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A kind of preparation method of xanthate compound

A technology for xanthates and compounds is applied in the field of green and efficient preparation of xanthates, and can solve the problems of waste water, low product yield and purity, loss of organic solvents, and the like

Active Publication Date: 2021-09-14
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The synthesis of the above-mentioned xanthate formate and allyl xanthate reacts in water or an organic solvent, or produces waste water, or causes organic solvent loss, pollutes the environment, or product yield and purity are not high

Method used

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  • A kind of preparation method of xanthate compound
  • A kind of preparation method of xanthate compound
  • A kind of preparation method of xanthate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation of embodiment 1 allyl isopropyl xanthate

[0033] Add 8.2 parts of allyl chloride with a purity of 98% and 0.6 parts of cetyltrimethylammonium bromide into the reaction kettle, stir evenly and start adding 18.6 parts of isopropyl chloride with a purity of 84.9% in batches after cooling down to 10-20°C. Sodium propyl xanthate, after all the reactants have been added, the temperature rises to 25°C to start the reaction timing. After 6.5h of reaction, the allyl isopropyl xanthate product with a purity of 97.54% is obtained (see figure 2 ), the yield based on sodium isopropyl xanthate is 96.2%. The yield and the purity of the allyl isopropyl xanthate product are significantly higher than the test results of Comparative Example 1.

Embodiment 2-5

[0034] The preparation of embodiment 2-5 allyl isopropyl xanthate

[0035] Change 0.6 parts of cetyltrimethylammonium bromide in Example 1 into triethylamine, benzyltriethylammonium chloride, benzyltrimethylammonium chloride or cetyl trimethylammonium chloride of the same quality respectively Trimethyl ammonium chloride, the allyl isopropyl xanthate product that makes is shown in Table 1.

[0036] Table 1 The influence of the type of phase transfer catalyst on the yield of allyl isopropyl xanthate

[0037]

Embodiment 6

[0038] The preparation of embodiment 6 allyl ethyl xanthate

[0039] Add 8.2 parts of allyl chloride with a purity of 98% and 0.6 parts of hexadecyltrimethylammonium bromide into the reaction kettle, stir well and start adding 16 parts of ethyl chloride with a purity of 90% in batches after cooling down to 10-20°C. Sodium xanthate, after all the reactants were added, the temperature rose to 25°C to start the reaction timing, and the reaction was stopped after 6.5 hours of reaction. The purity that makes allyl ethyl xanthate is 98.3% (see figure 1 ), the yield based on sodium ethyl xanthate is 95.3%.

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Abstract

The invention discloses a preparation method of xanthate compounds, which is characterized in that xanthate and chloride are reacted at 0-60°C in the presence of a phase transfer catalyst to obtain high-purity and high-yield xanthate compounds. xanthate compounds. Compared with the existing methods, the solvent-free (self-solvent) preparation of xanthate compounds by phase transfer catalysis has simple process, good product purity, high yield, economy and environmental protection, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a green and efficient preparation method of xanthate compounds. Background technique [0002] Alkyl xanthate refers to a class of compounds with the general formula ROC(=S)SR', which can be widely used in engineering fields such as flotation, and they are usually substituted by xanthate (ie xanthate) and chlorine compounds prepared by reaction. [0003] William A.Douglass reacts potassium ethyl xanthate and ethyl chloroformate in the organic solvent benzene to prepare ethyl xanthate ethyl formate (C 2 h 5 OC(=S)SC(=O)OC 2 h 5 ) (William A.Douglass.Process OfConcentrating Ores And Minerals By Flotation.US Patent 1652099,Dec.6,1927); Arthur H.Fischer used potassium butyl xanthate and allyl chloroformate (ClC(=O)OCH 2 CH=CH 2 ) is raw material, synthesizes allyl xanthate formate (C 4 h 9 OCSSCOOCH 2 CH=CH 2 ). (Arthur H.Fischer.XanthogenFormates.US P...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C329/16
CPCC07C329/16
Inventor 刘广义罗浩李江伟
Owner CENT SOUTH UNIV
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