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Preparation method of carbonate

A carbonate and carbonate technology, applied in the carbonate field, can solve the problems of high price and difficulty in synthesis, and achieve the effects of low cost, easy operation and high yield

Active Publication Date: 2007-10-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this reaction is that it needs to be carried out in two steps and uses expensive and difficult to synthesize amidine and guanidine bases.

Method used

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  • Preparation method of carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: in 50 milliliters autoclave, add 2.2g butanols (0.03mmol), 4.1g2-bromobutane (0.03mmol), 3.0g triethylamine (0.03mmol) and 0.1g cesium carbonate (3mmol) successively ×10 -4 mmol), seal the reactor, fill it with 3.5MPa carbon dioxide, raise the reaction to 60°C, cool to room temperature after 20 hours of reaction, unload the reactor, and steam the unreacted raw materials from the reaction solution by vacuum distillation to obtain the corresponding carbonic acid ester. Qualitative analysis was performed by HP6890 / 5793 mass spectrometer, and quantitative analysis was performed by Tianmei 7890II gas chromatograph. The yield of the product isobutyl butyl carbonate is 30.6%, and the selectivity is 95.4%.

Embodiment 2

[0024] Embodiment 2: in 50 milliliters autoclave, add 2.2g n-butanol (0.03mmol), 4.1g bromo-n-butane (0.03mmol), 5.6g tributylamine (0.03mmol) and 0.1g cesium carbonate successively (3×10 -4 mmol), seal the reaction kettle, fill it with 2.0MPa carbon dioxide, raise the reaction to 60°C, cool to room temperature after 20 hours of reaction, unload the kettle, and steam the unreacted raw materials from the reaction solution by vacuum distillation to obtain the corresponding carbonic acid ester. Qualitative analysis was performed by HP6890 / 5793 mass spectrometer, and quantitative analysis was performed by Tianmei 7890II gas chromatograph. The yield of the product dibutyl carbonate is 58.9%, and the selectivity is 96.3%.

Embodiment 3

[0025] Embodiment 3: in 50 milliliters autoclaves, add 2.2g butanols (0.03mmol), 4.1g bromo-n-butane (0.03mmol), 3.0g triethylamine (0.03mmol) and 0.1g cesium carbonate (0.03mmol) successively 3×10 -4 mmol), seal the reaction kettle, fill it with 3.0MPa carbon dioxide, raise the reaction to 60°C, cool to room temperature after 20 hours of reaction, unload the kettle, and steam the unreacted raw materials from the reaction solution through vacuum distillation to obtain the corresponding carbonic acid ester. Qualitative analysis was performed by HP6890 / 5793 mass spectrometer, and quantitative analysis was performed by Tianmei 7890II gas chromatograph. The yield of the product dibutyl carbonate is 75.0%, and the selectivity is 97.6%.

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Abstract

The present invention discloses a method for preparing correspondent carbonic ester by means of one-step reaction of alcohol and halohydrocarbon in the presence of catalyst. Said invention uses carbonate as catalyst, uses organic alkali as adjuvant and utilizes alcohol, carbon dioxide and halohydrocarbon to prepare carbonic ester by means of one-step reaction.

Description

technical field [0001] The present invention relates to a method for forming the corresponding carbonate by one-step reaction of alcohol and brominated hydrocarbon in the presence of carbon dioxide. Background technique [0002] In general, the methods for preparing carbonates are divided into phosgene method and non-phosgene method. In the phosgene process, phosgene is reacted with alcohols to produce carbonate compounds without catalyst and at low temperature. However, there are also a series of problems in this process such as: using highly toxic phosgene as a starting material, and because the highly corrosive hydrochloric acid produced in the reaction process has extremely high requirements on equipment, and another point is that the produced There is a large amount of chlorine in the produced carbonate products. [0003] The non-phosgene process can be roughly divided into the oxidative carbonylation process of alcohol, the nitrite process of alkyl hydrocarbon group ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/04
CPCY02P20/141
Inventor 许传芝夏春谷张愔
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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