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Method for preparing solid acid catalyst of esterification

A technology of solid acid catalyst and esterification reaction, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, and preparation of organic compounds, etc. It can solve the problems of complex preparation process, high cost of esterification reaction catalyst, and poor activity. Achieve the effect of good selectivity, long life and high activity

Inactive Publication Date: 2010-05-12
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a solid acid catalyst system that does not pollute the environment, is convenient to prepare, has high catalytic activity, good selectivity, and long service life in view of the shortcomings of the existing esterification reaction catalysts, such as high cost, poor activity, and complicated preparation process. and preparation method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 100g of tetraethyl orthosilicate, add 100g of deionized water under magnetic stirring at room temperature, and hydrolyze for 1.5h; h. The above two solutions were mixed and heated to 85°C to remove alcohol for 6 hours, and 110 g of deionized water was added. Afterwards, the above solution was put into a reaction kettle and heated to 170° C. for crystallization, and the crystallization time was 48 hours. The obtained white powder was washed to neutrality, then impregnated in 0.5mol.L -1 in sulfuric acid solution for 2 hours, dried and calcined at 450°C for 4 hours to obtain catalyst sample a.

Embodiment 2

[0025] Weigh 100g of silica sol, add 100g of deionized water under magnetic stirring at room temperature, and hydrolyze for 1.5h; dissolve 8g of butyl titanate in 30g of anhydrous propanol, add 50g of deionized water while stirring, and hydrolyze for 0.5h. The above two solutions were mixed and heated to 85°C to remove alcohol for 6h. Afterwards, the above solution was put into a reaction kettle and heated to 190° C. for crystallization, and the crystallization time was 48 hours. The obtained white powder was washed to neutrality, then impregnated in 0.5mol.L -1 in sulfuric acid solution for 2h, dried, and roasted at 450°C for 4h to obtain catalyst sample b.

Embodiment 3

[0027] Weigh 100g tetraethyl orthosilicate, add 100g deionized water with magnetic stirring at room temperature, and hydrolyze for 2.5h; h. The above two solutions were mixed and heated to 90°C to remove alcohol for 6h. Afterwards, put the above solution into the reaction kettle and raise the temperature to 200°C for crystallization, and the crystallization time is 48h. The obtained white powder was washed to neutrality, then impregnated in 0.5mol.L -1 in sulfuric acid solution for 2 hours, dried and calcined at 550°C for 5 hours to obtain catalyst sample c.

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Abstract

The invention relates to a method for preparing a solid acid catalyst used in esterification. The method takes organic titanium ester and silicone ester as raw materials and prepares a SO42- / TiO2-SiO2 novel solid acid by a hydrothermal method. If the solid acid catalyst is used in a reflux device to catalyze acetic acid / n-butanol esterification reaction, the yield and selectivity of n-butyl acetate can reach 98.9 percent and 99.5 percent respectively. The catalyst is characterized in simple preparation process, low cost, high activity and selectivity, long lifespan and the like, overcomes the disadvantage that concentrated sulfuric acid used as the catalyst is poor in selectivity, low in esterification yield, severe in equipment corrosion, large amount of waste liquid produced, environmental pollution and the like, and has good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of solid catalyst preparation and application, and in particular relates to a method for preparing a solid acid catalyst for esterification reaction. Background technique [0002] Organic esters are widely used in organic synthesis industries such as solvents, plasticizers, resins, coatings, flavors and fragrances, cosmetics, medicines, and surfactants. Therefore, esterification has become an important way to synthesize raw materials and intermediates. In modern industry play a pivotal role. The traditional synthetic method of this product is to use corresponding carboxylic acid and alcohol as raw materials, and adopts concentrated sulfuric acid as catalyst to prepare. Although the use of concentrated sulfuric acid as catalyst has the advantages of low price and high activity, this method is not ideal. The following points are insufficient: firstly, the oxidation and dehydration of the concentrated sulfuric...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J37/10B01J35/10C07C67/08C07C69/14
Inventor 许岩郑书忠于海斌刘敬利杨玉旺戴清
Owner CHINA NAT OFFSHORE OIL CORP
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