Method for simultaneously preparing glycol and carbonate by catalysis

A technology of ethylene glycol and carbonate, applied in chemical instruments and methods, preparation of organic carbonates, preparation of oxygenates, etc., can solve problems such as harsh reaction conditions, low equilibrium conversion rate, and reduced alcohol activity

Active Publication Date: 2011-06-15
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The currently reported catalysts for the synthesis of ethylene glycol and carbonate by transesterification include: alkali metal hydroxides, alkaline earth metal carbonates, organic bases, quaternary ammonium salts, quaternary phosphonium salts, imidazole tetrafluoroborate, solid bases (such as metal oxides), triphenylphosphine supported by crosslinking resin, sodium silicate supported by silica, quaternary ammonium salt of ion exchange resin, quaternary ammonium salt supported by chitosan, etc., these catalytic systems may be more There are some problems such as low catalytic activity, low stability, harsh reaction conditions, high catalyst cost, etc.
In addition, the transesterification reaction is an equilibrium reaction, and the equilibrium conversion rate is generally low, and the activity of the alcohol generally decreases with the increase of the carbon number of the alcohol.

Method used

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  • Method for simultaneously preparing glycol and carbonate by catalysis
  • Method for simultaneously preparing glycol and carbonate by catalysis
  • Method for simultaneously preparing glycol and carbonate by catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The first type of basic catalyst takes the synthesis of 1,3-dimethylimidazole-2-carboxylate as an example: in a 100mL reactor, add 15mL dimethyl carbonate and 10mL methylimidazole, under the protection of nitrogen, the temperature The reaction was carried out at 120°C for 24 hours, and the resulting solid was recrystallized with methanol to obtain white 1,3-dimethylimidazole-2-carboxylate.

[0014] Type 2-8 basic catalysts are triethylmethylammonium methyl carbonate [(C 2 H 5 ) 3 CH 3 NCO 3 CH 3 ] As an example: in a 100mL reactor, add 17.8g of dimethyl carbonate, 20g of triethylamine and 20g of methanol, at a temperature of 120℃, react for 12h, distill off unreacted raw materials, and use methanol for the remaining solid Recrystallization gave white triethylmethylammonium methyl carbonate.

[0015] The method of the present invention for catalyzing the simultaneous preparation of ethylene glycol and carbonate is illustrated by the following examples, but the present inventi...

Embodiment 3

[0017]

[0018] Implementation method: In a 100mL stainless steel autoclave, add 1.2mmol of catalyst 1,3-dimethylimidazole-2-carboxylate, 10.5g (0.12mol) of ethylene carbonate and 38mL (0.96mol) of methanol, and seal the reactor. The temperature was slowly raised to 383K controlled by a temperature controller, the pressure was 0.3MPa, the reaction was for 1 hour, and then cooled to room temperature. The resulting mixture was analyzed by gas chromatography. The conversion rate of ethylene carbonate was 72% and the selectivity of ethylene glycol was 99%. The selectivity of dimethyl carbonate is 99%.

Embodiment 4

[0020] Same as Example 3, the catalyst used was tributyl methyl ammonium methyl carbonate [(C 4 H 9 ) 3 CH 3 NCO 3 CH 3 ], the amount of the catalyst is 1.2 mmol, the others remain unchanged, the conversion rate of ethylene carbonate is 60%, the selectivity of ethylene glycol is 98%, and the selectivity of dimethyl carbonate is 99%.

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Abstract

The invention relates to a method for simultaneously preparing glycol and carbonate by catalysis, which is characterized in that ethylene carbonate and fatty alcohol are used as raw materials; and in the reaction process, a basic catalyst is used, the reaction pressure is 0.1-1.0 MPa, the temperature is 333-433K, the reaction time is 0.25-6 hours, and the mol ratio of the ethylene carbonate to the fatty alcohol is 1:4-1:32, so that glycol and carbonate can be selectively synthesized at high conversion rate.

Description

Technical field: [0001] The present invention relates to the technical field of green and clean catalysis, and specifically refers to a method for synthesizing ethylene glycol and carbonate through transesterification reaction with ethylene carbonate and fatty alcohol as raw materials under alkali catalysis. Background technique: [0002] Ethylene glycol is an important organic chemical raw material, mainly used to produce polyester. With the rapid development of my country's polyester industry in recent years and the increasing demand for antifreeze driven by the expansion of automobile production and sales, the consumption of ethylene glycol continues to increase. Dimethyl carbonate is a non-toxic, easily biodegradable and environmentally friendly green basic chemical raw material. It can be used as a solvent, gasoline additive, lithium ion battery electrolyte, bisphenol A polycarbonate monomer, and carbonylation, methyl Alkylation and carbonyl methylation reagents are widely ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/128C07C27/00C07C69/96C07C68/06B01J31/04B01J31/02
Inventor 张锁江王金泉孙剑成卫国张香平张增亮张学辉
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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