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Method for synthesizing diethyl carbonate and coproducing diol by using carbon dioxide

A technology of diethyl carbonate and carbon dioxide is applied in the field of synthesis of diethyl carbonate, direct esterification to prepare diethyl carbonate and co-production of diol, which can solve the problems that do not conform to the development direction of green chemical industry, the by-product hydrochloric acid corrodes equipment, Environmental pollution and other problems, to achieve excellent catalytic performance, avoid separation problems, and reduce equipment investment.

Active Publication Date: 2015-03-18
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in terms of economy and technology, there are certain shortcomings in the first few routes: the raw material phosgene in the phosgene method is highly toxic, and the by-product hydrochloric acid corrodes equipment, causing serious environmental pollution, which does not conform to the development direction of green chemical industry
However, due to the chemical inertness of carbon dioxide, direct utilization of carbon dioxide and ethanol to synthesize diethyl carbonate is limited by thermodynamic equilibrium, and the yield is very low (Topics in Catalysis, 55(2012) 668-672)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 150mL stainless steel autoclave, add 2.0g ethylene oxide, 31.4g ethanol, add 0.1g KI and 0.1g K 2 CO 3 Composite catalyst. After sealing the reactor, fill it with carbon dioxide with a purity of 3Mpa and 99.9%, and under the condition of the magneton rotating speed of 500rpm, the temperature controller controls the temperature to rise to 150°C, react for 3 hours, and cool to room temperature. The gas in the reactor is slowly discharged from the reactor through the pressure control valve. Absorb with ethanol solvent. After the gas in the kettle is released, open the kettle to collect the reaction mixture and absorption solution. A certain amount of product was taken, and after constant volume in a volumetric flask, it was analyzed by a Shimadzu gas chromatograph equipped with a hydrogen flame ionization detector (FID) and a polar capillary column (Rtx-WAX30m×0.25mm×0.25μm).

[0024] The analysis results showed that the conversion rate of ethylene oxide was 94.7%, ...

Embodiment 2

[0026] Adopt the described step of example 1, only change catalyst composition, add 0.1g KI and 0.1g Na 2 CO 3 catalyst. The results of chromatographic analysis showed that the conversion rate of ethylene oxide was 97.6%, the yield of DEC was 52.9%, the yield of ethylene glycol was 58.5%, the yield of ethylene carbonate was 37.0%, and the yield of 2-ethoxyethanol was 3.2%.

Embodiment 3

[0028] Adopt the procedure described in Example 1, only change the catalyst composition, add 0.1g KI and 0.1g NaOH catalyst. The results of chromatographic analysis showed that the conversion rate of ethylene oxide was 96.9%, the yield of DEC was 48.8%, the yield of ethylene glycol was 58.8%, the yield of ethylene carbonate was 29.2%, and the yield of 2-ethoxyethanol was 3.2%.

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Abstract

The invention discloses a method for synthesizing diethyl carbonate and coproducing diol by using carbon dioxide, belonging to the field of synthesis of organic chemicals. An epoxy compound, the carbon dioxide and ethanol are used as raw materials and directly esterified in the presence of a catalyst to prepare the diethyl carbonate, and the diol is also coproduced; and the catalyst is characterized by consisting of an alkali metal halide and an alkali catalyst which are used as active ingredients, wherein the weight ratio of the epoxy compound to the catalyst is 100: (1-5), the reaction temperature is 80-230 DEG C, the reaction pressure is 0.5-15MPa, and the reaction time is 0.01-5h. The diethyl carbonate is synthesized by directly using the CO2, the epoxy compound and the ethanol, so the yield and selectivity of the target product are relatively high, the production cost of the diethyl carbonate can be reduced, and the diethyl carbonate has good industrial application value.

Description

technical field [0001] The present invention relates to a synthesis method of diethyl carbonate, in particular to a method of directly esterifying diethyl carbonate and co-producing dihydric alcohols with epoxy compounds, carbon dioxide and ethanol as raw materials in the presence of a catalyst, which belongs to organic chemicals The field of synthetic technology. Background technique [0002] Diethyl carbonate, referred to as DEC, the carbonyl, ethoxy, and ethyl groups in the molecule have good reactivity, and can be used as carbonylation and ethylation reagents, and have important applications in the fields of organic synthesis, pharmaceuticals, and engineering plastics. DEC itself is a low-toxic substance that will gradually decompose when released into the environment to produce ethanol and carbon dioxide. It is an environmentally friendly chemical and can be used as a green solvent for resins, oils, nitrocellulose, and cellulose ether. Diethyl carbonate has a higher ox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/00C07C69/96C07C68/04C07C31/20C07C29/128C07C41/03C07C43/13C07D317/38
CPCC07C29/128C07C41/03C07C68/04C07C69/96C07C31/202C07C31/205C07C43/13Y02P20/141
Inventor 李会泉王利国辛淑敏李凤姣贺鹏曹妍
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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