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Heterogeneous acid catalyst, and preparation method and application thereof

An acid catalyst, heterogeneous technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of large environmental pollution of waste acid, high corrosion of equipment, deepening of product color, etc. The preparation method is simple, the catalytic efficiency is high, and the effect of easy recycling

Inactive Publication Date: 2014-01-15
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hydroxycarboxylate mainly adopts catalytic method synthesis in industry now, and its catalyzer is based on concentrated sulfuric acid, and this method has following shortcoming: 1. concentrated sulfuric acid has strong oxidizing property, can cause a lot of side reactions to produce and the generation of carbonization, make product The color deepens; 2. Concentrated sulfuric acid is more corrosive to equipment; 3. The discharge of a large amount of waste acid is more polluting to the environment
However, ionic liquids are difficult to recover due to their homogeneous catalysts, thus limiting their application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation of mesoporous material-modified SBA-15 is as follows: Add 125g of 1.9M HCl aqueous solution and 4g of P123 (M=5800) into a 250mL three-necked flask equipped with magnetic stirring and a thermometer, stir and dissolve at 40°C, After adding 6.83g of TEOS (tetraethyl orthosilicate) and hydrolyzing for 45min, 1.61g of MPTMS (γ-mercaptopropyltrimethoxysilane) was added and stirred. Keep stirring at 40°C for 20h, then raise the temperature to 100°C under static conditions for 24h, and recover the solid product. Reflux in 500ml of absolute ethanol for 20h to remove the template agent, recover the solid matter, wash it several times with water, and dry it under reduced pressure at 60°C to obtain the modified SBA-15.

[0026] The preparation of the acidic ionic liquid is as follows: take 3g of N-allylimidazole and 3.39g of 1,3-propane sultone in a 100ml three-necked flask, add 30ml of acetonitrile and stir at 25°C for 24h, filter the obtained solid product with ...

Embodiment 2

[0029] The preparation of SBA-15 modified by mesoporous materials is as follows: Add 125g of 3.0M HCl aqueous solution and 2.5g of P123 (M=5800) into a 250mL three-necked flask equipped with magnetic stirring and a thermometer, and stir to dissolve at 40°C , Add 5.0g of TEOS (tetraethyl orthosilicate) for hydrolysis for 45min, then add 1.25g of MPTMS (γ-mercaptopropyltrimethoxysilane) and stir. Keep stirring at 40°C for 20h, then raise the temperature to 100°C under static conditions for 24h, and recover the solid product. Reflux in 500ml of absolute ethanol for 20h to remove the template agent, recover the solid matter, wash it several times with water, and dry it under reduced pressure at 60°C to obtain the modified SBA-15.

[0030] The preparation of the acidic ionic liquid is as follows: take 3g of N-allylimidazole and 3.39g of 1,3-propane sultone in a 100ml three-necked flask, add 30ml of acetonitrile and stir at 20°C for 30h, filter the obtained solid product with Wash ...

Embodiment 3

[0033] The preparation of mesoporous material-modified SBA-15 is as follows: Add 125g of 1.5M HCl solution and 6.25g of P123 (M=5800) into a 250mL three-neck flask equipped with magnetic stirring and a thermometer, and stir to dissolve at 40°C , 8.75g of TEOS (tetraethyl orthosilicate) was added for hydrolysis for 45min, and then 2.5g of MPTMS (γ-mercaptopropyltrimethoxysilane) was added and stirred. Keep stirring at 30°C for 24h, then raise the temperature to 90°C under static conditions for 30h, and recover the solid product. Reflux in 500ml of absolute ethanol for 20h to remove the template agent, recover the solid matter, wash it several times with water, and dry it under reduced pressure at 60°C to obtain the modified SBA-15.

[0034] The preparation of the acidic ionic liquid is as follows: take 3g of N-allylimidazole and 3.39g of 1,3-propane sultone in a 100ml three-necked flask, add 30ml of acetonitrile and stir at 30°C for 18h, filter the obtained solid product with ...

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PUM

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Abstract

The invention provides a heterogeneous acid catalyst which is formed by linking an acidic ionic liquid on a mesoporous material through chemical bonds. The invention further provides a preparation method of the heterogeneous acid catalyst and the application of the heterogeneous acid catalyst in a catalytic esterification reaction. The heterogeneous acid catalyst is simple in preparation method and stable in structure, can be used as a heterogeneous catalyst to be repeatedly used, and is high in catalytic efficiency. Side reactions such as oxidation reactions, sulfonation reactions and the like are not likely to happen when the heterogeneous acid catalyst is used for synthesize an ester. A catalyzed product is good in quality, no acid regurgitation phenomenon happens, the heterogeneous acid catalyst does not corrode equipment, recycle is easy after a catalytic reaction, and the cost of an esterification reaction is greatly reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a heterogeneous acidic catalyst, a preparation method of the catalyst, and an application of the catalyst in catalyzing esterification reactions. Background technique [0002] Hydroxycarboxylates are a class of organic compounds with a wide range of uses, and are widely used in food, medical, daily chemical and other industries. Hydroxycarboxylate mainly adopts catalytic method synthesis in industry now, and its catalyzer is based on concentrated sulfuric acid, and this method has following shortcoming: 1. concentrated sulfuric acid has strong oxidizing property, can cause a lot of side reactions to produce and the generation of carbonization, make product The color deepens; 2. Concentrated sulfuric acid is more corrosive to equipment; 3. The discharge of a large amount of waste acid is more polluting to the environment. Therefore, searching for new esterification c...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C67/08C07C69/704C07C69/50
Inventor 郭凯袁爱邦李昕唐拾贵欧阳平凯
Owner NANJING UNIV OF TECH
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