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Solid base catalyst for synthesizing dimethyl carbonate by transesterification method and its preparation method and application

A solid base catalyst, technology of dimethyl carbonate, applied in the preparation of carbonate/haloformate, organic carbonate, preparation of organic compounds, etc., can solve the problem of difficulty in synthesizing dimethyl carbonate, high reaction temperature, etc. To achieve the effect of efficient catalysis, high selectivity and easy recovery of regeneration capacity

Active Publication Date: 2019-06-07
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction temperature of the solid base catalysts studied at present is usually high, so it is difficult to be suitable for the synthesis of dimethyl carbonate by catalytic distillation technology (Zhang Sujuan, preparation of solid base catalysts for the synthesis of dimethyl carbonate by transesterification, China University of Petroleum)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1. With 20mmol CaCl 2 and 40mmolAlCl 3 ·6H 2 O was dissolved in 100ml of deionized water as solution A; 0.14mol NaOH was dissolved in 100ml of deionized water as solution B. Subsequently, solution A and solution B are added dropwise in the water-ethanol (volume ratio is 1) solution of 250ml simultaneously with peristaltic pump, control pH at 10, in N 2 Stir continuously at 40°C for 36h under protection, wash the precipitate with deionized water until the pH value is 7, and dry in a vacuum oven at 80°C for 24h. Finally, the 27.3%Ca-12.4%Al-54.2%O-6.1%Cl catalyst was obtained by calcining in a nitrogen atmosphere at 700°C for 6h. Get 0.25g of catalyst and add in catalytic rectification reactor, add 9.23g methyl alcohol and 3.27g propylene carbonate, react 0.5h under stirring at 60 ℃, after the product is cooled, analyze with gas chromatography, the conversion rate of propylene carbonate of this catalyst is 32.4%, and the yield of dimethyl carbonate is 30.7%. ...

Embodiment 2

[0019] Example 2. With 50mmol CaCl 2 and 20mmolAlCl 3 ·6H 2 O was dissolved in 100ml of deionized water as solution A; 0.13mol NaOH and 0.01mol NaBr were dissolved in 100ml of deionized water as solution B. Subsequently, solution A and solution B are added dropwise in the water-ethanol (volume ratio of 0.8) solution of 250ml with peristaltic pump simultaneously, control pH at 13, in N 2 Stir continuously at 100°C for 6h under protection, wash the precipitate with deionized water until the pH value is 8, and dry in a vacuum oven at 160°C for 6h. Finally, 27.3%Ca-12.7%Al-56.5%O-3.5%Br was obtained by roasting at 900°C for 2h in a nitrogen atmosphere. Get 0.12g of catalyst and add in catalytic rectification reactor, add 10.30g methyl alcohol and 2.19g propylene carbonate, react 3h under stirring at 70 ℃, after the product is cooled, analyze with gas chromatography, the conversion rate of propylene carbonate is 44.7%, carbonic acid Dimethyl ester yield was 40.2%.

Embodiment 3

[0020] Example 3. With 40mmol CaCl 2 and 20mmolAlCl 3 ·6H 2 O was dissolved in 100ml of deionized water as solution A; 0.11mol NaOH and 0.02mol NaF were dissolved in 100ml of deionized water as solution B. Subsequently, solution A and solution B are added dropwise in the water-ethanol (volume ratio is 0.5) solution of 250ml with peristaltic pump simultaneously, control pH at 7, in N 2 Stir continuously at 60°C for 24h under protection, wash the precipitate with deionized water until the pH value is 7, and dry in a vacuum oven at 60°C for 24h. Finally, calcined in nitrogen atmosphere at 300℃ for 4h to obtain 16.2%Ca-8.4%Al-67.1%O-8.3%F catalyst. Get 0.63g of catalyst and add in catalytic rectification reactor, add 9.88g of methanol and 2.62g of propylene carbonate, react for 2h under stirring at 50°C, and analyze with gas chromatography after the product is cooled, the conversion rate of propylene carbonate is 46.1%. The yield of dimethyl ester was 43.7%.

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Abstract

The invention provides a solid base catalyst for synthesizing dimethyl carbonate through a transesterification method. The components are Ca-Al-O-X, wherein the mole content of Ca ranges from 15% to 35%, the mole content of Al ranges from 5% to 30%, the mole content of X ranges from 0.1% to 10%, the balance is O, and X is CO3<2-> or NO3<-> or F<-> or Cl<-> or Br<->. The solid base catalyst has the advantages that the use temperature is low, the conversion rate of propylene carbonate under the low-temperature condition is high, and the yield of dimethyl carbonate is high.

Description

technical field [0001] The invention belongs to a catalyst and a preparation method, in particular to a solid base catalyst for synthesizing dimethyl carbonate by transesterification, a preparation method and application. Background technique [0002] Dimethyl carbonate (DMC), as a non-toxic, non-corrosive green chemical intermediate, has been widely used in many fields such as pesticides, medicines, and fine chemicals. The current method of producing dimethyl carbonate is mainly transesterification. Patents CN101774888A and CN1569807A use methanol and propylene carbonate as raw materials and use homogeneous catalysts such as sodium methylate. The DMC yield is higher, but the catalyst is not easy to remove from the reaction mixture. separation, and the catalyst cannot be regenerated after the reaction. Compared with homogeneous catalysts, solid base catalysts have the advantages of easy separation of products and recyclability, so they have very broad application and develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/232B01J27/138B01J27/25C07C69/96C07C68/06
CPCB01J27/138B01J27/232B01J27/25C07C68/065C07C69/96
Inventor 肖福魁李枫廖云辉赵宁蒲彦锋王峰杨金海王太英陈兰光李建明银海
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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