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High-yield environment-friendly oxygen oxidation method for synthesis of accelerator DPG

A technology of oxygen oxidation and accelerator, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as water pollution and waste water, and achieve the effect of avoiding risk factors, avoiding waste water and improving yield

Active Publication Date: 2015-11-11
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 2. The synthesis of this process will produce a large amount of waste water, and the acid-soluble alkali precipitation and salt washing of the product will generate a large amount of waste water, causing serious water pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Mix 220g of carbon disulfide and 32g of sulfur under ultra-sound conditions to obtain a mixture of carbon disulfide and sulfur. Sulfur mixture, 40g sodium hydroxide, 2g sodium dodecylsulfonate, start stirring, heat up to 65°C, keep warm for 4 hours, then filter and dry to obtain diphenylthiourea, and store the mother liquor carbon disulfide after filtration for future use ,

[0043](2) In an autoclave equipped with a thermometer, mechanical stirring, and a heating device, add 230 g of diphenylthiourea, 360 g of ethanol, and 3 g of copper acetate-ethanol mixture in sequence, close the autoclave, and then pass into the autoclave Ammonia gas, the pressure in the kettle is raised to 0.5Mpa, and then the pressure in the kettle is raised to 1.0Mpa through ammonia gas, the temperature is raised to 35°C, the heat preservation reaction is carried out for 7.5 hours, the oxidation synthesis is completed, and the primary product of the accelerator DPG is obtained;

[0044] (3)...

Embodiment 2

[0048] (1) Mix 220g of carbon disulfide and 32g of sulfur under ultra-sound conditions to obtain a mixture of carbon disulfide and sulfur. Sulfur mixture, 50g sodium hydroxide, 4g sodium dodecylsulfonate, start stirring, heat up to 65°C, keep warm for 5 hours, then filter and dry to obtain diphenylthiourea, and store the mother liquor carbon disulfide after filtration for future use ,

[0049] (2) In an autoclave equipped with a thermometer, mechanical stirring, and a heating device, add 230 g of diphenylthiourea, 360 g of ethanol, and 3 g of copper acetate-ethanol mixture in sequence, close the autoclave, and then pass into the autoclave Ammonia gas, the pressure in the kettle is raised to 0.5Mpa, and then the pressure in the kettle is raised to 1.0Mpa by passing through the ammonia gas, the temperature is raised to 40°C, the heat preservation reaction is carried out for 6 hours, the oxidation synthesis is completed, and the primary product of the accelerator DPG is obtained;...

Embodiment 3

[0054] (1) Mix 220g of carbon disulfide and 32g of sulfur under ultra-sound conditions to obtain a mixture of carbon disulfide and sulfur. Sulfur mixture, 50g sodium hydroxide, 2g sodium dodecylsulfonate, start stirring, heat up to 60°C, keep warm for 4 hours, then filter and dry to obtain diphenylthiourea, and store the mother liquor carbon disulfide after filtration for future use ,

[0055] (2) In an autoclave equipped with a thermometer, mechanical stirring, and a heating device, add 230 g of diphenylthiourea, 360 g of ethanol, and 3 g of copper acetate-ethanol mixture in sequence, close the autoclave, and then pass into the autoclave Ammonia gas, the pressure in the kettle is raised to 0.4Mpa, then the pressure in the kettle is raised to 0.9Mpa by passing through ammonia gas, the temperature is raised to 35°C, the heat preservation reaction is carried out for 7.5 hours, the oxidation synthesis is completed, and the primary product of the accelerator DPG is obtained;

[0...

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PUM

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Abstract

The present invention relates to a high-yield environment-friendly oxygen oxidation method for synthesis of accelerator DPG. The method comprises: (1) preparation of an intermediate diphenyl thiourea; (2) synthesis of a target product accelerator DPG; (3) recovery of part of the solvent and recrystallization of the product; and (4) removal of the remaining ethanol by filtration, and drying and crushing to obtain the product. The preparation process of the present invention prepares diphenyl thiourea at low pressure, avoids the risk factor of high pressure reaction; the insolubility of diphenyl thiourea in carbon disulfide is taken into consideration that carbon disulfide is used as solvent to improve the conversion rate of the raw material aniline, increase the yield, avoid generation of wastewater, and benefit the environment.

Description

technical field [0001] The invention relates to an environment-friendly method for synthesizing accelerator DPG by a high-yield oxygen oxidation method, which belongs to the technical field of fine chemicals. Background technique [0002] Accelerator DPG is an important rubber medium-speed vulcanization accelerator, mainly used as a vulcanization accelerator for natural rubber and synthetic rubber. It can also be used as an activator for thiazole thiurams and sulfenamide accelerators. When it is used together with DM.TMTD, it can be used for continuous vulcanization. There are also plasticizers and peptizers in chloroprene rubber, which are mainly used in the manufacture of rubber products such as tires and rubber soles. Early accelerator DPG was prepared by using lead oxide as a desulfurizer, but due to the use of heavy metal lead in this method, which caused great harm to human body and environment, its use has been basically stopped. There are reports on the use of zin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/18C07C277/08
Inventor 吕寻伟马松潘林琳杜孟成孙庆刚
Owner SHANDONG YANGGU HUATAI CHEM
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