CN109179392A - A kind of technique of improved chemical method production graphene - Google Patents
A kind of technique of improved chemical method production graphene Download PDFInfo
- Publication number
- CN109179392A CN109179392A CN201811029228.8A CN201811029228A CN109179392A CN 109179392 A CN109179392 A CN 109179392A CN 201811029228 A CN201811029228 A CN 201811029228A CN 109179392 A CN109179392 A CN 109179392A
- Authority
- CN
- China
- Prior art keywords
- temperature
- reaction kettle
- added
- graphene
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses a kind of techniques of improved chemical method production graphene, include the following steps: step 1, raw material proportioning；Step 2, low-temperature oxidation；Step 3, medium temperature reaction；Step 4, washing and separation；Step 5, it is dry；Step 6, redox；In the step one, raw material selects the 96%-98% concentrated sulfuric acid, potassium permanganate, natural flake graphite, sodium nitrate, 30% hydrogen peroxide, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol, in the step two, select the graininess natural flake graphite of 60g, 30g sodium nitrate is added into 10L double-layer glass reaction kettle, 0 DEG C is cooled to reaction kettle, the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle again, it carries out that 30min is sufficiently stirred in a kettle, cooled down by cryostat to reaction kettle, the temperature of reaction system is kept to be not higher than 4 DEG C, then 180g potassium permanganate is added in reaction kettle, temperature in reaction kettle is kept to be not higher than 8 DEG C simultaneously.
Description
Technical field
The present invention relates to graphene production technical field, specially a kind of technique of improved chemical method production graphene.
Background technique
Graphene be one kind by carbon atom with sp2Hybridized orbit forms the Two-dimensional Carbon nanometer material that hexangle type is in honeycomb lattice
Material, graphene have excellent optics, electricity, mechanical characteristic, pass in materialogy, micro-nano technology, the energy, biomedicine and drug
Pass etc. is with important application prospects, it is considered to be a kind of future revolutionary material.
In the prior art, the quality of graphene can be improved without a kind of manufacture craft, cannot effectively save equipment at
Originally and noise pollution, and high process cost are reduced, therefore designing the new graphene production technology of one kind is prior art needs
The technical issues of solution.
Summary of the invention
The purpose of the present invention is to provide a kind of techniques of improved chemical method production graphene, to solve above-mentioned background skill
The problem of being proposed in art.
In order to solve the above technical problem, the present invention provides following technical solutions: a kind of improved chemical method production graphite
The technique of alkene, includes the following steps:
1) raw material proportioning: the raw material selection 96%-98% concentrated sulfuric acid, potassium permanganate, natural flake graphite, sodium nitrate, 30%
Hydrogen peroxide, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol；
2) low-temperature oxidation: selecting the graininess natural flake graphite of 60g, and 30g sodium nitrate, which is added to 10L double glazing, to react
In kettle, it is cooled to 0 DEG C to reaction kettle, then the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle, is filled in a kettle
Divide stirring 30min, cooled down by cryostat to reaction kettle, keeps the temperature of reaction system not higher than 4 DEG C, then by 180g high
Potassium manganate is added in reaction kettle, and carries out that 60min is sufficiently stirred, while temperature in reaction kettle being kept to be not higher than 8 DEG C；
3) medium temperature is reacted: withdrawing cryostat, the temperature in reaction kettle is heated to 35 DEG C using high temperature constant temperature circulating pump, is used
The solution in reaction kettle is sufficiently stirred in turbine agitator, persistently stirs 3h and obtains brown suspension, is slow added into
90g potassium permanganate reacts 12h, keeps the temperature in reaction kettle to be not higher than 40 DEG C, persistently carries out medium temperature reaction；
4) it washs and separates: withdrawing high temperature constant temperature circulating pump, using sub-cooled circulating pump by the temperature control in reaction kettle
It makes at 5 DEG C hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and companion
With there is a bulk gas generation, diluted suspension pass through at this temperature turbine agitator to the suspension inside reaction kettle into
Row stirs, and after 60min, 30% hydrogen peroxide of 50mL is slowly added into suspension, and be slowly stirred 60min in room temperature, obtained
To glassy yellow graphite oxide dispersion, there is lamination after dispersion liquid to be stood to 2h at room temperature, after removing supernatant, is added
A certain amount of deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then
Disperse filter cake in 5000mL deionized water, by filtering, and washed using a large amount of deionized waters, until in solution without chlorine from
Son, and close neutrality；
5) dry: above-mentioned generated solid product to be placed in 60 DEG C of vacuum oven, by constant temperature to solid
Product is dried, and is shaken while dry, after drying for 24 hours, obtains graphite oxide after being ground up, sieved, is recycled with sub-cooled
Pump at a certain temperature liquefies high-purity ammon in a sealed container, and the graphite oxide that a certain amount of drying is added is vortexed with vacuum to be removed
Machine removes 1h, and a certain amount of metal clang is put into liquid nitrogen, and solution becomes blue, continues to keep vacuum vortex stripping machine work
30min solution blackening, stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion, filtering are added into obtained black solid
It is washed with deionized to neutrality, 60 DEG C of vacuum dry 12h obtain the graphene oxide of black；
6) redox: being heat-treated under atmosphere protection, removes graphene oxide functional group, obtains Graphene powder
Can same decentralized medium be added according to a certain percentage in body, dry graphene oxide powder, prepare the NMP type dispersion of various concentration
Liquid, aqueous liquid dispersion etc., while the graphene powder after thermal reduction can prepare different graphene slurries in the method and divide
Dispersion liquid；
According to the above technical scheme, during the step 5) prepares graphene oxide, removing is vortexed with vacuum and is replaced
Previous intrinsic ultrasonic disperse.
According to the above technical scheme, the drying of graphene oxide is carried out in the step 5) using the drying process of vibration.
According to the above technical scheme, in the step 4) after washed, by silver nitrate solution monitor Chlorine in Solution from
Son.
According to the above technical scheme, the filter screen mesh number that filtering uses in the step 4) is 100 mesh.
Compared with prior art, the beneficial effects obtained by the present invention are as follows being: raw material selects the 96%-98% concentrated sulfuric acid, Gao Meng
Sour potassium, natural flake graphite, sodium nitrate, 30% hydrogen peroxide, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol are selected
The graininess natural flake graphite of 60g, 30g sodium nitrate are added into 10L double-layer glass reaction kettle, are cooled to 0 DEG C to reaction kettle,
The 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle again, carries out that 30min is sufficiently stirred in a kettle, by cryostat to anti-
It answers kettle to cool down, keeps the temperature of reaction system not higher than 4 DEG C, then 180g potassium permanganate is added in reaction kettle, goes forward side by side
60min is sufficiently stirred in row, while temperature in reaction kettle being kept to be not higher than 8 DEG C, withdraws cryostat, will be anti-using high temperature constant temperature circulating pump
It answers the temperature in kettle to be heated to 35 DEG C, the solution in reaction kettle is sufficiently stirred using turbine agitator, it is lasting to stir
3h obtains brown suspension, is slow added into 90g potassium permanganate reaction 12h, keeps the temperature in reaction kettle to be not higher than 40 DEG C, hold
It is continuous to carry out medium temperature reaction, high temperature constant temperature circulating pump is withdrawn, is controlled the temperature in reaction kettle at 5 DEG C using sub-cooled circulating pump
Hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and with a large amount of
Gas generates, and diluted suspension passes through turbine agitator at this temperature and is stirred to the suspension inside reaction kettle,
After 60min, it is slowly added to 30% hydrogen peroxide of 50mL into suspension, and be slowly stirred 60min in room temperature, obtains glassy yellow
There is lamination after dispersion liquid to be stood to 2h at room temperature in graphite oxide dispersion, after removing supernatant, is added a certain amount of
Deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then by filter cake point
It dissipates in 5000mL deionized water, by filtering, and is washed using a large amount of deionized waters, until without chloride ion in solution, and connect
Above-mentioned generated solid product is placed in 60 DEG C of vacuum oven by weakly acidic pH, is carried out by constant temperature to solid product
