Method for preparation of methyl alkyl carbonate

A technology of methyl alkyl carbonate and dimethyl carbonate, applied in the field of preparation of methyl alkyl carbonate, can solve the problems of difficult catalyst recovery, high catalyst toxicity, high reaction temperature, etc., and achieve high conversion rate and selectivity , Environmental friendliness and high catalytic activity

Inactive Publication Date: 2013-04-17
WUHAN UNIV
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Problems solved by technology

The relative use of chemical methods to catalyze the synthesis of methyl alkyl carbonate has the following defects: high reaction temperature (generally higher than 170°C), high pressure, high catalyst

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  • Method for preparation of methyl alkyl carbonate
  • Method for preparation of methyl alkyl carbonate
  • Method for preparation of methyl alkyl carbonate

Examples

Experimental program
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Example Embodiment

[0038] Example 1

[0039] In ionic liquid [Emim][PF 6 ]The reaction conditions for the preparation of methyl butyl carbonate by the reaction of dimethyl carbonate and butanol catalyzed by the lipase CAL of Candida antarctica are: the molar ratio of alcohol to ester is 1:12, the amount of enzyme is 12% by mass fraction of reactant, and the ionic liquid is 2mL / g (based on ester weight, v / w), water content 1% (based on ester weight, w / w), reaction temperature 55°C, and regularly take the reaction solution for analysis of methyl alkyl carbonate content. Take 50μL of the reaction solution by centrifugation, take 10μL of the upper liquid sample, dissolve it with 290μL of cyclohexane, shake it well, add 300μL of n-heptane (2mg / mL) as the internal standard; take 1μL of the sample into the sample, and determine the reaction by gas chromatography The yield of methyl butyl carbonate in the chromatographic column is SE-54. The specific test conditions are: the column chamber adopts a progr...

Example Embodiment

[0042] Example 2

[0043] In ionic liquid [Bmim][PF 6 ] The reaction conditions for the preparation of methyl lauric carbonate by the reaction of dimethyl carbonate and lauryl alcohol catalyzed by the lipase CAL of Candida antarctica are: the molar ratio of alcohol to ester is 1:20, the amount of enzyme is 1% of the mass fraction of the reactant, and the ionic liquid is 2 mL / g (based on the weight of the ester, v / w), water content 1% (based on the weight of the ester, w / w), the reaction temperature is 45°C, and the reaction solution is regularly taken for the analysis of the asymmetric ester content. Take 50μL of the reaction solution by centrifugation, take 10μL of the upper liquid sample, dissolve it with 290μL of cyclohexane, shake it well, add 300μL of n-heptane (2mg / mL) as the internal standard; take 1μL of the sample into the sample, and determine the reaction by gas chromatography The yield of asymmetric esters in the chromatographic column is SE-54. The specific test co...

Example Embodiment

[0045] Example 3

[0046] In ionic liquid [Emim][BF 4 ]The reaction conditions for the preparation of methyl propyl carbonate by the reaction of dimethyl carbonate and n-propanol catalyzed by the lipase CAL of Candida antarctica are: the molar ratio of alcohol to ester is 1:12, the amount of enzyme is 8% of the mass fraction of reactant, and 2 mL of ionic liquid / g (based on ester weight, v / w), water content 1% (based on ester weight, w / w), reaction temperature 25-75°C, reaction time 48 hours, take the reaction solution for analysis of methyl propyl carbonate content. Take 50μL of the reaction solution by centrifugation and layer, take 10μL of the upper liquid sample, dissolve it with 290μL of cyclohexane, shake well, and add 300μL of n-heptane (2mg / mL) as the internal standard; take 1μL of the sample into the sample and determine the reaction by gas chromatography The yield of methyl propyl carbonate in the chromatographic column is SE-54. The specific test conditions are: the ...

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Abstract

The invention belongs to the field of biochemical industry and provides a method for preparation of methyl alkyl carbonate. The method comprises the following steps of: using ion liquid as a reactant medium or adding dimethyl carbonate instead of a solvent, adding alkyl alcohol of which the mol ratio of alcohol to ester is 1:1-1:20, adding 1%-25% of candida antarctica lipase by mass percentage in the reactant, performing transesterification reaction after stirring, and then obtaining a product of methyl alkyl carbonate by means of treatment after the reaction. The method disclosed by the invention has the advantages of high transformation rate, high selectivity, high universality, simple technique, environmental friendliness and the like.

Description

technical field [0001] The invention belongs to the field of biochemical industry, and relates to a method for preparing methyl alkyl carbonate, Background technique [0002] Carbon dioxide is the most abundant source of C1 in nature. Dimethyl carbonate is currently one of the main products synthesized using carbon dioxide as a raw material, and is widely used in synthetic fibers, synthetic resins, medicine, pesticides and other industries. However, due to the excess production of dimethyl carbonate, the synthesis of other types of dialkyl carbonates from dimethyl carbonate is a hot spot in current research and application. [0003] There are many synthesis methods of dialkyl carbonate, mainly including phosgene method, carbonyl oxidation method, transesterification method and so on. The phosgene method (such as JP 6410l9 (1994)) is to generate methyl chloroformate by reacting phosgene with boiling alcohol first, and then continue to react with the corresponding alcohol to...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
Inventor 张海波周耀靓刘骏
Owner WUHAN UNIV
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