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Method for preparing tert-butyl carboxylate by using dual-modified SBA mesoporous molecular sieve catalyst

A technology of tert-butyl carboxylate and mesoporous molecular sieve, applied in the chemical industry, can solve the problems of high energy consumption for product separation and high investment in anti-corrosion equipment, and achieve the effects of high conversion rate, reduced energy consumption for separation and high selectivity

Active Publication Date: 2014-07-23
安徽百昊晟科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the production process of above-mentioned several carboxylic acids and olefin esterification synthesis carboxylate, in order to improve the selectivity of carboxylate, all must add polar solvents such as tert-butanol or carboxylic acid greatly excessive to suppress olefin polymerization, this just causes Subsequent product separation requires high energy consumption or high investment in anti-corrosion equipment
Therefore, in the reaction process of isobutene and carboxylic acid addition esterification to synthesize tert-butyl carboxylate, how to suppress the dimerization side reaction of isobutene and improve the selectivity of tert-butyl carboxylate is a challenge

Method used

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  • Method for preparing tert-butyl carboxylate by using dual-modified SBA mesoporous molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] With 4g P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer, the molecular formula is PEO 20 PPOs 70 PEOs 20 , average molecular weight 5800) is dissolved in 97g distilled water at room temperature, then adding 23.50g mass concentration is 37% hydrochloric acid aqueous solution, adjusts H in the solution + The concentration is 1M, heat the solution to 40°C and stir to dissolve, add 0.01g aluminum isopropoxide after dissolution, then add 7.65g tetraethyl orthosilicate dropwise; continue to stir the obtained mixture at 40°C for 4h, add 2.16g of γ-mercaptopropyltrimethoxysilane and 24.33g of 30% H 2 o 2 Continue to stir the resulting mixture at 40°C for 24h, crystallize at 80°C in a hydrothermal synthesis kettle for 24h, filter the crystallized solid-liquid mixture, and wash the filter cake with deionized water until neutral; use ethanol Wash the mixed solution with hydrochloric acid for 48 hours under heating, stirring and reflux conditions to re...

Embodiment 2

[0027] Dissolve 4g of P123 in 97g of distilled water at room temperature, then add 23.50g of 37% aqueous hydrochloric acid to adjust the H + The concentration is 1M, heat the solution to 40°C and stir to dissolve, add 1.41g of stannous chloride after dissolution, then add 7.65g of tetraethyl orthosilicate dropwise; continue to stir the resulting mixture at 40°C for 4h, add 0.07g γ-mercaptopropyltrimethoxysilane and 0.81g30% H 2 o 2Continue to stir the resulting mixture at 40°C for 36h, crystallize at 90°C in a hydrothermal synthesis tank for 48h, filter the crystallized solid-liquid mixture, and wash the filter cake with deionized water until neutral; use ethanol The mixed solution with hydrochloric acid was washed under reflux conditions for 48 hours to remove the surfactant, and dried in vacuum at 70°C for 10 hours to obtain a mesoporous Sn-SBA- 15-SO 3 H.

Embodiment 3

[0029] Dissolve 4g of P123 in 97g of distilled water at room temperature, then add 23.50g of 37% aqueous hydrochloric acid to adjust the H + The concentration is 1M, heat the solution to 40°C and stir to dissolve, add 0.55g ferric chloride hexahydrate after dissolution, then add 7.65g tetraethyl orthosilicate dropwise; continue to stir the obtained mixture at 40°C for 4h , adding 0.72g of γ-mercaptopropyltrimethoxysilane and 8.11g of 30% H 2 o 2 Continue to stir the resulting mixture at 40°C for 20h, crystallize in a hydrothermal synthesis kettle at 100°C for 72h, filter the crystallized solid-liquid mixture, and wash the filter cake with deionized water until neutral; use ethanol The mixed solution with hydrochloric acid was washed under reflux conditions for 48 hours to remove the surfactant, and dried in vacuum at 80°C for 12 hours to obtain a mesoporous Fe-SBA- 15-SO 3 H.

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Abstract

The invention discloses a method for preparing tert-butyl carboxylate by using a dual-modified SBA mesoporous molecular sieve catalyst. According to the method, carboxylic acid and isobutylene are subjected to addition esterification by using a dual-modified SBA mesoporous molecular sieve as a catalyst to synthesize the tert-butyl carboxylate. The molecular sieve catalyst is a metal-doped sulfonate-grafted dual-modified SBA mesoporous molecular sieve catalyst prepared by a one-step cocondensation process. When the dual-modified SBA mesoporous molecular sieve catalyst is used in the addition esterification reaction process of synthesizing tert-butyl carboxylic acid from carboxylic acid and isobutylene, no polar solvent (such as tert-butyl alcohol, methyl tert-butyl ether or the like) is needed as an isobutylene polymerization inhibitor, and the quantity of the carboxylic acid is not excessive, thereby reducing the energy consumption for separating the reaction product. The catalyst has the advantages of high conversion rate, high selectivity, non-homogeneous phase, no corrosiveness, adjustable acid quantity and acid center and the like, and is recyclable.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a method for producing tert-butyl carboxylate by catalyzing the esterification of olefins with double-modified SBA mesoporous molecular sieves, in particular to a double-modified SBA mesoporous molecular sieve catalyst with metal doping and sulfonic acid grafting A method for synthesizing tert-butyl carboxylate through solvent-free addition and esterification of carboxylic acid and isobutene. Background technique [0002] As we all know, the reaction of olefins and carboxylic acids to prepare carboxylic acid esters is an atom-economical reaction, which has the advantages of anhydrous formation in the reaction process and simple process flow. It gradually replaces the traditional production process of acid alcohol esterification and is an environmentally friendly Economical carboxylate production process. [0003] U.S. Patent No. 5,994,578 uses sulfonic acid modified cation exchang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/04C07C69/003C07C69/24C07C69/06C07C69/54C07C69/63C07C69/14B01J29/03
CPCC07C67/04C07C69/003B01J29/0308B01J2229/32B01J2229/186C07C69/24C07C69/06C07C69/54C07C69/63C07C69/14Y02P20/584
Inventor 汤吉海乔旭艾胜兰费兆阳崔咪芬陈献冯静远陈幸福齐敏吴明昆
Owner 安徽百昊晟科技有限公司
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