CN109824037A - A kind of preparation method of graphene aerogel electrode material - Google Patents
A kind of preparation method of graphene aerogel electrode material Download PDFInfo
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- CN109824037A CN109824037A CN201910265864.9A CN201910265864A CN109824037A CN 109824037 A CN109824037 A CN 109824037A CN 201910265864 A CN201910265864 A CN 201910265864A CN 109824037 A CN109824037 A CN 109824037A
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Abstract
The present invention provides a kind of preparation method of graphene aerogel electrode material, includes the following steps: the preparation of (1) ionic liquid mixture；(2) preparation of graphene oxide；(3) preparation of graphene oxide water solution；(4) preparation of hydrogel；(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, it is transferred to after dialysing 3-6 days in bag filter and filters, by material much be transferred in vacuum freeze drier, freeze 45-70h at -20 DEG C, obtain graphene aerogel electrode material.A kind of preparation method of graphene aerogel electrode material has high specific capacity, excellent conductivity；Graphene aerogel is prepared by ionic liquid composites and graphite oxide alkene reaction, the ionic liquid composites of reproducibility and graphene oxide are generated into graphene hydrogel by one step hydro thermal method, graphene aerogel electrode material is obtained after freeze-drying.
Description
Technical field
The invention belongs to new energy materials preparation fields, and in particular to a kind of preparation side of graphene aerogel electrode material
Method.
Background technique
Graphene aerogel electrode material itself has good elastic characteristic, is very suitable for the electricity as flexible battery
Pole material comes using can be used for graphene aerogel composite material as the electrode material of lithium ion battery and construct a kind of flexible lithium
Ion battery, make full use of the bi-dimensional cellular shape structure of graphene, very high conductivity, functionalized surface, simultaneously easy processing at
The features such as fexible film, big specific surface area can load more active materials further increases it on the basis of realizing flexibility
Electrochemistry is surely.Not only it had been able to achieve flexibility when grapheme material is as electrode but also the integral energy density of battery can be improved.
Currently, the preparation method of graphene aerogel electrode material is mainly in the majority with self assembly and phase transfer method, hydro-thermal system
Preparation Method is less.Self assembly and phase transfer method preparation process are complicated, and process is not easy to control, and high production cost, to environment
There is certain pollution.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphene aerogel electrode material, have high specific volume
Amount, excellent conductivity.
To achieve the goals above, the invention adopts the following technical scheme: a kind of system of graphene aerogel electrode material
Preparation Method includes the following steps:
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 10-20min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N-
Methylimidazole is added in acetonitrile, stirs 20-30 minutes, N- methylimidazole/acetonitrile mixed solution is obtained, by N- methylimidazole/second
Nitrile mixed solution is added in the bromo- 4- chlorobutane of the good 1- of constant temperature, and ultrasonic disperse 1-3h is then transferred in 35 DEG C of water-bath and reacts
2-5 days, then revolving removed solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to quiet in separatory funnel
Separation is set, removes supernatant liquid to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, by lower water
Water mutually is evaporated off in 60 DEG C of backspins, is then placed into drying 2-5 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixing
Object；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(3) graphene oxide for obtaining step 2 is added in deionized water, and ultrasonic disperse 1-3h obtains graphene oxide
Aqueous solution；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), adds step 1
Liner, is transferred in reaction kettle tightens later by obtained ionic liquid mixture, dry 1-3h in anti-corrosion air dry oven, so
1-2h is stirred with glass bar afterwards, obtains hydrogel；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred in bag filter and is dialysed 3-6 days
After filter, by material much be transferred in vacuum freeze drier, freeze 45-70h at -20 DEG C, obtain graphene airsetting
Gel electrode material.
Preferably, in step 1, the bromo- 4- chlorobutane of N- methylimidazole, acetonitrile, 1-, ethyl acetate, water mass ratio be 1-
5:30-120:1-5:80-180:90-200。
Preferably, in step 2, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, quality point
The mass ratio for the hydrogen peroxide that Particle density is 30% is 1-5:3-6:100-180:1-4:150-200:1-4.
Preferably, in step 3, graphene oxide, deionized water quality ratio are 2-5:80-120.
Preferably, in step 4, graphene oxide water solution, ionic liquid mixture mass ratio be 80-100:6-12.
The invention has the following advantages: a kind of preparation method of graphene aerogel electrode material, has high ratio
Capacity, excellent conductivity；Graphene has preferable electric conductivity, chemical stability and higher specific surface area；Pass through ion
Liquid complex and graphite oxide alkene reaction prepare graphene aerogel, by the ionic liquid composites and graphite oxide of reproducibility
Alkene generates graphene hydrogel by one step hydro thermal method, and graphene aerogel electrode material is obtained after freeze-drying.
