Novel method for preparing potassium thioacetate

A technology of potassium thioacetate and thioacetic acid, which is applied in the direction of organic chemistry, can solve problems such as low purity of potassium thioacetate, easy oxidation of air, and catalyst poisoning, so as to improve equipment use efficiency, prevent products from absorbing moisture, Reduce the effect of mother liquor residue

Pending Publication Date: 2020-06-19
陶陈丁
View PDF3 Cites 1 Cited by
  • 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 reac

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Novel method for preparing potassium thioacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Turn on the tail gas absorption system, add 550kg of absolute ethanol to the 1500L jacketed glass-lined reactor, put refrigerant ice salt water into the jacket, start stirring, the speed is 50-90 rpm, add 360kg Potassium carbonate, and the temperature in the reactor is controlled at -15 to 20°C;

[0053] (2) Slowly add 400kg of thioacetic acid dropwise to the reaction kettle at a rate of 80Kg / hour; the reaction is exothermic, and the temperature of the kettle is controlled at -15 to 20°C by using jacketed ice salt water. ~20°C constant temperature reaction for 10 hours; after the constant temperature reaction, control the temperature in the reactor at -10~10°C and prepare for centrifugation;

[0054] (3) Turn on the centrifuge, make it run slowly, and flush nitrogen into the centrifuge to improve the safety factor and reduce the contact between the product and the air. Slowly put the reactants obtained in step (2) into the centrifuge In the centrifuge, the potassiu...

Embodiment 2

[0059] (1) Turn on the tail gas absorption system, add 500kg of absolute ethanol to the 1500L jacketed glass-lined reactor, put refrigerant ice salt water into the jacket, start stirring, the speed is 50-90 rpm, add 355kg Potassium carbonate, and the temperature in the reactor is controlled at -10 to 30°C;

[0060] (2) Slowly add 400kg of thioacetic acid dropwise to the reaction kettle at a rate of 80Kg / hour; the reaction is exothermic, and the temperature of the kettle is controlled at -10 to 30°C by using jacketed ice salt water. After the addition of thioacetic acid is completed, the temperature is controlled at -10 React at a constant temperature of ~30°C for 10 hours; after the constant temperature reaction is completed, control the temperature in the reactor at -10-20°C and prepare for centrifugation;

[0061] (3) Turn on the centrifuge, make it run slowly, and flush nitrogen into the centrifuge to improve the safety factor and reduce the contact between the product and ...

Embodiment 3

[0066] (1) Turn on the tail gas absorption system, add 550kg of absolute ethanol to the 1500L jacketed glass-lined reactor, put refrigerant ice salt water into the jacket, start stirring, the speed is 50-90 rpm, add 360kg Potassium carbonate, and the temperature in the reactor is controlled at 0~40°C;

[0067] (2) Slowly add 400kg of thioacetic acid dropwise to the reaction kettle, and the dropping rate is 80Kg / hour; the reaction is exothermic, and the temperature of the kettle is controlled by jacketed ice salt water at 0-40°C. After the addition of thioacetic acid is completed, the temperature is controlled at 0-40 ℃ constant temperature reaction for 10 hours; after the constant temperature reaction is completed, control the temperature in the reactor at -5 ~ 30 ℃, and prepare for centrifugation;

[0068] (3) Turn on the centrifuge, make it run slowly, and flush nitrogen into the centrifuge to improve the safety factor and reduce the contact between the product and the air. ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a novel preparation method of potassium thioacetate, and belongs to the technical field of synthesis and purification. The method comprises the following steps: by taking high-concentration ethanol as a solvent, reacting thioacetic acid and potassium carbonate and crystallizing synchronously in the same reaction kettle in a low-temperature environment, and carrying out centrifugation, leaching, vacuum drying, vacuum packaging and other operations on the reaction product to obtain high-quality potassium thioacetate. According to the invention, the preparation method is simple in operation process, the product is high in yield, good in quality and beneficial to storage, the centrifuged mother liquor treatment method is environment-friendly, the product is subjected tovacuum drying and vacuum packaging, moisture absorption, hydrolysis, oxidation, discoloration and the like can be effectively prevented, the product quality is ensured, the purity of potassium thioacetate prepared by the method can reach 99.0% or above, and in a pharmaceutical process taking potassium thioacetate as a raw material, feeding is convenient, quality guarantee period is long, and customer use effect is good.

Description

technical field [0001] The invention relates to a new method for preparing potassium thioacetate, which belongs to the technical field of organic synthesis and purification. Background technique [0002] Potassium thioacetate (CAS No.: 10387-40-3), also known as potassium ethylthiolate, potassium thioacetate, etc., is a white crystalline powder with a melting point of 173°C to 176°C. It is mainly used for sulfur in the molecular structure. The introduction of 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 potassium carbonate in 200kg water, add 100kg thioacetic acid dropwise, the temperature is 80℃; [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 obtai...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C327/06
CPCC07C327/06
Inventor 陶陈丁
Owner 陶陈丁
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap