CN210480876U - System for preparing graphene powder by redox method - Google Patents
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- CN210480876U CN210480876U CN201921096656.2U CN201921096656U CN210480876U CN 210480876 U CN210480876 U CN 210480876U CN 201921096656 U CN201921096656 U CN 201921096656U CN 210480876 U CN210480876 U CN 210480876U
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Abstract
The utility model relates to a system for redox method preparation graphite alkene powder belongs to graphite alkene preparation technical field. Including reduction reation kettle, reduction reation kettle upper portion links to each other with the condenser, and the reduction reation kettle lower part passes through the pipeline and links to each other with one-level centrifuge, and one-level centrifuge passes through the pipeline and links to each other with second grade centrifuge, and second grade centrifuge passes through the pipeline and links to each other with the freeze dryer. System of redox method preparation graphite alkene powder, the practicality is strong, equipment is simple, the simple operation, factor of safety is high, the graphite alkene dispersibility of preparation is good, it is low to pile up the degree, difficult reunion can be applicable to extensive industrial production.
Description
Technical Field
The utility model relates to a system for redox method preparation graphite alkene powder belongs to graphite alkene preparation technical field.
Background
Graphene, which is a carbon atom in sp2A two-dimensional atomic crystal of a thickness of hybridized monoatomic bonds. The special structure enables the graphene to show a plurality of excellent properties, such as ultrahigh specific surface area, ultrahigh electrical characteristics, ultrahigh electron transport capacity, ultrahigh mechanical properties and the like, is a leading-edge new material, and has profound influence in a plurality of scientific fields.
Patent CN 105047255a discloses a crystalline silicon solar cell aluminum paste containing highly dispersed graphene and a preparation method thereof, wherein the glass powder is adsorbed on the surface of graphene by mixing and ball-milling the glass powder and the graphene, so as to prevent aggregation of the graphene, better maintain the conjugated structure of the graphene, and ensure excellent conductivity of an aluminum back surface field.
At present, in a system for producing graphene powder, equipment connection is complicated, the preparation period is long, operation is inconvenient, the yield is low, and the system is not suitable for the requirement of large-scale industrial production.
Therefore, a new system for preparing graphene powder by a redox method is needed.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the not enough of prior art, provide a system for preparation graphite alkene powder of redox method. The system has the advantages of strong practicability, simple equipment, convenience and rapidness in operation, high safety factor, good dispersity of the prepared graphene, low stacking degree, difficulty in agglomeration and suitability for large-scale industrial production.
System of redox method preparation graphite alkene powder, including reduction reation kettle, reduction reation kettle upper portion links to each other with the condenser, and the reduction reation kettle lower part passes through the pipeline and links to each other with one-level centrifuge, and one-level centrifuge passes through the pipeline and links to each other with second grade centrifuge, and second grade centrifuge passes through the pipeline and links to each other with the freeze drier.
And a feeding port at the upper part of the reduction reaction kettle is respectively connected with a graphene oxide solution feeding pipe and a hydrazine hydrate feeding pipe.
The upper part of the condenser is connected with the first condensing pipe, and the lower part of the condenser is connected with the second condensing pipe.
The rotating speed of the primary centrifuge is 19000r/min-25000 r/min.
The rotation speed of the secondary centrifuge is 19000r/min-25000 r/min.
