Thiocarbamic acid derivative and preparation method thereof

A technology of thiocarbamic acid and derivatives, applied in organic chemistry and other fields, can solve problems such as easy contact with air, reduce safety, and pollute the environment, and achieve the effects of simple operation, reduced energy consumption, and lowered reaction temperature

Active Publication Date: 2014-03-05
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Organic solvent can be aromatic solvent, aliphatic hydrocarbon or alicyclic hydrocarbon in the technical scheme disclosed by this patent (referring to description page 11-16), as toluene, chlorobenzene, normal hexane, hexanaphthene, these several solvents all It is a flammable liquid, which reduces the safety in the production process; moreover, solvents s...

Method used

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  • Thiocarbamic acid derivative and preparation method thereof
  • Thiocarbamic acid derivative and preparation method thereof
  • Thiocarbamic acid derivative and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The first reaction process: use water as solvent.

[0033]Using a 250mL four-neck flask equipped with a stirring device, a thermometer and a reflux condenser, weigh 14.2g of hexamethylene dihydrate 1,6-dithiosulfate disodium salt (Duralink HTS, purchased from Flexsys) and add it to the flask , add 36.4g of water, stir to dissolve HTS, add 3.2g of sodium bicarbonate, 3.4g of formaldehyde solution with a concentration of 35% by mass, stir at 20°C for 30min, then add 9.2g of dichloromethane. Then 94.5 g of a sodium dibenzyl dithiocarbamate solution (sodium dibenzyl dithiocarbamate, purchased from Bailingwei Technology Co., Ltd., purity: 98%) with a mass percentage concentration of 25% was added dropwise, and the reaction was stirred at 20° C. for 5 h . Suction filter the above solution, wash the obtained solid product with water, and dry it in an oven at 60°C to constant weight to obtain 26.4g of 1,6-bis(N,N-dibenzylthiocarbamoyl disulfide)hexane solid powder , The calcu...

Embodiment 2

[0037] The first reaction process: use water as solvent.

[0038] Using a 250mL four-neck flask equipped with a stirring device, a thermometer and a reflux condenser, weigh 8.2g of HTS and add it to the flask, add 80g of water, stir to dissolve the HTS, add 1.0g of sodium bicarbonate, 3.5g of mass percent 20% formaldehyde aqueous solution, stirred at 20°C for 30min, and added 5.9g of dichloromethane. Then 60.0 g of 20% by mass concentration of sodium dibenzyl dithiocarbamate solution was added dropwise, and stirred at 20° C. for 5 h. Suction filter the above solution, wash the obtained solid product with water, and dry it in an oven at 60°C to constant weight to obtain 6.6g of 1,6-bis(N,N-dibenzylthiocarbamoyl disulfide)hexane solid powder , The calculated product yield is about 92.7%.

[0039] The second reaction process: using the filtrate after suction filtration as a solvent to continuously prepare 1,6-bis(N,N-dibenzylthiocarbamoyl disulfide)hexane.

[0040] Weigh 80g o...

Embodiment 3

[0042] The first reaction process: use water as solvent.

[0043] Using a 250mL four-necked flask equipped with a stirring device, a thermometer and a reflux condenser, weigh 14.5g of HTS and add it to the flask, add 24g of water, stir to dissolve the HTS, add 5.2g of sodium bicarbonate, 9.2g of mass percent concentration 20% aqueous formaldehyde solution, stirred at 25°C for 30min, and added 1.7g of dichloromethane. Then 102.0 g of sodium dibenzyl dithiocarbamate solution with a concentration of 25% by mass was added dropwise, and stirred at 25° C. for 4 h. Suction filter the above solution, wash the obtained solid product with water, and dry it in an oven at 70°C to constant weight to obtain 13.6g of 1,6-bis(N,N-dibenzylthiocarbamoyl disulfide)hexane solid powder , The calculated product yield is about 95.4%.

[0044] The second reaction process: using the filtrate after suction filtration as a solvent to continuously prepare 1,6-bis(N,N-dibenzylthiocarbamoyl disulfide)hex...

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Abstract

The invention provides a preparation method, which is simple in operation and is green and environment-friendly, for preparing a thiocarbamic acid derivative. According to the preparation method, organic thiosulfate and sodium thiocarbamate are used as raw materials, dichloromethane and formaldehyde can be added during reaction to accelerate the reaction, suction filtration is performed after reaction to separate out a solid product, and the filtrate can be recycled to continuously prepare the thiocarbamic acid derivative. The boiling point of the dichloromethane added during the reaction is low, so that the reaction temperature can be reduced, the energy consumption is reduced, and the dichloromethane is difficult to burn to ensure that the safety performance during production is improved.

Description

technical field [0001] The invention belongs to the field of processing aids for the rubber industry, and in particular relates to an anti-reversion agent thiocarbamic acid derivative and a preparation method thereof. Background technique [0002] Rubber is a chain-like polymer material, adding a vulcanizing agent can cause a cross-linking reaction with it to form a three-dimensional network structure, making the rubber change from a plastic material to an elastic material, making the rubber highly elastic and flexible in a wide temperature range. Small plasticity, high strength performance. Sulfur vulcanized compounds undergo vulcanization reversion when the vulcanizate is overvulcanized during production or exposed to anaerobic heat aging conditions during use. In addition, the heat generated during use by many compounds is sufficient to cause crosslinking Network degradation, so that the product is easily damaged, the service life is shortened, and vulcanization reversio...

Claims

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Application Information

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IPC IPC(8): C07C333/30C07D295/21
Inventor 董栋甄博鸣赵丽丽
Owner BEIJING RED AVENUE INNOVA
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