CN108962623A - A kind of graphene composite material and preparation method thereof and device - Google Patents

A kind of graphene composite material and preparation method thereof and device Download PDF

Info

Publication number
CN108962623A
CN108962623A CN201810964125.4A CN201810964125A CN108962623A CN 108962623 A CN108962623 A CN 108962623A CN 201810964125 A CN201810964125 A CN 201810964125A CN 108962623 A CN108962623 A CN 108962623A
Authority
CN
China
Prior art keywords
composite material
graphene
mixed liquor
centrifugation
inner cylinder
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.)
Granted
Application number
CN201810964125.4A
Other languages
Chinese (zh)
Other versions
CN108962623B (en
Inventor
武建军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Xinfeng Power Supply Technology Co ltd
Original Assignee
Datong Xincheng New Material Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Datong Xincheng New Material Co Ltd filed Critical Datong Xincheng New Material Co Ltd
Priority to CN201810964125.4A priority Critical patent/CN108962623B/en
Publication of CN108962623A publication Critical patent/CN108962623A/en
Application granted granted Critical
Publication of CN108962623B publication Critical patent/CN108962623B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/38Carbon pastes or blends; Binders or additives therein
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G13/00Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The present invention discloses a kind of graphene composite material and preparation method thereof and device, and wherein graphene composite material is prepared from the following raw materials: crystalline graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water, graphene suspension is prepared first, by CoCl2·6H2O is dissolved in graphene suspension, stirs 15~25min, secondary mixed liquor is obtained, by Co (OH)2、MoS2、CO(NH2)2It is added in secondary mixed liquor, stir 15~25min, mixed liquor three times is obtained, will be poured into stainless steel cauldron mixed liquor three times, pressure condition is 20MPa~25MPa, temperature condition is 25~35 DEG C, graphene compound mixture is obtained, graphene compound mixture is filtered, after being washed with deionized, it is put into drying in drying oven, obtains graphene composite material;The composite material of obtained metal oxide and graphene, it is metal oxide supported on the surface of graphene on improve the chemical property of composite material, specific capacity significantly improves, improve as electrode of super capacitor significant effect.

