Method for preparing thionocarbamate and trithiocarbonate

A technology of trithiocarbonate and thiocarbamate, applied in the field of preparing thiocarbamate and co-producing trithiocarbonate, producing thiocarbamate and trithiocarbamate, which can solve the problem that has not yet been widely used , high cost of raw materials and other issues, to achieve the effect of high reactivity, increased yield, and easy precipitation

Active Publication Date: 2017-02-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high raw material cost of the existing preparation technology, it has not been widely used

Method used

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  • Method for preparing thionocarbamate and trithiocarbonate
  • Method for preparing thionocarbamate and trithiocarbonate
  • Method for preparing thionocarbamate and trithiocarbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0060] Synthesis of O-isopropyl-N-ethylthiocarbamate and co-production of benzyl sodium trithiocarbonate:

[0061] 30.32 parts of purity are 95.12% of O-isopropyl-N-ethyl thiocarbamate and 17.53 parts of purity of 90.27% sodium isopropyl xanthate are added to the reactor, fully stirred, and then Add 12.79 parts of benzyl chloride with a purity of 99.0% into the pressure dropping funnel, control the reaction temperature to 75°C, and cool to room temperature after 3 hours of reaction, then add 6.68 parts of ethylamine aqueous solution (with a content of 65% to 70% %), warming up to 70 ° C, reacted for 2 hours, cooled to room temperature and filtered to remove sodium chloride, the filtrate was transferred to the reactor, and 8.08 parts of carbon disulfide with a purity of 99.0% were added to the reactor, and 4.38 parts of powdered hydroxide were added. Sodium (purity: 96.0%), after adding sodium hydroxide, stirred and reacted at 30° C. for 4 hours, and the reaction ended. Filter...

Embodiment 2

[0063] Synthesis of O-isobutyl-N-ethylthiocarbamate and co-production of benzyl sodium trithiocarbonate:

[0064] 25.30 parts of O-isobutyl-N-ethyl thiocarbamate with a purity of 94.77% and 18.84 parts of sodium isobutyl xanthate with a purity of 91.41% were added to the reactor, fully stirred, and then Add 12.79 parts of benzyl chloride with a purity of 99.0% to the pressure dropping funnel, control the reaction temperature to 65°C, react for 2 hours, cool to room temperature, and then add 6.68 parts of ethylamine aqueous solution (with a content of 65% to 70% %), warming up to 70 ° C, reacted for 2 hours, cooled to room temperature and filtered to remove sodium chloride, the filtrate was transferred to the reactor, and 8.08 parts of carbon disulfide with a purity of 99.0% were added to the reactor, and 4.38 parts of powdered hydroxide were added. Sodium (purity: 96%), after adding the caustic, stirred and reacted at 30° C. for 4 hours, and the reaction ended. Filter to obta...

Embodiment 3

[0066] Synthesis of O-isopropyl-N-propylthiocarbamate and co-production of benzyl sodium trithiocarbonate:

[0067] 114.95 parts of O-isopropyl-N-propyl thiocarbamate with a purity of 95.12% and 53.59 parts of sodium isopropyl xanthate with a purity of 90.27% were added to the reactor, fully stirred, and then Add 38.37 parts of purity to 99.0% benzyl chloride into the pressure dropping funnel, control the reaction temperature to be 75°C, react for 3 hours, cool to room temperature, then add 18.09 parts of 98.0% n-propylamine with a constant pressure dropping funnel, and heat up to 70 ℃, reacted 3 hours, cooled to room temperature and filtered to remove sodium chloride, the filtrate was transferred to the reactor, added 25.38 parts of carbon disulfide with a purity of 99.0% in the reactor, and added 13.13 parts of powdered sodium hydroxide (purity is 96 %), after adding the caustic alkali, stirred and reacted at 30°C for 4 hours, and the reaction ended. Filter to obtain benzyl...

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Abstract

The invention discloses a method for preparing thionocarbamate and trithiocarbonate. The method comprises the following steps: carrying out an esterification reaction on alkyl xanthate salt and a halogenation reagent to obtain alkyl xanthate ester; carrying out an aminolysis reaction on the alkyl xanthate ester and fatty amine to obtain a thionocarbamate and mercaptan compound mixture; and carrying out an addition reaction on the thionocarbamate and mercaptan compound mixture and carbon disulfide in the presence of caustic alkali, and carrying out solid-liquid separation to obtain a liquid phase which is the thionocarbamate product and a solid phase which is the trithiocarbonate product. The products prepared through the preparation method have high yield and high purity, and the method allows the two high-efficiency collectors comprising thionocarbamate and trithiocarbonate to be simultaneously produced, and has the advantages of easiness in separation of the products, high atom economy property, low production cost, and easiness in realization of industrial production.

Description

technical field [0001] The invention relates to a method for preparing thiourethane and co-producing trithiocarbonate, in particular to a method using alkyl xanthate and benzyl halide, propenyl halide or β-halogenated propionitrile as raw materials, The method for simultaneously producing thiourethane and trithiocarbonate belongs to the field of preparation of flotation collectors. Background technique [0002] Thiurethane, the scientific name is O-alkyl-N-alkylthiocarbamate, is a kind of sulfide ore flotation agent with excellent performance, which has excellent chelating effect on copper, gold, silver and other metal ions. Compared with conventional sulfide mineral collectors such as xanthate and black powder, it has good selectivity, small dosage, foaming property, and can effectively separate valuable minerals and gangue minerals under low alkali conditions. And other advantages, so it is widely used in the flotation of various copper ore, gold ore, lead-zinc ore. It is...

Claims

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Application Information

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IPC IPC(8): C07C329/00C07C333/04
CPCC07C319/02C07C329/00C07C333/04C07C321/10
Inventor 钟宏马鑫王帅曹占芳刘广义
Owner CENT SOUTH UNIV
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