It is dry, it is shaken while dry, after drying for 24 hours, graphite oxide is obtained after being ground up, sieved, with sub-cooled circulating pump certain
At a temperature of high-purity ammon is liquefied in a sealed container, the graphite oxide of a certain amount of drying vacuum is added and is vortexed stripping machine removing
A certain amount of metal clang is put into liquid nitrogen by 1h, and solution becomes blue, continues to keep vacuum vortex stripping machine work 30min molten
Liquid blackening, stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion is added into obtained black solid, deionization is used in filtering
Water washing obtains the graphene oxide of black, is heat-treated under atmosphere protection to neutrality, 60 DEG C of vacuum dry 12h, removes
Graphene oxide functional group, obtains graphene powder, and dry graphene oxide powder can be added with dispersion according to a certain percentage
Medium prepares NMP type dispersion liquid, aqueous liquid dispersion of various concentration etc., while the graphene powder after thermal reduction is according to the party
Method can prepare different graphene slurry and dispersion liquid, the graphene produced in the process flow, after Strong oxdiative, without strong reduction
Agent reduction, reduces the number of cleaning, separation and concentration, with the removing of vacuum vortex instead of previous ultrasonic disperse, saves
Equipment cost and reduction noise pollution, this method controllability is strong, and process costs are low, is to be suitble to graphene and its interphase product big
One of method of large-scale production.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is process flow chart of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of technique of improved chemical method production graphene, packet
Include following steps:
Embodiment 1
1) raw material proportioning: raw material selects 98% concentrated sulfuric acid, potassium permanganate, natural flake graphite, sodium nitrate, 30% dioxygen
Water, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol；
2) low-temperature oxidation: selecting the graininess natural flake graphite of 60g, and 30g sodium nitrate, which is added to 10L double glazing, to react
In kettle, it is cooled to 0 DEG C to reaction kettle, then the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle, is filled in a kettle
Divide stirring 30min, cooled down by cryostat to reaction kettle, keeps the temperature of reaction system not higher than 4 DEG C, then by 180g high
Potassium manganate is added in reaction kettle, and carries out that 60min is sufficiently stirred, while temperature in reaction kettle being kept to be not higher than 8 DEG C；
3) medium temperature is reacted: withdrawing cryostat, the temperature in reaction kettle is heated to 35 DEG C using high temperature constant temperature circulating pump, is used
The solution in reaction kettle is sufficiently stirred in turbine agitator, persistently stirs 3h and obtains brown suspension, is slow added into
90g potassium permanganate reacts 12h, keeps the temperature in reaction kettle to be not higher than 40 DEG C, persistently carries out medium temperature reaction；
4) it washs and separates: withdrawing high temperature constant temperature circulating pump, using sub-cooled circulating pump by the temperature control in reaction kettle
It makes at 5 DEG C hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and companion
With there is a bulk gas generation, diluted suspension pass through at this temperature turbine agitator to the suspension inside reaction kettle into
Row stirs, and after 60min, 30% hydrogen peroxide of 50mL is slowly added into suspension, and be slowly stirred 60min in room temperature, obtained
To glassy yellow graphite oxide dispersion, there is lamination after dispersion liquid to be stood to 2h at room temperature, after removing supernatant, is added
A certain amount of deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then
Disperse filter cake in 5000mL deionized water, by filtering, and washed using a large amount of deionized waters, until in solution without chlorine from
Son, and close neutrality；
5) dry: above-mentioned generated solid product to be placed in 60 DEG C of vacuum oven, by constant temperature to solid
Product is dried, and is shaken while dry, after drying for 24 hours, obtains graphite oxide after being ground up, sieved, is recycled with sub-cooled
Pump at a certain temperature liquefies high-purity ammon in a sealed container, and the graphite oxide that a certain amount of drying is added is vortexed with vacuum to be removed
Machine removes 1h, and a certain amount of metal clang is put into liquid nitrogen, and solution becomes blue, continues to keep vacuum vortex stripping machine work
