CN102586922A - 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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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 Graphene fiber preparation method, relate in particular to a kind of preparation method of polyacrylonitrile graft grapheme macroscopic fibres.
Background technology
2010, two of Univ Manchester UK professor Andre Geim obtained Nobel Prize in physics with Konstantin Novoselov because successfully isolate stable Graphene first, had started the upsurge that the whole world is studied Graphene.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.With the native graphite is raw material, can produce the Graphene presoma of grapheme material and chemistry functional in batches.In up-to-date research, the Graphene through chemical oxidation has prepared macroscopical Graphene fiber (Nature communication, 2011; 2:571); But, improve the graphene film interlayer and interact, prepare more high performance Graphene fiber and remain a challenge.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of preparation method of polyacrylonitrile graft grapheme macroscopic fibres is provided.
The preparation method's of polyacrylonitrile graft grapheme macroscopic fibres step is following:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, nitrogen protection add the initator of 0.01 ~ 10 weight portion down, are heated to 50 ~ 95 ℃; Reacted 1 ~ 60 hour; Through deposition, 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 sonicated 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; Extruded velocity with 1 ~ 100 mL/h is the spinning capillary of 5 ~ 500 μ m through diameter; In 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk; The use wrapping head is collected, and obtains polyacrylonitrile graft grapheme macroscopic fibres after the drying.
Described graphene oxide is that natural flake graphite is peeled off method through chemical oxidation and made.
The solvent of said step 1) is methyl alcohol, ethanol, N-Methyl pyrrolidone, acetone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone second, glycol, diethylene glycol (DEG) or their mixed liquor.
Said step 2) solvent is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
Described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, 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 a graphite, raw material sources extensively, be easy to get, with low cost;
2) Graphene presoma and the Graphene colloidal sol of stable polyacrylonitrile grafting of the polyacrylonitrile grafting of highly dissoluble have been prepared simplely;
3) adopt the method for solvent spinning to prepare the Graphene fiber, easy and simple to handle;
4) the Graphene fiber that makes has good intensity and toughness, and excellent electric conductivity is arranged simultaneously;
Description of drawings
Fig. 1: the digital camera photo of Graphene fiber roll on the glass roller bearing, fibre length reaches several meters;
Fig. 2: the electron scanning micrograph of Graphene tensile fiber section show that it has good stratiform orientation arrangement structure, and interlayer has tangible polyacrylonitrile crystallization crosslinked.
The specific embodiment
The preparation method's of polyacrylonitrile graft grapheme macroscopic fibres step is following:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, nitrogen protection add the initator of 0.01 ~ 10 weight portion down, are heated to 50 ~ 95 ℃; Reacted 1 ~ 60 hour; Through deposition, 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 sonicated 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; Extruded velocity with 1 ~ 100 mL/h is the spinning capillary of 5 ~ 500 μ m through diameter; In 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk; The use wrapping head is collected, and obtains polyacrylonitrile graft grapheme macroscopic fibres after the drying.
Described graphene oxide is that natural flake graphite is peeled off method through chemical oxidation and made.
The solvent of said step 1) is methyl alcohol, ethanol, N-Methyl pyrrolidone, acetone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, ethylene glycol, diethylene glycol (DEG) or their mixed liquor.
