CN104817067A - Preparation method of porous carbon - Google Patents
Preparation method of porous carbon Download PDFInfo
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- CN104817067A CN104817067A CN201510273178.8A CN201510273178A CN104817067A CN 104817067 A CN104817067 A CN 104817067A CN 201510273178 A CN201510273178 A CN 201510273178A CN 104817067 A CN104817067 A CN 104817067A
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Abstract
The invention relates to a preparation method of a carbon material, particularly a preparation method of porous carbon. The preparation method comprises the following steps: uniformly dispersing modified graphene in a high-flowability substrate, mixing the substrate with alkali metal oxide, carrying out carbonization, washing to remove the metal oxide, and carrying out high-temperature graphitization to obtain the porous carbon. The novel material graphene is mainly utilized for modification to firstly form a support framework in the substrate, so that the formed porous carbon maintains favorable mechanical strength and has the advantages of higher specific area, lower resistivity and higher mesopore rate.
Description
Technical field
The present invention relates to a kind of preparation method of carbon material, particularly a kind of preparation method of porous carbon.
Background technology
The manufacture method of porous carbon, by cellulosics such as timber slurries, sawdust, Exocarpium cocois (Cocos nucifera L), rice husks as everyone knows, or paddy, barnyard grass, corn and other starches matter, the vegetable raw material of xylogen etc., the mineral raw materials such as coal, tar, petroleum pitch, and the synthetic resins such as resol, polyacrylonitrile etc. is as raw material, and under non-oxidizing atmosphere, the method making its carbonization is heated to it, in addition, also there will be a known and make with medicament process these carbide (activated carbon) and make it compose the method for activation.
Summary of the invention
Technical barrier to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of preparation method of porous carbon.The novel porous carbon material of one adopting the present invention to prepare, can be used as the field such as the negative material of gas adsorption material, nonaqueous electrolyte battery, the electrode materials of electrical condenser, have Research Prospects widely.
Technical solution of the present invention is, is dispersed in the base material of high workability by the graphene uniform of modification, and this base material mixes with alkaline metal oxide and carries out carbonizing treatment, and metal oxide is removed in washing, then obtains porous carbon through high temperature graphitization process.
Concrete steps are as follows:
(1) modification of Graphene: Graphene is placed in plasma reaction chamber, first pass into high-purity argon gas 10 ~ 15min wherein, then purity oxygen 2 ~ 10min is passed into, 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 the condition 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 workability, alkaline metal oxide is positioned in container with modified graphene and mixes;
(3) carbonization: be positioned in carbide furnace by the mixture of gained in step (2), carries out carbonization 1 ~ 5h under the condition of 1000 ~ 1200 DEG C and inert atmosphere or vacuum;
(4) with the product in detergent washing step (3), amorphousness porous carbon is obtained;
(5) greying: be positioned in graphitizing furnace by amorphous porous carbon, carries out greying 1 ~ 8h, obtains porous carbon under the condition of inert atmosphere and 2000 DEG C ~ 2600 DEG C;
Described high workability base material is imide series resin, or acrylic resin, or resol.
Described alkaline metal oxide is magnesium oxide, or calcium oxide, or caoxalate.
Washing composition described in above-mentioned steps (4) is hydrochloric acid, or sulfuric acid, or formic acid.
The advantage that the present invention is compared with prior art possessed is:
(1) Graphene through modification can improve the physical strength of porous carbon and reduce resistivity;
(2) porous carbon that this technique is prepared possesses many laminate structures, the advantage such as high mesoporosity and high-specific surface area.
Embodiment
Embodiment 1
First Graphene is placed in plasma reaction chamber, first pass into high-purity argon gas 10min wherein, pass into 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 the condition of 120 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active.Then by 90 parts of polyimide, 10 parts of magnesium oxide and 5 parts of modified graphenes are positioned in container and carry out dry type and mix, then the mixture of gained is positioned in carbide furnace, carbonization 1h is carried out under the condition of 1000 DEG C and argon gas, with 4 parts of salt acid elution carbonized products, obtain amorphousness porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under the condition of argon gas atmosphere and 2000 DEG C, carry out greying 1h, obtain porous carbon.
Embodiment 2
First Graphene is placed in plasma reaction chamber, first pass into high-purity argon gas 13min wherein, pass into 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 the condition 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 and mix, then the mixture of gained is positioned in carbide furnace, carbonization 3h is carried out under the condition of 1100 DEG C and argon gas, with 7 parts of sulfuric acid scrubbing carbonized products, obtain amorphousness porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under the condition of argon gas atmosphere and 2300 DEG C, carry out greying 5h, obtain porous carbon.