Specific embodiment
Embodiment 1
A kind of preparation method of graphene aerogel electrode material, includes the following steps:
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 10min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N- first
Base imidazoles is added in acetonitrile, stirs 20 minutes, obtains N- methylimidazole/acetonitrile mixed solution, and N- methylimidazole/acetonitrile is mixed
Solution is added in the bromo- 4- chlorobutane of the good 1- of constant temperature, ultrasonic disperse 1h, is then transferred in 35 DEG C of water-bath and is reacted 2 days, then
Revolving removes solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to settle and separate in separatory funnel, removes
Supernatant liquid is to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, by lower layer's water phase at 60 DEG C
Revolving water removal is then placed into drying 2 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixture；N- methyl miaow
The bromo- 4- chlorobutane of azoles, acetonitrile, 1-, ethyl acetate, water mass ratio be 1:30:1:80:90；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1h, and it is 35 DEG C and magnetic agitation 1h that mixed solution temperature is then controlled under condition of ice bath；Add again into mixed solution
Entering temperature is 70 DEG C of deionized waters, obtains bright orange color contamination liquor after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%,
Graphene oxide is obtained after being 6 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate,
The mass ratio for the hydrogen peroxide that 70 DEG C of deionized waters, mass fraction concentration are 30% is 1:3:100:1:150:1；
(3) graphene oxide for obtaining step 2 is added in deionized water, and ultrasonic disperse 1h obtains graphene oxide water
Solution；Graphene oxide, deionized water quality ratio are 2:80；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), adds step 1
Liner, is transferred in reaction kettle tightens later by obtained ionic liquid mixture, dry 1h in anti-corrosion air dry oven, then
1h is stirred with glass bar, obtains hydrogel；Graphene oxide water solution, ionic liquid mixture mass ratio be 80:6；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred to after dialysing 3 days in bag filter
Filter, by material much be transferred in vacuum freeze drier, freeze 45h at -20 DEG C, obtain graphene aerogel electrode
Material.
Embodiment 2
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 20min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N- first
Base imidazoles is added in acetonitrile, stirs 30 minutes, obtains N- methylimidazole/acetonitrile mixed solution, and N- methylimidazole/acetonitrile is mixed
Solution is added in the bromo- 4- chlorobutane of the good 1- of constant temperature, ultrasonic disperse 3h, is then transferred in 35 DEG C of water-bath and is reacted 5 days, then
Revolving removes solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to settle and separate in separatory funnel, removes
Supernatant liquid is to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, by lower layer's water phase at 60 DEG C
Revolving water removal is then placed into drying 5 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixture；N- methyl miaow
The bromo- 4- chlorobutane of azoles, acetonitrile, 1-, ethyl acetate, water mass ratio be 5:120:5:180:200；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 5:6:180:4:200:4；
(3) graphene oxide for obtaining step 2 is added in deionized water, and ultrasonic disperse 3h obtains graphene oxide water
Solution；Graphene oxide, deionized water quality ratio are 5:120；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), adds step 1
Liner, is transferred in reaction kettle tightens later by obtained ionic liquid mixture, dry 3h in anti-corrosion air dry oven, then
2h is stirred with glass bar, obtains hydrogel；Graphene oxide water solution, ionic liquid mixture mass ratio be 100:12；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred to after dialysing 6 days in bag filter
Filter, by material much be transferred in vacuum freeze drier, freeze 70h at -20 DEG C, obtain graphene aerogel electrode
Material.
Embodiment 3
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 14min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N- first
Base imidazoles is added in acetonitrile, stirs 24 minutes, obtains N- methylimidazole/acetonitrile mixed solution, and N- methylimidazole/acetonitrile is mixed
Solution is added in the bromo- 4- chlorobutane of the good 1- of constant temperature, ultrasonic disperse 2h, is then transferred in 35 DEG C of water-bath and is reacted 3 days, then
Revolving removes solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to settle and separate in separatory funnel, removes
Supernatant liquid is to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, by lower layer's water phase at 60 DEG C
Revolving water removal is then placed into drying 3 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixture；N- methyl miaow
The bromo- 4- chlorobutane of azoles, acetonitrile, 1-, ethyl acetate, water mass ratio be 2:60:2:90:130；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 2:4:140:2:175:2；
(3) graphene oxide for obtaining step 2 is added in deionized water, and ultrasonic disperse 2h obtains graphene oxide water
Solution；Graphene oxide, deionized water quality ratio are 3:100；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), adds step 1
Liner, is transferred in reaction kettle tightens later by obtained ionic liquid mixture, dry 2h in anti-corrosion air dry oven, then
1h is stirred with glass bar, obtains hydrogel；Graphene oxide water solution, ionic liquid mixture mass ratio be 88:8；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred to after dialysing 4 days in bag filter
Filter, by material much be transferred in vacuum freeze drier, freeze 50h at -20 DEG C, obtain graphene aerogel electrode
Material.
