Preparation method of thioacetic acid potassium

A technology of potassium thioacetate and thioacetic acid, which is applied in the direction of organic chemistry, can solve the problems of high cost, many wastes, and low utilization rate, and achieve the effect of mild reaction conditions, less environmental pollution, and complete reaction

Inactive Publication Date: 2007-10-03
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned reaction, because its used 1-butanol is a water-containing alcoholic solvent (generally 70% concentration), the yield of potassium thioacetate is low and repeated operations are difficult, and because hydrogen sulfide is not obtained more in this reaction Adequate reaction, low utilization rate, resulting in a large amount of hydrogen sulfide, high cost, and a lot of three wastes, especially waste gas, causing serious pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation of embodiment 1 thioacetic acid

[0016] In a 1000ml autoclave, put 4.2g of sodium polysulfide, 168.2g (2.0mol) of diketene, and 1.0g of dibutylhydroxytoluene (BHT) into 168ml of isobutanol solution, cool with refrigerated brine, and feed hydrogen sulfide gas to Stir at 0.1Mpa, keep the pressure for 2 hours, control the temperature at 0-5°C, take a sample of GC and analyze the diketene below 1%, indicating that the thiolation is complete, release the pressure to another reactor of the same type, return to normal pressure, and turn to 500ml intermittent distillation In the bottle, add 0.5ml of dichloroacetic acid as a stabilizer, recover under reduced pressure to obtain 420 g of a mixture of thioacetic acid and isobutanol, and the thioacetic acid content is 70% according to GC analysis. Atmospheric distillation collected fractions at 89-92°C to obtain 273.6 g (3.6 mol) of thioacetic acid, with a yield of 90%. GC analysis content was 99%.

Embodiment 2

[0017] The preparation of embodiment 2 potassium thioacetate

[0018] Add potassium hydroxide 168.2g in 2000ml flask, butylated hydroxytoluene (BHT) 0.2g and anhydrous isobutanol 1500ml stir and dissolve, cool to about 0 ℃ with frozen brine, add dropwise the thioacetic acid that embodiment 1 reclaims and The mixture of isobutanol is 260g, containing 182g (2.4mol) of thioacetic acid, and the time of dropping is controlled to be 1.5 hours. After the drop is completed, stir at room temperature for 1 hour, control the temperature below 60°C, and recover isobutanol under reduced pressure until white The crystals were frozen to 0°C, filtered, washed with isobutanol, and dried to obtain 251.7 g of white crystals, with a yield as high as 92%.

Embodiment 3

[0019] The preparation of embodiment 3 potassium thioacetate

[0020] Add potassium hydroxide 40g in 1000ml flask, butylated hydroxyanisole (BHA) 0.5g and anhydrous n-butanol 500ml stir and dissolve, cool to about 5 ℃ with freezing brine, dropwise add the thioacetic acid 50g that embodiment 1 prepares ( 0.658mol), control the dropping time for 1 hour, after the dropping, stir at room temperature for 1 hour, control the temperature below 50°C, recover n-butanol under reduced pressure until white crystals are precipitated, freeze to 0°C, filter, and wash with n-butanol , dried to obtain 72 g of white powder, based on thioacetic acid yield of 96%.

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Abstract

This invention relates to a preparation method of thioacetic acid kalium. In existing method, hydrogen sulfide does not has plenary reaction, so utilization ratio is low, result in hydrogen sulfide dosage is large, cost high and three waste are too many, especially in exhaust gas, has serious pollution to environment. This invention uses ketene dimer and sodium polysulfide to inlet hydrogen sulfide gas to absolute alcohol solvent, add antioxidant, after completeness thio reaction, rectify to gain thioacetic acid and absolute alcohol solvent; add thioacetic acid or its hybrid with absolute alcohol solvent by distribution droplets to absolute alcohol solvent of potassium hydroxide, whipping, decompress and reclaim absolute alcohol solvent, and the precipitable white crystal is thioacetic acid kalium.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a preparation method of potassium thioacetate. Background technique [0002] Potassium thioacetate is an important thio reagent in organic compound reactions, and has a wide range of uses. Organic.Syntheses, CV4, 928 describes the use of acetic anhydride to feed the required H under the condition of a small amount of sodium hydroxide. 2 S, then fast distillation to separate thioacetic acid and acetic acid from sodium salt, and then rectify and separate thioacetic acid with a yield of 72-76%. In the literature, acetic acid and phosphorus pentoxide, acetyl chloride and thiocyanate are also used Potassium sulfur, diacetyl sulfide hydrolysis, acetic anhydride and hydrogen sulfide react in acidic medium or under triethylamine and pyridine, and acetyl chloride and hydrogen sulfide react in the presence of aluminum trichloride, acetic anhydride and hydrogen sulfi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C327/06
Inventor 陈建辉王红卫丁建清
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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