CN107053817A - A kind of continuous coiled preparation method of flexible multi-layered graphene - Google Patents
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Abstract
Pin of the present invention is related to a kind of continuous coiled preparation method of flexible multi-layered graphene, comprises the following steps：(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, film is pressed into after roll-in, film is subjected to high-temperature process under argon gas, graphene film is obtained；(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, cans again, the flexible multi-layered graphene film of long size is made, production efficiency is greatly improved, at the same time, graphene film is gapless to be fitted on electrostatic film, directly cutting can be used, and improve precision, it is to avoid waste product occur, reduce manually, reduce cost.
Description
Technical field
The present invention relates to a kind of continuous coiled method of graphene, and in particular to a kind of flexible multi-layered graphene is continuously coiled
Preparation method.
Background technology
Graphite is a kind of allotrope of elemental carbon, and the periphery of each carbon atom, which links, writes the other three carbon atom (row
Row mode is in cellular multiple hexagons) with Covalent bonding together, constitute covalent molecule.Graphite belongs to typical layer structure,
Carbon atom aligned in layers, is equidistantly connected between each carbon and adjacent carbon, and the carbon in each layer is arranged by hexagonal ring shape, up and down phase
The carbon hexagonal ring of adjacent bed forms layer structure by being stacked again after the parallel mutual displacement in wire side direction.Due to its special construction, stone
Ink has heat-resisting quantity, electric conductivity, thermal conductivity, lubricity, chemical stability, plasticity and thermal shock resistance etc., can be as resistance to
Fiery material, lubriation material, conductive heat conducting material etc. are applied in the industry such as metallurgy, chemical industry, machinery, electronics, atomic energy and national defence.
Its thermal conductivity exceedes the metal materials such as steel, iron, lead.But thermal conductivity factor is raised and reduced with temperature, at very high temperatures, graphite
Can also be into heat guard.Graphite film material is because with the heat conductivility for surmounting metal material, also with as organic plastics
Plasticity, and can be coated in the characteristic of the surface of solids, in all electronical display products if desired for radiating and need what is heated
Electronic component field, which is obtained for, to be widely applied.
It is well known that at present graphene and graphene microchip graphite furnace or other increase temperature technique and vaporize other elements
Leave carbon to form, and be sheet stock, sheet stock due to be limited to shape cannot automated production, therefore can only it is single plus
Work, spillage of material is very big, it is impossible to form the coiled strip having an economic benefit.
Graphite film is mainly produced with sheet form, and this brings inconvenience to the cross cutting processing in later stage, is characterized in the reality of material
Border utilization rate can not be improved, and the graphite film of sheet needs a piece of connect of graphite film a piece of being affixed on diaphragm or electrostatic before cross cutting
So as to form package structure on film, then cut.But it is to connect a piece of by flake graphite film is a piece of the problem of be primarily present at present
When being affixed on diaphragm or electrostatic film, piece and the distance between piece are uncontrollable, cause the distance between graphite film and piece
, it is impossible to cutting accuracy is controlled, waste product easily occurs, virtually improves production cost.
The content of the invention
The present invention proposes a kind of continuous coiled preparation method of flexible multi-layered graphene regarding to the issue above, makes long chi
Very little flexible multi-layered graphene film, greatly improves production efficiency, at the same time, and graphene film is gapless to be fitted in electrostatic
On film, directly cutting can be used, and improve precision, it is to avoid waste product occur, reduces manually, reduces cost.
Specific technical scheme is as follows：
A kind of continuous coiled preparation method of flexible multi-layered graphene, comprises the following steps：
(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, be pressed into after roll-in
Film, high-temperature process is carried out by film under argon gas, and 1300 DEG C -1800 DEG C are warming up to 15 DEG C/min speed, is incubated 1-3h
Obtain graphene film；
(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；
(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；
(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, then cans.
A kind of continuous coiled preparation method of above-mentioned flexible multi-layered graphene, wherein, the length of the electrostatic film is more than
100m, the length of flexible multi-layered graphene film is more than 100m, flexible multi-layered graphene film laminating absorption curl shape on electrostatic film
Into coil structure.
A kind of continuous coiled preparation method of above-mentioned flexible multi-layered graphene, wherein, the preparation method of the phase change layer is：
(1) solidification liquid is prepared, coagulant liquid is first warming up to 800- under atmosphere of inert gases with 10-15 DEG C/min speed
1200 DEG C, it is incubated 1-2h；
(2) 1800-2200 DEG C is warming up to 5-8 DEG C/min speed under atmosphere of inert gases, is incubated 2-3h；
(3) 2800-3200 DEG C is warming up to 1-3 DEG C/min speed under atmosphere of inert gases, is incubated 3-4h, obtains gas
Gel mould；
(4) aerogel film is soaked into 1-10h in dichloromethane solution of the concentration for 1-100g/ml paraffin, then be put in
Dried in 20-40 DEG C of vacuum drying oven, obtain phase change layer.
