CN104817067B - A kind of preparation method of porous carbon - Google Patents
A kind of preparation method of porous carbon Download PDFInfo
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- CN104817067B CN104817067B CN201510273178.8A CN201510273178A CN104817067B CN 104817067 B CN104817067 B CN 104817067B CN 201510273178 A CN201510273178 A CN 201510273178A CN 104817067 B CN104817067 B CN 104817067B
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Abstract
The present invention relates to the preparation method of a kind of material with carbon element, the preparation method of a kind of porous carbon.Its process route is, is dispersed in the base material of high fluidity by modified graphene uniform, then is mixed with alkaline metal oxide by this base material, then carries out carbonization treatment, is washed out removing metal-oxide, then obtains porous carbon through high temperature graphitization process.The present invention mainly uses grapheme material modified to it, first forms support frame in base material, makes the mechanical strength that the porous carbon holding of formation is good, possesses higher specific surface area, relatively low resistivity and higher mesoporous.
Description
Technical field
The present invention relates to the preparation method of a kind of material with carbon element, the preparation method of a kind of porous carbon.
Background technology
The manufacture method of porous carbon, it is well known as cellulosics such as timber serosity, sawdust, Exocarpium cocois (Cocos nucifera L), rice husks, or paddy, barnyard grass, corn and other starches matter, the vegetable raw material of lignin etc., the mineral raw materials such as coal, tar, asphalt, and the synthetic resin such as phenolic resin, polyacrylonitrile etc. is as raw material, and under non-oxidizing atmosphere, it is heated the method making its carbonization, it is also known that there is use medicament that these carbides (activated carbon) are processed and make its method composing activation.
Summary of the invention
Technical barrier to be solved by this invention is to overcome the deficiencies in the prior art, it is provided that the preparation method of a kind of porous carbon.Use a kind of porous carbon materials of preparing of the present invention, can serve as the field such as electrode material of gas adsorption material, the negative material of nonaqueous electrolyte battery, capacitor, there is Research Prospects widely.
The technical solution of the present invention is, is dispersed in the base material of high fluidity by modified graphene uniform, and this base material mix with alkaline metal oxide and carries out carbonization treatment, washs removal metal-oxide, then obtains porous carbon through high temperature graphitization process.
Specifically comprise the following steps that
(1) modification of Graphene: Graphene is placed in plasma reaction chamber, first it is passed through high-purity argon gas 10～15min wherein, then pass to purity oxygen 2～10min, discharge process 3～10min under power 70～120W, obtain plasma-activated Graphene, and the plasma-activated Graphene obtained is placed in maleic anhydride xylene solvent carries out supersound process, finally under conditions of 120 DEG C～180 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active；
(2) preparation of mixture: by the base material of high fluidity, alkaline metal oxide is positioned in container with modified graphene mixs homogeneously；
(3) carbonization: the mixture of gained in step (2) is positioned in carbide furnace, carries out carbonization 1～5h under conditions of 1000～1200 DEG C and inert atmosphere or vacuum；
(4) with the product in detergent washing step (3), noncrystalline porous carbon is obtained；
(5) graphitization: be positioned in graphitizing furnace by amorphous porous carbon, carries out graphitization 1～8h under conditions of inert atmosphere and 2000 DEG C～2600 DEG C, obtains porous carbon；
Described high fluidity base material is imide series resin, or acrylic resin, or phenolic resin.
Described alkaline metal oxide is magnesium oxide, or calcium oxide, or calcium oxalate.
Detergent described in above-mentioned steps (4) is hydrochloric acid, or sulphuric acid, or formic acid.
The advantage that the present invention is compared with prior art possessed is:
(1) mechanical strength of porous carbon can be improved through modified Graphene and reduce resistivity；
(2) porous carbon that this technique is prepared possesses many layer structures, the advantage such as high mesoporosity and high-specific surface area.
Detailed description of the invention
Embodiment 1
First Graphene is placed in plasma reaction chamber, first it is passed through high-purity argon gas 10min wherein, it is passed through purity oxygen 2min, discharge process 3min under power 70W, obtain plasma-activated Graphene, and the plasma-activated Graphene obtained is placed in maleic anhydride xylene solvent carries out supersound process, under conditions of 120 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active.Then by 90 parts of polyimides, 10 parts of magnesium oxide and 5 parts of modified graphenes are positioned in container and carry out dry type mixing, then the mixture of gained is positioned in carbide furnace, carbonization 1h is carried out under conditions of 1000 DEG C and argon, with 4 parts of salt acid elution carbonized products, obtain noncrystalline porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under conditions of argon gas atmosphere and 2000 DEG C, carry out graphitization 1h, obtain porous carbon.
