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Process for the preparation of olefinic esters from epoxides and carbon dioxide

An epoxide and carbon dioxide technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc., can solve the problem of easy loss of active components, low activity of heterogeneous catalysts, etc. question

Active Publication Date: 2016-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is the problem of low activity of heterogeneous catalysts and easy loss of active components in the prior art, and a new method for preparing ethylene carbonate from epoxide and carbon dioxide is provided

Method used

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  • Process for the preparation of olefinic esters from epoxides and carbon dioxide
  • Process for the preparation of olefinic esters from epoxides and carbon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] At room temperature, 12.4gKNO 3 and 106.9gAl(NO 3 ) 3 9H 2 O was dissolved in 200mL of deionized water, and then 10g of SBA-15 (specific surface area 671m 2 / g), after stirring for 0.5h, slowly evaporate to dryness at 50°C. The obtained solid was dried overnight in an oven at 90°C, and then calcined at 350°C for 10 hours to obtain the catalyst. The catalyst is used for the reaction of propylene oxide and carbon dioxide, the conditions are as follows: add 150.0g propylene oxide and 5.0g catalyst in a 300mL autoclave, fill with 1.0MPaCO 2 , heated up to 140°C, and filled with CO 2 , maintain the reaction pressure at 4.0MPa, remove the catalyst by filtration after 3 hours of reaction, the measured conversion rate of propylene oxide is 81.2%, the selectivity of propylene carbonate is 99.1%, and the yield is 80.5%.

Embodiment 2

[0019] At room temperature, 0.5gNa 2 SO 4 and 1.4gGa(NO 3 ) 3 9H 2 O was dissolved in 200 mL of deionized water, and then 10 g of SiO 2 (DegussaA380, specific surface area 376m 2 / g), after stirring for 5h, evaporate to dryness at 120°C. The obtained solid was dried overnight in an oven at 140°C, and then calcined at 800°C for 10 hours to obtain the catalyst. The catalyst was used for the reaction of propylene oxide and carbon dioxide under the same conditions as [Example 1], the conversion rate of propylene oxide was 24.1%, the selectivity of propylene carbonate was 99.2%, and the yield was 23.9%.

Embodiment 3

[0021] At room temperature, 2.7gLiNO 3 and 8.7gAl(NO 3 ) 3 9H 2 O was dissolved in 200mL of deionized water, and then 10g of MCM-41 (specific surface area 1012m 2 / g), stirred for 3 hours, and evaporated to dryness at 100°C. The obtained solid was dried overnight in an oven at 120°C, and then calcined at 500°C for 5 hours to obtain the catalyst. The catalyst was used for the reaction of propylene oxide and carbon dioxide under the same conditions as [Example 1], the conversion rate of propylene oxide was 59.1%, the selectivity of propylene carbonate was 98.4%, and the yield was 58.2%.

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Abstract

The invention relates to a method for preparing alkenyl carbonate from epoxide and carbon dioxide, and mainly solves the problems of low activity of heterogeneous catalyst and easy loss of active components in the prior art. The method comprises the following steps: taking epoxide and carbon dioxide as the raw materials, controlling the reaction temperature in a range of 50 to 200 DEG C, the reaction pressure in a range of 0.1 to 10.0 MPa, and the weight ratio of the catalyst to epoxide in a range of 0.005 to 0.5, and contacting the reaction raw materials with the catalyst to carry out reactions so as to obtain the alkenyl carbonate; wherein the catalyst is composed of the following components in percentage by weight: (a) 0.5 to 20% of alkali metal oxides M2O, wherein M is selected from Li, Na, K, Rb, or Cs; (b) 0.5 to 50% of metal oxides X2O3, wherein the X is selected from Al or Ga; (c) 30 to 99% of carrier, wherein the carrier is selected from at least one component of SiO2, SBA-15, MCM-41, MCF, HMS, KIT-6, SBA-16 and diatomite. The method solves the problems mentioned above and is capable of being applied to the industrial alkenyl carbonate production using epoxide and carbon oxide as the raw materials.

Description

technical field [0001] The present invention relates to a method for preparing olefinic esters from epoxides and carbon dioxide. Background technique [0002] Ethylene carbonate is a kind of excellent solvent and fine chemical intermediate, and is a potential basic raw material of organic chemical industry. At the same time CO 2 It is a kind of greenhouse gas, how to effectively fix it has become one of the most challenging topics in this century, and through epoxide and CO 2 The reaction synthesis of olefinic ester is one of the good immobilization methods. As the recent co-production of dimethyl carbonate, ethylene glycol, and propylene glycol using ethylene carbonate as raw material has attracted increasing attention, the fixation of CO by cyclic olefinic ester 2 approach has also received increasing attention. [0003] The method majority of reported production cyclic olefinic carbonate is to use the binary homogeneous catalyst that Lewis acid metal compound and Lewi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36C07D317/38B01J29/03B01J23/08B01J29/70B01J23/04
CPCC07D317/36C07D317/38
Inventor 陈梁锋何文军
Owner CHINA PETROLEUM & CHEM CORP