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Preparation method of dicaprolactam disulfide

A technology of dicaprolactam disulfide and caprolactam, which is applied in the preparation of dicaprolactam disulfide (DTDC) and the field of dicaprolactam disulfide preparation, which can solve the problems of prolonging the reaction time, potential safety hazards, increasing the difficulty of reaction operation, etc., and achieve high melting point , less pollution, improved physical and chemical properties

Active Publication Date: 2019-08-23
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This mode of operation prolongs the reaction time, increases the difficulty of the reaction operation, and has certain potential safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of dicaprolactam disulfide, the steps are as follows:

[0029] 1. Weigh 100g of sulfur monochloride, 343.6g of caprolactam, and 1000g of 120# solvent oil for later use.

[0030] 2. Add 343.6g of caprolactam into 1000g of 120# solvent oil, start to stir and cool down.

[0031] 3. When the temperature drops to 10°C, add 100g of sulfur monochloride to the reaction system at one time, and then use constant temperature water with a temperature lower than 50°C to slowly raise the temperature of the reaction system at a rate of 1°C / min.

[0032] 4. Stop the temperature rise when the temperature rises to 45°C, and keep warm at this temperature for 2 hours; after the heat preservation is completed, start to add 996.2g of sodium hydroxide aqueous solution (6.3wt%) to the reaction system for alkali washing, and the alkali washing time is 1h , The reaction solution is neutral (weakly alkaline) after alkali washing.

[0033] 5. After the alkali washing, the so...

Embodiment 2

[0035] 1. Weigh 100g of sulfur monochloride, 343.6g of caprolactam, and 1000g of 120# solvent oil for later use.

[0036] 2. Add 343.6g of caprolactam into 1000g of 120# solvent oil, start to stir and cool down.

[0037] 3. When the temperature drops to 10°C, add 100g of sulfur monochloride to the reaction system at one time; then use constant temperature water with a temperature lower than 50°C to slowly raise the temperature of the reaction system at a rate of 1°C / min.

[0038] 4. Stop heating when the temperature rises to 43°C, and keep warm at this temperature for 2 hours; after the heat preservation is completed, start to add 996.2g of sodium hydroxide aqueous solution (6.3wt%) to the reaction system for alkali washing, and the alkali washing time is 1h , the reaction solution was neutral after alkali washing.

[0039] 5. After the alkali washing, the solid in the reaction system was suction filtered, rinsed with 200 g of water, and dried under vacuum to obtain 178.9 g o...

Embodiment 3

[0041] 1. Weigh 100g of sulfur monochloride, 343.6g of caprolactam, and 1000g of 120# solvent oil for later use.

[0042] 2. Add 343.6g of caprolactam into 1000g of 120# solvent oil, start to stir and cool down.

[0043] 3. When the temperature drops to 10°C, add 100g of sulfur monochloride to the reaction system at one time; then use constant temperature water with a temperature lower than 50°C to slowly raise the temperature of the reaction system at a rate of 1°C / min.

[0044] 4. Stop heating when the temperature rises to 47°C, and keep warm at this temperature for 2 hours; after the heat preservation is completed, start to add 996.2g of sodium hydroxide aqueous solution (6.3wt%) to the reaction system for alkali washing, and the alkali washing time is 1h , the reaction solution was neutral after alkali washing.

[0045] 5. After the alkali washing, the solid in the reaction system was suction filtered, rinsed with 200 g of water, and dried under vacuum to obtain 179.2 g of ...

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Abstract

The invention discloses a preparation method of dicaprolactam disulfide. The method comprises adding sulfur monochloride only one time at a low temperature, and then raising the temperature to a reaction temperature according to a heating rate of 1-3 DEG C / min to carry out a reaction to obtain dicaprolactam disulfide. The method replaces slow dropping by directly inputting sulfur monochloride, shortens the time required for the synthesis process, and at the same time makes the operation of operators be relatively simple; and the pollution is small, the energy is saved and the environment is protected, the production cost is reduced, the process safety hidden dangers are reduced, and the product yield is high, so that the method adapts to national green chemical policy requirements.

Description

technical field [0001] The invention relates to a preparation method of dicaprolactam disulfide, in particular to a preparation method of dicaprolactam disulfide (DTDC) which is less time-consuming, highly safe and easy to operate, and belongs to the technical field of fine chemicals. Background technique [0002] In recent years, with the rapid development of the automobile industry and the communication industry, the rapid development of the rubber processing industry has provided a good opportunity for the development of the domestic rubber additives industry. However, the production of rubber additives in my country has been greatly improved. However, in terms of environmental protection, especially in terms of green additives, there is still a big gap with foreign countries. The production and application of the vulcanizing agent DTDM and thiuram products are due to the fact that the secondary oxygen released by the cracking of the vulcanizing agent DTDM and thiuram pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10
CPCC07D223/10
Inventor 孟祥克马德龙杜孟成王才朋徐思明李庆朝王克军崔亭亭
Owner SHANDONG YANGGU HUATAI CHEM
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