Description

A kind of graphene composite material and preparation method thereof and device
Technical field
The present invention relates to field of material technology, in particular to a kind of graphene composite material and preparation method thereof and device.
Background technique
Carbon material is to be used as electrode material for super capacitor earliest, has stability and electric conductivity good, specific surface area The advantages that high.Since carbon material is by being formed on its surface electric double layer capacitance, the specific surface area of material gets over the electricity of large capacitor Capacitive can be better, and therefore, the specific surface area for improving carbon material is to improve the effective way of carbon electrode material capacitor specific capacity.Stone Black alkene is a kind of two-dimensional slice structure, only one carbon atom of thickness is thick, the hexagonal network knot that surface is made of carbon atom Structure.Graphene has special physical and chemical properties, and graphene is as a kind of carbon material, and specific surface area is high, in super capacitor The application of device electrode material above has good prospect.But graphene specific capacity is lower, and chemical property is poor, as super capacitor Device electrode effect is poor.
Summary of the invention
To overcome the problems in correlation technique, the present invention provide a kind of graphene composite material and preparation method thereof and Device.
According to the first aspect of the embodiments of the present disclosure, a kind of graphene composite material, the graphene composite material are provided It is prepared from the following raw materials: crystalline graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO (NH2)2And deionized water.
A kind of graphene composite material of first aspect,.
Optionally, the CoCl2·6H2The additive amount of O is 3.5mmol.
According to the second aspect of the disclosure, a kind of preparation method of graphene composite material is provided, comprising the following steps:
Crystalline graphite powder and the concentrated sulfuric acid are uniformly mixed, NaNO is added in stirring while3And KMnO4, it is 5 DEG C~-5 DEG C in temperature Under the conditions of stir 3h, obtain preliminary mixed liquor;
The preliminary mixed liquor is heated to 45 DEG C~50 DEG C, deionized water dilution is added, obtains dilution mixed liquor;
H is added in the dilution mixed liquor2O2, it is washed after filtering with HCl, is washed with deionized later, after dry, Obtain graphite oxide powder;
The graphite oxide powder is dissolved in deionized water, and is centrifuged 20~30min under 3000rpm~4000rpm speed conditions, Obtain graphene suspension;
By CoCl2·6H2O is dissolved in the graphene suspension, stirs 15~25min, obtains secondary mixed liquor;
By Co (OH)2、MoS2、CO(NH2)2It is added in the secondary mixed liquor, stirs 15~25min, mixed three times Liquid;
The mixed liquor three times is poured into stainless steel cauldron, pressure condition be 20MPa~25MPa, temperature condition be 25~ 35 DEG C, obtain graphene compound mixture;
The graphene compound mixture is filtered, after being washed with deionized, drying in drying oven is put into, obtains the graphite Alkene composite material.
Using second aspect provide carbon brush preparation method, crystalline graphite powder and the concentrated sulfuric acid are uniformly mixed first, stirring it is same When NaNO is added3And KMnO4, 3h is stirred under the conditions of temperature is 5 DEG C~-5 DEG C, preliminary mixed liquor is obtained, by the preliminary mixing Liquid is heated to 45 DEG C~50 DEG C, and deionized water dilution is added, and obtains dilution mixed liquor, H is added in the dilution mixed liquor2O2, It is washed after filtering with HCl, is washed with deionized later, after dry, graphite oxide powder is obtained, by the graphite oxide Powder is dissolved in deionized water, and 20~30min is centrifuged under 3000rpm~4000rpm speed conditions, obtains graphene suspension, By CoCl2·6H2O is dissolved in the graphene suspension, stirs 15~25min, secondary mixed liquor is obtained, by Co (OH)2、MoS2、 CO(NH2)2It is added in the secondary mixed liquor, stirs 15~25min, obtain mixed liquor three times, the mixed liquor three times is fallen Enter in stainless steel cauldron, pressure condition is 20MPa~25MPa, and temperature condition is 25~35 DEG C, obtains the compound mixing of graphene Object filters the graphene compound mixture, after being washed with deionized, is put into drying in drying oven, obtains the graphite Alkene composite material;The composite material of obtained metal oxide and graphene, it is metal oxide supported to come up on the surface of graphene The chemical property of composite material is improved, specific capacity significantly improves, and improves as electrode of super capacitor significant effect.
Optionally, described by CoCl2·6H2O is dissolved in the graphene suspension, and the temperature condition of 15~25min of stirring is 90~100 DEG C.
Optionally, the inner wall of the stainless steel cauldron is provided with polytetrafluoroethylene ethylene layer.
Optionally, described to pour into the mixed liquor three times in stainless steel cauldron, reaction time 8.5h.
According to the third aspect of the disclosure, a kind of preparation facilities of graphene composite material is provided, is used for the oxidation Graphite powder is dissolved in deionized water, and 20~30min is centrifuged under 3000rpm~4000rpm speed conditions, which is characterized in that institute Stating preparation facilities includes: centrifugal device, feeding device and feeding device, and the feeding device and the feeding device are all provided with It is placed in the top of the centrifugal device;
The centrifugal device include centrifugation outer cylinder and centrifugation inner cylinder, it is described centrifugation inner cylinder facility in it is described centrifugation outer cylinder inside, The bottom of the centrifugation outer cylinder is provided with rotary shaft, and the rotary shaft is fixedly connected with the centrifugation inner cylinder, the centrifugation inner cylinder Volume be less than it is described centrifugation inner cylinder bottom to it is described be centrifuged outer cylinder bottom region volume;
