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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, thereby solving the cumbersome process steps and operating environment of the current preparation methods. Poor quality, high production cost, difficult wastewater treatment, environmental pollution and other problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 0.1 mol of proxanthate 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 manganese acetate as a catalyst (the amount of catalyst is 1% of the molar amount of xanthate) and triethylamine , react at 30-35°C for 1 hour under stirring, then raise the temperature to 50°C, and continue to keep warm for 1-4 hours;

[0029] Then the reaction solution is filtered, and 50 milliliters of ethyl acetate is added to the filtrate to extract as an organic extractant, and the water phase is removed by standing for liquid separation; the organic phase is distilled under reduced pressure to remove ethyl acetate as an organic extractant, and the remainder is The target product is thiocarbamate; analysis shows that the product yield is above 92.0%, and the purity is 98.2%.

Embodiment 2

[0031] Dissolve 0.1 mol of isobutyl 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 manganese acetate as a catalyst (the amount of catalyst is 1% of the molar amount of xanthate) and triethyl For amine, react at 30-35°C for 1 hour under stirring, then raise the temperature to 50°C, and continue to keep warm for 1-4 hours. Then the reaction solution is filtered, 50 milliliters of ethyl acetate is added to the filtrate as an organic extractant for extraction, the water phase is removed by standing for liquid separation, and the organic phase is distilled under reduced pressure to remove ethyl acetate as an organic extractant, and the remainder is The target product is thiocarbamate; analysis shows that the product yield is above 90.0%, and the purity is 97.9%.

Embodiment 3

[0033] Dissolve 0.1 mol of proxanthate 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), and stir React at 30-35°C for 1 hour, then raise the temperature to 50°C, and continue to keep warm for 1-4 hours;

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

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PUM

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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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