A kind of continuous coiled preparation method of above-mentioned flexible multi-layered graphene, wherein, the inert gas is by argon gas, helium
With nitrogen according to 3:4:1 volume ratio is mixed.
A kind of continuous coiled preparation method of above-mentioned flexible multi-layered graphene, wherein, the preparation method of the solidification liquid is：
(1) count 0.5-2.4 parts of zinc oxide, 5-18 parts of sodium citrate, 3-9 parts of glycerine, butanediamine by weight
2.2-4.5 parts, 15-32 parts of vinyl acetate-ethylene copolymerization emulsions, carry out ultrasound after the mixing of 22-38 parts of dioctyl phthalate
Wavelength-division dissipates 20-50min and obtains mixed liquor A；
(2) expanded graphite is added in mixed liquor A, solidification liquid is can obtain after stirring 2-3h；The weight of expanded graphite is
The 0.1%-1.3% of mixed liquor A weight.
A kind of continuous coiled preparation method of above-mentioned flexible multi-layered graphene, wherein, the preparation method of the bonding agent is：
Count 15-28 parts of Kynoar, 3-9 parts of Ludox, 10-16 parts of naphthenic oil, ethylene glycol 8-16 by weight
Part mixes 1-2h at a temperature of 60-80 DEG C can obtain bonding agent.
Beneficial effects of the present invention are：
Graphene press mold is fixed between two phase change layers by the present invention by gluing, and bonding agent is coated in graphene press mold
Upper and lower two end faces on, bonding agent realize being adhesively fixed effect, fix it is more firm.
The splendid heat sink material of graphene effect propety, serves radiating effect, realizes quick conductive well, with phase
Change layer is coordinated, and is realized the storage of potential, is put, improves economic value, production efficiency greatly improved, reduce cost,
Have wide range of applications, can be widely used for equipment cooling.
The present invention sets unique phase change layer and bonding agent, heat dispersion is greatly improved, while having certain heat accumulation
Effect, further adds the application of graphene composite film
Graphene coil stock of the present invention is adapted to substantial amounts of and automated production, and can make bigger longer size, therefore greatly
Improve production efficiency；
The present invention presses coiled flexible multi-layered graphene film and electrostatic film in rolls by calender, and machine is cut i.e. by film
Can fine cut cutting, it is to avoid waste product occur, reduce artificial, reduce cost.
Embodiment
To make technical scheme become apparent from clearly, below the present invention is described further, it is any to this
The scheme that the technical characteristic progress equivalencing of inventive technique scheme and conventional reasoning are drawn each falls within the scope of the present invention.
Embodiment one
A kind of continuous coiled preparation method of flexible multi-layered graphene, comprises the following steps：
(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, be pressed into after roll-in
Film, high-temperature process is carried out by film under argon gas, is warming up to 1500 DEG C with 20 DEG C/min speed, insulation 2h obtains graphene
Film；
(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；
(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；
(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, then cans.
The length of the electrostatic film is 300m, and the length of flexible multi-layered graphene film is 300m, flexible multi-layered graphene film
Laminating absorption curls into coil structure on electrostatic film.
The preparation method of the phase change layer is：
(1) solidification liquid is prepared, coagulant liquid is first warming up to 950 DEG C under atmosphere of inert gases with 13 DEG C/min speed,
It is incubated 1.5h；
(2) 2000 DEG C are warming up to 7 DEG C/min speed under atmosphere of inert gases, are incubated 2.2h；
(3) 3000 DEG C are warming up to 2 DEG C/min speed under atmosphere of inert gases, are incubated 3.5h, obtain aerogel film；
(4) aerogel film is soaked into 4h in dichloromethane solution of the concentration for 38g/ml paraffin, then is put in 30 DEG C very
Dried in empty baking oven, obtain phase change layer.
The inert gas is by argon gas, helium and nitrogen according to 3:4:1 volume ratio is mixed.
The preparation method of the solidification liquid is：
(1) count 1.5 parts of zinc oxide, 12 parts of sodium citrate, 7.5 parts of glycerine, 3.5 parts of butanediamine, vinegar by weight
The scattered 30min of ultrasonic wave, which is carried out, after sour 22 parts of ethylene-vinyl copolymer emulsion, 34 parts of mixing of dioctyl phthalate obtains mixed liquor
A；
(2) expanded graphite is added in mixed liquor A, solidification liquid is can obtain after stirring 2.5h；The weight of expanded graphite is
The 0.8% of mixed liquor A weight.
