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Method for preparing sodium thiocarbonate by phase transfer catalytic method

A technology of phase transfer catalysis and sodium perthiocarbonate, which is applied in chemical instruments and methods, alkali metal carbonates, inorganic chemistry, etc., can solve the problems of long reaction time and low efficiency of phase transfer agent, and reduce the cost of preparation , rapid and efficient preparation, and the effect of reducing costs

Inactive Publication Date: 2007-11-28
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the synthesis of sodium perthiocarbonate still has a long reaction time, indicating that the efficiency of alcohol as a phase transfer agent is not high, and a condensing reflux device needs to be used for separation in the later stage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: 24gNa 2 S·9H 2 O solid was dissolved in 50mL distilled water, and the prepared sodium sulfide solution was filled into a three-necked flask; add 25mL CS 2 And 1.25mL pyrimidine borofluorotetraionic liquid. After the reaction system was reacted at room temperature and normal pressure for 10 minutes, the solution was transferred to a separatory funnel and allowed to stand for liquid separation. Then, crystallization of sodium perthiocarbonate was obtained after low temperature crystallization. Analysis by spectrophotometry showed that the conversion rate of sodium sulfide was 95.8%.

Embodiment 2

[0020] Embodiment 2: 24gNa 2 S·9H 2 O solid was dissolved in 50mL distilled water, and the sodium sulfide solution was filled into a three-necked flask; add 25mL CS 2 And 2.5mL pyrimidoborofluoro tetraionic liquid. After the reaction system was reacted at room temperature and normal pressure for 5 minutes, the solution was transferred to a separatory funnel and allowed to stand for liquid separation. Then, crystallization of sodium perthiocarbonate was obtained after low temperature crystallization. Analysis by spectrophotometry showed that the conversion rate of sodium sulfide was 94.7%.

Embodiment 3

[0021] Embodiment 3: 30gNa 2 S·9H 2 O solid was dissolved in 50mL distilled water, and the sodium sulfide solution was filled into a three-necked flask, and 30mL CS was added 2 and 2.4ml of pyrimidium chloride ionic liquid. The reaction system was irradiated under the microwave power of 1000W for 1min, the solution was transferred to a separatory funnel, and the liquid was separated by standing. Then, crystallization of sodium perthiocarbonate was obtained after low temperature crystallization. Analysis by spectrophotometry showed that the conversion of sodium sulfide was 99.5%.

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Abstract

The present invention discloses phase transfer catalysis process of preparing sodium sulfocarbonate. The process is one normal temperature and normal pressure reaction process of sodium sulfide and carbon disulfide in the presence of ionic liquid as the phase transfer catalyst. The process includes the steps of: mixing industrial pure carbon disulfide and sodium sulfide water solution, adding ionic liquid in 5-10 vol% of the carbon disulfide, reacting for 5-10 min, and cooling to separate out sodium sulfocarbonate crystal. The present invention has lowered phase interface between sodium sulfide or sodium hydroxide water solution and carbon disulfide, raised reaction rate at normal temperature and normal pressure, low sodium sulfocarbonate preparing cost.

Description

technical field [0001] The invention relates to a method for synthesizing sodium perthiocarbonate using ionic liquid as a phase transfer catalyst. Background technique [0002] Ionic liquids are substances composed of ions that are liquid at or near room temperature, and are also called room temperature ionic liquids, room temperature molten salts, or organic ionic liquids. Room temperature ionic liquids refer to ionic compounds that are liquid in a large temperature range near room temperature. It solves the instability problem of substances under high temperature conditions, so room temperature ionic liquids have great research and market potential. At present, domestic and foreign studies on ionic liquid chemistry mainly focus on the preparation of ionic liquids, characterization of physical and chemical properties, catalytic synthesis, extraction and separation, and electrochemistry. [0003] There are many kinds of ionic liquids, and different ionic liquids can be desi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D7/00
Inventor 刘作华杜军陶长元孙大贵李泽全张样盛
Owner CHONGQING UNIV