Technology for synthesizing glycol dibenzenesulfonate from nano-solid alkali catalyst

A technology of ethylene glycol dibenzenesulfonate and solid base catalyst, which is applied in the direction of physical/chemical process catalyst, sulfonate ester preparation, metal/metal oxide/metal hydroxide catalyst, etc., and can solve the problem of glycol diphenylsulfonate The sulfonate process route is complex and the yield is not good, etc., to achieve the effects of easy acquisition, reduced side reactions, and simple operation

Inactive Publication Date: 2017-04-26
盐城市胜达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the process route of synthesizing glycol dibenzene

Method used

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  • Technology for synthesizing glycol dibenzenesulfonate from nano-solid alkali catalyst
  • Technology for synthesizing glycol dibenzenesulfonate from nano-solid alkali catalyst

Examples

Experimental program
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Embodiment 1

[0021] Cesium-modified nano-scale Ti / Al composite solid base catalyst, the preparation process is as follows:

[0022] Step 1. Treat alumina and titanium dioxide under ultrasonic waves for 2 hours;

[0023] Step 2, then calcining treatment: first calcining in air at 500°C and 0.2kpa for 4h, then calcining in nitrogen at 600°C and 0.4kpa for 3h;

[0024] Step 3, after the calcination, purging under helium atmosphere for 3h;

[0025] Step 4, then introduce cesium element by impregnation method: mix 10g of alumina and 5g of titanium dioxide in a mass ratio of 2:1, and then immerse in 0.5mol / L Cs2CO3 solution for 12h;

[0026] Step 5, then use hot alkali treatment, treat it under hot air at 180°C for 2h, then soak it in 5% sodium hydroxide solution for 5h, and then transfer it to a beaker;

[0027] Step 6. Perform coupling treatment: add 0.05mol coupling agent kh500 dropwise to the mixture after hot alkali treatment, and magnetically stir while adding;

[0028] Step 7, adding 0...

Embodiment 2

[0037] Example 2 Prepare glycol, benzenesulfonyl chloride, and self-made cesium-modified nano-scale Ti / Al composite solid base catalyst with a mass ratio of 26:100:0.5. Glycol 26g, benzenesulfonyl chloride 100g, self-made cesium-modified nano-scale Ti / Al composite solid base catalyst 0.5g. Pyridine 1.1mol, chloroform 160ml. The operation steps are the same as in Example 1.

Embodiment 3

[0038] Example 3 Prepare glycol, benzenesulfonyl chloride, and self-made cesium-modified nano-scale Ti / Al composite solid base catalyst with a mass ratio of 18:105:0.5. Glycol 18g, benzenesulfonyl chloride 105g, self-made cesium-modified nano-scale Ti / Al composite solid base catalyst 0.5g. Other raw materials, operation steps are the same with embodiment 1.

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Abstract

The invention discloses a technology for synthesizing glycol dibenzenesulfonate from a nano-solid alkali catalyst. Glycol dibenzenesulfonate is prepared from raw materials including glycol, pyridine, benzene sulfonyl chloride, the home-made caesium modified nano-scale Ti/Al composite solid alkali catalyst and the like through operating means including ice-water bath, reduced-pressure distillation, magnetic stirring and the like.

Description

technical field [0001] The invention relates to a process for synthesizing ethylene glycol dibenzenesulfonate through a nanometer solid base catalyst, which belongs to the field of organic synthesis. Background technique [0002] Since Pedersen discovered the first crown ether compound in 1967, the research and development of macrocyclic polyether compounds has developed rapidly. People's in-depth research on its specific structure and complexing properties not only created new fields of "crown ether chemistry", "host-guest chemistry" and "supramolecular chemistry" for organic chemistry, but also a large number of crown ethers with different functions and their functions Derivatives are synthesized. One of the most commonly used intermediates for crown ethers is polyethylene glycol dibenzenesulfonate. At present, the process route of synthesizing glycol dibenzenesulfonate is relatively complicated, and the yield is not good. I have invented a process for synthesizing ethy...

Claims

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Application Information

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IPC IPC(8): C07C303/28C07C309/73B01J23/04B01J21/06B01J21/04
CPCY02P20/584C07C303/28B01J21/04B01J21/063B01J23/04C07C309/73
Inventor 吴思敏刘威远
Owner 盐城市胜达化工有限公司
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