Method for preparing mesopore-micropore composite porous carbon on basis of vinylidene chloride polymers

A technology of vinylidene chloride and partial vinylidene chloride, which is applied in the field of preparation of porous carbon materials to achieve the effects of narrow pore size distribution, good application prospects and good correspondence

Active Publication Date: 2012-12-05
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Deng et al. (Chemistry of Materials, 2008, 20(23): 7281-7286) used the ATRP method to prepare polyethylene glycol-polyacrylonitrile block copolymers. The carbonization of acrylonitrile, adjusting the ratio of pyrolysis segment and carbon source segment in the block, has successfully prepared mesoporous carbon with a pore size of 20nm~90nm and a single size; but it has not yet been prepared by RAFT polymerization from vinylidene chloride ( Block copolymers composed of co)polymers and PEG and reports on the preparation of porous carbons from block copolymers

Method used

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  • Method for preparing mesopore-micropore composite porous carbon on basis of vinylidene chloride polymers
  • Method for preparing mesopore-micropore composite porous carbon on basis of vinylidene chloride polymers
  • Method for preparing mesopore-micropore composite porous carbon on basis of vinylidene chloride polymers

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preparation example Construction

[0024] The steps of a preparation method of a vinylidene chloride polymer-based mesopore-microporous composite porous carbon are as follows:

[0025]1) Add 50-100 parts by mass of 1,4-dioxane, 5-20 parts by mass of vinylidene chloride, 2-7 parts by mass of polyethylene glycol-based macromolecular RAFT reagent, 0.016-0.16 parts by mass Azobisisobutyronitrile, stir at room temperature for 10-30 minutes to dissolve and mix the reactants, pass nitrogen to remove oxygen, heat to 60-70°C, and polymerize for 18-24 hours; add a precipitant to the reaction solution, precipitate, separate, and dry Obtain a block copolymer composed of vinylidene chloride (co)polymer and polyethylene glycol;

[0026] 2) Put the prepared block copolymer of vinylidene chloride (co)polymer and polyethylene glycol into a crucible, put it into a high-temperature furnace, and first pass a protective inert gas into the high-temperature furnace for 30-60 minutes, and take 2 ℃ / min~10℃ / min to raise the temperature...

Embodiment 1

[0032] Add 0.007mol of polyethylene glycol with a molecular weight of 2000 and 0.0156mol of S-1-dodecyl-S'-(α,α'-dimethyl-α''-acetic acid) trithiocarbonate Reactor, use 1.1mol of dichloromethane as solvent, stir and disperse, then add 0.003mol of catalyst 4-dimethylaminopyridine, continue to stir and disperse evenly, then add 0.0155mol of water remover dicyclohexylcarbodiimide, 25℃ Stirring and reacting for 24 hours, the product was precipitated and filtered, and the precipitated solid was dissolved with dichloromethane and precipitated with petroleum ether. This operation was repeated three times, and finally the product was dried to obtain a macromolecular RAFT chain transfer agent.

[0033] 2 grams of modified polyethylene glycol 2000 macromolecule RAFT chain transfer agent, 0.015 grams of azobisisobutyronitrile, 10.8 grams of vinylidene chloride and 1.2 grams of methyl acrylate were added to a 200 milliliter reactor, and then Add 100 ml of reaction solvent 1,4-dioxane, sti...

Embodiment 2

[0036] Add 0.007mol of polyethylene glycol with a molecular weight of 6000 and 0.0156mol of S-1-dodecyl-S'-(α,α'-dimethyl-α''-acetic acid) trithiocarbonate Reactor, use 0.91mol of dichloromethane as solvent, stir and disperse, then add 0.003mol of catalyst 4-dimethylaminopyridine, continue to stir and disperse evenly, add 0.0155mol of water remover dicyclohexylcarbodiimide, 25℃ Stirring and reacting for 48 hours, the product was precipitated and filtered, and the precipitated solid was dissolved with dichloromethane and precipitated with petroleum ether. This operation was repeated three times, and finally the product was dried to obtain a macromolecular RAFT chain transfer agent.

[0037] 6.4 gram of modified polyethylene glycol 6000 macromolecule RAFT chain transfer agent, 0.015 gram of azobisisobutyronitrile, 10.8 gram of vinylidene chloride and 1.2 gram of methyl acrylate are added to 200 milliliters of autoclave, and then Add 100 ml of reaction solvent 1,4-dioxane, stir a...

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Abstract

The invention discloses a method for preparing mesopore-micropore composite porous carbon on the basis of vinylidene chloride. The method includes steps of 1), adding 1,4-dioxane, vinylidene chloride, polyethylene-glycol-based macromolecular RAFT (reversible addition-fragmentation transfer) reagents and azodiisobutyronitrile into a reaction kettle, stirring the reactants at the room temperature to dissolve and mix the reactants together, charging nitrogen, removing oxygen, heating the mixture, enabling the reactants to have polymerization reaction to generate reaction liquid, adding precipitating agents into the reaction liquid, depositing the reaction liquid to obtain deposits, separating the deposits and drying the separated deposits to obtain segmented copolymers comprising vinylidene chloride polymers (copolymers) and polyethylene glycol; and 2), placing the segmented copolymers into a crucible, placing the crucible in a high-temperature furnace, heating the high-temperature furnace, keeping the temperature of the high-temperature furnace constant, and then slowly reducing the temperature of the high-temperature furnace to reach the constant temperature so as to obtain the mesopore-micropore composite porous carbon. The method is simple, a synthetic carbon precursor structure effectively corresponds to a porous carbon material structure, and the mesopore-micropore composite porous carbon has a mesopore-micropore aperture structure with narrow aperture distribution, and has a good application prospect in fields such as electrodes of super-capacitors, gas adsorption and industrial catalysis.

Description

technical field [0001] The invention relates to a preparation method of a porous carbon material, in particular to a preparation method of a vinylidene chloride polymer-based mesopore-micropore composite porous carbon. Background technique [0002] Porous carbon is a carbon material with rich pore structure, large specific surface area, stable physical and chemical properties, high temperature resistance, and recyclability. It is widely used in battery electrode materials, supercapacitors (EDLC), gas storage and Separation of adsorbents and catalyst supports, etc. In recent years, the research on porous carbon materials mainly focuses on the improvement of the existing porous carbon preparation technology and the development of new porous carbon preparation technology. According to the size of the pores, the International Union of Fine Applied Chemistry (IUPAC) classified the pores of porous carbon as follows: macropores >50nm, mesopores 2-50nm, micropores <2nm. Trad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 杨杰包永忠
Owner ZHEJIANG UNIV
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