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Solid basic catalyst, preparation method of solid basic catalyst and application of solid basic catalyst in ester exchange reaction

A solid base catalyst, a technology for transesterification, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. Reduce catalytic performance, basic site aggregation and other problems to achieve ideal catalytic effect, low operating cost and good stability

Inactive Publication Date: 2012-10-03
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of solid bases in the prior art requires high-temperature roasting to generate basic sites, and the resulting basic sites will aggregate, reducing catalytic performance, and the basic sites lack interaction with the carrier and are easy to lose. This method of preparing solid bases method needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix 0.0153 g of lithium tert-butoxide and 0.1296 g of mesoporous silica SBA-15 with 10 mL of benzene solution, stir for about 1 h under Ar atmosphere at room temperature and normal pressure, then add benzene to wash 3 times, The samples obtained by washing were successively vacuum-dried at a temperature of 25, 50 and 60° C. for 0.5, 0.5 and 2.5 h to obtain a solid base catalyst. The content of lithium element in the solid base catalyst was 1.4mmol / g as measured by plasma coupled spectroscopy (ICP) (all the following examples were measured by this method).

[0026] 20mL of methanol, 8.7076g of ethylene carbonate and 0.0796g of catalyzer were added into the flask, the reaction temperature was 60°C, and the pressure was normal pressure. After reacting for 4h under stirring conditions, the product was centrifuged, and the supernatant was analyzed by gas chromatography. The yield of methyl ester was 16.7%.

Embodiment 2

[0028] Mix 0.0334 g of lithium tert-butoxide and 0.1294 g of mesoporous silica SBA-15 with 10 mL of benzene solution, stir for about 1 h under Ar atmosphere at room temperature and normal pressure, then add benzene to wash 3 times, The samples obtained by washing were successively vacuum-dried at a temperature of 25, 50 and 60° C. for 0.5, 0.5 and 2.5 h to obtain a solid base catalyst. The content of lithium element in the solid base catalyst is 3.1 mmol / g.

[0029] 20mL of methanol, 8.7076g of ethylene carbonate and 0.0790g of catalyzer were added into the flask, the reaction temperature was 60°C, the pressure was normal pressure, and after stirring for 4 hours, the product was centrifuged, and the supernatant was analyzed by gas chromatography. The yield of methyl ester was 26.3%.

Embodiment 3

[0031] Mix 0.0602g of lithium tert-butoxide and 0.1299g of mesoporous silica SBA-15 with 10mL of benzene solution, stir for about 1h under Ar atmosphere at room temperature and normal pressure, then add benzene to wash 3 times, The samples obtained by washing were successively vacuum-dried at a temperature of 25, 50 and 60° C. for 0.5, 0.5 and 2.5 h to obtain a solid base catalyst. The content of lithium element in the solid base catalyst is 4.8mmol / g.

[0032] 20mL of methanol, 8.7076g of ethylene carbonate and 0.0789g of catalyzer were added to the flask, the reaction temperature was 60°C, the pressure was normal pressure, and after stirring for 4 hours, the product was centrifuged, and the supernatant was analyzed by gas chromatography. The yield of methyl ester was 28.0%.

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Abstract

The invention discloses a solid basic catalyst, a preparation method of the solid basic catalyst and an application of the solid basic catalyst in ester exchange reaction. The solid basic catalyst catalyzes the ester exchange reaction by the reaction of metal organic compound and hydroxyl on a carrier under the moderate conditions to synthesize dimethyl carbonate. The solid basic catalyst provided by the invention consists of metal organic alkali and the carrier. The metal organic alkali is linked to the carrier in bond-forming manner; the metal organic alkali is one or more of lithium methoxide, lithium ethoxide, lithium isopropoxide, lithium n-butoxide, lithium tert-butoxide, sodium methoxide, sodium ethoxide, sodium isopropoxide, sodium n-butoxide, sodium tert-butoxide, potassium methoxide, potassium ethoxide, potassium isopropoxide, potassium n-butoxide and potassium tert-butoxide; the carrier is one or more of silicon oxide, aluminium oxide, titanium oxide, zirconia, mesoporous silicon oxide synthesized by the template method, mesoporous aluminium oxide synthesized by the template method, mesoporous titanium oxide synthesized by the template method, and mesoporous zirconia synthesized by the template method.

Description

technical field [0001] The present invention relates to a kind of catalyst, preparation method and application thereof, more specifically relate to a kind of solid base catalyst, preparation method and application in transesterification reaction. Background technique [0002] Dimethyl carbonate (DMC) is an environmentally friendly green chemical product that has attracted widespread attention at home and abroad. Because of its structure containing oxymethyl and carbonyl groups, it is expected to completely replace highly toxic or toxic substances such as phosgene and dimethyl sulfate in many fields. Carcinogens undergo carbonylation, methylation, methyl esterification and transesterification reactions to produce many important chemical products. At present, the methods for synthesizing dimethyl carbonate can be divided into three categories: phosgene method, methanol oxidative carbonylation method, and transesterification method. The phosgene method is not easy to populariz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J31/26B01J31/02B01J35/02C07C69/96C07C68/06B01J35/00
Inventor 孙林兵刘晓勤李田田刘定华
Owner NANJING UNIV OF TECH
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