The feeding device includes feed pipe, and one end of the feed pipe protrudes from the top of the centrifugation outer cylinder, the charging The other end of pipe is set to the inside of the centrifugation inner cylinder, and the feeding device includes feeding pipe, and one end of the feeding pipe is set It is placed in the inside of the centrifugation inner cylinder, the other end of the feeding pipe is connected with dispenser, and the side of the dispenser is connected with Vacuum pump.
Optionally, multiple nozzles, pipe of multiple nozzles in the feed pipe are provided on the tube wall of the feed pipe It is evenly distributed on wall.
Optionally, multiple nozzles are in circular cone shape.
Optionally, baffle, the vertical section of the baffle and the centrifugation inner cylinder are provided at the top of the centrifugation inner cylinder The angle in vertical section is in 45 °
The preparation facilities of a kind of graphene composite material of the third aspect, in use, the oxidation stone of deionized water will be dissolved in first Ink powder pours into feed pipe, and graphite oxide powder enters centrifugation inner cylinder, and rotary shaft drives centrifugation inner cylinder rotating, graphite oxide powder compared to Hydrone particle is bigger, graphite oxide powder stay in centrifugation inner cylinder inside, extra water by the hole on the barrel of centrifugation inner cylinder into Enter and be centrifuged outer cylinder, and due to centrifugation inner cylinder volume be less than centrifugation inner cylinder bottom to be centrifuged outer cylinder bottom region appearance Product, the water being centrifuged in outer cylinder will not flow back into centrifugation inner cylinder, complete centrifugally operated, finally open vacuum pump, vacuum pump will be complete Enter in dispenser at the graphite oxide powder suspension of centrifugally operated via feeding pipe, not having to opening equipment in this way can complete Liquid is taken, the graphene composite material that the third aspect provides enables to the graphene-structured after centrifugation more stable, of graphene Granularity is more uniform, improves the properties of composite material.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, letter will be made to attached drawing needed in the embodiment below Singly introduce, it should be apparent that, for those of ordinary skills, without any creative labor, It is also possible to obtain other drawings based on these drawings.
Fig. 1 is that a kind of process of the preparation method of the graphene composite material provided according to an exemplary embodiment is illustrated Figure;
Fig. 2 is a kind of overall schematic of the preparation facilities of the graphene composite material provided according to an exemplary embodiment.
Specific embodiment
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.Following exemplary embodiment Described in embodiment do not represent all embodiments consistented with the present invention.On the contrary, they be only with it is such as appended The example of device and method being described in detail in claims, some aspects of the invention are consistent.
A kind of graphene composite material, the graphene composite material are made of raw material from the following weight: crystalline graphite powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water.Composite material Microstructure have a great impact to the chemical property of electrode, the crystal of the microscopic appearance of the composite material of the present embodiment is clear Clear, crystal perfection is presented good fascicular texture, the meso-hole structure that fascicular texture is made of some little particles, and these small The diameter dimension of kernel structure is uniform, and is evenly distributed.This arrangement reduces the resistances of ion transport to surface of active material, mention The high utilization rate of bioactive molecule, can significantly improve the capacitive property and chemical property of composite material.
In addition, showing the CoCl by experimental study2·6H2The additive amount of O is 3.5mmol, CoCl2·6H2O's adds Dosage is different, and anodizing reduction current is different, CoCl2·6H2When the additive amount of O is smaller, anodizing reduction current is smaller, Chemical property is relatively weak, with raising CoCl2·6H2The additive amount of O, the redox ability enhancing of composite material, still CoCl2·6H2When the adding too much of O, the impedance that electronics and ion transport surface of active material will increase again, and then specific volume Amount will be with reduction, so it was proved that CoCl2·6H2It is obtained composite wood when the additive amount of O is 3.5mmol The specific capacity of material is maximum, and chemical property is best.
Fig. 1 is the flow diagram of the preparation method of the graphene carbon brush provided according to an exemplary embodiment, including such as Lower step:
In step sl, crystalline graphite powder and the concentrated sulfuric acid are uniformly mixed, NaNO is added in stirring while3And KMnO4, in temperature 3h is stirred under the conditions of being 5 DEG C~-5 DEG C, obtains preliminary mixed liquor.
In step s 2, the preliminary mixed liquor is heated to 45 DEG C~50 DEG C, deionized water dilution is added, is diluted Mixed liquor.
In step s3, H is added in the dilution mixed liquor2O2, washed after filtering with HCl, use deionization later Water washing obtains graphite oxide powder after dry.
In step s 4, the graphite oxide powder is dissolved in deionized water, and in 3000rpm~4000rpm speed conditions 20~30min of lower centrifugation, obtains graphene suspension.
In step s 5, by CoCl2·6H2O is dissolved in the graphene suspension, stirs 15~25min, obtains secondary mixed Close liquid.