The system for preparing graphene powder by the redox method disclosed by the invention has the following working principle and process:
adding a graphene oxide solution into a reduction reaction kettle through a graphene oxide feeding pipe, wherein the reduction reaction kettle is provided with a heat-preservation jacket, circulating water is arranged in the heat-preservation jacket, the temperature of the reduction reaction kettle is controlled to be 60-90 ℃ through the heat-preservation jacket, and the graphene oxide solution is subjected to heat treatment, so that oxygen-containing functional groups in a graphene oxide structure are removed, and graphene oxide sheets are crosslinked with one another to form reduced graphene oxide with a three-dimensional structure; then adding hydrazine hydrate into a reduction reaction kettle through a hydrazine hydrate feeding pipe, controlling the temperature of the reduction reaction kettle to be 75-85 ℃ through a jacket, evaporating the hydrazine hydrate in the reaction process, allowing the evaporated hydrazine hydrate to enter a condenser for condensation, and reducing the loss of the hydrazine hydrate, wherein the upper part of the condenser is connected with a first condensation pipe, the lower part of the condenser is connected with a second condensation pipe, and normal-temperature tap water is introduced into the first condensation pipe and the second condensation pipe to realize the cooling of the hydrazine hydrate volatilized into the condenser, and the water bath backflow is continuously carried out for 12 hours; the following reactions take place in the reduction reactor: hydrazine hydrate molecules react with epoxy groups in a graphene oxide structure in a nucleophilic substitution mode to enable the epoxy groups to generate an open loop reaction to form carbocations, oxygen anions capture hydrogen in the hydrazine molecules to form hydroxyl groups, the hydrazine molecules losing the hydrogen are combined with the carbocations, and then oxygen-containing functional groups in the structure are removed through an intramolecular condensation reaction, so that the graphene oxide is reduced; after the reduction reaction is finished, the material enters a primary centrifuge from the outlet of a reduction reaction kettle for centrifugation, the centrifugation is carried out for alkali removal, the rotation speed of the centrifuge is controlled to be 19000r/min-25000r/min, then the material enters a secondary centrifuge for further centrifugation and impurity removal, the rotation speed of the centrifuge is controlled to be 19000r/min-25000r/min, the centrifuged material enters a freeze dryer for drying through a feeding pipe, the drying temperature of the freeze dryer is-70 ℃, the drying time is 70-80 hours, and after the drying is finished, the graphene oxide powder is prepared.
Compared with the prior art, the utility model, following beneficial effect has:
system of redox method preparation graphite alkene powder, the practicality is strong, equipment is simple, the simple operation, factor of safety is high, the graphite alkene dispersibility of preparation is good, it is low to pile up the degree, difficult reunion can be applicable to extensive industrial production.
Drawings
Fig. 1 is a schematic structural diagram of a system for preparing graphene powder by a redox method.
In the figure: 1. a reduction reaction kettle; 2. a graphene oxide solution feeding pipe; 3. a hydrazine hydrate feed pipe; 4. a condenser; 5. a first condenser pipe; 6. a primary centrifuge; 7. a secondary centrifuge; 8. a second condenser pipe; 9. a freeze dryer; 10. and (4) feeding a pipe.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Embodiments of the present invention are further described below with reference to the accompanying drawings: as shown in fig. 1, redox method preparation graphite alkene powder's system, including reduction reation kettle 1, reduction reation kettle 1 upper portion links to each other with condenser 4, and reduction reation kettle 1 lower part passes through the pipeline and links to each other with one-level centrifuge 6, and one-level centrifuge 6 passes through the pipeline and links to each other with second grade centrifuge 7, and second grade centrifuge 7 passes through the pipeline and links to each other with freeze dryer 9.
The upper feed inlet of the reduction reaction kettle 1 is respectively connected with a graphene oxide solution feed pipe 2 and a hydrazine hydrate feed pipe 3.
The upper part of the condenser 4 is connected with the first condensation pipe 5, and the lower part of the condenser 4 is connected with the second condensation pipe 8.
The rotating speed of the primary centrifuge 6 is 19000r/min-25000 r/min.
The rotation speed of the secondary centrifuge 6 is 19000r/min-25000 r/min.
