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Preparation method of porous polymer

A technology of a porous polymer and a synthesis method is applied in the field of the preparation of porous polymers to achieve the effects of low cost of raw materials, strong hydrogen storage capacity and short time.

Active Publication Date: 2015-04-29
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, hydrogen storage methods mainly include gaseous compressed hydrogen storage, liquefied hydrogen storage, glass microsphere hydrogen storage, and porous material adsorption hydrogen storage. Among them, gaseous compressed hydrogen storage and liquefied hydrogen storage are more traditional hydrogen storage methods, but considering storage costs And storage conditions and other factors, the application of these two hydrogen storage methods is subject to certain limitations, and there are still certain defects in the technology of glass microsphere hydrogen storage. However, due to factors such as economy, safety and reliability, and storage efficiency, porous materials currently on the market for hydrogen adsorption and storage cannot be applied industrially.

Method used

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  • Preparation method of porous polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: the synthesis of MDI trimer

[0019] Mix 44.4g of MDI monomer (MDI is 4,4'-diphenylmethane diisocyanate) with 50mL of toluene, turn on the stirrer, and add 2,4,6-tris(dimethylamino Methyl) phenol, when the molar content of isocyanate is 8% at 60°C, add polymerization inhibitor benzoyl chloride, and react at constant temperature for 30 minutes, cool, filter, rinse with toluene to remove MDI monomer and catalyzer, obtain MDI trimer, the mass addition of described 2,4,6-tris(dimethylaminomethyl)phenol, benzoyl chloride is respectively 0.05%, 0.05% of MDI monomer , wherein, the molar content of isocyanate in the reactant is determined by di-n-butylamine titration.

Embodiment 2

[0020] Example 2: Synthesis of Porous Polymers

[0021] 1) Weigh 1.44g of melamine and 30mL of dimethyl sulfoxide (DMSO for English abbreviation) and mix, turn on the stirrer, and after dissolving, add 1g of MDI trimer, react at 180°C for 24h, and filter with suction. Rinse the sample with acetone for 3 times, and then dry it for 24 hours at a temperature of 180°C and a vacuum of -0.1MPa to obtain the intermediate product;

[0022] 2) Put the intermediate product in chloroform, and reflux at 70°C for 12 hours to form a porous polymer. After testing, the specific surface area of ​​the porous polymer is 144m 2 / g, the micropore volume accounts for 12.5% ​​of the total pore volume, the most probable pore diameter in the micropore is 0.88nm, the hydrogen adsorption capacity under the conditions of 77K and 1.5MPa is 0.13wt%, and when the maximum constant volume pressure is 7MPa, The hydrogen adsorption amount under the condition of 5.1MPa is 8.6wt%.

Embodiment 3

[0023] Example 3: Synthesis of Porous Polymers

[0024] 1) Weigh 1.8g of melamine and 30mL of dimethyl sulfoxide and mix it, turn on the stirrer, after dissolving, add 1g of MDI trimer, react at 180°C for 24h, filter with suction, and rinse the sample with acetone for 3 times , and then dried for 24 hours at a temperature of 180°C and a vacuum of -0.1MPa to obtain the medium product;

[0025] 2) Put the intermediate product in chloroform, and reflux at 70°C for 12 hours to form a porous polymer. After testing, the specific surface area of ​​the porous polymer is 276m 2 / g, the micropore volume accounts for 18.3% of the total pore volume, the most probable pore diameters in the micropores are 0.85nm, the hydrogen adsorption capacity under the conditions of 77K and 1.5MPa is 0.95wt%, and the maximum constant volume pressure is 7MPa , the hydrogen adsorption amount under the equilibrium condition of 5.8MPa is 5.8wt%.

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Abstract

The invention belongs to the technical field of chemical industry, and particularly discloses a preparation method of a porous polymer for adsorbing hydrogen. The method comprises the following steps: a) weighing melamine and an aprotic polar solvent, mixing, stirring, dissolving, adding an MDI tripolymer (namely 4,4'-diphenyl-methane-diisocyanate tripolymer), reacting at 150-190 DEG C for 18-36 hours, carrying out suction filtration, washing a sample with acetone, and drying to obtain an intermediate product; and b) putting the intermediate product into a solvent, and refluxing at 40-80 DEG C for 10-15 hours, so as to obtain the porous polymer. The method disclosed by the invention has the advantages of low cost of raw materials for preparing a hydrogen storage material, simple process and short time; the technological conditions are easy to control; the prepared porous polymer can adsorb a great amount of hydrogen under high pressure; through detection, the specific surface area of the porous polymer can be up to 270m<2> / g; the micropore volume accounts for 12%-20% of total pore volume; when the maximal constant volume pressure is 7MPa, the adsorbing capacity of the porous polymer prepared by the method on hydrogen can be up to 8wt%; and the hydrogen storage capacity is high.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of a porous polymer used for absorbing hydrogen. Background technique [0002] With the development of society and the increasing seriousness of environmental problems, the research on clean and renewable energy has been widely concerned by people. Hydrogen is a renewable energy source with a wide range of uses. It is stable at room temperature, but it can chemically react with many substances under ignited or heated conditions. Therefore, how to ensure the safe and effective storage of hydrogen when using hydrogen is an important issue. It is a question that must be considered. [0003] At present, hydrogen storage methods mainly include gaseous compressed hydrogen storage, liquefied hydrogen storage, glass microsphere hydrogen storage, and porous material adsorption hydrogen storage. Among them, gaseous compressed hydrogen storage and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/79C08G18/32C08J9/28B01J20/26C01B3/56C08G101/00
CPCB01J20/262C01B3/56C08G18/092C08G18/3851C08G18/794C08J9/286C08J2375/04
Inventor 刘瑾张景肖胜宝李真
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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