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Method for preparing dibasic alcohol

A diol and carbon dioxide technology, which is applied in the field of diol preparation, can solve problems such as difficulty in obtaining high-quality ethylene glycol, incomplete conversion of cyclic carbonates, and low selectivity of diols, and achieve effective The effect of utilization, high stability, and convenient circulation

Inactive Publication Date: 2011-05-18
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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AI Technical Summary

Problems solved by technology

Dow Chemical Company [WO: 98 / 14419, 1999] reported the conditions for the synthesis of ethylene glycol by catalyzing the hydrolysis of ethylene carbonate by alkali metal carbonate or bicarbonate, and improved the conversion rate of ethylene carbonate by increasing the reaction time, but it is difficult to obtain high quality ethylene glycol
[0005] And use the method for transesterification of cyclic carbonate and methyl alcohol to prepare dibasic alcohol because can co-produce dimethyl carbonate and also receive general attention at present, but there is incomplete conversion of cyclic carbonate in this method, and the selectivity of dibasic alcohol is not good. high disadvantage
[0006] There have been reports on the method of synthesizing cyclic carbonates in China, but the research on the synthesis of diols by hydrolysis of cyclic carbonates has not been reported yet.

Method used

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  • Method for preparing dibasic alcohol
  • Method for preparing dibasic alcohol
  • Method for preparing dibasic alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]

[0042] In a 100 ml autoclave, add 0.05 mmol of metal salt zinc chloride, 0.5 mmol of ionic liquid 1-methyl-3-butylimidazolium bromide and 0.4 mmol of tetrabutylammonium bromide, and finally add 20 ml of epoxy Propane (1a), a closed reaction kettle, the temperature is controlled by a temperature controller to slowly rise to 100 ° C, maintain a reaction pressure of 1.5 MPa, react for 1 hour, cool to room temperature, unload the kettle, and separate the catalyst from the reaction liquid through vacuum distillation. The corresponding cyclic carbonate (2a) is then obtained. In the autoclave, 2.8 grams of polystyrene-supported N-methylimidazolium bicarbonate ionic liquid and 12.96 grams of water were successively added to generate 40.9 grams of propylene carbonate (2a). Close the reaction kettle, the temperature is controlled by the temperature controller to rise slowly to 140°C, keep the reaction pressure at 1.5MPa, react for 4 hours, cool to room temperature, collect t...

Embodiment 2

[0044] With embodiment 1, used synthetic reaction metal salt is zinc bromide, and the selectivity of propylene glycol (3a) is 99%, and yield is 99%;

Embodiment 3

[0046] Same as Example 1, the cocatalyst used in the synthesis reaction is 0.05 mmol of 1-methyl-3-butyl imidazolium chloride salt, N-butyl pyrimidine bromide salt, the selectivity of propylene glycol (3a) is 99%, and the yield is 99%;

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Abstract

The invention discloses a method for preparing dibasic alcohol by hydrolyzing cyclic carbonate prepared from an epoxy compound and carbon dioxide. A system consisting of metal salt, ionic liquid and quaternary ammonium salt is taken as a catalyst in addition reaction, the cycloaddition of the carbon dioxide and the compound is catalyzed to prepare the cyclic carbonate, and the cyclic carbonate from which the catalyst is separated is subjected to hydrolysis reaction in the presence of a supported alkaline ionic liquid catalyst. The method can overcome the defects of high energy consumption and water ratio in the process of directly hydrating the epoxy compound, and also can overcome the defects of low conversion rate and selectivity of the method for preparing the dibasic alcohol through the ester exchange of the cyclic carbonate and methanol.

Description

technical field [0001] The present invention relates to a kind of preparation method of dibasic alcohol, more specifically, the present invention relates to a kind of method of preparing dibasic alcohol by hydrolysis of cyclic carbonate by epoxy compound and carbon dioxide. Background technique [0002] Dihydric alcohols, especially ethylene glycol, are widely used. They can be used to synthesize polymer compounds such as "polyester" (dacron), and can also be used as raw materials for films, rubber, plasticizers, desiccants, and brake fluids. Boiling point solvents, antifreeze for car radiators and refrigerants for aircraft engines. Ethylene glycol can also be used as a wetting agent for cellophane, fibers, leather, and adhesives. The vapor produced by heating ethylene glycol can be used as a stage smoke screen, and the nitrate ester of ethylene glycol is an explosive. [0003] China's large-scale ethylene glycol production mainly adopts the patented technologies of the wo...

Claims

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Application Information

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IPC IPC(8): C07C29/09C07C31/20
Inventor 夏春谷许传芝张愔陈静
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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