Embodiment 3
First Graphene is placed in plasma reaction chamber, first pass into high-purity argon gas 15min wherein, pass into 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 the condition of 180 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active.Then by 120 parts of resol, 30 parts of caoxalates and 10 parts of modified graphenes are positioned in container and carry out dry type and mix, then the mixture of gained is positioned in carbide furnace, carbonization 5h is carried out under the condition of 1200 DEG C and argon gas, with 8 parts of formic acid washing carbonized products, obtain amorphousness porous carbon, finally amorphous porous carbon is positioned in graphitizing furnace, under the condition of argon gas atmosphere and 2600 DEG C, carry out greying 8h, obtain porous carbon.
Claims (5)
1. a preparation method for porous carbon, is characterized in that: by the Graphene of modification and high workability base material, alkaline metal oxide Homogeneous phase mixing, after carbonizing treatment, and metal oxide is removed in washing, then obtains porous carbon through high temperature graphitization process.
2. the preparation method of a kind of porous carbon as claimed in claim 1, it is characterized in that, concrete steps are as follows:
(1) modification of Graphene: Graphene is placed in plasma reaction chamber, first pass into high-purity argon gas 10 ~ 15min wherein, then purity oxygen 2 ~ 10min is passed into, 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 the condition of 120 DEG C ~ 180 DEG C, carry out grafted maleic anhydride, obtain the Graphene of surface active;
(2) preparation of mixture: high workability base material, alkaline metal oxide and modified graphene are positioned in container and carry out Homogeneous phase mixing;
(3) carbonization: be positioned in carbide furnace by the mixture of gained in step (2), carries out carbonization 1 ~ 5h under the condition of 1000 ~ 1200 DEG C and inert atmosphere or vacuum;
(4) wash: with the product in detergent washing step (3), obtain amorphousness porous carbon;
(5) greying: be positioned in graphitizing furnace by amorphous porous carbon, carries out greying 1 ~ 8h, obtains porous carbon under the condition of inert atmosphere and 2000 DEG C ~ 2600 DEG C.
3. the preparation method of a kind of porous carbon as described in claim 1 or 2, is characterized in that: described high workability base material is imide series resin or acrylic resin or resol.
4. the preparation method of a kind of porous carbon as described in claim 1 or 2, is characterized in that: described alkaline metal oxide is magnesium oxide or calcium oxide or caoxalate.
5. the preparation method of a kind of porous carbon as described in claim 2, is characterized in that the washings described in step (4) is hydrochloric acid or sulfuric acid or formic acid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| 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 |
| CN111344254A (en) * | 2018-06-29 | 2020-06-26 | 东洋炭素株式会社 | Method for producing porous carbon, and electrode and catalyst carrier comprising porous carbon produced by the production method |
-
2015
- 2015-05-26 CN CN201510273178.8A patent/CN104817067B/en active Active
Cited By (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 |
| CN111344254A (en) * | 2018-06-29 | 2020-06-26 | 东洋炭素株式会社 | Method for producing porous carbon, and electrode and catalyst carrier comprising porous carbon produced by the production method |
| US11235978B2 (en) | 2018-06-29 | 2022-02-01 | Toyo Tanso Co., Ltd. | Method of producing porous carbon, and electrode and catalyst carrier containing porous carbon produced by the method |
| US11702344B2 (en) | 2018-06-29 | 2023-07-18 | Toyo Tanso Co., Ltd. | Method of producing porous carbon, and electrode and catalyst carrier containing porous carbon produced by the 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 |
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| CN104817067B (en) | 2016-09-21 |
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Effective date of registration: 20170602 Address after: 201209, A252, building 1, building 2588, Golden Sea Road, Shanghai, Pudong New Area Patentee after: Shanghai Yueda New Material Technology Co., Ltd. Address before: 224007 Yancheng City economic and Technological Development Zone, East Ring Road, Jiangsu, No. 69 Patentee before: Jiangsu Yueda novel material Science and Technology Ltd. |
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Effective date of registration: 20180523 Address after: 201822 J3330 room 912, Yecheng Road, Jiading Industrial Zone, Jiading District, Shanghai. Patentee after: Shanghai Mstar Technology Ltd Address before: 201209 room 1, building 1, Jinhai Road, Pudong New Area, Shanghai, A252 Patentee before: Shanghai Yueda New Material Technology Co., Ltd. |
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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. |