In step s 6, by Co (OH)2、MoS2、CO(NH2)2It is added in the secondary mixed liquor, stirring 15~ 25min obtains mixed liquor three times.
In the step s 7, the mixed liquor three times being poured into stainless steel cauldron, pressure condition is 20MPa~25MPa, Temperature condition is 25~35 DEG C, obtains graphene compound mixture.
In step s 8, the graphene compound mixture is filtered, after being washed with deionized, is put into drying oven and does It is dry, obtain the graphene composite material.
In step s 5, described by CoCl2·6H2O is dissolved in the graphene suspension, stirs the temperature strip of 15~25min Part is 90~100 DEG C.Temperature is too low, and the cobalt for reacting not thorough enough, only a small amount of adheres on the surface of graphene, and temperature is excessively high and holds Graphene oxide is easily led to adequately to be restored, surface loses activity functional group, it was proved that, the optimum temperature of reaction is 90~100 DEG C.
In the step s 7, the inner wall of the stainless steel cauldron is provided with polytetrafluoroethylene ethylene layer, and polytetrafluoroethylene ethylene layer can It prevents graphene from reacting with stainless steel inner wall, enables the substance in mixed liquor three times sufficiently compound.
In the step s 7, described to pour into the mixed liquor three times in stainless steel cauldron, reaction time 8.5h, reaction Time is too short, and graphene and other materials are compound not thorough enough, and the reaction time is too long, and graphene oxide is also easy adequately to be gone back Original, surface lose activity functional group, and specific capacity declines instead, thus the reaction time it was proved that, 8.5h is optimum response Time.
Fig. 2 is that a kind of the whole of the preparation facilities of the graphene composite material provided according to an exemplary embodiment is illustrated Figure, for the graphite oxide powder to be dissolved in deionized water, and under 3000rpm~4000rpm speed conditions centrifugation 20~ 30min, the preparation facilities include: centrifugal device 1, feeding device 2 and feeding device 3, the feeding device 2 and described Feeding device 3 is all set in the top of the centrifugal device 1;
The centrifugal device 1 includes centrifugation outer cylinder 11 and centrifugation inner cylinder 12, and 12 facility of centrifugation inner cylinder is in the centrifugation outer cylinder 11 inside, the bottom of the centrifugation outer cylinder 11 are provided with rotary shaft 13, and the rotary shaft 13 and the centrifugation inner cylinder 12 are fixed Connection, the volume of the centrifugation inner cylinder 12 are less than the bottom of the centrifugation inner cylinder 12 to the region of the bottom of the centrifugation outer cylinder 11 Volume;
The feeding device 2 includes feed pipe 21, and one end of the feed pipe 21 protrudes from the top of the centrifugation outer cylinder 11, institute The other end for stating feed pipe 21 is set to the inside of the centrifugation inner cylinder 12, and the feeding device 3 includes feeding pipe 31, described to take One end of expects pipe 31 is set to the inside of the centrifugation inner cylinder 12, and the other end of the feeding pipe 31 is connected with dispenser 32, institute The side for stating dispenser 32 is connected with vacuum pump 33.
In use, the graphite oxide powder for being dissolved in deionized water is first poured into feed pipe 21, graphite oxide powder enters in centrifugation Cylinder 12, rotary shaft 13 drive centrifugation inner cylinder 12 to rotate, and graphite oxide powder is bigger compared to hydrone particle, and graphite oxide powder stays in It is centrifuged the inside of inner cylinder 12, extra water enters centrifugation outer cylinder 11 by the hole on the barrel of centrifugation inner cylinder 12, and due to centrifugation The volume of inner cylinder 12 be less than centrifugation inner cylinder 12 bottom to centrifugation outer cylinder 11 bottom region volume, centrifugation outer cylinder 11 in Water will not flow back into centrifugation inner cylinder 12, complete centrifugally operated, finally open vacuum pump 33, and vacuum pump 33 will complete centrifugally operated Graphite oxide powder suspension via feeding pipe 31 enter dispenser 32 in, in this way do not have to opening equipment can complete to take liquid, The graphene composite material that the third aspect provides enables to the graphene-structured after centrifugation more stable, and the granularity of graphene is more Add uniformly, improves the properties of composite material.
Fig. 2 shows feed pipe 21 another embodiment, be provided with multiple nozzles on the tube wall of the feed pipe 21 211, multiple nozzles 211 are evenly distributed on the tube wall of the feed pipe.Multiple nozzles 211 are in the frustum of a cone Shape, such structure setting is conducive to the spraying of graphite oxide powder uniform suspension into centrifugation inner cylinder 12, so that graphite oxide The centrifugation of powder suspension is more uniform.
Fig. 2 shows another embodiment, be provided with baffle, the vertical section of the baffle at the top of the centrifugation inner cylinder Angle with the vertical section of the centrifugation inner cylinder is in 45 °, and when baffle can prevent centrifugation inner cylinder 12 from rotating, graphite oxide powder suspends Liquid splashes from the top of centrifugation inner cylinder 12, leads to the waste of raw material.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to of the invention its Its embodiment.This application is intended to cover any variations, uses, or adaptations of the invention, these modifications, purposes or Person's adaptive change follows general principle of the invention and including the undocumented common knowledge in the art of the disclosure Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following Claim is pointed out.
It should be understood that the present invention is not limited to the precise structure already described above and shown in the accompanying drawings, and And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.

