Method for fast synthesizing mesoporous solid acid catalyst immobilized with sulfonic acid

A solid acid catalyst and sulfonic acid-carrying technology, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve obstacles to popularization and application, high production costs, Complicated process and other issues, to achieve good reactivity, large immobilization capacity, and simple separation

Inactive Publication Date: 2012-12-12
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of many expensive organic reagents in the synthesis leads to high production costs, complicated processes and long time, which greatly hinders its popularization and application in industrial production.

Method used

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  • Method for fast synthesizing mesoporous solid acid catalyst immobilized with sulfonic acid
  • Method for fast synthesizing mesoporous solid acid catalyst immobilized with sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 1.0 g of SBA-15 mesoporous molecular sieve without template removal to 100 ml of sulfuric acid solution with a sulfuric acid mass fraction of 80%, heat the sulfuric acid solution to 190 ° C, stir for 3 h, cool to room temperature, suction filter, and wash until the filtrate is Neutral, the obtained solid is dried at 100°C; each gram of solid is extracted with 200ml ethanol for 24 hours, and dried at 100°C for 24 hours to obtain a mesoporous solid acid catalyst immobilized with sulfonic acid.

[0018] Catalytic effect: Add 0.20g of catalyst, 20ml of n-hexane as solvent, 100mmol of n-heptanal, 110mmol of ethylene glycol in a three-necked flask, reflux for 120min, the conversion rate of n-heptanal is 92%, and the selectivity of product acetal is 98%.

Embodiment 2

[0020] Add 5.0 g of SBA-15 mesoporous molecular sieves without template removal to 200 ml of sulfuric acid solution with a sulfuric acid mass fraction of 80%, heat the sulfuric acid solution to 190 ° C, stir for 3 h, cool to room temperature, suction filter, and wash until the filtrate is Neutral, the obtained solid is dried at 100°C; each gram of solid is extracted with 200ml of ethanol for 48 hours, and dried at 100°C for 36 hours to obtain a mesoporous solid acid catalyst immobilized with sulfonic acid.

[0021] Catalytic effect: Add 0.20g of catalyst, 20ml of n-hexane as solvent, 50mmol of n-heptanal, 55mmol of ethylene glycol in a three-necked flask, and reflux for 120min. The conversion rate of n-heptanal is 86%, and the selectivity of product acetal is 98%.

Embodiment 3

[0023] Add 10.0 g of SBA-15 mesoporous molecular sieves without template removal to 500 ml of sulfuric acid solution with a sulfuric acid mass fraction of 90%, heat the sulfuric acid solution to 195°C, stir for 4 hours, cool to room temperature, suction filter, and wash until the filtrate is Neutral, the obtained solid is dried at 100°C; each gram of solid is extracted with 200ml of ethanol for 48 hours, and dried at 100°C for 24 hours to obtain a mesoporous solid acid catalyst immobilized with sulfonic acid.

[0024] Catalytic effect: add catalyst 0.20g, 20ml n-hexane as solvent, 50mmol n-heptanal, 55mmol ethylene glycol in a three-necked flask, reflux for 120min, the conversion rate of n-heptanal is 82%, and the selectivity of product acetal is 98%.

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Abstract

The invention relates to a method for fast synthesizing a mesoporous solid acid catalyst immobilized with sulfonic acid, which comprises the following steps of: heating mesoporous molecular sieves with template agents, which are used as raw materials, in sulfuric acid solution with certain concentration so that the template agents in molecular sieve pore paths are carbonized and sulfonated; then,carrying out suction filtration, extraction and baking to obtain the mesoporous solid acid catalyst immobilized with the sulfonic acid. Compared with the tradiational mesoporous solid acid catalysts,the catalyst has simple preparation method and little time consumption. Sulfonic acid base groups are prepared through carbonizing and sulfonating the template agents, the use of expensive organic reagents is avoided, the production cost is greatly reduced, and the goal of waste utilization is also reached. In addition, the catalyst has orderly height distribution of the pore pathes, uniform porediameter and large specific surface area, is simple to separate and easy to store and shows good reaction activity when applied to the catalysis of aldolization.

Description

technical field [0001] The invention belongs to the technical field of new materials and catalysts, and relates to a method for rapidly synthesizing a mesoporous solid acid catalyst immobilized with sulfonic acid. Background technique [0002] Traditional liquid acids such as sulfuric acid, nitric acid, p-toluenesulfonic acid, and hydrochloric acid are frequently used as catalysts in many important organic reactions such as preparation of acetals, alkylation of aromatics, polymerization of olefins, cracking of hydrocarbons, and esterification. Among them, sulfuric acid is the most widely used. But the liquid acid catalyst itself also has some obvious defects. At present, the problems to be solved are as follows: 1. Liquid acid catalyst is difficult to separate from the product as a homogeneous catalyst, and the reuse of the catalyst is very difficult, resulting in acidic waste liquid polluting the environment; 2. Some liquid acids, such as concentrated sulfuric acid, have s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J35/10C07D317/12
Inventor 刘双喜杜斌张轩李金涛
Owner NANKAI UNIV
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