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Preparation method of potassium thioacetate

A technology of potassium thioacetate and potassium carbonate, which is applied in the field of preparation of potassium thioacetate, can solve the problems of high production cost, reaction with water, and easy oxidation of air, etc., to reduce production cost, increase yield, and reduce loss Effect

Pending Publication Date: 2017-06-13
绍兴市上虞区耕创化工技术服务部
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] 1. The obtained potassium thioacetate has low purity and contains more potassium carbonate and potassium bicarbonate
[0012] 2. High energy consumption and low yield
[0013] 3. CH3COSK is highly water-absorbing, easy to oxidize when exposed to air, and will react with water for a long time at high temperature
However, due to the reaction between thioacetic acid and potassium hydroxide, a large amount of water is generated, alcohols need to be recycled and reused, and more expensive potassium hydroxide is used, so the production cost is relatively high
Owing to decompressing and reclaiming anhydrous alcohol solvent first, the potassium thioacetate that separates out contains unreacted potassium hydroxide, causes the purity of potassium thioacetate to be not high

Method used

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  • Preparation method of potassium thioacetate
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  • Preparation method of potassium thioacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Please refer to figure 1 , the preparation method of potassium thioacetate in the figure, comprises the steps:

[0042] a, forming potassium thioacetate synthetic material:

[0043] In a 500L conical ribbon vacuum dryer, add 190kg of potassium carbonate or potassium bicarbonate, start the ribbon stirring, add 200kg of thioacetic acid, after stirring evenly, add 10kg of water by spraying, then turn on the vacuum, the vacuum degree -0.01MPa, heat up to 40°C, heat up for 20 minutes, after the temperature reaches 40°C, keep warm for 2 hours, ready for use;

[0044] b. Dissolution and separation:

[0045] In a 1000L reaction pot, add 200L of anhydrous solvent, start stirring, put in the above synthetic material, stir for half an hour, and filter after potassium thioacetate is fully dissolved; the filter residue is washed with anhydrous solvent, due to potassium carbonate and bicarbonate Potassium is almost insoluble in this anhydrous solvent, so the filter residue is pota...

Embodiment 2

[0055] Please refer to figure 1 , the preparation method of potassium thioacetate in the figure, comprises the steps:

[0056] a, forming potassium thioacetate synthetic material:

[0057] In a 500L conical ribbon vacuum dryer, add 240kg of potassium carbonate or potassium bicarbonate, start the ribbon stirring, add 200kg of thioacetic acid, after stirring evenly, add 20kg of water by spraying, then turn on the vacuum, the vacuum degree 0.09MPa, heat up to 80°C, heat up for 30 minutes, after the temperature reaches 80°C, keep warm for 5 hours, ready for use;

[0058] b. Dissolution and separation:

[0059] In a 1000L reaction pot, add 800L of anhydrous solvent, start stirring, put in the above synthetic material, stir for half an hour, and filter after potassium thioacetate is fully dissolved; the filter residue is washed with anhydrous solvent, due to potassium carbonate and bicarbonate Potassium is almost insoluble in this anhydrous solvent, so the filter residue is potassi...

Embodiment 3

[0069] Please refer to figure 1 , the preparation method of potassium thioacetate in the figure, comprises the steps:

[0070] a, forming potassium thioacetate synthetic material:

[0071] In a 500L conical ribbon vacuum dryer, add 220kg of potassium carbonate or potassium bicarbonate, start ribbon stirring, add 200kg of thioacetic acid, after stirring evenly, add 15kg of water by spraying, then turn on the vacuum, the vacuum degree -0.06MPa, heat up to 60°C, heat up for 25 minutes, after the temperature reaches 60°C, keep warm for 3 hours, ready for use;

[0072] b. Dissolution and separation:

[0073] In a 1000L reaction pot, add 600L of anhydrous solvent, start stirring, put in the above synthetic material, stir for half an hour, and filter after potassium thioacetate is fully dissolved; the filter residue is washed with anhydrous solvent, due to potassium carbonate and bicarbonate Potassium is almost insoluble in this anhydrous solvent, so the filter residue is potassiu...

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Abstract

The invention discloses a preparation method of potassium thioacetate. The method comprises the following steps of adding 190-240kg of potassium carbonate or potassium bicarbonate to a 500L tapered helical tape vacuum drier, and starting helical tape stirring; adding 200kg of thioacetic acid, stirring evenly, and then adding 10-20kg of water in a spray manner; starting vacuum, wherein the vacuum degree is -0.01MPa to -0.09MPa; and heating to 40-80 DEG C for 20-30min and carrying out heat preservation reaction for 2-5h after the temperature reaches 40-80 DEG C for later use. The technical problem of how to efficiently prepare the potassium thioacetate at low cost can be solved.

Description

technical field [0001] The invention relates to a preparation method of potassium thioacetate. Background technique [0002] Potassium thioacetate is also called potassium thioacetate, potassium ethyl thiolate, potassium thioacetate, potassium thioacetate, etc. It is a white crystalline powder with a melting point of 173°C-176°C. It is mainly used in molecular structure The introduction of sulfur atoms and the synthesis of anti-AIDS drugs, etc. [0003] The traditional process step of making above-mentioned potassium thioacetate is: [0004] 1. Dissolve 100kg of potassium carbonate in 200kg of water, add 100kg of thioacetic acid dropwise, and the temperature is 80°C; [0005] 2. Add 5kg of activated carbon to the above synthetic liquid, and reflux for decolorization; [0006] 3. Cool the decolorizing solution, separate out and filter unreacted excess potassium carbonate, potassium bicarbonate, and activated carbon to obtain a clear solution; [0007] 4. Concentrate the c...

Claims

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Application Information

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IPC IPC(8): C07C327/06
CPCC07C327/06
Inventor 陶陈丁
Owner 绍兴市上虞区耕创化工技术服务部
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