CN108314023A - A method of preparing graphene using special graphite powder - Google Patents
A method of preparing graphene using special graphite powder Download PDFInfo
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- CN108314023A CN108314023A CN201810271845.2A CN201810271845A CN108314023A CN 108314023 A CN108314023 A CN 108314023A CN 201810271845 A CN201810271845 A CN 201810271845A CN 108314023 A CN108314023 A CN 108314023A
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Abstract
The invention discloses a kind of methods preparing graphene using special graphite powder, and steps are as follows for specific method：Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50 100 mesh, step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate and phosphorus pentoxide is added in 60 70 DEG C of the concentrated sulfuric acid, is stirred evenly, 8 hours cooling or more, is then filtered and washed work, is washed to neutrality, is finally dried, and mixing sample, step 3 are obtained：The mixing sample obtained in step 2 is added in 05 DEG C of the concentrated sulfuric acid, step 4：Potassium permanganate is added, the temperature of system is maintained at 10 20 DEG C.The present invention prepares graphene using special graphite powder, and there is reliable stability, adsorptivity and electrical and thermal conductivity, the no heat treatment process in whole preparation process to reduce energy consumption, entire preparation process is simple, preparation method is economical and practical, and production cost is low, can be mass-produced.
Description
Technical field
The present invention relates to graphene preparation method field, more particularly to a kind of side preparing graphene using special graphite powder
Method.
Background technology
Graphene be it is a kind of it is two-dimensional accumulated by hexatomic ring made of carbon material.Graphene has good electric conductivity, machine
Tool intensity, optical property, absorption property, heat conductivility and very high transparency, graphene is most light, strong in known materials at present
Maximum material is spent, to which graphene is applied to the industries such as the energy, machinery, electronics.
Glue is used for the first time with Kostya Novoselov from the Andre Geim professors of Univ Manchester UK in 2004
Band stripping obtains graphene（Graphene,GN）Think, the research of graphene is just paid attention to and studied by vast scientific researcher.
Traditional graphene preparation method has：Micromechanics stripping method, ultrahigh vacuum graphene epitaxial growth method, chemical gaseous phase
Sedimentation, solution stripping method etc., but there is also many disadvantages for these methods, preparation process is complicated, and production cost is higher, and
It is unfavorable for mass producing.
Therefore, invent that a kind of using special graphite powder to prepare the method for graphene necessary to solve the above problems.
Invention content
The purpose of the present invention is to provide a kind of methods preparing graphene using special graphite powder, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the present invention provides the following technical solutions：It is a kind of to prepare graphene using special graphite powder
Method, steps are as follows for specific method：
Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50-100 mesh；
Step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate
It is added in 60-70 DEG C of the concentrated sulfuric acid, stirs evenly with phosphorus pentoxide, it is 8 hours cooling or more, it is then filtered and is washed
Work is washed to neutrality, is finally dried, and mixing sample is obtained；
Step 3：The mixing sample obtained in step 2 is added in 0-5 DEG C of the concentrated sulfuric acid；
Step 4：Potassium permanganate is added, the temperature of system is maintained at 10-20 DEG C；
Step 5：Then it is kept for 5 hours in 20-35 DEG C of oil bath, is slowly added to deionized water；
Step 6：After 30min, the deionized water containing hydrogen peroxide is added, until the color of solution becomes glassy yellow, is taken out while hot
Filter；
Step 7：It is washed, is filtered with a concentration of 10% hydrochloric acid again；
Step 8：Last 40-60 DEG C of vacuum drying obtains graphene oxide；
Step 9：The graphene oxide obtained in step 8 is added in sodium hydroxide, in one ultrasound 30- of vacuum condition
120min is washed 5-7 times, gained is deposited in then with the rotating speed magnetic agitation 24-72h of 250-300r/min with absolute ethyl alcohol
Dry 24-48h, obtains graphene in the vacuum drying chamber that temperature is 50-80 DEG C.
Preferably, concentrated sulfuric acid addition is 200-250ml in the step 3.
Preferably, deionized water addition is 900-1000ml in the step 5.
Preferably, deionized water addition is 2.5-3.0L in the step 6, is wherein contained in 50-100ml deionized waters
There is the hydrogen peroxide of 30% concentration.
Preferably, hydrochloric acid addition is 5-7L in the step 7.
Preferably, the ratio of graphene oxide and sodium hydroxide solution is 150mg in the step 9:150-300ml.
The technique effect and advantage of the present invention：
1, entire prepare in raw material prepares graphene using special graphite powder, and the graphene of production has reliable stability, suction
Attached property and electrical and thermal conductivity；
2, in entire graphene preparation process, by the addition of the concentrated sulfuric acid, potassium permanganate and deionized water, it is eventually adding hydrogen
Sodium oxide molybdena is simultaneously ultrasonically treated under vacuum, is washed through absolute ethyl alcohol after magnetic agitation, and reprecipitation is dried to obtain graphene, whole
No heat treatment process, easy to operate in a preparation process, reduces energy consumption；
3, entire preparation process is simple, and preparation method is economical and practical, and production cost is low, can be mass-produced.
