Method for synthesizing xanthate

A synthesis method and technology of xanthate, applied in the direction of organic chemistry, etc., can solve the problems of incomplete xanthate reaction, low purity and yield of xanthate products, save raw materials, efficient reaction, eliminate combustion, and reduce volatilization loss. Effect

Active Publication Date: 2012-09-26
CENT SOUTH UNIV
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Problems solved by technology

Due to containing carbon disulfide and solvent acetone in the reaction mixture, they did not reclaim excessive carbon disulfide raw material, meanwhile, they only

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  • Method for synthesizing xanthate

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Embodiment 2

[0029] The preparation of embodiment 2 sodium isobutyl xanthate

[0030] 46.13 parts of purity are 99% carbon disulfide and 14.98 parts of purity are 99% isobutanol to add in the reactor (the ratio of the amount of substance of alcohol and carbon disulfide is n (alcohol): n (carbon disulfide)=1: 3), in Cool the mixture to about 15°C under stirring, then add 3 parts, 3 parts and 2.34 parts of flaky sodium hydroxide (96% purity) into the reactor in 3 times, and stir for 10 minutes after each addition About, control the temperature when adding the alkali to be 15°C-30°C, after adding caustic alkali, stir and react at 25°C for 2 hours, and the reaction ends. The excess carbon disulfide solvent is recovered by step-by-step distillation under normal pressure and then under reduced pressure to obtain the desired sodium isobutyl xanthate product. Analysis showed that the purity of sodium isobutyl xanthate was 88.9%, and the product yield based on isobutanol was 95.4%.

Embodiment 3

[0031] The preparation of embodiment 3 sodium isobutyl xanthate

[0032] Add 46.13 parts of carbon disulfide with a purity of 99% and 8.34 parts of granular sodium hydroxide (with a purity of 96%) into the reactor, and cool the mixture to about 15°C under stirring, and then use it under stirring at 15°C to 30°C 14.98 parts of purity is 99% isobutanol (the ratio of the amount of substance of alcohol and carbon disulfide is n (alcohol): n (carbon disulfide)=1: 3) to reactor dropwise, dropwise and keep reaction temperature is 25 ℃, The reaction was stirred for 4 hours, and the reaction was completed. The excess carbon disulfide solvent is recovered by step-by-step distillation under normal pressure and then under reduced pressure to obtain the desired sodium isobutyl xanthate product. Analysis showed that the purity of sodium isobutyl xanthate was 89.2%, and the product yield based on isobutanol was 96.8%.

Embodiment 4

[0033] The preparation of embodiment 4 sodium isobutyl xanthate

[0034] 46.13 parts of carbon disulfide in embodiment 2 are used as 61.50 parts of carbon disulfide (the ratio of the amount of substance of alcohol and carbon disulfide is n (alcohol): n (carbon disulfide)=1: 4), granular sodium hydroxide (purity is 96%) Use instead flake sodium hydroxide, other conditions remain unchanged, the purity of sodium isobutyl xanthate in the sodium isobutyl xanthate product obtained is 88.4%, and the product yield based on isobutanol is 97.1%.

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Abstract

Disclosed is a method for synthesizing xanthate, relating to a synthetic process of a flotation collector of metal mines. The invention provides a method for synthesizing xanthate with high yield and good quality. The xanthate of the invention is prepared by adopting the technical solution that raw materials comprise alcohol, carbon disulfide, and caustic alkali with a molar ratio of 1:3-9:1-1.1, wherein the caustic alkali is sodium hydroxide or potassium hydroxide, and the xanthate which is known as Huangyao is prepared by reacting the raw materials for 0.5-8 hours at a temperature ranged from 10 DEG C to 70 DEG C. The invention further discloses methods for recycling a carbon disulfide solvent. The first method comprises filtering materials from a reactor under the protection of nitrogen, and carrying out reduced pressure distillation on the obtained filter cake to acquire a xanthate product with high purity and a carbon disulfide solvent. A Filter liquor and the recycled carbon disulfide can be cycledly utilized. The second method comprises first carrying out an atmospheric distillation on materials from the reactor at a temperature ranged from 50 DEG C to 90 DEG C to recover most of the carbon disulfide, and then carrying out reduced pressure distillation to recover the rest of the carbon disulfide and acquire a xanthate product with high purity at the same time.

Description

technical field [0001] The invention relates to a solvent method synthesis process of xanthate. Background technique [0002] Xanthate ROCSSNa(K), commonly known as "xanthate", can form soluble compounds with various metal ions. In 1815, Zeise first synthesized xanthate, which was called xanthate because of its yellow color. Since Keller discovered that xanthate can be used as a flotation collector for sulfide minerals in 1925, xanthate has been widely used in metal sulfide mines to recover metal sulfide minerals. At present, xanthate is the most consumed sulfide ore flotation collector in the field of mineral processing. [0003] At present, the methods for synthesizing xanthate mainly include "kneading method" and "solvent method". The kneading method is to add alcohol and carbon disulfide to the kneader, then gradually add powder alkali (sodium hydroxide or potassium hydroxide), and react at 25°C to 35°C to form xanthate. Because it does not need other auxiliary raw m...

Claims

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Application Information

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IPC IPC(8): C07C329/14
Inventor 钟宏刘广义马鑫王帅曹占芳
Owner CENT SOUTH UNIV
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