Preparation of cyclic carbonic ester with high-activity catalyst

A high-activity catalyst, cyclic carbonate technology, used in clean catalysis and green fields, can solve the problems of harsh reaction conditions, high catalytic cost, low stability, etc., and achieve convenient preparation, high catalytic activity, and good thermal stability. Effect

Inactive Publication Date: 2006-08-16
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology

[0003] The currently reported catalysts for the production of cyclic carbonates mainly include: alkali metal halides, alkaline earth metal halides, organic bases, quaternary ammonium salts, imidazolium salts, metal oxides, transition metal complexes, and tetradentate Schiff alkali metal complexes. However, these catalyst systems have more or less problems such as low catalytic activity, low stability, harsh reaction conditions, use of highly toxic organic solvents, and high catalytic costs.

Method used

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  • Preparation of cyclic carbonic ester with high-activity catalyst
  • Preparation of cyclic carbonic ester with high-activity catalyst
  • Preparation of cyclic carbonic ester with high-activity catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]

[0027] Implementation method: In a 100ml stainless steel autoclave, add 0.059mmol of zinc bromide and 0.35mmol of triphenylhexylphosphine bromide in sequence, and finally add 20ml of propylene oxide (1a), seal the autoclave, and fill it with an appropriate amount of carbon dioxide , the temperature is controlled by the temperature controller to slowly rise to 120 ° C, and then the carbon dioxide pressure is controlled to 1.5 MPa, react for 1 hour, cool to room temperature, unload the kettle, and after the excess carbon dioxide is absorbed by saturated sodium carbonate solution, the obtained liquid is distilled under reduced pressure Get the product propylene carbonate (2a), weigh it, and calculate the yield and conversion frequency (TOF) (TOF=product amount / transition metal salt amount / reaction time). After chromatographic mass spectrometry and nuclear magnetic analysis, the product purity is greater than 99.0%, the best separation yield is 98.0%, the selectivity is...

Embodiment 2

[0029] Same as Example 1, the binary catalyst system used is zinc chloride and triphenylhexylphosphine bromide to obtain propylene carbonate (2a). The selectivity is 99.0%, and the conversion frequency (TOF) is 4638.4h -1 .

Embodiment 3

[0031] Same as Example 1, the binary catalyst system used is zinc iodide and triphenylhexylphosphine bromide to obtain propylene carbonate (2a). The selectivity is 99.0%, and the conversion frequency (TOF) is 4807.5h -1 .

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Abstract

Production of cyclic carbonic acid ester from high-activity catalyst is carried out by utilizing efficient binary catalyst with transition metal salt and quaternary alkylphosphonium salt halide ionic liquid, cycloaddition reacting at 313.15-483.15K and 0.1-5.0Mpa and synthesizing cyclic carbonic acid ester. It is simple and clean, has recovery rate and selectivity and can be re-used.

Description

Technical field: [0001] The invention relates to the technical field of green and clean catalysis, in particular to a method for synthesizing carbonates by cycloaddition reaction of carbon dioxide and epoxy compounds. Background technique: [0002] Carbon dioxide is a greenhouse gas and an inexhaustible C1 resource. The effective fixation of carbon dioxide has become one of the most challenging issues in this century. The synthesis of cyclic carbonates is one of the good immobilization approaches. Cyclic carbonate is a very good polar solvent, and it has been widely used in the synthesis of pharmaceutical and fine chemical intermediates. Especially recently, the economic value and industrial demand of ethene carbonate as raw material for the preparation of carbonic acid diester and the synthesis of ethylene glycol with water by using methanol transesterification are increasing. In recent years, research on this aspect has received more and more attention. [0003] The cur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/34B01J31/02
Inventor 张锁江孙剑张香平李增喜成卫国
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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