30min solution blackening, stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion, filtering are added into obtained black solid
It is washed with deionized to neutrality, 60 DEG C of vacuum dry 12h obtain the graphene oxide of black；
6) redox: being heat-treated under atmosphere protection, removes graphene oxide functional group, obtains Graphene powder
Can same decentralized medium be added according to a certain percentage in body, dry graphene oxide powder, prepare the NMP type dispersion of various concentration
Liquid, aqueous liquid dispersion etc., while the graphene powder after thermal reduction can prepare different graphene slurries in the method and divide
Dispersion liquid；
Embodiment 2
1) raw material proportioning: raw material selects 96% concentrated sulfuric acid, potassium permanganate, natural flake graphite, sodium nitrate, 30% dioxygen
Water, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol；
2) low-temperature oxidation: selecting the graininess natural flake graphite of 60g, and 30g sodium nitrate, which is added to 10L double glazing, to react
In kettle, it is cooled to 0 DEG C to reaction kettle, then the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle, is filled in a kettle
Divide stirring 30min, cooled down by cryostat to reaction kettle, keeps the temperature of reaction system not higher than 4 DEG C, then by 180g high
Potassium manganate is added in reaction kettle, and carries out that 60min is sufficiently stirred, while temperature in reaction kettle being kept to be not higher than 8 DEG C；
3) medium temperature is reacted: withdrawing cryostat, the temperature in reaction kettle is heated to 35 DEG C using high temperature constant temperature circulating pump, is used
The solution in reaction kettle is sufficiently stirred in turbine agitator, persistently stirs 3h and obtains brown suspension, is slow added into
90g potassium permanganate reacts 12h, keeps the temperature in reaction kettle to be not higher than 40 DEG C, persistently carries out medium temperature reaction；
4) it washs and separates: withdrawing high temperature constant temperature circulating pump, using sub-cooled circulating pump by the temperature control in reaction kettle
It makes at 5 DEG C hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and companion
With there is a bulk gas generation, diluted suspension pass through at this temperature turbine agitator to the suspension inside reaction kettle into
Row stirs, and after 60min, 30% hydrogen peroxide of 50mL is slowly added into suspension, and be slowly stirred 60min in room temperature, obtained
To glassy yellow graphite oxide dispersion, there is lamination after dispersion liquid to be stood to 2h at room temperature, after removing supernatant, is added
A certain amount of deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then
Disperse filter cake in 5000mL deionized water, by filtering, and washed using a large amount of deionized waters, until in solution without chlorine from
Son, and close neutrality；
5) dry: above-mentioned generated solid product to be placed in 60 DEG C of vacuum oven, by constant temperature to solid
Product is dried, and is shaken while dry, after drying for 24 hours, obtains graphite oxide after being ground up, sieved, is recycled with sub-cooled
Pump at a certain temperature liquefies high-purity ammon in a sealed container, and the graphite oxide that a certain amount of drying is added is vortexed with vacuum to be removed
Machine removes 1h, and a certain amount of metal clang is put into liquid nitrogen, and solution becomes blue, continues to keep vacuum vortex stripping machine work
30min solution blackening, stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion, filtering are added into obtained black solid
It is washed with deionized to neutrality, 60 DEG C of vacuum dry 12h obtain the graphene oxide of black；
6) redox: being heat-treated under atmosphere protection, removes graphene oxide functional group, obtains Graphene powder
Can same decentralized medium be added according to a certain percentage in body, dry graphene oxide powder, prepare the NMP type dispersion of various concentration
Liquid, aqueous liquid dispersion etc., while the graphene powder after thermal reduction can prepare different graphene slurries in the method and divide
Dispersion liquid；
According to the above technical scheme, during the step 5) prepares graphene oxide, removing is vortexed with vacuum and is replaced
Previous intrinsic ultrasonic disperse.
According to the above technical scheme, the drying of graphene oxide is carried out in the step 5) using the drying process of vibration.
According to the above technical scheme, in the step 4) after washed, by silver nitrate solution monitor Chlorine in Solution from
Son.
According to the above technical scheme, the filter screen mesh number that filtering uses in the step 4) is 100 mesh.
