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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 toxicity, low conversion rate, poor selectivity, and difficult recovery of the catalyst, etc.
The most widely used commercialized CALB is Novozym 435 fixed in macroporous acrylic resin, which is expensive

Method used

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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
Comparison scheme
Effect test

Embodiment 1

[0039] In the ionic liquid [Emim][PF 6 ] The reaction conditions of Candida antarctica lipase CAL catalyzed the reaction of dimethyl carbonate and butanol to prepare methyl butyl carbonate were as follows: the molar ratio of alcohol to ester was 1:12, the amount of enzyme was 12% of the reactant mass fraction, and the ionic liquid was 2 mL / g (based on ester weight, v / w), water content 1% (based on ester weight, w / w), and reaction temperature at 55°C, the reaction solution was taken regularly for analysis of methyl alkyl carbonate content. Take 50 μL of the reaction solution and centrifuge to separate layers, take 10 μL of the upper liquid sample, dissolve it in 290 μL cyclohexane, shake well, then add 300 μL of n-heptane (2 mg / mL) as an internal standard; take 1 μL of the sample for injection, and measure the reaction by gas chromatography The yield of methyl butyl carbonate in the product, the chromatographic column is SE-54 type. The specific test conditions are: the tempe...

Embodiment 2

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

Embodiment 3

[0046] In ionic liquids [Emim][BF 4 ]Candida antarctica lipase CAL catalyzes the reaction of dimethyl carbonate and n-propanol to prepare methyl propyl carbonate. The reaction conditions are: the molar ratio of alcohol to ester is 1:12, the amount of enzyme is 8% of the reactant mass fraction, and the ionic liquid is 2mL / 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, the reaction solution was used for analysis of methyl propyl carbonate content. Take 50 μL of the reaction solution and centrifuge to separate layers, take 10 μL of the upper liquid sample, dissolve it in 290 μL cyclohexane, shake well, then add 300 μL of n-heptane (2 mg / mL) as an internal standard; take 1 μL of the sample for injection, and measure the reaction by gas chromatography The yield of methyl propyl carbonate in the product, the chromatographic column is SE-54 type. The specific test conditions are as follows: th...

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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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