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Benzenesulfonic acid catalyst supported on silica gel, as well as preparation and application thereof

A technology of benzenesulfonic acid and catalyst, which is applied in the field of preparation of silica gel-supported benzenesulfonic acid catalyst, can solve the problems of unstable catalyst and easy hydrolysis, does not meet environmental protection requirements, cannot be recycled, etc., and achieves stable and efficient catalytic activity and cost. Low, easy to recycle effect

Inactive Publication Date: 2012-01-04
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the Claisen rearrangement reaction often uses Lewis acids such as boron trichloride, aluminum trichloride, titanium tetrachloride, tin tetrachloride and Bronsted acids such as sulfuric acid and trifluoroacetic acid as catalysts. Stable and easy to hydrolyze, some are highly corrosive, and they are difficult to separate from the system after the reaction, and they cannot be recycled, which does not meet environmental protection requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment one, the preparation of silica gel immobilized benzenesulfonic acid

[0029] Preparation of silica gel chloride: Weigh 5 g of macroporous silica gel, place it in a muffle furnace, dry it at 120°C for 8 h, and then add it to a reactor equipped with a reflux condenser and a drying tube; add 10 mL of thionyl chloride was refluxed in an oil bath at 80°C for 24 h, the color of the system turned yellow during the reaction, and the color continued to deepen as time went by. After the reaction was completed, it was filtered, and the obtained solid product was fully washed three times with dichloromethane. After removing the solvent, it was dried in a vacuum oven at 60° C. for 10 h to obtain 5.3 g of a light yellow solid product. According to the analysis and calculation, the solid loading capacity of Cl in silica gel chloride is 2.43 mmol / g.

[0030] Preparation of silica gel-supported benzene: Add silica gel chloride (5.3 g, 0.013 mol of immobilized chlorine) and p...

Embodiment 2

[0032] Embodiment two, the preparation of silica gel immobilized benzenesulfonic acid

[0033] Preparation of silica gel chloride: Weigh 10 g of coarse-pore silica gel, put it in a muffle furnace, dry it at 120°C for 8 h, and then add it to a reactor equipped with a reflux condenser and a drying tube; add 20 g of silica gel to the container mL of thionyl chloride was refluxed in an oil bath at 80°C for 24 h, the color of the system turned yellow during the reaction, and the color continued to deepen as time went by. After the reaction was completed, it was filtered, and the obtained solid product was fully washed three times with dichloromethane. After removing the solvent, it was dried in a vacuum oven at 60° C. for 10 h to obtain 10.5 g of a light yellow solid product. According to the analysis and calculation, the solid loading capacity of Cl in silica gel chloride is 2.37 mmol / g.

[0034] Preparation of silica gel-supported benzene: silica gel chloride (10.5 g, 0.025 mol ...

Embodiment 3

[0036] Embodiment three, the preparation of silica gel immobilized benzenesulfonic acid

[0037]Preparation of silica gel chloride: Weigh 15 g of fine-pore silica gel, place it in a muffler furnace, dry it at 120°C for 8 h, and then add it to a reactor equipped with a reflux condenser and a drying tube; add 30 g of silica gel to the container mL of thionyl chloride was refluxed in an oil bath at 80°C for 24 h, the color of the system turned yellow during the reaction, and the color continued to deepen as time went by. After the reaction was completed, it was filtered, and the obtained solid product was fully washed three times with dichloromethane. After removing the solvent, it was dried in a vacuum oven at 60° C. for 10 h to obtain 15.4 g of a light yellow solid product. According to the analysis and calculation, the solid loading capacity of Cl in silica gel chloride is 2.24 mmol / g.

[0038] Preparation of silica gel-supported benzene: Add silica gel chloride (15.4 g, 0.03...

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PUM

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Abstract

The invention discloses a benzenesulfonic acid catalyst supported on silica gel, which is prepared by adopting silica gel to react with thionyl chloride, phenol and chlorosulfonic acid sequentially. In the catalyst, the silica gel and benzenesulfonic acid are bonded in a covalent bond mode, so that the supporting capacity is stable, and the supporting capacity of the benzenesulfonic acid is about 2.25mmol / g in the benzenesulfonic acid catalyst supported on silica gel through analysis and calculation. Experiments prove that: the prepared catalyst has efficient catalytic activity to two kinds of atom economic reactions, namely Beckmann rearrangement reaction and Claisen rearrangement reaction, is non-toxic, harmless and noncorrosive, is easily separated, can be recycled, and accords with green and environmentally-friendly national industrial policy.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of a silica gel immobilized benzenesulfonic acid catalyst; at the same time, the invention also relates to the use of the catalyst in the Beckmann rearrangement reaction of ketoxime and the Claisen heavy reaction of allyl aryl ether. Application in row reaction. Background technique [0002] As a liquid acid, benzenesulfonic acid is often used as a catalyst. It has high activity and wide applicability. However, it has the common disadvantages of traditional liquid acids, such as the difficulty of separating the catalyst after the reaction is completed, strong corrosiveness, and pollution to the environment. With the rapid development of green chemical technology today, using pure liquid benzenesulfonic acid as a catalyst to catalyze chemical reactions will inevitably bring great harm to the environment. Therefore, the development of non-toxic, harmle...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C231/10C07C233/07C07D201/04C07D223/10C07C233/65C07C37/00C07C39/19
Inventor 李政王略杨靖亚
Owner NORTHWEST NORMAL UNIVERSITY
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