Claims (10)

1. a kind of graphene composite material, which is characterized in that the graphene composite material is made of raw material below: scale stone Ink powder, H2SO4、NaNO3、KMnO4、H2O2、HCl、CoCl2·6H2O、Co(OH)2、MoS2、CO(NH2)2And deionized water.
2. a kind of graphene composite material as described in claim 1, which is characterized in that the CoCl2·6H2The additive amount of O is 3.5mmol。
3. a kind of preparation method of graphene composite material, which comprises the following steps:
Crystalline graphite powder and the concentrated sulfuric acid are uniformly mixed, NaNO is added in stirring while3And KMnO4, it is 5 DEG C~-5 DEG C in temperature Under the conditions of stir 3h, obtain preliminary mixed liquor;
The preliminary mixed liquor is heated to 45 DEG C~50 DEG C, deionized water dilution is added, obtains dilution mixed liquor;
H is added in the dilution mixed liquor2O2, it is washed after filtering with HCl, is washed with deionized later, after dry, Obtain graphite oxide powder;
The graphite oxide powder is dissolved in deionized water, and is centrifuged 20~30min under 3000rpm~4000rpm speed conditions, Obtain graphene suspension;
By CoCl2·6H2O is dissolved in the graphene suspension, stirs 15~25min, obtains secondary mixed liquor;
By Co (OH)2、MoS2、CO(NH2)2It is added in the secondary mixed liquor, stirs 15~25min, obtain mixed liquor three times;
The mixed liquor three times is poured into stainless steel cauldron, pressure condition be 20MPa~25MPa, temperature condition be 25~ 35 DEG C, obtain graphene compound mixture;
The graphene compound mixture is filtered, after being washed with deionized, drying in drying oven is put into, obtains the graphite Alkene composite material.
4. a kind of preparation method of graphene composite material as claimed in claim 3, which is characterized in that described by CoCl2· 6H2O is dissolved in the graphene suspension, and the temperature condition of 15~25min of stirring is 90~100 DEG C.
5. a kind of preparation method of graphene composite material as claimed in claim 3, which is characterized in that the stainless steel reaction The inner wall of kettle is provided with polytetrafluoroethylene ethylene layer.
6. a kind of preparation method of graphene composite material as claimed in claim 3, which is characterized in that the general is described three times Mixed liquor pours into stainless steel cauldron, reaction time 8.5h.
7. a kind of preparation facilities of graphene composite material, for the graphite oxide powder to be dissolved in deionized water, and 20~30min is centrifuged under 3000rpm~4000rpm speed conditions, which is characterized in that the preparation facilities includes: centrifugal device (1), feeding device (2) and feeding device (3), the feeding device (2) and the feeding device (3) are all set in described The top of centrifugal device (1);
The centrifugal device (1) includes centrifugation outer cylinder (11) and centrifugation inner cylinder (12), and centrifugation inner cylinder (12) facility is in described It is centrifuged the inside of outer cylinder (11), the bottom of centrifugation outer cylinder (11) is provided with rotary shaft (13), the rotary shaft (13) and institute It states centrifugation inner cylinder (12) to be fixedly connected, the volume of centrifugation inner cylinder (12) is less than the bottom of centrifugation inner cylinder (12) described in It is centrifuged the volume in the region of the bottom of outer cylinder (11);
The feeding device (2) includes feed pipe (21), and one end of the feed pipe (21) protrudes from the centrifugation outer cylinder (11) Top, the other end of the feed pipe (21) is set to the inside of centrifugation inner cylinder (12), and the feeding device (3) includes Feeding pipe (31), one end of the feeding pipe (31) are set to the inside of centrifugation inner cylinder (12), the feeding pipe (31) The other end is connected with dispenser (32), and the side of the dispenser (32) is connected with vacuum pump (33).
8. a kind of preparation facilities of graphene composite material as claimed in claim 7, which is characterized in that the feed pipe (21) Tube wall on be provided with multiple nozzles (211), multiple nozzles (211) on the tube wall of the feed pipe (21) in uniformly point Cloth.
9. such as a kind of preparation facilities for graphene composite material that claim 8 is stated, which is characterized in that multiple nozzles It (211) is in circular cone shape.
10. a kind of preparation facilities of graphene composite material as described in claim 7 to 9 any one claim, special Sign is, is provided with baffle (121) at the top of the centrifugation inner cylinder (12), the vertical section of the baffle (121) and the centrifugation The angle in the vertical section of inner cylinder (12) is in 45 °.
CN201810964125.4A 2018-08-23 2018-08-23 Graphene composite material and preparation method and device thereof Active CN108962623B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810964125.4A CN108962623B (en) 2018-08-23 2018-08-23 Graphene composite material and preparation method and device thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810964125.4A CN108962623B (en) 2018-08-23 2018-08-23 Graphene composite material and preparation method and device thereof

