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

A solid acid catalyst, a technology for carrying sulfonic acid, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the obstacles to popularization and application, high production cost, Complex process and other problems, to achieve the effects of good reactivity, large immobilization capacity and simple separation

Inactive Publication Date: 2011-04-20
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
  • Method for fast synthesizing mesoporous solid acid catalyst immobilized with sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 1.0g of SBA-15 mesoporous molecular sieve without removing template agent to 100ml sulfuric acid solution with 80% sulfuric acid mass fraction. Heat the sulfuric acid solution to 190℃, stir for 3h, cool to room temperature, filter with suction, 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 24h and dried at 100°C for 24h to obtain a mesoporous solid acid catalyst supported by sulfonic acid.

[0018] Catalytic effect: Add 0.20 g of catalyst, 20 ml of n-hexane as solvent, 100 mmol n-heptanal, 110 mmol ethylene glycol, reflux for 120 min in a three-necked flask, 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 sieve without removing the template agent to 200 ml of sulfuric acid solution with 80% sulfuric acid mass fraction. The sulfuric acid solution is heated to 190°C, stirred for 3 hours, cooled to room temperature, filtered with suction, and washed until the filtrate is Neutral, the obtained solid is dried at 100°C; each gram of solid is extracted with 200ml ethanol for 48h and dried at 100°C for 36h to obtain a mesoporous solid acid catalyst supported by sulfonic acid.

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

Embodiment 3

[0023] Add 10.0g of SBA-15 mesoporous molecular sieve without removing template agent to 500ml sulfuric acid solution with 90% sulfuric acid mass fraction. Heat the sulfuric acid solution to 195℃, stir for 4h, cool to room temperature, filter with suction, 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 48h and dried at 100°C for 24h to obtain a mesoporous solid acid catalyst supporting sulfonic acid.

[0024] Catalytic effect: Add 0.20 g of catalyst, 20 ml of n-hexane as solvent, 50 mmol n-heptanal, 55 mmol ethylene glycol, reflux for 120 min in a three-necked flask, 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 supporting 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 the preparation of acetals, aromatic alkylation, olefin polymerization, hydrocarbon cracking and esterification. Among them, sulfuric acid is the most widely used. However, the liquid acid catalyst itself has some obvious defects. At present, the problems that need to be solved are as follows: 1. Liquid acid catalyst is difficult to separate from the product as a homogeneous catalyst, and it is very difficult to reuse the catalyst, resulting in acidic waste liquid polluting the environment; 2. Some liquid acids, such as concentrated sulfuric acid, have strong oxidi...

Claims

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Application Information

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Patent Type & Authority Applications(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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