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Application of Ca-based solid alkali heterogeneous catalyst in preparation of dimethyl carbonate

A heterogeneous catalyst, dimethyl carbonate technology, applied in catalyst activation/preparation, organic compound preparation, physical/chemical process catalyst, etc., can solve the difficulty of accurate control of hydrotalcite-like structure, loss of catalyst active component Ca , the catalyst preparation process is complicated and other problems, to achieve the effect of stable reuse performance, easy industrial scale-up, and simple preparation method

Active Publication Date: 2021-04-09
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalyst can synthesize DMC at low temperature, the yield of dimethyl carbonate dropped from 55.7% to 47.2% after 5 times of repeated use, and the active component Ca of the catalyst was still lost, and the preparation process of the catalyst was complex and water-like. Accurate control of talc structure is difficult
[0005] Generally speaking, the existing heterogeneous solid base catalysts generally require a higher reaction temperature, and high temperature can easily lead to the formation of by-products, and at the same time, high temperature can easily lead to the polymerization of polyols.

Method used

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  • Application of Ca-based solid alkali heterogeneous catalyst in preparation of dimethyl carbonate
  • Application of Ca-based solid alkali heterogeneous catalyst in preparation of dimethyl carbonate
  • Application of Ca-based solid alkali heterogeneous catalyst in preparation of dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The catalyst was prepared by sol-gel method, and 10.12 g of Ca(NO 3 ) 2 ·4H 2 O, 16.63g of Co (NO 3 ) 2 ·6H 2 O salt, 19.21 g of citric acid, and 54 mL of deionized water were jointly transferred to a 250 mL three-necked flask, refluxed at 80 °C for 6 h under magnetic stirring, then heated to 105 °C, and 5.76 g of dispersant ethylene glycol was added, and the reflux stirring was continued. 6 h. Then the formed gel was dried in a blast drying oven at 110 °C for 12 h, ground into fine powder, and then calcined in a muffle furnace at 800 °C for 4 h at a heating rate of 2 °C / min to obtain Ca. 3 Co 4 O 9 catalyst.

[0031] Take 0.20g of catalyst and put it into the tank reactor, add 6.40g of methanol and 2.55g of propylene carbonate raw materials, and react under stirring at 60 ° C for 2 hours. After the product is cooled, it is analyzed by gas chromatography. The conversion rate of propylene carbonate is 57.5%. The yield of dimethyl ester was 53.9%.

Embodiment 2

[0033] The catalyst was prepared by sol-gel method, and 10.12 g of Ca(NO 3 ) 2 ·4H 2 O, 16.63g of Co (NO3 ) 2 ·6H 2 O salt, 28.82 g of citric acid, and 90 mL of deionized water were jointly transferred to a 250 mL three-necked flask, refluxed at 80 °C for 6 h under magnetic stirring, then heated to 105 °C, and 8.64 g of dispersant ethylene glycol was added, and the reflux stirring was continued. 6 h. Then the formed gel was dried in a blast drying oven at 110 °C for 12 h, ground into fine powder, and then calcined in a muffle furnace at 800 °C for 4 h at a heating rate of 2 °C / min to obtain Ca. 3 Co 4 O 9 catalyst.

[0034] Take 0.20g of catalyst and put it into the kettle reactor, add 6.40g of methanol and 2.55g of propylene carbonate raw materials, and react under stirring at 60 ° C for 2 hours. After the product is cooled, it is analyzed by gas chromatography. The yield of dimethyl ester was 52.7%.

Embodiment 3

[0036] The catalyst was prepared by sol-gel method, and 10.12 g of Ca(NO 3 ) 2 ·4H 2 O, 16.63g of Co (NO 3 ) 2 ·6H 2 O salt, 24.01 g of citric acid, and 90 mL of deionized water were jointly transferred to a 250 mL three-necked flask, refluxed at 80 °C for 6 h under magnetic stirring, then heated to 105 °C, and 9.0 g of dispersant ethylene glycol was added, and the reflux stirring was continued. 6 h. Then the formed gel was dried in a blast drying oven at 110 °C for 12 h, ground into fine powder, and then calcined in a muffle furnace at 800 °C for 4 h at a heating rate of 2 °C / min to obtain Ca. 3 Co 4 O 9 catalyst.

[0037] Take 0.20g of catalyst and put it into the tank reactor, add 6.40g of methanol and 2.55g of propylene carbonate raw materials, and react under stirring at 60 ° C for 2 hours. After the product is cooled, it is analyzed by gas chromatography. The conversion rate of propylene carbonate is 71.2%. The yield of dimethyl ester was 70.3%.

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Abstract

The invention provides an application of a Ca-based solid base heterogeneous catalyst in preparation of dimethyl carbonate. The Ca-based solid base heterogeneous catalyst is a Ca3Co4O9 catalyst and is used in a reaction for preparing dimethyl carbonate through transesterification of cyclic carbonate and methanol. The Ca-based solid alkali heterogeneous catalyst Ca3Co4O9 has the advantages of high temperature resistance, oxidation resistance, good thermal stability, high chemical stability and the like, loss of Ca active components can be effectively inhibited, high dimethyl carbonate yield is realized under normal-pressure and low-temperature reaction conditions, and in addition, the catalyst is simple in preparation method, stable in repeated use performance and suitable for industrial production. The industrial amplification is facilitated.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to the application of a Ca-based solid base heterogeneous catalyst in the preparation of dimethyl carbonate. Background technique [0002] Dimethyl carbonate (DMC for short) is a new, low-polluting, environment-friendly basic chemical raw material with a wide range of applications, large market capacity, green, low toxicity and high added value. It can effectively promote the development of green solvent, non-phosgene polycarbon, non-phosgene polyurethane, new energy lithium battery, green drug synthesis and other industries. In recent years, the United States proposed to use DMC to gradually replace MTBE as a gasoline additive to improve the octane number, which has attracted the attention of scholars from all over the world on DMC. [0003] At present, most of the domestic processes for producing DMC by transesterification use sodium methoxide or potassium methoxide as catalysts. For exa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/065C07C69/96B01J23/78B01J37/03B01J37/08
CPCC07C68/065B01J23/78B01J23/002B01J37/03B01J37/036B01J37/082C07C69/96
Inventor 蒲彦锋翟明路王甜金文雅杨浩霍琳梦乔聪震柏
Owner HENAN UNIVERSITY
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