Based on above-mentioned, it is an advantage of the current invention that the graphene production technology, raw material selects the 96%-98% concentrated sulfuric acid, high
Potassium manganate, natural flake graphite, sodium nitrate, 30% hydrogen peroxide, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol, choosing
With the graininess natural flake graphite of 60g, 30g sodium nitrate is added into 10L double-layer glass reaction kettle, is cooled to 0 to reaction kettle
DEG C, then the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle, it carries out that 30min is sufficiently stirred in a kettle, passes through cryostat
Cool down to reaction kettle, keep the temperature of reaction system not higher than 4 DEG C, then 180g potassium permanganate is added in reaction kettle,
And carry out that 60min is sufficiently stirred, while temperature in reaction kettle being kept to be not higher than 8 DEG C, cryostat is withdrawn, high temperature constant temperature circulating pump is used
Temperature in reaction kettle is heated to 35 DEG C, the solution in reaction kettle is sufficiently stirred using turbine agitator, is continued
Stirring 3h obtains brown suspension, is slow added into 90g potassium permanganate reaction 12h, the temperature in reaction kettle is kept to be not higher than 40
DEG C, medium temperature reaction is persistently carried out, high temperature constant temperature circulating pump is withdrawn, is controlled the temperature in reaction kettle using sub-cooled circulating pump
At 5 DEG C hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and adjoint
There is bulk gas generation, diluted suspension passes through turbine agitator at this temperature carries out the suspension inside reaction kettle
It stirs, after 60min, 30% hydrogen peroxide of 50mL is slowly added into suspension, and be slowly stirred 60min in room temperature, obtained
There is lamination after dispersion liquid to be stood to 2h at room temperature in glassy yellow graphite oxide dispersion, after removing supernatant, is added one
Quantitative deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then will
Filter cake is scattered in 5000mL deionized water, by filtering, and is washed using a large amount of deionized waters, until in solution without chlorine from
Son, and close to neutrality, above-mentioned generated solid product is placed in 60 DEG C of vacuum oven, solid is produced by constant temperature
Object is dried, and is shaken while dry, after drying for 24 hours, graphite oxide is obtained after being ground up, sieved, with sub-cooled circulating pump
High-purity ammon is liquefied in a sealed container at a certain temperature, the graphite oxide that a certain amount of drying is added is vortexed stripping machine with vacuum
1h is removed, a certain amount of metal clang is put into liquid nitrogen, solution becomes blue, continues to keep vacuum vortex stripping machine work
30min solution blackening, stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion, filtering are added into obtained black solid
It is washed with deionized to neutrality, 60 DEG C of vacuum dry 12h obtain the graphene oxide of black, and heat is carried out under atmosphere protection
Reduction, remove graphene oxide functional group, obtain graphene powder, dry graphene oxide powder can according to a certain percentage,
Same decentralized medium is added, prepares NMP type dispersion liquid, aqueous liquid dispersion of various concentration etc., while the Graphene powder after thermal reduction
Body can prepare different graphene slurry and dispersion liquid in the method, the graphene produced in the process flow, after Strong oxdiative,
It is restored without strong reductant, reduces the number of cleaning, separation and concentration, with vacuum vortex removing instead of previous ultrasound point
It dissipates, saved equipment cost and reduces noise pollution, this method controllability is strong, and process costs are low, is to be suitble to graphene and wherein
Between one of the method that is mass produced of phase product.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (5)
1. a kind of technique of improved chemical method production graphene, includes the following steps: step 1, raw material proportioning；Step 2 is low
Temperature oxidation；Step 3, medium temperature reaction；Step 4, washing and separation；Step 5, it is dry；Step 6, redox；Its feature exists
In:
In the step one, the raw material selection 96%-98% concentrated sulfuric acid, potassium permanganate, natural flake graphite, sodium nitrate,