Publications (2)

Publication Number Publication Date
CN108962623A true CN108962623A (en) 2018-12-07
CN108962623B CN108962623B (en) 2020-02-28

Family

ID=64473872

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810964125.4A Active CN108962623B (en) 2018-08-23 2018-08-23 Graphene composite material and preparation method and device thereof

Country Status (1)

Country Link
CN (1) CN108962623B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109786136A (en) * 2019-02-25 2019-05-21 天津艾克凯胜石墨烯科技有限公司 The method of Ni-Co-Mn nanoneedle is grown on a kind of 3D graphene
RU2729880C1 (en) * 2019-11-05 2020-08-13 Объединенный Институт Ядерных Исследований (Оияи) Solid-state capacitor-ionistor with dielectric layer made of dielectric nanopowder

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006322034A (en) * 2005-05-18 2006-11-30 Mitsubishi Electric Corp Electrode for discharge surface treatment, coated film for discharge surface treatment and treatment method
CN102347143A (en) * 2011-07-11 2012-02-08 中国科学院上海硅酸盐研究所 Graphene composite porous counter electrode, preparation method and application thereof
CN102891016A (en) * 2012-10-19 2013-01-23 常州大学 Nickel cobaltate-graphene composite material and application and preparation method thereof
CN104157850A (en) * 2014-07-07 2014-11-19 青岛大学 Application of cell-structured M<2+>/MoS2 and graphene composite material in lithium ion battery
CN105375061A (en) * 2015-12-09 2016-03-02 宋宏婷 Graphene electrode
CN106504907A (en) * 2016-12-02 2017-03-15 东华大学 A kind of molybdenum sulfide/cobaltosic oxide composite material and its preparation method and application
US20170338472A1 (en) * 2016-05-17 2017-11-23 Aruna Zhamu Chemical-Free Production of Graphene-Encapsulated Electrode Active Material Particles for Battery Applications