The preparation method of the bonding agent is：
Count 23 parts of Kynoar, 6 parts of Ludox, 13 parts of naphthenic oil, 12 parts of ethylene glycol by weight at 75 DEG C
At a temperature of mix 1.5h can obtain bonding agent.
Embodiment two
A kind of continuous coiled preparation method of flexible multi-layered graphene, comprises the following steps：
(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, be pressed into after roll-in
Film, high-temperature process is carried out by film under argon gas, is warming up to 1300 DEG C with 15 DEG C/min speed, insulation 1h obtains graphene
Film；
(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；
(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；
(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, then cans.
The length of the electrostatic film is 200m, and the length of flexible multi-layered graphene film is 200m, flexible multi-layered graphene film
Laminating absorption curls into coil structure on electrostatic film.
The preparation method of the phase change layer is：
(1) solidification liquid is prepared, coagulant liquid is first warming up to 800 DEG C under atmosphere of inert gases with 10 DEG C/min speed,
It is incubated 1h；
(2) 1800 DEG C are warming up to 5 DEG C/min speed under atmosphere of inert gases, are incubated 2h；
(3) 2800 DEG C are warming up to 1 DEG C/min speed under atmosphere of inert gases, are incubated 3h, obtain aerogel film；
(4) aerogel film is soaked into 1.5h in dichloromethane solution of the concentration for 20g/ml paraffin, then is put in 25 DEG C
Dried in vacuum drying oven, obtain phase change layer.
The inert gas is by argon gas, helium and nitrogen according to 3:4:1 volume ratio is mixed.
The preparation method of the solidification liquid is：
(1) count 0.5 part of zinc oxide, 5 parts of sodium citrate, 3 parts of glycerine, 2.2 parts of butanediamine, acetic acid second by weight
The scattered 30min of ultrasonic wave, which is carried out, after 15 parts of alkene-ethylene copolymerization emulsions, 22 parts of mixing of dioctyl phthalate obtains mixed liquor A；
(2) expanded graphite is added in mixed liquor A, solidification liquid is can obtain after stirring 2h；The weight of expanded graphite is mixed
Close the 0.3% of liquid A weight.
The preparation method of the bonding agent is：
The temperature at 60 DEG C by 15 parts of Kynoar, 3 parts of Ludox, 10 parts of naphthenic oil, 8 parts of ethylene glycol is counted by weight
The lower mixing 1h of degree can obtain bonding agent.
Embodiment three
A kind of continuous coiled preparation method of flexible multi-layered graphene, comprises the following steps：
(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, be pressed into after roll-in
Film, high-temperature process is carried out by film under argon gas, is warming up to 1800 DEG C with 25 DEG C/min speed, insulation 3h obtains graphene
Film；
(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；
(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；
(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, then cans.
The length of the electrostatic film is 320m, and the length of flexible multi-layered graphene film is 320m, flexible multi-layered graphene film
Laminating absorption curls into coil structure on electrostatic film.
The preparation method of the phase change layer is：
(1) solidification liquid is prepared, coagulant liquid is first warming up to 200 DEG C under atmosphere of inert gases with 15 DEG C/min speed,
It is incubated 2h；
(2) 2200 DEG C are warming up to 8 DEG C/min speed under atmosphere of inert gases, are incubated 3h；
(3) 3200 DEG C are warming up to 3 DEG C/min speed under atmosphere of inert gases, are incubated 4h, obtain aerogel film；
(4) aerogel film is soaked into 7h in dichloromethane solution of the concentration for 76g/ml paraffin, then is put in 40 DEG C very
Dried in empty baking oven, obtain phase change layer.
The inert gas is by argon gas, helium and nitrogen according to 3:4:1 volume ratio is mixed.
The preparation method of the solidification liquid is：
(1) count 2.4 parts of zinc oxide, 18 parts of sodium citrate, 9 parts of glycerine, 4.5 parts of butanediamine, acetic acid by weight
The scattered 50min of ultrasonic wave, which is carried out, after 32 parts of ethylene-vinyl copolymer emulsion, 38 parts of mixing of dioctyl phthalate obtains mixed liquor A；
(2) expanded graphite is added in mixed liquor A, solidification liquid is can obtain after stirring 3h；The weight of expanded graphite is mixed
Close the 1.2% of liquid A weight.
The preparation method of the bonding agent is：
Count 28 parts of Kynoar, 9 parts of Ludox, 16 parts of naphthenic oil, 16 parts of ethylene glycol by weight at 80 DEG C
At a temperature of mix 2h can obtain bonding agent.