30% hydrogen peroxide, 10% dilute hydrochloric acid, deionized water, liquefied ammonia, metal clang, ethyl alcohol；
In the step two, the graininess natural flake graphite of 60g is selected, 30g sodium nitrate is added anti-to 10L double glazing
It answers in kettle, is cooled to 0 DEG C to reaction kettle, then the 2500mL98% concentrated sulfuric acid is slowly added in reaction kettle, carries out in a kettle
30min is sufficiently stirred, is cooled down by cryostat to reaction kettle, keeps the temperature of reaction system not higher than 4 DEG C, then by 180g
Potassium permanganate is added in reaction kettle, and carries out that 60min is sufficiently stirred, while temperature in reaction kettle being kept to be not higher than 8 DEG C；
In the step three, cryostat is withdrawn, the temperature in reaction kettle is heated to 35 DEG C using high temperature constant temperature circulating pump, is made
The solution in reaction kettle is sufficiently stirred with turbine agitator, 3h is persistently stirred and obtains brown suspension, then slowly add
Enter 90g potassium permanganate reaction 12h, keeps the temperature in reaction kettle to be not higher than 40 DEG C, persistently carry out medium temperature reaction；
In the step four, high temperature constant temperature circulating pump is withdrawn, using sub-cooled circulating pump by the temperature control in reaction kettle
It makes at 5 DEG C hereinafter, 7L deionized water is slowly added dropwise in brown suspension, temperature of reaction kettle increases suddenly at this time, and companion
With there is a bulk gas generation, diluted suspension pass through at this temperature turbine agitator to the suspension inside reaction kettle into
Row stirs, and after 60min, 30% hydrogen peroxide of 50mL is slowly added into suspension, and be slowly stirred 60min in room temperature, obtained
To glassy yellow graphite oxide dispersion, there is lamination after dispersion liquid to be stood to 2h at room temperature, after removing supernatant, is added
A certain amount of deionized water, by the way that yellowish-brown filter cake is obtained by filtration, after being washed with 5000mL10% dilute hydrochloric acid to filter cake, then
Disperse filter cake in 5000mL deionized water, by filtering, and washed using a large amount of deionized waters, until in solution without chlorine from
Son, and close neutrality；
In the step five, above-mentioned generated solid product is placed in 60 DEG C of vacuum oven, constant temperature is passed through
Solid product is dried, is shaken while dry, after drying for 24 hours, graphite oxide is obtained after being ground up, sieved, uses low temperature cold
But circulating pump at a certain temperature liquefies high-purity ammon in a sealed container, and the graphite oxide vacuum whirlpool of a certain amount of drying is added
It flows stripping machine and removes 1h, a certain amount of metal clang is put into liquid nitrogen, solution becomes blue, continues to keep vacuum vortex stripping machine
Work the blackening of 30min solution, and stopping cooling nature heating makes liquefied ammonia volatilize, and ethyl alcohol dispersion is added into obtained black solid,
Filtering is washed with deionized to neutrality, and 60 DEG C of vacuum dry 12h obtain the graphene oxide of black；
It in the step six, is heat-treated under atmosphere protection, removes graphene oxide functional group, obtain Graphene powder
Can same decentralized medium be added according to a certain percentage in body, dry graphene oxide powder, prepare the NMP type dispersion of various concentration
Liquid, aqueous liquid dispersion etc., while the graphene powder after thermal reduction can prepare different graphene slurries in the method and divide
Dispersion liquid.
2. a kind of technique of improved chemical method production graphene according to claim 1, it is characterised in that: described
In step 5, during preparing graphene oxide, removing is vortexed with vacuum and replaces previous intrinsic ultrasonic disperse.
3. a kind of technique of improved chemical method production graphene according to claim 1, it is characterised in that: described
In step 5, the drying of graphene oxide is carried out using the drying process of vibration.
4. a kind of technique of improved chemical method production graphene according to claim 1, it is characterised in that: described
In step 4, after washed, Chlorine in Solution ion is monitored by silver nitrate solution.