Embodiment 4
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 27min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N- first
Base imidazoles is added in acetonitrile, stirs 27 minutes, obtains N- methylimidazole/acetonitrile mixed solution, and N- methylimidazole/acetonitrile is mixed
Solution is added in the bromo- 4- chlorobutane of the good 1- of constant temperature, ultrasonic disperse 2h, is then transferred in 35 DEG C of water-bath and is reacted 4 days, then
Revolving removes solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to settle and separate in separatory funnel, removes
Supernatant liquid is to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, by lower layer's water phase at 60 DEG C
Revolving water removal is then placed into drying 4 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixture；N- methyl miaow
The bromo- 4- chlorobutane of azoles, acetonitrile, 1-, ethyl acetate, water mass ratio be 4:100:5:160:180；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 4:5:160:3:180:3；
(3) graphene oxide for obtaining step 2 is added in deionized water, and ultrasonic disperse 2h obtains graphene oxide water
Solution；Graphene oxide, deionized water quality ratio are 4:100；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), adds step 1
Liner, is transferred in reaction kettle tightens later by obtained ionic liquid mixture, dry 2h in anti-corrosion air dry oven, then
2h is stirred with glass bar, obtains hydrogel；Graphene oxide water solution, ionic liquid mixture mass ratio be 80:10；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred to after dialysing 5 days in bag filter
Filter, by material much be transferred in vacuum freeze drier, freeze 62h at -20 DEG C, obtain graphene aerogel electrode
Material.
Claims (5)
1. a kind of preparation method of graphene aerogel electrode material, which comprises the steps of:
(1) the bromo- 4- chlorobutane of 1- is set into constant temperature 10-20min in the cold-trap for be put into a round bottom flask 0 DEG C, later by N- methyl
Imidazoles is added in acetonitrile, stirs 20-30 minutes, obtains N- methylimidazole/acetonitrile mixed solution, N- methylimidazole/acetonitrile is mixed
It closes solution to be added in the bromo- 4- chlorobutane of the good 1- of constant temperature, ultrasonic disperse 1-3h is then transferred in 35 DEG C of water-bath and reacts 2-5
It, then revolving removes solvent, and ethyl acetate and water are added into the head product after revolving, is transferred to stand in separatory funnel and divide
From removing supernatant liquid to remove the bromo- 4- chlorobutane of the extra 1- in reactant and collect lower layer's water phase, lower layer's water phase existed
Water is evaporated off in 60 DEG C of backspins, is then placed into drying 2-5 days in 60 DEG C of vacuum oven, finally obtains ionic liquid mixture；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in condition of ice bath
Uniform magnetic agitation down；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic force stirs
1-3h is mixed, it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；Again into mixed solution
Addition temperature is 70 DEG C of deionized waters, and it is molten to obtain bright orange color contamination liquid after 30% hydrogen peroxide to be eventually adding mass fraction concentration
Liquid obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(3) graphene oxide for obtaining step 2 is added in deionized water, and it is water-soluble to obtain graphene oxide by ultrasonic disperse 1-3h
Liquid；
(4) graphene oxide water solution for obtaining step 3 is added in the liner of polytetrafluoroethylene (PTFE), is added step 1 and is obtained
Ionic liquid mixture, liner is transferred in reaction kettle tightens later, dry 1-3h, is then used in anti-corrosion air dry oven
Glass bar stirs 1-2h, obtains hydrogel；
(5) hydrogel for obtaining step 4 is filtered, and is cleaned with deionized water, is transferred to after dialysing 3-6 days in bag filter and is taken out
Filter, by material much be transferred in vacuum freeze drier, freeze 45-70h at -20 DEG C, obtain graphene aerogel electricity
Pole material.
2. a kind of preparation method of graphene aerogel electrode material according to claim 1, which is characterized in that step 1
In, the bromo- 4- chlorobutane of N- methylimidazole, acetonitrile, 1-, ethyl acetate, water mass ratio be 1-5:30-120:1-5:80-180:
90-200。
3. a kind of preparation method of graphene aerogel electrode material according to claim 1, which is characterized in that step 2
In, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, the hydrogen peroxide that mass fraction concentration is 30%
Mass ratio be 1-5:3-6:100-180:1-4:150-200:1-4.
4. a kind of preparation method of graphene aerogel electrode material according to claim 1, which is characterized in that step 3
In, graphene oxide, deionized water quality ratio are 2-5:80-120.
5. a kind of preparation method of graphene aerogel electrode material according to claim 1, which is characterized in that step 4
In, graphene oxide water solution, ionic liquid mixture mass ratio be 80-100:6-12.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111086985A (en) * | 2019-12-31 | 2020-05-01 | 江西宏柏新材料股份有限公司 | Preparation method of graphene carbon nanotube composite aerogel electrode material |
| CN111326818A (en) * | 2020-03-07 | 2020-06-23 | 杨富强 | Treatment method of lithium battery production waste |
-
2019
- 2019-04-03 CN CN201910265864.9A patent/CN109824037A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111086985A (en) * | 2019-12-31 | 2020-05-01 | 江西宏柏新材料股份有限公司 | Preparation method of graphene carbon nanotube composite aerogel electrode material |
| CN111086985B (en) * | 2019-12-31 | 2021-11-02 | 江西宏柏新材料股份有限公司 | Preparation method of graphene carbon nanotube composite aerogel electrode material |
| CN111326818A (en) * | 2020-03-07 | 2020-06-23 | 杨富强 | Treatment method of lithium battery production waste |
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Application publication date: 20190531 |