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Process for synthesizing cyclic carbonate

A technology of cyclic carbonate and complex, applied in the field of synthesizing cyclic carbonate, can solve the problems of difficult separation of product and catalyst, high catalyst cost, harsh conditions, etc., and achieves low cost, simple catalyst system and mild reaction conditions. Effect

Inactive Publication Date: 2005-01-19
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these catalyst systems have more or less problems such as low activity, harsh conditions, use of highly toxic organic solvents, high catalyst cost, and difficulty in separating the product from the catalyst.

Method used

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  • Process for synthesizing cyclic carbonate
  • Process for synthesizing cyclic carbonate
  • Process for synthesizing cyclic carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]

[0021] In a 70ml autoclave, add nickel chloride triphenylphosphine 0.05mmol, zinc powder 1mmol, n-Bu 4 NBr 0.2mmol, finally add 12.5 milliliters of propylene oxide (1a), replace the air in the kettle with carbon dioxide on the Schleck pipeline for three times, then continue to feed carbon dioxide under a certain pressure to make the system reach a dissolution equilibrium, and finally fill to Specifies the pressure. Close the reaction kettle, control the temperature by a temperature controller to slowly rise to 120°C for 1 hour, cool to room temperature, slowly release excess carbon dioxide, and distill the reaction liquid under reduced pressure to obtain propylene carbonate (2a). The selectivity is 99%, and the conversion frequency (TOF) is 3544h -1 .

Embodiment 2

[0023] Same as Example 1, the complex used is nickel chloride 1,3 diphenylphosphinopropane to obtain propylene carbonate (2a). The selectivity is 99%, and the conversion frequency (TOF) is 3401h -1 .

Embodiment 3

[0025] With embodiment 1, complex used is nickel chloride 1, and 1' diphenylphosphinoferrocene obtains propylene carbonate (2a). The selectivity is 99%, and the conversion frequency (TOF) is 3437h -1 .

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Abstract

The invention relates to a process for preparing cyclic carbonates from carbon dioxide and epoxy compound, wherein nickel-phosphonium complex and zinc powder reducing agent are used as the catalyst, quaternary ammonium salt is used as the catalyst promoter at a reaction temperature of 50-150 deg. C, the initial pressure of CO2 is 1.5-5Mpa, the reacting time is 0.5-6 hours.

Description

technical field [0001] The invention relates to a method for synthesizing cyclic carbonate from carbon dioxide and epoxy compound through cycloaddition reaction. Background technique [0002] Cyclic carbonate is a very good polar solvent, which is widely used in the synthesis of pharmaceuticals and fine chemical intermediates. Especially recently, people use ethylene carbonate as raw material to prepare dimethyl carbonate by transesterification with methanol, so that the demand for cyclic carbonate is increasing day by day. In recent decades, research in this area has received more and more attention. The reported catalyst systems include organic bases, quaternary ammonium salts, transition metal complexes, and MgO-Al 2 o 3 etc. (X.Yin, J.R.Moss, Coord.Chem.Rev.1999, 181, 27; R.L.Paddock, S.T.Nguyen, J.Am.Chem.Soc.2001, 121, 11498; Y.M.Shen, W.L.Duan, M.Shi , J. Org. Chem. 2003, 68, 1559). However, these catalyst systems have more or less problems such as low activity, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/34
Inventor 夏春谷李福伟胡斌陈革新
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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