5. a kind of technique of improved chemical method production graphene according to claim 1, it is characterised in that: described
In step 4, filtering the filter screen mesh number used is 100 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811029228.8A CN109179392A (en) | 2018-09-05 | 2018-09-05 | A kind of technique of improved chemical method production graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811029228.8A CN109179392A (en) | 2018-09-05 | 2018-09-05 | A kind of technique of improved chemical method production graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109179392A true CN109179392A (en) | 2019-01-11 |
Family
ID=64914688
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811029228.8A Pending CN109179392A (en) | 2018-09-05 | 2018-09-05 | A kind of technique of improved chemical method production graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109179392A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111724954A (en) * | 2020-02-07 | 2020-09-29 | 宴晶科技(北京)有限公司 | Graphene oxide magnetic bead, antibody-coupled graphene oxide magnetic bead, preparation methods of graphene oxide magnetic bead and antibody-coupled graphene oxide magnetic bead and application of graphene oxide magnetic bead in cell sorting |
| CN112479196A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide and preparation method thereof |
| CN112473641A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide COD adsorption fixing agent, preparation method and application thereof |
| CN112473642A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide modified attapulgite, and preparation method and application thereof |
| CN113194556A (en) * | 2021-04-20 | 2021-07-30 | 广东温道百镒健康科技有限公司 | Graphene radiation heating film and preparation method thereof |
| CN113371702A (en) * | 2021-05-11 | 2021-09-10 | 施亮 | Preparation process of composite graphene back gel for rubber filler |
| CN117601456A (en) * | 2024-01-22 | 2024-02-27 | 四川省宜宾普什建材有限责任公司 | Processing technology of large-caliber electric melting type plastic pipe fitting |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602504A (en) * | 2009-07-16 | 2009-12-16 | 上海交通大学 | Graphene preparation method based on xitix |
| CN102320598A (en) * | 2011-07-26 | 2012-01-18 | 河南大学 | Preparation method of graphene |
| CN103382026A (en) * | 2012-05-02 | 2013-11-06 | 中国科学院上海硅酸盐研究所 | Low-cost mass preparation method of high-quality graphene |
| CN204034664U (en) * | 2014-08-19 | 2014-12-24 | 青岛金墨自动化科技有限公司 | A kind of graphene oxide vacuum eddy current stripping off device |
| CN105883790A (en) * | 2016-05-26 | 2016-08-24 | 同济大学 | Low-temperature-stripping modified graphene and preparation method thereof |
| CN107934946A (en) * | 2017-12-13 | 2018-04-20 | 北京大学 | Graphene powder and preparation method thereof |
| CN108314021A (en) * | 2017-01-16 | 2018-07-24 | 山东恒华新材料有限公司 | The batch production method of high-quality graphene |
-
2018
- 2018-09-05 CN CN201811029228.8A patent/CN109179392A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602504A (en) * | 2009-07-16 | 2009-12-16 | 上海交通大学 | Graphene preparation method based on xitix |
| CN102320598A (en) * | 2011-07-26 | 2012-01-18 | 河南大学 | Preparation method of graphene |
| CN103382026A (en) * | 2012-05-02 | 2013-11-06 | 中国科学院上海硅酸盐研究所 | Low-cost mass preparation method of high-quality graphene |
| CN204034664U (en) * | 2014-08-19 | 2014-12-24 | 青岛金墨自动化科技有限公司 | A kind of graphene oxide vacuum eddy current stripping off device |
| CN105883790A (en) * | 2016-05-26 | 2016-08-24 | 同济大学 | Low-temperature-stripping modified graphene and preparation method thereof |
| CN108314021A (en) * | 2017-01-16 | 2018-07-24 | 山东恒华新材料有限公司 | The batch production method of high-quality graphene |
| CN107934946A (en) * | 2017-12-13 | 2018-04-20 | 北京大学 | Graphene powder and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 谢炜 等: "《微晶石墨深加工及应用》", 31 August 2016, 湖南大学出版社 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111724954A (en) * | 2020-02-07 | 2020-09-29 | 宴晶科技(北京)有限公司 | Graphene oxide magnetic bead, antibody-coupled graphene oxide magnetic bead, preparation methods of graphene oxide magnetic bead and antibody-coupled graphene oxide magnetic bead and application of graphene oxide magnetic bead in cell sorting |