Said step 2) solvent is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
Described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, 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 specifically described; Present embodiment only is used for the present invention is done further explanation; Can not be interpreted as restriction to protection domain of the present 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 N of 20 mL, dinethylformamide (DMF), the acrylonitrile monemer of 15 g; Nitrogen protection adds the initator of 0.01 g weight portion down, is heated to 60 ℃, reacts 48 hours, through deposition; 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 sonicated 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; Extruded velocity with 10 mL/h is the spinning capillary of 30 μ m through diameter; In 20 ℃ water and methyl-sulfoxide (DMSO) mixed liquor, stop 50 s and be frozen into silk, use wrapping head to collect, obtain the Graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols in methyl-sulfoxide (DMSO), shows good shear flowability equally.The Graphene fibre strength 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, nitrogen protection adds down the initator of 0.01 g weight portion, is heated to 50 ℃, react 48 hours, and is centrifugal through deposition, washs, and drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene with 50 mg polyacrylonitrile grafting adds 3 mL oxolanes, in 30 ℃ with the sonicated 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; Extruded velocity with 10 mL/h is the spinning capillary of 30 μ m through diameter, in 20 ℃ water and N, stops 50 s in the dinethylformamide mixed liquor and is frozen into silk; The use wrapping head is collected, and obtains the Graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols in oxolane, shows good shear flowability equally.The Graphene fibre strength 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) employing prepares the Graphene of polyacrylonitrile grafting with embodiment 1 identical reactions step;
2) Graphene with 50 mg polyacrylonitrile grafting adds 5 mL N-Methyl pyrrolidone, in 30 ℃ with the sonicated 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, be the spinning capillary of 50 μ m with the extruded velocity of 10 mL/h through diameter, in 20 ℃ butanone, stop 50 s and be frozen into silk, use wrapping head to collect, obtain the Graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols in N-Methyl pyrrolidone, shows good shear flowability equally.The Graphene fibre strength 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 DMAC N,N of 20 mL, the acrylonitrile monemer of 10 g; Nitrogen protection adds the initator of 0.01 g weight portion down, is heated to 50 ℃, reacts 60 hours, through deposition; Centrifugal, washing, drying obtains the Graphene of polyacrylonitrile grafting;
2) Graphene with 50 mg polyacrylonitrile grafting adds 10 mL N, dinethylformamide (DMF), in 50 ℃ with the sonicated of 30 KHz 10 hours, obtain the Graphene spinning solution colloidal sol of polyacrylonitrile grafting;
3) adopt the step spinning identical, prepare the Graphene fiber with embodiment 1.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols at N in the dinethylformamide, shows good shear flowability equally.The Graphene fibre strength 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) employing prepares the Graphene of polyacrylonitrile grafting with embodiment 1 identical reactions step;
2) employing prepares the Graphene spinning solution colloidal sol of polyacrylonitrile grafting with embodiment 1 identical reactions step;
3) with the Graphene spinning solution colloidal sol of polyacrylonitrile grafting; Extruded velocity with 10 mL/h is the spinning capillary of 30 μ m through diameter; 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 the Graphene fiber after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols at N in the dinethylformamide, shows good shear flowability equally.The Graphene fibre strength 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, nitrogen protection add the initator of 0.01 weight portion down, are heated to 50 ℃; Reacted 1 hour, through deposition, 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 sonicated 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; Extruded velocity with 1 mL/h is the spinning capillary of 5 μ m through diameter; In 10 ℃ solidification liquid, stop 1s and be frozen into silk, use wrapping head to collect, obtain polyacrylonitrile graft grapheme macroscopic fibres after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols in acetone, shows good shear flowability equally.The Graphene fibre strength 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, nitrogen protection add the initator of 10 weight portions down, are heated to 95 ℃; Reacted 60 hours, through deposition, 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 sonicated 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; Extruded velocity with 100 mL/h is the spinning capillary of 500 μ m through diameter; In 80 ℃ solidification liquid, stop 100s and be frozen into silk, use wrapping head to collect, obtain polyacrylonitrile graft grapheme macroscopic fibres after the drying.
Through above step, the polyacrylonitrile graft grapheme of preparation forms stable sols in dioxane, shows good shear flowability equally.The Graphene fibre strength 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 polyacrylonitrile graft grapheme macroscopic fibres is characterized in that its step is following:
1) acrylonitrile monemer of the solvent of the Graphene of 1 weight portion or graphene oxide, 10-1000 weight portion, 10-1000 weight portion, nitrogen protection add the initator of 0.01 ~ 10 weight portion down, are heated to 50 ~ 95 ℃; Reacted 1 ~ 60 hour; Through deposition, 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 sonicated 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; Extruded velocity with 1 ~ 100 mL/h is the spinning capillary of 5 ~ 500 μ m through diameter; In 10 ~ 80 ℃ solidification liquid, stop 1 ~ 100s and be frozen into silk; The use wrapping head is collected, and obtains polyacrylonitrile graft grapheme macroscopic fibres after the drying.