Specific implementation mode
Below in conjunction with the embodiment in the present invention, technical solution in the embodiment of the present invention carries out clearly and completely
Description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this hair
Embodiment in bright, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1：
The present invention provides a kind of methods preparing graphene using special graphite powder, and steps are as follows for specific method：
Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50-100 mesh；
Step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate
It is added in 60 DEG C of the concentrated sulfuric acid, stirs evenly with phosphorus pentoxide, it is 8 hours cooling or more, then carry out suction filtration and washers
Make, wash to neutrality, be finally dried, obtains mixing sample；
Step 3：The mixing sample obtained in step 2 is added in 0 DEG C of the concentrated sulfuric acid, concentrated sulfuric acid addition is 200ml；
Step 4：Potassium permanganate is added, the temperature of system is maintained at 10 DEG C；
Step 5：Then it is kept for 5 hours in 20 DEG C of oil bath, is slowly added to deionized water, deionized water addition is
900ml；
Step 6：After 30min, the deionized water containing hydrogen peroxide is added, until the color of solution becomes glassy yellow, is taken out while hot
Filter, deionized water addition are 2.5-3.0L, the wherein hydrogen peroxide containing 30% concentration in 50ml deionized waters；
Step 7：It is washed, is filtered with a concentration of 10% hydrochloric acid again, hydrochloric acid addition is 5L；
Step 8：Last 40 DEG C of vacuum drying obtain graphene oxide；
Step 9：The graphene oxide obtained in step 8 is added in sodium hydroxide, in one ultrasound 120min of vacuum condition, so
It afterwards with the rotating speed magnetic agitation 72h of 250-300r/min, is washed 7 times with absolute ethyl alcohol, it is 50 DEG C true that gained, which is deposited in temperature,
Dry 48h in empty drying box obtains graphene, and the wherein ratio of graphene oxide and sodium hydroxide solution is 150mg:150ml.
Embodiment 2：
The present invention provides a kind of methods preparing graphene using special graphite powder, and steps are as follows for specific method：
Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50-100 mesh；
Step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate
It is added in 65 DEG C of the concentrated sulfuric acid, stirs evenly with phosphorus pentoxide, it is 8 hours cooling or more, then carry out suction filtration and washers
Make, wash to neutrality, be finally dried, obtains mixing sample；
Step 3：The mixing sample obtained in step 2 is added in 2.5 DEG C of the concentrated sulfuric acid, concentrated sulfuric acid addition is 225ml；
Step 4：Potassium permanganate is added, the temperature of system is maintained at 15 DEG C；
Step 5：Then it is kept for 5 hours in 27.5 DEG C of oil bath, is slowly added to deionized water, deionized water addition is
950ml；
Step 6：After 30min, the deionized water containing hydrogen peroxide is added, until the color of solution becomes glassy yellow, is taken out while hot
Filter, deionized water addition are 2.75L, the wherein hydrogen peroxide containing 30% concentration in 75ml deionized waters；
Step 7：It is washed, is filtered with a concentration of 10% hydrochloric acid again, hydrochloric acid addition is 6L；
Step 8：Last 50 DEG C of vacuum drying obtain graphene oxide；
Step 9：The graphene oxide obtained in step 8 is added in sodium hydroxide, in one ultrasound 75min of vacuum condition, so
It afterwards with the rotating speed magnetic agitation 42h of 250-300r/min, is washed 6 times with absolute ethyl alcohol, it is 65 DEG C true that gained, which is deposited in temperature,
Dry 36h in empty drying box obtains graphene, and the wherein ratio of graphene oxide and sodium hydroxide solution is 150mg:225ml.
Embodiment 3：
The present invention provides a kind of methods preparing graphene using special graphite powder, and steps are as follows for specific method：
Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50-100 mesh；
Step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate
It is added in 70 DEG C of the concentrated sulfuric acid, stirs evenly with phosphorus pentoxide, it is 8 hours cooling or more, then carry out suction filtration and washers
Make, wash to neutrality, be finally dried, obtains mixing sample；
Step 3：The mixing sample obtained in step 2 is added in 5 DEG C of the concentrated sulfuric acid, concentrated sulfuric acid addition is 250ml；
Step 4：Potassium permanganate is added, the temperature of system is maintained at 20 DEG C；
Step 5：Then it is kept for 5 hours in 35 DEG C of oil bath, is slowly added to deionized water, deionized water addition is
1000ml；
Step 6：After 30min, the deionized water containing hydrogen peroxide is added, until the color of solution becomes glassy yellow, is taken out while hot
Filter, deionized water addition are 3.0L, the wherein hydrogen peroxide containing 30% concentration in 100ml deionized waters；
Step 7：It is washed, is filtered with a concentration of 10% hydrochloric acid again, hydrochloric acid addition is 7L；
Step 8：Last 60 DEG C of vacuum drying obtain graphene oxide；
Step 9：The graphene oxide obtained in step 8 is added in sodium hydroxide, in one ultrasound 30min of vacuum condition, so
Afterwards for 24 hours with the rotating speed magnetic agitation of 250-300r/min, it is washed 5 times with absolute ethyl alcohol, it is 80 DEG C true that gained, which is deposited in temperature,
Dry in empty drying box to obtain graphene for 24 hours, the wherein ratio of graphene oxide and sodium hydroxide solution is 150mg:300ml.