| CN111724954B (en) * | 2020-02-07 | 2023-01-20 | 宴晶科技(北京)有限公司 | Graphene oxide magnetic bead, antibody-coupled graphene oxide magnetic bead and application of graphene oxide magnetic bead in cell sorting |
| CN112479196A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide and preparation method thereof |
| CN112473641A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide COD adsorption fixing agent, preparation method and application thereof |
| CN112473642A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Graphene oxide modified attapulgite, and preparation method and application thereof |
| CN112473641B (en) * | 2020-06-11 | 2023-09-01 | 中科远方(北京)科技有限公司 | Graphene oxide COD adsorption fixing agent, preparation method and application thereof |
| CN112473642B (en) * | 2020-06-11 | 2023-10-03 | 中科远方(北京)科技有限公司 | Graphene oxide modified attapulgite, preparation method and application thereof |
| CN113194556A (en) * | 2021-04-20 | 2021-07-30 | 广东温道百镒健康科技有限公司 | Graphene radiation heating film and preparation method thereof |
| CN113371702A (en) * | 2021-05-11 | 2021-09-10 | 施亮 | Preparation process of composite graphene back gel for rubber filler |
| CN117601456A (en) * | 2024-01-22 | 2024-02-27 | 四川省宜宾普什建材有限责任公司 | Processing technology of large-caliber electric melting type plastic pipe fitting |
| CN117601456B (en) * | 2024-01-22 | 2024-03-26 | 四川省宜宾普什建材有限责任公司 | Processing technology of large-caliber electric melting type plastic pipe fitting |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109179392A (en) | A kind of technique of improved chemical method production graphene | |
| CN106684485B (en) | Method for recycling waste lithium iron phosphate anode material by acid leaching method | |
| CN104787759B (en) | A kind of impurity-removing method in graphene preparation process | |
| CN105664902A (en) | Trivalent titanium ion self-doped titanium dioxide nanosheet catalyst | |
| CN105347339A (en) | Preparation method of expanded graphite | |
| CN111883869A (en) | Method for recycling lithium by using graphite cathode of waste power battery and preparing graphene by using lithium | |
| CN104209119A (en) | Mn3O4-MnO2 nano rod composite oxide as well as preparation method and application of Mn3O4-MnO2 nano rod composite oxide | |
| CN106672975A (en) | Preparation method of low-cost nano-porous silica powder | |
| CN110540200A (en) | method for etching diamond (100) surface in high orientation | |
| CN110898794A (en) | Preparation method of lithium ion sieve | |
| CN109665525A (en) | A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon | |
| CN114477320B (en) | Preparation method of PEM water electrolysis oxygen desorption catalyst iridium oxide | |
| CN110492076B (en) | Preparation method of two-dimensional porous hexagonal metal oxide nanosheet composite material and application of composite material in potassium ion battery | |
| CN107352519B (en) | A kind of C3N4The preparation method of nano wire | |
| CN104495835A (en) | Method for preparing multilayer graphene through step-by-step oxidization and step-by-step dissociation | |
| CN106848309B (en) | The composite mixed iron manganese phosphate material and preparation method thereof of metal/carbon nanotube | |
| CN105923657A (en) | Preparation method of monoclinic tungsten trioxide | |
| CN111250146A (en) | Preparation method of oxygen-enriched BiOI-BiOBr/SBA-16 composite photocatalytic material | |
| CN104525114A (en) | Method for treating isopropanol-containing wastewater by using modified activated carbon | |
| CN104051731B (en) | A kind of method that LiFePO4 is prepared in pollution-free zero-emission | |
| CN109616668A (en) | The micro- preparation method for expanding layer natural graphite of lithium cell negative pole material manganese oxide-small size | |
| CN105013516A (en) | Supported multistage structure silver-silver halide-titanium dioxide composite light visible catalytic material and preparation method therefor | |
| CN105271443A (en) | Method for preparing flaky nano CoO or Co3O4 through assistant microwave heating | |
| CN109420491A (en) | A kind of preparation method of carbon nanotube-manganese dioxide composite catalyst | |
| CN105271198B (en) | The preparation of graphene oxide and the preparation of graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190111 |
|
| WD01 | Invention patent application deemed withdrawn after publication |