2. the preparation method of a kind of polyacrylonitrile graft grapheme macroscopic fibres according to claim 1 is characterized in that described graphene oxide is that natural flake graphite is peeled off method through chemical oxidation and made.
3. the preparation method of a kind of polyacrylonitrile graft grapheme macroscopic fibres according to claim 1; The solvent that it is characterized in that said step 1) is methyl alcohol, ethanol, N-Methyl pyrrolidone, acetone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, ethylene glycol, diethylene glycol (DEG) or their mixed liquor.
4. the preparation method of a kind of polyacrylonitrile graft grapheme macroscopic fibres according to claim 1; It is characterized in that said step 2) solvent be water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
5. the preparation method of a kind of polyacrylonitrile graft grapheme macroscopic fibres according to claim 1; It is characterized in that described solidification liquid is water, methyl alcohol, ethanol, isopropyl alcohol, n-butanol, N-Methyl pyrrolidone, methyl-sulfoxide, pyridine, dioxane, N; Dinethylformamide, DMAC N,N, oxolane, butanone, glycol, diethylene glycol (DEG) or their mixed liquor.
6. the preparation method of a kind of polyacrylonitrile graft grapheme macroscopic fibres 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, and TENSILE STRENGTH is 100 ~ 700MPa; Elongation at break is 0.3-15%, and conductance is greater than 10000S/m.
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| CN104264260A (en) * | 2014-07-28 | 2015-01-07 | 四川大学 | Graphene/nanometer cellulose composite fibers and preparation method thereof |
| CN105624830A (en) * | 2016-01-06 | 2016-06-01 | 东华大学 | Ultraviolet-resistant PAN/GO coaxial nano fibers and preparation method thereof |
| CN105732917A (en) * | 2016-04-28 | 2016-07-06 | 北京理工大学 | Preparation method of reduced graphene oxide-grafted polyacrylonitrile |
| CN105932101A (en) * | 2016-05-20 | 2016-09-07 | 广东蒙泰纺织纤维有限公司 | Polypropylene fiber solar microcell and manufacturing method thereof |
| CN106012099A (en) * | 2016-07-15 | 2016-10-12 | 东华大学 | Conductive PAN/rGO coaxial nanofiber 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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| 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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| CN105624830A (en) * | 2016-01-06 | 2016-06-01 | 东华大学 | Ultraviolet-resistant PAN/GO coaxial nano fibers and preparation method thereof |
| CN105732917A (en) * | 2016-04-28 | 2016-07-06 | 北京理工大学 | Preparation method of reduced graphene oxide-grafted polyacrylonitrile |
| CN105932101A (en) * | 2016-05-20 | 2016-09-07 | 广东蒙泰纺织纤维有限公司 | Polypropylene fiber solar microcell and manufacturing method thereof |
| CN106012099A (en) * | 2016-07-15 | 2016-10-12 | 东华大学 | Conductive PAN/rGO coaxial nanofiber 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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| CN108221370B (en) * | 2018-01-23 | 2020-04-14 | 长兴德烯科技有限公司 | Environment-stable high-conductivity graphene composite fiber and preparation method thereof |
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| CN109280994A (en) * | 2018-09-03 | 2019-01-29 | 北京化工大学 | Graphene fiber and preparation method thereof |
| CN109280994B (en) * | 2018-09-03 | 2020-12-15 | 北京化工大学 | Graphene fiber and preparation method thereof |
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Effective date of registration: 20190903 Address after: 313199 Room 830, 8th Floor, Changxing World Trade Building, 1278 Mingzhu Road, Changxing Economic Development Zone, Huzhou City, Zhejiang Province Patentee after: Changxin de Technology Co., Ltd. Address before: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Patentee before: Zhejiang University |