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Method used for preparing dimethyl carbonate via direct reaction of carbon dioxide with methanol

A technology of dimethyl carbonate and carbon dioxide, applied in the preparation of carbon dioxide or inorganic carbonate, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high dehydration cost, non-renewable, cumbersome and lengthy separation process, etc.

Active Publication Date: 2017-07-14
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these additional methods of adding chemical dehydrating agents have an inherent defect, that is, the dehydrating agent will be converted into other organic compounds after reacting with water, such as phenacetin and water reacting into amide, dimethoxypropane and water reacting into It is acetone, so that the dehydrating agent loses its dehydration ability and cannot be regenerated
Therefore, dehydration is costly
In addition, the catalysts and dehydrating agents used in all the above methods are different substances, making the subsequent separation process cumbersome and lengthy

Method used

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  • Method used for preparing dimethyl carbonate via direct reaction of carbon dioxide with methanol
  • Method used for preparing dimethyl carbonate via direct reaction of carbon dioxide with methanol
  • Method used for preparing dimethyl carbonate via direct reaction of carbon dioxide with methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a 100ml stainless steel autoclave, add 5mmol methanol, 10ml methylene bromide, 5mmol 1-methyl-3-butylimidazole bicarbonate ionic liquid [C 1 C 4 Im] [HCO 3 ], 5mmol cesium carbonate, carbon dioxide at 1MPa pressure. After stirring and reacting at room temperature for 24 hours, the conversion rate of methanol was 45% and the selectivity of dimethyl carbonate was 99% through gas chromatography analysis.

Embodiment 2-10

[0026] Similar to Example 1, the results of operating under different conditions are shown in the table below:

[0027]

[0028] Remarks: DBU means 1,8-diazabicycloundec-7-ene; BABCO means 1,4-diazabicyclo[2.2.2]octane; HTMP means 2,2,6,6- Tetramethylpiperidine. C 4 is n-butyl, C 6 For n-hexyl.

Embodiment 18

[0030] The imidazolium bicarbonate ionic liquid with catalysis and dehydration ability can be regenerated by the following method: after the reaction shown in Example 1 finishes, dimethyl carbonate, methyl alcohol, methylene bromide are removed by distillation, and the residue (containing ionic liquid and cesium carbonate) After vacuum drying at 50 °C for 24 hours, the imidazolium bicarbonate ionic liquid with catalytic and dehydrating ability can be regenerated. Add 5 mmol of methanol, 10 ml of methylene bromide, and carbon dioxide at a pressure of 1 MPa to the regenerated ionic liquid and cesium carbonate mixture. After stirring and reacting at room temperature for 24 hours, the conversion rate of methanol was 43% and the selectivity of dimethyl carbonate was 97% through gas chromatography analysis.

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Abstract

The invention relates to a method used for preparing dimethyl carbonate via direct reaction of carbon dioxide with methanol. According to the method, a midazole bicarbonate ionic liquid is taken as a catalyst and a dehydrating agent, direct reaction of carbon dioxide with methanol at mild conditions is carried out so as to obtain dimethyl carbonate. Compared with the prior art, the method possesses following advantages: the midazole bicarbonate ionic liquid is taken as both as the catalyst and the dehydrating agent, so that the production process of dimethyl carbonate is simplified; the method is green and economical; the conversion rate of methanol is as high as 54%; and the selectivity of dimethyl carbonate production is as high as 99%.

Description

technical field [0001] The invention relates to ionic liquid catalysis, in particular to a new method for preparing dimethyl carbonate through the direct reaction of carbon dioxide and methanol. [0002] technical background [0003] Dimethyl carbonate is an environmentally friendly chemical raw material, which can be used to synthesize polymer compounds, as battery electrolyte, as a reaction solvent, as an intermediate in organic synthesis, etc. [0004] At present, there are many synthetic methods of dimethyl carbonate, including the direct reaction of methanol and phosgene to prepare dimethyl carbonate, and the preparation of dimethyl carbonate by transesterification of methanol and carbonate (CN201410300187.7, CN201210226548.9, CN201110415385.4), Methanol and ethylene carbonate react to prepare dimethyl carbonate (CN201410677148.9, CN201410428934.5, CN201410497814.0, CN201410195315.6), methanol and urea react to prepare dimethyl carbonate (CN201410585479.X), methanol and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/04C07C69/96B01J31/02
CPCC07C68/04B01J31/0284C07C69/96Y02P20/141
Inventor 胡兴邦赵天祥吴有庭李锐
Owner NANJING UNIV
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