Method of manufacturing thioacetic acid

A technology of thioacetic acid and hydrogen sulfide, applied in the direction of organic chemistry, can solve the problems of low yield, low yield and content, and high cost

Inactive Publication Date: 2008-01-23
WEIFANG HAISHUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the methods used by people to synthesize thioacetic acid mainly include the reaction of glacial acetic acid and phosphorus pentasulfide to produce, because of its difficult separation, low yield, poor quality, high cost, and serious environmental pollution, or the synthesis reaction of acetic anhydride and hydrogen sulfide Production of thioacetic acid, but this method is technically difficult, difficult to operate, and in the process of synthesis and preparation, it is easy to generate H 2 The leakage of S gas and waste glacial acetic acid by-products cause pollution to the external environment, and the thioacetic acid produced by synthesis is severely decomposed and separated in the subsequent purification process, and the yield and content are very low, and the content is lower than 93%. , not only reduces the quality of the product, but also causes a certain waste of materials

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  • Method of manufacturing thioacetic acid

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Experimental program
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Effect test

Embodiment 1

[0026] Sodium sulfide sodium sulfide is produced by using carbon and Glauber's salt;

[0027] First check the airtightness of all operating equipment to ensure that there are no leak points. Put 800 kilograms of industrial acetic anhydride into the 1000L glass-lined reaction tank, and after sealing it, start stirring. Pour two prepared liquids (1300 kg 50% sulfide lye and 2000 kg 30% hydrochloric acid) into the measuring cylinders of sulfide alkali and hydrochloric acid respectively, turn on the gas generator to stir, and put sulfide lye into the gas generator at the same time And hydrochloric acid liquid, at this time will react to generate hydrogen sulfide gas. Open the exhaust valve, pass into the reaction tank through 20 kg of calcium chloride-dried hydrogen sulfide gas, pay attention to keep the reaction temperature in the glass-lined reaction tank, and keep the liquid at 50 ° C, (because the low temperature will affect the reaction speed, the temperature If it is too h...

Embodiment 2

[0031] Sodium sulfide sodium sulfide is produced by using carbon and Glauber's salt;

[0032] First check the airtightness of all operating equipment to ensure that there are no leak points. Put 750 kilograms of industrial acetic anhydride into the 1000L glass-lined reaction tank, and after sealing it, start stirring. Pour two prepared liquids (1250 kg of 50% sulfide lye and 1950 kg of 30% hydrochloric acid) into the measuring cylinders of sulfide alkali and hydrochloric acid respectively, turn on the gas generator to stir, and put sulfide lye into the gas generator at the same time And hydrochloric acid liquid, at this time will react to generate hydrogen sulfide gas. Open the exhaust valve, pass into the reaction tank through 19 kg of calcium chloride-dried hydrogen sulfide gas, pay attention to keep the reaction temperature in the glass-lined reaction tank, and keep the liquid at 55 ° C, (because the low temperature will affect the reaction speed, the temperature If it is...

Embodiment 3

[0036] First check the airtightness of all operating equipment to ensure that there are no leak points. Put 850 kilograms of industrial acetic anhydride into the 1000L glass-lined reaction tank, and after sealing it, start stirring. Pour two prepared liquids (1350 kg 50% sulfide lye and 2050 kg 30% hydrochloric acid) into the measuring cylinders of sulfide alkali and hydrochloric acid respectively, turn on the gas generator to stir, and put sulfide lye into the gas generator at the same time And hydrochloric acid liquid, at this time will react to generate hydrogen sulfide gas. Open the exhaust valve, pass into the reaction tank through 21 kg of calcium chloride-dried hydrogen sulfide gas, pay attention to keep the reaction temperature in the glass-lined reaction tank, and keep the liquid at 60 ° C, (because the low temperature will affect the reaction speed, the temperature If it is too high, it will be difficult to ventilate, and a bumping accident will occur) After reactin...

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Abstract

The invention discloses a preparation method of the thioacetic acid. The method is that the sodium sulphide produced by the carbon and the mirabilite is adopted to react with the hydrochloric acid to prepare the hydrogen sulfide, and then under the good air-tightness, the hydrogen sulphide gas processed by the dryer reacts with the acetic anhydride to gain the nearly colorless thioacetic acid with content not less than 95 per cent, boiling range of 88 DEG C. to 91DEG C., heavy metals less than 0.0002 per cent, melting point less than minus 17 DEG C. and flash point less than 1 DEG C. through reduced pressure distillation and rectification. The preparation method has convenient operation, which avoids the pollution on the external environment during production, greatly increases the purification of the product content and the product quality and lowers the production cost.

Description

technical field [0001] The present invention relates to a kind of preparation method of thioacetic acid. Background technique [0002] Thioacetic acid is a basic industrial raw material used in flavors, fragrances, pharmaceutical and chemical industries, molecular formula: C 2 h 4 OS, structural formula: [0003] [0004] Molecular weight: 76, content ≥98% (or ≥95%); color GB5, almost colorless; heavy metal <0.0001% (or <0.0002%); boiling range 87-91°C; specific gravity 1.075; melting point <-17°C ; Flash point 1°C. At present, the methods used to synthesize thioacetic acid mainly include the reaction of glacial acetic acid and phosphorus pentasulfide to produce, because of its difficult separation, low yield, poor quality, high cost, and serious environmental pollution, or the synthesis reaction of acetic anhydride and hydrogen sulfide Production of thioacetic acid, but this method is technically difficult, difficult to operate, and in the process of synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C327/06
Inventor 王俊刚
Owner WEIFANG HAISHUN CHEM
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