Adding a graphene oxide solution into a reduction reaction kettle 1 through a graphene oxide feeding pipe 2, wherein the reduction reaction kettle 1 is provided with a heat-preservation jacket, circulating water is arranged in the heat-preservation jacket, the temperature of the reduction reaction kettle 1 is controlled to be 60-90 ℃ through the heat-preservation jacket, and the graphene oxide solution is subjected to heat treatment, so that oxygen-containing functional groups in a graphene oxide structure are removed, and graphene oxide sheets are crosslinked with one another to form reduced graphene oxide with a three-dimensional structure; then adding hydrazine hydrate into a reduction reaction kettle 1 through a hydrazine hydrate feeding pipe 3, controlling the temperature of the reduction reaction kettle 1 to be 75-85 ℃ through a jacket, evaporating the hydrazine hydrate in the reaction process, condensing the evaporated hydrazine hydrate in a condenser 4, reducing the loss of the hydrazine hydrate, connecting a first condensing pipe 5 to the upper part of the condenser 4, connecting a second condensing pipe 8 to the lower part of the condenser 4, introducing normal-temperature tap water into the first condensing pipe 5 and the second condensing pipe 8, realizing the cooling of the hydrazine hydrate volatilized into the condenser 4, and continuously carrying out water bath reflux for 12 hours; the following reaction takes place in reduction reactor 1: hydrazine hydrate molecules react with epoxy groups in a graphene oxide structure in a nucleophilic substitution mode to enable the epoxy groups to generate an open loop reaction to form carbocations, oxygen anions capture hydrogen in the hydrazine molecules to form hydroxyl groups, the hydrazine molecules losing the hydrogen are combined with the carbocations, and then oxygen-containing functional groups in the structure are removed through an intramolecular condensation reaction, so that the graphene oxide is reduced; after the reduction reaction is finished, the material enters a primary centrifuge 6 from an outlet of a reduction reaction kettle 1 for centrifugation, alkali removal treatment is carried out by centrifugation, the rotating speed of the primary centrifuge 6 is controlled to be 19000r/min-25000r/min, then the material enters a secondary centrifuge 7 for further centrifugation and impurity removal, the rotating speed of the secondary centrifuge 7 is controlled to be 19000r/min-25000r/min, the centrifuged material enters a freeze dryer 9 through a feeding pipe 10 for drying, the drying temperature of the freeze dryer 9 is-70 ℃, the drying time is 70-80 hours, and graphene oxide powder is prepared after the drying is finished.
Claims (5)
1. A system for preparing graphene powder by a redox method is characterized in that: including reduction reation kettle (1), reduction reation kettle (1) upper portion links to each other with condenser (4), and reduction reation kettle (1) lower part passes through the pipeline and links to each other with one-level centrifuge (6), and one-level centrifuge (6) pass through the pipeline and link to each other with second grade centrifuge (7), and second grade centrifuge (7) pass through the pipeline and link to each other with freeze drier (9).
2. The system for preparing graphene powder according to claim 1, wherein: the upper feed inlet of the reduction reaction kettle (1) is respectively connected with a graphene oxide solution feed pipe (2) and a hydrazine hydrate feed pipe (3).
3. The system for preparing graphene powder according to claim 1, wherein: the upper part of the condenser (4) is connected with the first condensing pipe (5), and the lower part of the condenser (4) is connected with the second condensing pipe (8).
4. The system for preparing graphene powder according to claim 1, wherein: the rotating speed of the primary centrifuge (6) is 19000r/min-25000 r/min.
5. The system for preparing graphene powder according to claim 1, wherein: the rotation speed of the secondary centrifuge (7) is 19000r/min-25000 r/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921096656.2U CN210480876U (en) | 2019-07-12 | 2019-07-12 | System for preparing graphene powder by redox method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921096656.2U CN210480876U (en) | 2019-07-12 | 2019-07-12 | System for preparing graphene powder by redox method |
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| CN210480876U true CN210480876U (en) | 2020-05-08 |
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| CN201921096656.2U Active CN210480876U (en) | 2019-07-12 | 2019-07-12 | System for preparing graphene powder by redox method |
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Effective date of registration: 20210617 Address after: 255000 Gaocheng Town Industrial Park, Gaoqing County, Zibo City, Shandong Province Patentee after: SHANDONG HAIMAI NEW MATERIAL Co.,Ltd. Address before: 256301 Taiwan Industrial Park, Gaocheng Town, Gaoqing County, Zibo City, Shandong Province Patentee before: Zibo Lianke graphene Technology Service Center |
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