Preparation method and production device of thioacetic acid

A technology for thioacetic acid and production equipment, applied in chemical instruments and methods, organic chemistry, phosphorus compounds, etc., can solve problems such as complex production equipment, unsatisfactory yield and purity of thioacetic acid, and difficult control of the reaction process , to achieve high economical effect

Pending Publication Date: 2018-07-24
兖矿水煤浆气化及煤化工国家工程研究中心有限公司 +1
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Problems solved by technology

[0003] The process of using hydrogen sulfide as raw material is relatively complicated and dangerous, and generally requires an independent hydrogen sulfide preparation device
Using the synthesis process of phosphorus pentasulfide and acetic acid as raw materials, it is obtained by co-heating distillation of acetic acid and phosphorus pentasulfide, heating to 91 ° C to start distilling thioacetic acid, the co-heating process needs to monitor the temperature from time to time not to be higher than 100 ° C, and at the same time to prevent bumping, Therefore, the

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  • Preparation method and production device of thioacetic acid
  • Preparation method and production device of thioacetic acid
  • Preparation method and production device of thioacetic acid

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preparation example Construction

[0064] The invention provides a kind of preparation method of thioacetic acid, comprising:

[0065] A) Mix the acetic acid solution, phosphorus pentasulfide and the catalyst to obtain a mixed solution after the reaction; the temperature of the reaction is not higher than 50° C., the pressure of the reaction is -0.1 to 0.5 MPa, and the reaction time is 1 to 12 hours;

[0066] The catalyst is selected from one or more of low molecular alcohol, acid solution and water;

[0067] B) The mixed solution is subjected to solid-liquid separation for the first time, and the obtained liquid phase substance is rectified to obtain thioacetic acid.

[0068] In the invention, the acetic acid solution, the phosphorus pentasulfide and the catalyst are firstly mixed, and the mixed solution is obtained after the reaction.

[0069] The present invention has no special limitation on the preparation method of the acetic acid solution, and the preparation method of the solution well known to those s...

Embodiment 1

[0156] Mix 1000 g of fresh acetic acid solution with a content of 95 wt %, 400 g of flaky phosphorus pentasulfide from which metal impurities have been removed, and 20 g of aqueous methanol solution with a mass fraction of 95 wt %, and react in a reactor at 45 ° C and normal pressure for 3 to 5 hours to obtain a mixed solution. The mixed solution is carried out solid-liquid separation for the first time in the first filter, and the obtained liquid phase material is carried out rectification for the first time in the first rectification tower, and the tower bottom temperature of the rectification for the first time is The temperature at the top of the first rectification is 115.5°C, the pressure of the first rectification is -0.05MPa, the time of the first rectification is 30min, and the light components with a boiling point of 60-119°C are obtained . The heavy component obtained after the first rectification is mixed with water according to the mass ratio of 65:1, hydrolyzed ...

Embodiment 2

[0159] Mix 400 g of fresh acetic acid solution with a content of 95 wt%, 600 g of rectified acetic acid solution for reuse, 400 g of flaky phosphorus pentasulfide for removal of metal impurities, and 20 g of ethylene glycol, and react in a reaction kettle at 35° C. under normal pressure for 3 to 5h, a mixed solution was obtained. The mixed solution is carried out solid-liquid separation for the first time in the first filter, and the obtained liquid phase material is carried out rectification for the first time in the first rectification tower, and the tower bottom temperature of the rectification for the first time is The temperature at the top of the first rectification is 115°C, the pressure of the first rectification is -0.05MPa, the time of the first rectification is 30min, and the light components with a boiling point of 60-119°C are obtained . The heavy component obtained after the first rectification is mixed with water according to the mass ratio of 65:1, hydrolyzed ...

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Abstract

The invention discloses a preparation method and a production device of thioacetic acid. The thioacetic acid is obtained through carrying out low temperature reaction by adopting acetic acid and phosphorus pentasulfide under the action of a specific catalyst, carrying out solid-liquid separation, and carrying out distillation separation on a liquid phase. A solid-phase substance obtained through solid-liquid separation for the first time is further extracted and purified, so that a byproduct potassium phosphate is obtained. Low-price and easy-to-get raw materials and the catalyst are adopted and can be reacted to synthesize to obtain the thioacetic acid at lower temperature and pressure intensity and even at normal pressure and temperature, solid-liquid separation is carried out to obtainthe liquid phase, and the liquid phase is subjected to distillation separation so as to obtain the thioacetic acid with high purity and high yield. Through further extracting and purifying the solid-phase substance obtained through solid-liquid separation for the first time, the high-value-added byproduct potassium phosphate with high purity and high yield is obtained from the waste liquid, so that the preparation method is friendly to the environment and has higher economical efficiency.

Description

technical field [0001] The invention relates to the technical field of preparing chemical intermediates, in particular to a preparation method and production device of thioacetic acid. Background technique [0002] Thioacetic acid is a fine chemical intermediate with certain corrosiveness and wide application. The synthesis process of thioacetic acid is mainly divided into two routes, one is to use hydrogen sulfide and acetic anhydride to react to generate thioacetic acid. The second is to use phosphorus pentasulfide to react with acetic acid to generate thioacetic acid. [0003] The process of using hydrogen sulfide as raw material is relatively complicated and dangerous, and generally requires an independent hydrogen sulfide preparation device. Using the synthesis process of phosphorus pentasulfide and acetic acid as raw materials, it is obtained by co-heating distillation of acetic acid and phosphorus pentasulfide, heating to 91 ° C to start distilling thioacetic acid, ...

Claims

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Application Information

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IPC IPC(8): C07C327/06C01B25/30
CPCC01B25/30C07C327/06C01P2006/80
Inventor 李智吴永国王艳李涛王振华刘海燕赵梅梅王红星刘峰张彦路文学郭宝贵
Owner 兖矿水煤浆气化及煤化工国家工程研究中心有限公司
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