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006322034A (en) * 2005-05-18 2006-11-30 Mitsubishi Electric Corp Electrode for discharge surface treatment, coated film for discharge surface treatment and treatment method
CN102347143A (en) * 2011-07-11 2012-02-08 中国科学院上海硅酸盐研究所 Graphene composite porous counter electrode, preparation method and application thereof
CN102891016A (en) * 2012-10-19 2013-01-23 常州大学 Nickel cobaltate-graphene composite material and application and preparation method thereof
CN104157850A (en) * 2014-07-07 2014-11-19 青岛大学 Application of cell-structured M<2+>/MoS2 and graphene composite material in lithium ion battery
CN105375061A (en) * 2015-12-09 2016-03-02 宋宏婷 Graphene electrode
US20170338472A1 (en) * 2016-05-17 2017-11-23 Aruna Zhamu Chemical-Free Production of Graphene-Encapsulated Electrode Active Material Particles for Battery Applications
CN106504907A (en) * 2016-12-02 2017-03-15 东华大学 A kind of molybdenum sulfide/cobaltosic oxide composite material and its preparation method and application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109786136A (en) * 2019-02-25 2019-05-21 天津艾克凯胜石墨烯科技有限公司 The method of Ni-Co-Mn nanoneedle is grown on a kind of 3D graphene
RU2729880C1 (en) * 2019-11-05 2020-08-13 Объединенный Институт Ядерных Исследований (Оияи) Solid-state capacitor-ionistor with dielectric layer made of dielectric nanopowder

Also Published As

Publication number Publication date
CN108962623B (en) 2020-02-28

Similar Documents

Publication Publication Date Title
WO2018024196A1 (en) Preparation method for graphene nanometer material
CN204671927U (en) A kind of novel multifunctional tank
CN108929598A (en) A kind of preparation method of the MXene ink based on inkjet printing and its application in MXene flexible electrode
CN106430295B (en) A kind of micro-nano hierarchy BaTiO3Crystal and preparation method thereof
CN107867726B (en) A kind of preparation method of nano oxidized ruthenium
CN108962623A (en) A kind of graphene composite material and preparation method thereof and device
CN105600828B (en) A kind of porous nano CuFe2O4Preparation method
CN105664950B (en) A kind of porous nano ZnFe2O4Preparation method
CN105345023B (en) The preparation method of the super fine silver powder of good dispersion
CN102191389B (en) Rinsing method of potassium fluotantalate product obtained through sodium reduction
CN105780093A (en) Composite electroplating technology of high-wear-resisting nano diamond alkene
CN109243665A (en) A kind of preparation method of conductive uniformly monolithic layer transition metal carbide film
CN211226350U (en) Industrial equipment for preparing graphene oxide by one-step method under low-temperature condition
CN103273074B (en) Process method of continuously producing ultra-fine nickel powder
CN108435176A (en) A kind of Fe2O3 doping TiO2Octahedron nanometer particle and preparation method thereof
CN107742587B (en) A kind of three layers of Mn of height ratio capacity2O3@MoS2Nano-hollow ball electrode material and the preparation method and application thereof
CN104709913A (en) Novel nano silica powder preparation method
CN106809918B (en) A kind of carbon nano tube modified lead dioxide electrode and preparation method thereof
CN105198004B (en) A kind of Fe3O4‑SnO2Nano composite material and preparation method thereof
CN209423376U (en) Agitating paddle is used in a kind of processing of honey
CN107742585B (en) A kind of height ratio capacity MoS2/Mn2O3Nano-hollow ball combination electrode material and the preparation method and application thereof
CN101818365A (en) Method for preparing nano stibium powder
CN109119253A (en) Composition metal-organic framework materials, metal composite oxide-organic framework materials and preparation method and application
CN105692700B (en) In high ion concentration plating solution can stable suspersion tungsten trioxide nano particle preparation method and application
CN204699661U (en) Solid-liquid agitator

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
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20230419

Address after: 547000 Daren Industrial Park (Industrial Park), Hechi City, Guangxi Zhuang Autonomous Region

Patentee after: Guangxi Xinfeng Power Supply Technology Co.,Ltd.

Address before: 037002 Garden Village, Xinrong District, Datong, Shanxi

Patentee before: DATONG XINCHENG NEW MATERIAL Co.,Ltd.

TR01 Transfer of patent right