Claims (6)
1. a kind of continuous coiled preparation method of flexible multi-layered graphene, it is characterized in that, comprise the following steps：
(1) graphene powder is uniformly sprayed on the plastics base film of uniform forward motion, film is pressed into after roll-in,
Film is subjected to high-temperature process under argon gas, 1300 DEG C -1800 DEG C are warming up to 15 DEG C/min speed, insulation 1-3h obtains stone
Black alkene film；
(2) two layers of graphene film was entered to be pressed into integral structure after roll-in, and obtained graphene press mold；
(3) graphene press mold is fixed between two phase change layers by bonding agent and forms flexible multi-layered graphene film；
(4) pressing of flexible multi-layered graphene film is adsorbed on electrostatic film by calender, then cans.
2. the continuous coiled preparation method of a kind of flexible multi-layered graphene as claimed in claim 1, it is characterized in that, the electrostatic
The length of film is more than 100m, and the length of flexible multi-layered graphene film is more than 100m, and flexible multi-layered graphene film laminating absorption is quiet
Coil structure is curled on electrolemma.
3. the continuous coiled preparation method of a kind of flexible multi-layered graphene as claimed in claim 1, it is characterized in that the phase transformation
Layer preparation method be：
(1) solidification liquid is prepared, coagulant liquid is first warming up to 800-1200 under atmosphere of inert gases with 10-15 DEG C/min speed
DEG C, it is incubated 1-2h；
(2) 1800-2200 DEG C is warming up to 5-8 DEG C/min speed under atmosphere of inert gases, is incubated 2-3h；
(3) 2800-3200 DEG C is warming up to 1-3 DEG C/min speed under atmosphere of inert gases, is incubated 3-4h, obtains aeroge
Film；
(4) aerogel film is soaked into 1-10h in dichloromethane solution of the concentration for 1-100g/ml paraffin, then is put in 20-40
Dried in DEG C vacuum drying oven, obtain phase change layer.
4. the continuous coiled preparation method of a kind of flexible multi-layered graphene as claimed in claim 3, it is characterized in that, the inertia
Gas is by argon gas, helium and nitrogen according to 3:4:1 volume ratio is mixed.
5. the continuous coiled preparation method of a kind of flexible multi-layered graphene as claimed in claim 3, it is characterized in that the solidification
The preparation method of liquid is：
(1) count 0.5-2.4 parts of zinc oxide, 5-18 parts of sodium citrate, 3-9 parts of glycerine, butanediamine 2.2-4.5 by weight
Ultrasonic wave is carried out after part, 15-32 parts of vinyl acetate-ethylene copolymerization emulsions, 22-38 parts of mixing of dioctyl phthalate to disperse
20-50min obtains mixed liquor A；
(2) expanded graphite is added in mixed liquor A, solidification liquid is can obtain after stirring 2-3h；The weight of expanded graphite is mixing
The 0.1%-1.3% of liquid A weight.
6. the continuous coiled preparation method of a kind of flexible multi-layered graphene as claimed in claim 3, it is characterized in that, the bonding
The preparation method of agent is：
Count by weight and 15-28 parts of Kynoar, 3-9 parts of Ludox, 10-16 parts of naphthenic oil, 8-16 parts of ethylene glycol exist
1-2h is mixed at a temperature of 60-80 DEG C can obtain bonding agent.
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| CN (1) | CN107053817A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109119345A (en) * | 2018-08-09 | 2019-01-01 | 盐城美茵新材料有限公司 | A kind of membrane structure and preparation method thereof |
| CN113527825A (en) * | 2020-04-13 | 2021-10-22 | 中国科学院大连化学物理研究所 | Graphene-based flexible composite shaped phase-change material film and preparation and application thereof |
-
2016
- 2016-12-28 CN CN201611234381.5A patent/CN107053817A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109119345A (en) * | 2018-08-09 | 2019-01-01 | 盐城美茵新材料有限公司 | A kind of membrane structure and preparation method thereof |
| CN109119345B (en) * | 2018-08-09 | 2020-08-18 | 盐城美茵新材料有限公司 | Membrane structure and manufacturing method thereof |
| CN113527825A (en) * | 2020-04-13 | 2021-10-22 | 中国科学院大连化学物理研究所 | Graphene-based flexible composite shaped phase-change material film and preparation and application thereof |
| CN113527825B (en) * | 2020-04-13 | 2022-06-07 | 中国科学院大连化学物理研究所 | Graphene-based flexible composite shaped phase-change material film and preparation and application thereof |
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