Embodiment 2
First Graphene is placed in plasma reaction chamber, first it is passed through high-purity argon gas 13min wherein, it is passed through purity oxygen 6min, discharge process 5min under power 90W, obtain plasma-activated Graphene, and the plasma-activated Graphene obtained is placed in maleic anhydride xylene solvent carries out supersound process, under conditions of 150 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active.Then by 100 parts of polyacrylic resins, 20 parts of calcium oxide and 8 parts of modified graphenes are positioned in container and carry out dry type mixing, then the mixture of gained is positioned in carbide furnace, carbonization 3h is carried out under conditions of 1100 DEG C and argon, with 7 parts of sulfuric acid scrubbing carbonized products, obtain noncrystalline porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under conditions of argon gas atmosphere and 2300 DEG C, carry out graphitization 5h, obtain porous carbon.
Embodiment 3
First Graphene is placed in plasma reaction chamber, first it is passed through high-purity argon gas 15min wherein, it is passed through purity oxygen 10min, discharge process 10min under power 120W, obtain plasma-activated Graphene, and the plasma-activated Graphene obtained is placed in maleic anhydride xylene solvent carries out supersound process, under conditions of 180 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active.Then by 120 parts of phenolic resin, 30 parts of calcium oxalates and 10 parts of modified graphenes are positioned in container and carry out dry type mixing, then the mixture of gained is positioned in carbide furnace, carbonization 5h is carried out under conditions of 1200 DEG C and argon, with 8 parts of formic acid washing carbonized products, obtain noncrystalline porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under conditions of argon gas atmosphere and 2600 DEG C, carry out graphitization 8h, obtain porous carbon.
Claims (3)
1. the preparation method of a porous carbon, it is characterised in that: uniformly being mixed with high fluidity base material, alkaline metal oxide by modified Graphene, after carbonization treatment, metal-oxide is removed in washing, then obtains porous carbon through high temperature graphitization process；Specifically comprise the following steps that
(1) modification of Graphene: Graphene is placed in plasma reaction chamber, first it is passed through high-purity argon gas 10～15min wherein, then pass to purity oxygen 2～10min, discharge process 3～10min under power 70～120W, obtain plasma-activated Graphene, and the plasma-activated Graphene obtained is placed in maleic anhydride xylene solvent carries out supersound process, finally under conditions of 120 DEG C～180 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active；
(2) preparation of mixture: high fluidity base material, alkaline metal oxide are positioned in container with modified graphene and uniformly mix；
(3) carbonization: the mixture of gained in step (2) is positioned in carbide furnace, carries out carbonization 1～5h under conditions of 1000～1200 DEG C and inert atmosphere or vacuum；
(4) washing: with the product in detergent washing step (3), obtain noncrystalline porous carbon；
(5) graphitization: be positioned in graphitizing furnace by amorphous porous carbon, carries out graphitization 1～8h under conditions of inert atmosphere and 2000 DEG C～2600 DEG C, obtains porous carbon；
Described high fluidity base material is imide series resin or acrylic resin or phenolic resin.
The preparation method of a kind of porous carbon the most as claimed in claim 1, it is characterised in that: described alkaline metal oxide is magnesium oxide or calcium oxide；Or with the alkaline metal oxide described in calcium oxalate replacement.
The preparation method of a kind of porous carbon the most as claimed in claim 1, it is characterised in that: the detergent described in step (4) is hydrochloric acid or sulphuric acid or formic acid.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017028301A1 (en) * | 2015-08-20 | 2017-02-23 | Robert Bosch Gmbh | Sulfur-carbon composite comprising carbon substrate and sulfur for lithium-sulfur batteries and process for preparing the same |
| CN106115694A (en) * | 2016-06-20 | 2016-11-16 | 山东欧铂新材料有限公司 | The preparation method of a kind of composite type pitch matrix activated carbon and ultracapacitor |
| CN106673657A (en) * | 2016-12-30 | 2017-05-17 | 苏州高通新材料科技有限公司 | Special carbon material and production method thereof |
| EP4331720A3 (en) | 2018-06-29 | 2024-07-24 | Toyo Tanso Co., Ltd. | Method for producing porous carbon, and electrode and catalyst support containing porous carbon produced by said production method |
| CN109368620A (en) * | 2018-12-11 | 2019-02-22 | 中国科学院兰州化学物理研究所 | A kind of preparation method of extra small sub-nanometer hole porous graphene |
| JP7137713B2 (en) * | 2019-09-12 | 2022-09-14 | 株式会社カネカ | Surface layer porous graphite sheet |
| CN118702098A (en) * | 2024-08-28 | 2024-09-27 | 合肥工业大学 | Porous carbon material and preparation method and application thereof |
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Address after: Room j653, building 6, 1288 Yecheng Road, Jiading District, Shanghai, 201822 Patentee after: Zhongke Yueda (Shanghai) material technology Co.,Ltd. Address before: 201822 J3330 room 912, Yecheng Road, Jiading Industrial Zone, Jiading District, Shanghai. Patentee before: Shanghai Ewang Material Technology Co.,Ltd. |
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