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Green synthesis process of antimony mercaptide

A green synthesis, mercaptan antimony technology, which is applied in the production of antimony organic compounds, compounds of group 5/15 elements of the periodic table, bulk chemicals, etc., can solve the problems of non-recyclable reuse, corrosion of reaction equipment, and operational risks, etc. problems, to achieve the effect of shortened reaction time, reduced corrosion, and no by-products

Active Publication Date: 2018-09-28
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing catalytic synthesis method to produce antimony mercaptan uses concentrated sulfuric acid or concentrated hydrochloric acid as a catalyst, which belongs to precursor chemicals, has operational risks, high reaction temperature, and certain danger, and the catalyst used is severely corrosive to the reaction equipment. Also not recyclable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 5L three-necked flask with a stirrer and a thermometer, add isooctyl mercaptopropionate 1500g (content 99.0%), antimony trioxide 335.8g (99.5%), [BMIM][HSO 4 ]1640.6g, i.e. isooctyl mercaptopropionate: antimony trioxide: [BMIM][HSO 4 ] The mass ratio is 1600:360:1750, and the reaction is stirred at room temperature for 1 hour to obtain 3409.4 g of a crude antimony thiolate product, with a crude product yield of 99.8%.

[0020] The crude product was distilled under reduced pressure at -0.096MPa and 107°C for 1.5 hours, cooled to obtain the target product antimony thiolate 1751.1g, the product purity was 99.3%, and the yield was 99.7%; ionic liquid [BMIM][HSO was obtained 4 ] 1624.2g, the recovery rate of ionic liquid is 99.0%.

Embodiment 2

[0022] In Example 1, isooctyl mercaptopropionate: antimony trioxide: [BMIM][HSO 4 ] The mass ratio was adjusted to 1600:360:1800, and the rest remained unchanged to obtain the target product antimony thiolate 1752.9g, the product purity was 99.4%, and the yield was 99.8%, and the ionic liquid [BMIM][HSO was obtained. 4 ] 1672.3g, the recovery rate is 99.1%.

Embodiment 3

[0024] The mass ratio of isooctyl mercaptopropionate: antimony trioxide: [BMIM][HSO4] in Example 1 was adjusted to 1600:400:1800, and the rest remained unchanged to obtain the target product antimony thiolate 1742.3g, with a product purity of 99.1% , the yield was 99.2%, and the ionic liquid [BMIM][HSO was obtained 4 ] 1670.6g, the recovery rate is 99.0%.

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PUM

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Abstract

The invention provides a green synthesis method of antimony mercaptide. The antimony mercaptide is obtained by taking antimonous oxide and isooctyl 3-mercaptopropionate as raw materials, and reactingunder the action of an ionic liquid catalyst. The preparation method comprises the steps that ionic liquid is used as the catalyst and a reaction solvent and reacts for 0.5-2 h under the room temperature condition, and the yield being 95% or above can be reached. Accordingly, by means of the applied ionic liquid, a homogeneous system is formed through the reaction, mass transfer resistance of thereaction system is lowered, the antimony mercaptide synthesis reaction time is shortened, the reaction temperature is lowered, the yield is increased, and no by-product exists. Accordingly, the catalyst applied in the method can be separated, recycled and repeatedly used, and the phenomenon that for a traditional method, precursor chemicals such as concentrated sulfuric acid or concentrated hydrochloric acid are used as the catalyst is avoided; meanwhile, corrosion to carbon steel (iron nail) is lowered, and the green synthesis method of the antimony mercaptide is provided.

Description

technical field [0001] The invention relates to a synthesis method of fine chemicals, in particular to a green synthesis process of antimony thiolate. Background technique [0002] Antimony mercaptide is a new type of heat stabilizer, which has the advantages of good initial coloring performance, low price and non-toxicity. It is a good substitute for expensive organotin heat stabilizers. With the rapid growth of the market demand for antimony thiolate heat stabilizers, the industrialized production of antimony thiolate has attracted more and more attention. In its synthesis and production process, the most important thing is the choice of reaction environment and conditions. [0003] The existing catalytic synthesis method for producing antimony mercaptide uses concentrated sulfuric acid or concentrated hydrochloric acid as a catalyst, which is a precursor chemical, and has operational risks, high reaction temperature, and certain dangers, and the catalyst used is seriousl...

Claims

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Application Information

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IPC IPC(8): C07F9/90
CPCC07F9/902Y02P20/54
Inventor 程珍马韵升张建林陈梅梅许倩倩薛大永
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD