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Application of organic framework porous solid acid

A porous solid and organic framework technology, applied in the preparation of organic compounds, organic chemistry, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of lack of pore structure, low specific surface area, poor stability, etc.

Active Publication Date: 2013-01-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its low specific surface area, poor pore structure, and poorly stable framework structure limit its wide application.

Method used

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  • Application of organic framework porous solid acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] First, tetrahydrofuran and water are used as a mixed solvent to synthesize the mesoporous polydivinylbenzene material, which is PDVB.

[0020] Add 2g of DVB monomer to a mixed solvent containing 0.03-0.05g of azobisisobutyronitrile, 10-20ml of tetrahydrofuran, 1-2ml of water, and stir at room temperature and pressure for more than 3 hours, then 75-150°C water After heat treatment for 1-2 days, take it out, open the lid, and evaporate the dry solvent at room temperature to obtain a polydivinylbenzene material (PDVB) with high specific surface area and rich mesoporous structure.

Embodiment 2

[0022] Choose dichloromethane as the solvent and concentrated sulfuric acid as the sulfonation reagent for the sulfonation reaction.

[0023] (1) Grind 2-3g PDVB into ultrafine powder, and degas it under nitrogen at 100-150℃ for 10h;

[0024] (2) Swelling process: Adding 2.0 g of PDVB block to an excessive amount of solvent, the PDVB material quickly swells, and the PDVB quickly bursts into small pieces, accompanied by rapid volume expansion.

[0025] (3) Take 30mL of dichloromethane and 70mL of concentrated sulfuric acid and mix well, add 0.2g of silver sulfate as a catalyst. After stirring evenly, add the above PDVB, stir vigorously, and raise the temperature to 90℃ for 12h to complete the reaction and filter the product. Wash with dioxane, wash with water to neutral, dry at 80°C, activate with 0.1M sulfuric acid for 4 hours, wash with plenty of water to neutral, dry, and set aside.

Embodiment 3

[0027] Catalytic performance evaluation and its comparison with traditional catalytic materials

[0028] Esterification reaction conditions of acetic acid and cyclohexanol: 0.2g catalyst, 11.5mL cyclohexanol, 17.5mL glacial acetic acid were mixed uniformly, and the reaction was completed at 100°C for 5 hours, dodecane was used as the internal standard.

[0029] Esterification reaction conditions of n-hexanoic acid and ethanol: 0.3g catalyst, 6.26mL n-hexanoic acid, 11.67mL ethanol are mixed uniformly, and the reaction is completed at 80°C for 5h, dodecane is the internal standard.

[0030] The esterification reaction conditions of dodecanoic acid and ethanol: 0.15g catalyst, 4mmol dodecanoic acid, and 50mmol ethanol were mixed uniformly and the reaction was completed at 70°C for 5h, and dodecane was used as the internal standard.

[0031] Fuchs acylation reaction: 0.3g catalyst, 5.5mL anisole, 0.71mL acetyl chloride are mixed uniformly, and the reaction is completed at 60°C for 5h, dod...

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Abstract

The invention relates to application of organic framework porous solid acid. A catalyst for catalytic esterification and acylation reaction is prepared by the steps of adding a divinyl benzene monomer into a solvent prepared by mixing azobisisobutyronitrile, tetrahydrofuran and water, performing hydro-thermal treatment at the normal temperature under the constant pressure, and volatilizing the solvent at the room temperature to obtain polydivinylbenzene; grinding the polydivinylbenzene into 200-mesh powder and performing degassing treatment under the nitrogen condition; adding polydivinylbenzene blocks into 1,1',2-methyl chloroform to explode and crack into small blocks, wherein the small blocks swell; evenly mixing 1,1',2-methyl chloroform and concentrated sulfuric acid, adding silver sulfate serving as a catalyst, adding processed polydivinylbenzene, performing sulfonation, filtering and dioxane washing till a solution is neutral, performing drying, using dilute sulphuric acid to activate, performing washing till the solution is neutral and performing drying. The catalyst is used for the catalytic esterification and the acylation reaction and has high catalytic activity and conversion rate.

Description

Technical field [0001] The invention relates to the application of an organic framework porous solid acid. Background technique [0002] With the development of the chemical industry, solid acid catalysts have been widely used, especially in the petrochemical and fine chemical fields. Traditional acid catalysts include zeolite molecular sieves, sulfurized metal oxides, and acid-functionalized mesoporous materials. Heteropoly acids, etc., but their shortcomings such as hydrophilic framework structure and pore size limitation of zeolite materials have affected the wide application of inorganic solid acid materials. Compared with traditional inorganic framework acid catalysts, pure organic framework solid acid materials have received more and more extensive research due to their unique framework hydrophobic properties, simple and convenient functionalization process, and better catalytic performance. [0003] U.S. Patent: B01J31 / 10; B01J47 / 00; C07C37 / 20, etc., have published a strong...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10B01J35/10C08F112/36C08F8/36C08J9/28C07C67/08C07C69/14C07C69/24C07C45/46C07C49/84
CPCC07C49/84C07C45/65B01J35/023B01J35/10C08F112/36B01J37/0036C07C67/08B01J27/055C07C69/14C07C45/46C07C69/24B01J37/10C08J9/28C08F8/36B01J31/10C07C2601/14B01J35/40
Inventor 李文鹏肖丰收肖海成刘福建李影辉孟祥举徐显明郁向民徐可忠张伟宋国权裴皓天李方伟曾群英张志翔李月满
Owner PETROCHINA CO LTD
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