It is learnt according to embodiment 1-3：Processing preparation temperature is suitable in embodiment 2, and raw material usage amount is moderate, on the one hand not
The waste of material can be caused, and what can be maximized utilizes material, on the other hand, the graphene quality produced is high, success
Rate is higher, and utilization rate of raw materials is higher, maximumlly reduces production cost, economical and practical, is conducive to the extensive life of graphene
Production, in addition, in entire graphene preparation process, by the addition of the concentrated sulfuric acid, potassium permanganate and deionized water, is eventually adding
Sodium hydroxide is simultaneously ultrasonically treated under vacuum, is washed through absolute ethyl alcohol after magnetic agitation, and reprecipitation is dried to obtain graphene,
No heat treatment process in whole preparation process, it is easy to operate, reduce energy consumption.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, 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
With technical scheme described in the above embodiments is modified 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 the present invention's
Within protection domain.
Claims (6)
1. a kind of method preparing graphene using special graphite powder, steps are as follows for specific method：
Step 1：Prepare the special graphite powder that purity is 99.99%, particle is 50-100 mesh；
Step 2：Oxidation processes are carried out to the special graphite powder prepared in step 1, by 3:2:2 special graphite powder, potassium sulfate
It is added in 60-70 DEG C of the concentrated sulfuric acid, stirs evenly with phosphorus pentoxide, it is 8 hours cooling or more, it is then filtered and is washed
Work is washed to neutrality, is finally dried, and mixing sample is obtained；
Step 3：The mixing sample obtained in step 2 is added in 0-5 DEG C of the concentrated sulfuric acid；
Step 4：Potassium permanganate is added, the temperature of system is maintained at 10-20 DEG C；
Step 5：Then it is kept for 5 hours in 20-35 DEG C of oil bath, is slowly added to deionized water；
Step 6：After 30min, the deionized water containing hydrogen peroxide is added, until the color of solution becomes glassy yellow, is taken out while hot
Filter；
Step 7：It is washed, is filtered with a concentration of 10% hydrochloric acid again；
Step 8：Last 40-60 DEG C of vacuum drying obtains graphene oxide；
Step 9：The graphene oxide obtained in step 8 is added in sodium hydroxide, in one ultrasound 30- of vacuum condition
120min is washed 5-7 times, gained is deposited in then with the rotating speed magnetic agitation 24-72h of 250-300r/min with absolute ethyl alcohol
Dry 24-48h, obtains graphene in the vacuum drying chamber that temperature is 50-80 DEG C.
2. a kind of method preparing graphene using special graphite powder according to claim 1, it is characterised in that：The step
Concentrated sulfuric acid addition is 200-250ml in rapid three.
3. a kind of method preparing graphene using special graphite powder according to claim 1, it is characterised in that：The step
Deionized water addition is 900-1000ml in rapid five.
4. a kind of method preparing graphene using special graphite powder according to claim 1, it is characterised in that：The step
Deionized water addition is 2.5-3.0L, the wherein hydrogen peroxide containing 30% concentration in 50-100ml deionized waters in rapid six.
5. a kind of method preparing graphene using special graphite powder according to claim 1, it is characterised in that：The step
Hydrochloric acid addition is 5-7L in rapid seven.
6. a kind of method preparing graphene using special graphite powder according to claim 1, it is characterised in that：The step
The ratio of graphene oxide and sodium hydroxide solution is 150mg in rapid nine:150-300ml.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108862272A (en) * | 2018-08-21 | 2018-11-23 | 大同新成新材料股份有限公司 | A method of expanded graphite is prepared using graphene oxide, nano-carbon powder |
| CN112811416A (en) * | 2021-01-20 | 2021-05-18 | 陕西榆能集团能源化工研究院有限公司 | Preparation method of single-layer graphene oxide based on semi-coke |
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Patent Citations (4)
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| CN102126720A (en) * | 2011-04-14 | 2011-07-20 | 中国科学院理化技术研究所 | Method for synthesizing graphene |
| CN102674327A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Environment-friendly method for preparing water-soluble grapheme at normal temperature |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108862272A (en) * | 2018-08-21 | 2018-11-23 | 大同新成新材料股份有限公司 | A method of expanded graphite is prepared using graphene oxide, nano-carbon powder |
| CN112811416A (en) * | 2021-01-20 | 2021-05-18 | 陕西榆能集团能源化工研究院有限公司 | Preparation method of single-layer graphene oxide based on semi-coke |
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Application publication date: 20180724 |