Method for catalytically preparing propylene monothio-carbonate by ionic liquid

A technology of propylene monothiocarbonate and ionic liquid, which is applied in the field of ionic liquid catalyzed preparation of propylene monothiocarbonate, can solve the problems that ionic liquid catalysts have not yet been developed and applied, and achieve improved selectivity and conversion, reaction The effect of mild conditions and simple operation

Inactive Publication Date: 2018-09-04
CHANGSHU INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of monothiocarbonate requires the use of catalysts, and among the many catalysts that catalyze this reaction, ionic liquid catalysts have not been developed and applied yet.

Method used

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  • Method for catalytically preparing propylene monothio-carbonate by ionic liquid
  • Method for catalytically preparing propylene monothio-carbonate by ionic liquid
  • Method for catalytically preparing propylene monothio-carbonate by ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 2 grams of propylene oxide in a 10ml autoclave, add 1-butyl-3-methylimidazolium bromide borate ionic liquid catalyst by 2% of the mass of propylene oxide, under uniform stirring, feed carbon oxysulfide to 2 MPa pressure, reacted at 100°C for 1 hour, slowly degassed after cooling to room temperature, filtered to obtain the crude product liquid, and obtained propylene monothiocarbonate by distillation under reduced pressure, and the yield was measured by hydrogen nuclear magnetic spectrum, monothiocarbonic acid The yield results of propylene ester products are shown in Table 1 below.

Embodiment 2

[0022] Add 2 grams of propylene oxide in a 10ml autoclave, add 1-butyl-3-methylimidazolium fluoroborate ionic liquid catalyst according to 0.5% of the mass of propylene oxide, stir evenly, and feed carbon oxysulfide to 3 MPa pressure, react at 80°C for 2 hours, slowly release gas after cooling to room temperature, filter to obtain crude product liquid, obtain propylene monothiocarbonate through vacuum distillation, and measure the yield by hydrogen nuclear magnetic spectrum, monothiocarbonic acid The yield results of propylene ester products are shown in Table 1 below.

Embodiment 3

[0024] Add 2 grams of propylene oxide into a 10ml autoclave, add 1-butyl-3-methylimidazolium fluorophosphate ionic liquid catalyst according to 0.1% of the mass of propylene oxide, stir evenly, and feed carbon oxysulfide to 5 MPa pressure, reacted at 70°C for 6 hours, cooled to room temperature and slowly released gas, filtered to obtain the crude product liquid, and obtained monothiopropylene carbonate through vacuum distillation, and the yield was measured by nuclear magnetic hydrogen spectrum, monothiopropylene The ester product yield results are shown in Table 1 below.

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Abstract

The invention discloses a method for catalytically preparing propylene monothio-carbonate by ionic liquid. The method comprises the following steps: using carbon oxysulfide and epoxypropane as raw materials, and using the ionic liquid as a catalyst, reacting in a high-pressure reaction kettle, to obtain the propylene monothio-carbonate. The ionic liquid catalyst developed by the method has the advantages of high activity and high selectivity, and is capable of improving the selectivity and conversion rate of the carbon oxysulfide. The catalyst after vacuum distillation purification can be repeatedly used for a reaction of synthesizing the propylene monothio-carbonate by the carbon oxysulfide and the epoxypropane. A process of preparing the propylene monothio-carbonate is simple, the operation is simple and convenient, the reaction condition is gentle, a reaction rate is rapid, and the reaction process is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and in particular relates to a method for preparing propylene monothiocarbonate by catalyzing ionic liquids. Background technique [0002] Cyclic monothiocarbonate is a potential polar aprotic solvent, an intermediate in drug synthesis, and a monomer for preparing high refractive index resin polymonothiocarbonate. Therefore, it is of great value to study the synthesis of cyclic monothiocarbonates. [0003] Carbon oxysulfide is an air pollutant and an industrial waste gas, but it is also an important raw material for chemical synthesis. Cyclic monothiocarbonate is prepared by reacting carbon oxysulfide with epoxides. On the one hand, carbon oxysulfide can be effectively used to synthesize Valuable organic chemical products; on the other hand, this reaction has high atom economy and conforms to the principle of green chemistry. [0004] The inventor found in the experimental resea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 罗铭薛安琪左晓兵刘万辉杨刚周弟陈奠宇张黎伟余磊
Owner CHANGSHU INSTITUTE OF TECHNOLOGY
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