductance has good toughness simultaneously greater than 10000S/m.
Claims (6)
1. the preparation method of a macroscopic fiber of polyacrylonitrile grafted graphene is characterized in that its step is as follows:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, the initator that adds 0.01 ~ 10 weight portion under the nitrogen protection, be heated to 50 ~ 95 ℃, reacted 1 ~ 60 hour, through precipitation, centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene of 1 weight portion polyacrylonitrile grafting is added the solvent of 5 ~ 150 weight portions, in 30 ~ 80 ℃ with the ultrasonic processing of 5 ~ 50 KHz 0.1 ~ 10 hour, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting, take the extruded velocity of 1 ~ 100 mL/h by the spinning capillary of diameter as 5 ~ 500 μ m, in 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk, the use wrapping head is collected, and obtains macroscopic fiber of polyacrylonitrile grafted graphene after the drying.
2. the preparation method of a kind of macroscopic fiber of polyacrylonitrile grafted graphene according to claim 1 is characterized in that described graphene oxide is that natural flake graphite makes by the chemical oxidation stripping method.
3. the preparation method of a kind of macroscopic fiber of polyacrylonitrile grafted graphene according to claim 1, the solvent that it is characterized in that described step 1) is methyl alcohol, ethanol, 1-METHYLPYRROLIDONE, acetone, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, ethylene glycol or their mixed liquor.
4. the preparation method of a kind of macroscopic fiber of polyacrylonitrile grafted graphene according to claim 1, it is characterized in that described step 2) solvent be water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol or their mixed liquor.
5. the preparation method of a kind of macroscopic fiber of polyacrylonitrile grafted graphene according to claim 1, it is characterized in that described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 1-METHYLPYRROLIDONE, methyl-sulfoxide, pyridine, dioxane, N, dinethylformamide, DMA, oxolane, butanone, glycol or their mixed liquor.
6. the preparation method of a kind of macroscopic fiber of polyacrylonitrile grafted graphene according to claim 1, the macroscopic fibres that it is characterized in that described polyacrylonitrile graft grapheme is arranged vertically to pile up by Graphene and is formed, crosslinked by the crystalline polypropylene nitrile between graphene layer, the diameter of fiber is the 5-1000 micron, TENSILE STRENGTH is 100 ~ 700MPa, elongation at break is 0.3-15%, and electrical conductivity is greater than 10000S/m.
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| CN103408880B (en) * | 2013-06-27 | 2015-10-14 | 安徽百特新材料科技有限公司 | A kind of preparation method of polyacrylonitrile/grcomposite composite material |
| CN104264260B (en) * | 2014-07-28 | 2016-04-13 | 四川大学 | A kind of graphene/nanometer cellulose composite fiber and preparation method thereof |
| CN105624830B (en) * | 2016-01-06 | 2017-12-22 | 东华大学 | A kind of uvioresistant PAN/GO Coaxial Nanofibers and preparation method thereof |
| CN105732917B (en) * | 2016-04-28 | 2018-12-28 | 北京理工大学 | A kind of preparation method of redox graphene graft polypropylene nitrile |
| CN105932101B (en) * | 2016-05-20 | 2017-10-10 | 广东蒙泰高新纤维股份有限公司 | A kind of polypropylene fiber solar micro battery and its manufacture method |
| CN106012099B (en) * | 2016-07-15 | 2018-12-04 | 东华大学 | A kind of conduction PAN/rGO Coaxial Nanofibers and preparation method thereof |
| CN107475818A (en) * | 2017-08-18 | 2017-12-15 | 北京化工大学 | Compound carbon fiber of graphene polyacrylonitrile-radical and preparation method thereof |
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| CN109016549A (en) * | 2018-06-29 | 2018-12-18 | 成都市容德建筑劳务有限公司 | A kind of composite box processing method for building |
| CN109280994B (en) * | 2018-09-03 | 2020-12-15 | 北京化工大学 | Graphene fiber and preparation method thereof |
| CN113385153A (en) * | 2021-06-25 | 2021-09-14 | 南通强生石墨烯科技有限公司 | Graphene ion exchange fiber and preparation method thereof |
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