Method for preparing a 1,3-dioxolane compound

A technology of dioxolane and compound, applied in 1 field, can solve the problems of low ethylene glycol selectivity, high mass ratio, large energy consumption and the like

Active Publication Date: 2009-09-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the existing ethylene glycol production process is that the mass ratio of water to ethylene oxide is high (about 10:1), and at the same time, the selectivity of ethylene glycol is low, the process is long, and the energy consumption is large. A large amount of energy in the production is used for Moisture in evaporated products

Method used

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  • Method for preparing a 1,3-dioxolane compound
  • Method for preparing a 1,3-dioxolane compound
  • Method for preparing a 1,3-dioxolane compound

Examples

Experimental program
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Effect test

Embodiment 1

[0101] Embodiment 1: Preparation of 2,2-dimethyl-1,3-dioxolane

[0102] Add 21.2 grams of acetone and 4.4 grams of ethylene oxide into the 100ml polytetrafluoroethylene-lined reaction kettle, add 1.8 grams of zinc trifluoromethanesulfonate quickly, close the reaction kettle, and heat it in an oil bath at 55 ℃ magnetic stirring reaction for 8 hours, down to room temperature sampling analysis. The conversion rate is 98.77%, the selectivity is 99.06%, and the yield is 97.84%.

[0103] The composition of the reaction product liquid was analyzed by gas chromatography: the total content of by-products was 0.2%w. And it is 0.4%w in the document EP0448157B1.

Embodiment 2

[0104] Example 2: Preparation of 2,2-dimethyl-1,3-dioxolane

[0105] Add 11.6 grams of acetone and 4.4 grams of ethylene oxide into the reaction kettle with 100ml polytetrafluoroethylene lining, add 1.4 grams of zinc trifluoromethanesulfonate quickly, close the reaction kettle, heat in an oil bath, at 65 ℃ magnetic stirring reaction for 8 hours, down to room temperature sampling analysis. The conversion rate is 90.05%, the selectivity is 89.92%, and the yield is 80.97%.

Embodiment 3

[0106] Embodiment 3: Preparation of 2-methyl-2-ethyl-1,3-dioxolane

[0107] Add 28.8 grams of methyl ethyl ketone, 4.4 grams of ethylene oxide and 1.8 grams of zinc trifluoromethanesulfonate in a 100ml polytetrafluoroethylene-lined reaction kettle, close the reaction kettle, and react for 8 hours under heating in an oil bath at 55°C. Sample analysis at room temperature. The conversion rate is 99.71%, the selectivity is 96.69%, and the yield is 96.41%. Example 4: Preparation of 2-methyl-2-ethyl-1,3-dioxolane

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Abstract

The invention relates to a method for preparing a 1, 3-dioxolane compound. With the catalysis of zinc trifluoromethanesulfonate, an epoxy compound reacts with ketone or aldehyde to generate the 1, 3-dioxolane compound and the rate of conversion is increased. The method can be applied to the development of a new production technology that ethylene alcohol is prepared by the hydrolysis of epoxy ethane in the field of petrochemical industry, save energy and reduce investment in equipment.

Description

technical field [0001] The invention relates to a preparation method of 1,3-dioxolane compounds, in particular to a preparation method of 2,2-dialkyl-1,3-dioxolane and its hydrolysis method for preparing ethylene glycol. Background technique [0002] The preparation method of 1,3-dioxolane compounds is classified according to reactants, and generally has two kinds: the first, with adjacent diol compounds and carbonyl-containing compounds (aldehydes or ketones) as reactants, the reaction generates 1 , 3-dioxolane compounds and water; second, epoxy compounds react with aldehydes or ketones to generate 1,3-dioxolane compounds. In the field of organic synthesis, the first method is commonly used in the protection of ortho-dihydroxyl or carbonyl functional groups and the gas chromatography analysis of ortho-diol compounds; the second method is less reported in the literature, and the examples with potential industrial application value are in Under the action of catalyst, react ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/10
Inventor 谢伦嘉王伟亢宇赵思源田宇冯华升
Owner CHINA PETROLEUM & CHEM CORP
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