Thiocarbamate compound preparation method

A technology for thiocarbamic acid and ester compounds, applied in the direction of organic chemistry and the like, can solve the problems of cumbersome process, high production cost, poor operating environment, etc., and achieve the effects of improving environmental pollution, stable product quality, and improving production efficiency.

Active Publication Date: 2013-09-04
BEIJING MINING & METALLURGICAL TECH GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a preparation method of thiocarbamate compounds, which can realize simple and easy operation to prepare thiocarbamate compounds in one step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example one

[0028] Dissolve 0.1 mol of isopropylxanthate with a purity greater than 80.0% in 20 ml of water, then add 0.1-0.2 mol of ethylamine and an appropriate amount of manganese acetate as a catalyst (the amount of catalyst is 1% of the molar amount of xanthate) and triethylamine , React for 1 hour at 30-35°C with stirring, then heat up to 50°C, and continue to keep the temperature for 1 to 4 hours;

[0029] Then the reaction solution was filtered, 50 ml of ethyl acetate was added to the filtrate as an organic extractant for extraction, and the aqueous phase was removed by standing for liquid separation; the organic phase was distilled under reduced pressure to remove ethyl acetate as the organic extractant, and the rest was Target product thiocarbamate; analysis shows that the yield of the product is over 92.0% and the purity is 98.2%.

Example Embodiment

[0030] Example two

[0031] Dissolve 0.1 mole of isobutyl xanthate with a purity greater than 80.0% in 20 ml of water, then add 0.1 to 0.2 mole of ethylamine, add an appropriate amount of manganese acetate as a catalyst (the amount of catalyst is 1% of the molar amount of xanthate) and triethyl The amine is reacted at 30-35°C for 1 hour under stirring, then the temperature is raised to 50°C, and the temperature is kept for 1 to 4 hours. Then the reaction solution was filtered, and 50 ml of ethyl acetate was added to the filtrate as the organic extractant for extraction. The aqueous phase was removed by static separation, and the organic phase was distilled under reduced pressure to remove ethyl acetate as the organic extractant. The target product thiocarbamate; analysis shows that the yield of the product is over 90.0% and the purity is 97.9%.

Example Embodiment

[0032] Example three

[0033] Dissolve 0.1 mol of isopropyl xanthate with a purity greater than 80.0% in 20 ml of water, then add 0.1 to 0.2 mol of ethylamine, add an appropriate amount of active manganese dioxide as a catalyst (the amount of catalyst is 5% of the molar amount of xanthate), stir React at 30-35°C for 1 hour, then heat to 50°C, and continue to keep the temperature for 1 to 4 hours;

[0034] Then the reaction solution was filtered, 50 ml of ethyl acetate was added to the filtrate as an organic extractant for extraction, and the aqueous phase was removed by standing for liquid separation; the organic phase was distilled under reduced pressure to remove ethyl acetate as the organic extractant, and the rest was The target product thiocarbamate; analysis shows that the yield of the product is over 82.0% and the purity is 98.0%.

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Abstract

The invention discloses a thiocarbamate compound preparation method for preparation of a thiocarbamate flotation agent of sulfide ore. According to the preparation method, corresponding xanthate and amine are adopted as starting materials, water is adopted as a solvent, and a one-step method is adopted to synthesize the corresponding thiocarbamate compound. With the preparation method, the defect of the two-step reaction of the traditional method is overcome, the process is simplified, and a production operation environment is improved. The preparation method has characteristics of simpleness, easy operation, substantial synthesis process shortening, production efficiency improvement, and stable product quality, and provides a simple and feasible method for thiocarbamate flotation agent preparation.

Description

technical field [0001] The invention relates to the preparation of mine chemicals, in particular to a preparation method of a thiocarbamate compound used as a sulfide ore beneficiation agent. Background technique [0002] Thiocarbamate compounds are a very important class of sulfide ore beneficiation agents. At present, the main methods of producing this medicament mainly contain the following types: [0003] The most widely used method is xanthate esterification-amination method. This method is mainly carried out through two-step reaction. First, xanthate is esterified with haloalkane or chloroacetic acid to generate intermediate product xanthate; then add amines The compound undergoes aminolysis reaction with xanthate, and finally generates the target product thiocarbamate. When using the haloalkane method to prepare, there are disadvantages in the process that the by-product alkyl mercaptan is difficult to separate from the target product, and a large amount of mercapta...

Claims

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Application Information

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IPC IPC(8): C07C333/04
Inventor 张行荣刘龙利吴桂叶何伟张杰尹琨
Owner BEIJING MINING & METALLURGICAL TECH GRP CO LTD
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