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A method for preparing thiourethane and co-producing dibenzyl disulfide

A technology of dibenzyl disulfide and thiourethane is applied in the fields of producing thiourethane and dibenzyl disulfide, preparing thiourethane and producing dibenzyl disulfide, and can solve problems such as environmental pollution , to achieve the effect of large reaction activity, increased yield, and reduced temperature conditions

Active Publication Date: 2018-03-30
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthetic method of dibenzyl disulfide mainly contains: (1) mercaptan method, obtains by oxidative coupling of benzyl mercaptan, although this method is simple to operate, because raw material mercaptan has special odor, causes bigger to environment pollution
But with alkyl xanthate, benzyl halide, aliphatic amine etc. as raw material preparation thiourethane and co-production of dibenzyl disulfide method has no report

Method used

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  • A method for preparing thiourethane and co-producing dibenzyl disulfide
  • A method for preparing thiourethane and co-producing dibenzyl disulfide
  • A method for preparing thiourethane and co-producing dibenzyl disulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Synthesis of O-isopropyl-N-ethylthiocarbamate and co-production of dibenzyl disulfide:

[0059] 15.16 parts of O-isopropyl-N-ethyl thiocarbamate with a purity of 95.12% and 8.77 parts of sodium isopropyl xanthate with a purity of 90.27% were added to the reactor, fully stirred, and then Add 6.40 parts of benzyl chloride with a purity of 99.0% to the pressure dropping funnel, control the reaction temperature to 75°C, cool to room temperature after 3 hours of reaction, filter to remove sodium chloride, transfer the filtrate to the reactor, and then use a constant pressure dropping funnel to Add 3.34 parts of ethylamine aqueous solution (content: 65% to 70%), heat up to 70°C, react for 2 hours, cool to room temperature, add 0.19 parts of tetra-n-butylammonium iodide (purity: 99.0%) into the reactor, And add 89.27 parts of hydrogen peroxide with a concentration of 2.0% with a constant pressure dropping funnel, stir and react at room temperature for 20 minutes, and the react...

Embodiment 2

[0061] Synthesis of O-isopropyl-N-ethylthiocarbamate and co-production of dibenzyl disulfide:

[0062] 30.32 parts of purity of 95.12% O-isopropyl-N-ethyl thiocarbamate and 17.54 parts of purity of 90.27% sodium isopropyl xanthate were added to the reactor, fully stirred, and then Add 12.80 parts of benzyl chloride with a purity of 99.0% to the pressure dropping funnel, control the reaction temperature to 75°C, react for 3 hours and cool to room temperature, filter to remove sodium chloride, transfer the filtrate to the reactor, and then use a constant pressure dropping funnel to Add 6.68 parts of ethylamine aqueous solution (content: 65% to 70%), heat up to 70°C, react for 2 hours, cool to room temperature, add 0.25 parts of tetra-n-butylammonium iodide (purity: 99.0%) into the reactor, Get 11.30 parts of hydrogen peroxide with a concentration of 30%, add 87.11 parts of the separated water phase in Example 1, and add 60.26 parts of distilled water, and add it dropwise to the ...

Embodiment 3

[0064] Synthesis of O-isobutyl-N-ethylthiocarbamate and co-production of dibenzyl disulfide:

[0065] 20.00 parts of O-isobutyl-N-ethylthiocarbamate with a purity of 94.77% and 9.42 parts of sodium isobutyl xanthate with a purity of 91.41% were added to the reactor, fully stirred, and then Add 6.40 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, filter to remove sodium chloride, transfer the filtrate to the reactor, and then use a constant pressure dropping funnel to Add 3.35 parts of ethylamine aqueous solution (content: 65% to 70%), heat up to 70°C, react for 2 hours, cool to room temperature, add 0.48 parts of tetra-n-butylammonium bromide (purity: 99.0%) to the reactor, And add 35.71 parts of 5.0% hydrogen peroxide with a constant pressure dropping funnel, stir and react at room temperature for 20 minutes, and the reaction ends. Stand at room temperature...

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Abstract

The invention discloses a method for producing thionocarbamate and dibenzyl disulfide. The method comprises the following steps: carrying out an esterification reaction on alkyl xanthate and benzyl halide to obtain alkyl benzyl xanthate; carrying out an aminolysis reaction on the alkyl benzyl xanthate and fatty amine to obtain a thionocarbamate and benzyl mercaptan mixture; and carrying out an oxidation reaction on the thionocarbamate and benzyl mercaptan mixture and hydrogen peroxide, and carrying out liquid-solid separation to obtain a solid which is the dibenzyl disulfide product and a liquid, and allowing the liquid to stand for oil and water layering in order to obtain an oil phase which is the thionocarbamate product. The dibenzyl disulfide product and thionocarbamate product obtained through the method have high yield and high purity, and the method has the advantages of easiness in separation of the products in the preparation process, environmental protection, 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 dibenzyl disulfide, in particular to a method for simultaneously producing thiourethane and dibenzyl disulfide by using alkyl xanthate, benzyl halide and fatty amine as raw materials The method for disulfide-based, belongs to the field of preparation of fine chemical products. Background technique [0002] Sulfur urethane, scientific name is O-alkyl-N-alkyl thiocarbamate, is a kind of sulfide ore flotation agent with excellent performance, and it can be combined with conventional sulfide ore collectors such as xanthate, black medicine, etc. Compared with the advantages of good selectivity, small dosage, foaming, and effective separation of valuable minerals and gangue minerals under low alkali conditions, it is widely used in various copper mines, gold mines, lead-zinc mines, etc. Flotation is a kind of non-ionic sulfide ore collector that is widely used and studied in flota...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C329/00C07C319/14C07C321/20
CPCC07C319/02C07C319/14C07C329/00C07C321/20C07C321/10
Inventor 钟宏马鑫王帅曹占芳刘广义
Owner CENT SOUTH UNIV
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