Method for synthesizing accelerator DPTU

A technology of accelerators and mixtures, applied in the direction of organic chemistry, etc., can solve the problems of incomplete absorption of liquid caustic soda, and achieve the effects of improving production conditions, complete recovery and increased safety factor.

Active Publication Date: 2017-01-11
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional process has the following disadvantages: 1. High pressure reaction, carbon disulfide is a flammable and explosive raw material, which has a great risk factor under this condition; 2. The generated hydrogen sulfide gas is discharged through the tail gas, and the absorption with liquid alkali is not complete

Method used

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  • Method for synthesizing accelerator DPTU
  • Method for synthesizing accelerator DPTU
  • Method for synthesizing accelerator DPTU

Examples

Experimental program
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Effect test

Embodiment 1

[0037] (1) Take 150g of aniline and 250g of 30wt% sodium hydroxide aqueous solution, mix them evenly under ultrasonic conditions, and then put them into the reaction kettle;

[0038] (2) Take 73g of carbon disulfide and 52g of sulfur, mix them uniformly under ultrasonic conditions, then put them into the reaction kettle, and mix them with the materials in step (1);

[0039] (3) Turn on the reactor to stir, the stirring speed is controlled at 100 rpm, and then the temperature is raised to 40°C for 8 hours.

[0040] (4) After the reaction, filter, wash with water, and dry to obtain 171.8g of DPTU product. The filtered mother liquor contains sodium disulfide, which can be used as a raw material for preparing other products.

[0041] The obtained product is a silver-white solid powder with a purity (HPLC) of 99% and a yield of 93.4%.

Embodiment 2

[0043] (1) Take 150g of aniline and 250g of 30wt% sodium hydroxide aqueous solution, mix them evenly under ultrasonic conditions, and then put them into the reaction kettle;

[0044] (2) Take 73g of carbon disulfide and 52g of sulfur, mix them uniformly under ultrasonic conditions, then put them into the reaction kettle, and mix them with the materials in step (1);

[0045] (3) Turn on the reactor to stir, the stirring speed is controlled at 100 rpm, and then the temperature is raised to 70°C for 5 hours.

[0046] (4) After the reaction, filter, wash with water, and dry to obtain 163.8 g of DPTU product with a purity (HPLC) of 99.2% and a yield of 89.1%.

Embodiment 3

[0048] (1) Take 150g of aniline and 250g of 30wt% sodium hydroxide aqueous solution, mix them evenly under ultrasonic conditions, and then put them into the reaction kettle;

[0049] (2) Take 73g of carbon disulfide and 52g of sulfur, mix them uniformly under ultrasonic conditions, then put them into the reaction kettle, and mix them with the materials in step (1);

[0050] (3) Turn on the reactor to stir, the stirring speed is controlled at 100 rpm, and then the temperature is raised to 50°C for 8 hours.

[0051] (4) After the reaction, filter, wash with water, and dry to obtain 177.5 g of DPTU product with a purity (HPLC) of 99% and a yield of 96.5%.

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Abstract

The invention discloses a method for synthesizing an accelerator DPTU. The method comprises the following steps of: mixing aniline with an alkali aqueous solution uniformly; dissolving sulfur in carbon disulfide, and mixing until the sulfur completely dissolves; mixing the two mixtures uniformly, and then carrying out the reaction under normal pressure to obtain the accelerator DPTU. The invention adopts alkali aqueous solution as the solvent, and needs not to add an emulsifier, the generated hydrogen sulfide gas is absorbed and removed immediately during the reaction, so that the reaction is carried out toward the positive reaction direction to a greater extent, the reaction rate and the aniline conversion rate are improved, the yield is increased, the hydrogen sulfide gas recovery is more complete, the generation of hydrogen sulfide waste gas is reduced, and the production conditions are greatly improved.

Description

technical field [0001] The invention relates to a method for synthesizing accelerator DPTU, in particular to a relatively safe and environment-friendly method for synthesizing accelerator DPTU, and belongs to the technical field of fine chemicals. Background technique [0002] Accelerator DPTU, full name N, N'-diphenylthiourea, referred to as diphenylthiourea, is a medium-speed vulcanization accelerator for natural rubber and synthetic rubber, mainly used in natural latex and neoprene latex products, It can also be used in the manufacture of vulcanization bladders, water tires, tire sealants, wires and cables, industrial products, rubber shoes, etc. It is also an intermediate for the synthesis of vulcanization accelerator DPG. my country is a big rubber processing country in the world, and its annual rubber consumption ranks first in the world for four consecutive years. In 2013, China's rubber consumption was 8.3 million tons, an increase of 13.7% over the previous year, o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/16
CPCC07C335/16
Inventor 吕寻伟马松潘琳琳孙庆刚
Owner SHANDONG YANGGU HUATAI CHEM
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