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Synthetic method of vulcanizing agent 1,1-caprolactam disulfide

A technology for dithiodicaprolactam and a synthesis method, which is applied in the direction of organic chemistry and the like, can solve the problems of low product yield and melting point, high solvent toxicity, large amount of waste water, etc., and achieves less volatilization of solvent, cheap raw materials, and reduced waste water. The effect of discharge

Active Publication Date: 2016-03-02
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing dithiocaprolactam synthesis technology uses solvents such as trichlorethylene and DMF, which have the problems of high solvent toxicity and difficulty in recycling, low product yield and melting point, and a large amount of wastewater in the production process

Method used

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Examples

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Effect test

Embodiment 1

[0026] A synthetic method of vulcanizing agent 1,1-dithiodicaprolactam, the production process flow chart is shown in figure 1 As shown, the steps are as follows:

[0027] (1) After nitrogen replacement in the reactor, put in 900kg120# solvent oil, 210kg pyridine and 300kg caprolactam, after the temperature rises to 50°C, start to drop 170kgS 2 Cl 2 After 2 hours, the dropwise addition was completed, and after the addition was completed, stirring was continued at this temperature for 2.5 hours, and the mixture was obtained after the reaction was completed;

[0028] (2) Add a sodium hydroxide solution with a mass concentration of 15% in the kettle to adjust the pH value to 7, stir and heat up to 85°C, keep it standing at 85°C for half an hour, put the water phase clean, put the solvent oil phase into the cooling kettle, Cool down to 5°C with cooling water, and the product precipitates. After filtration, the wet product dithiodicaprolactam is obtained. The wet product is dried...

Embodiment 2

[0030] A kind of synthetic method of vulcanizing agent 1,1-dithiodicaprolactam, the steps are as follows:

[0031] (1) After nitrogen replacement in the reactor, put in 1252kg120# solvent oil, 219kg pyridine and 313kg caprolactam, after the temperature rises to 60°C, start to drop 170kgS 2 Cl 2 After 2 hours, the dropwise addition was completed, and after the addition was completed, stirring was continued at this temperature for 2.5 hours, and the mixture was obtained after the reaction was completed;

[0032] (2) Add a sodium hydroxide solution with a mass concentration of 14% in the kettle to adjust the pH value to 7, stir and heat up to 90°C, keep standing at 90°C for half an hour, put the water phase clean, put the solvent oil phase into the cooling kettle, Cool down to 10°C with cooling water, and the product precipitates. After filtration, the wet product dithiodicaprolactam is obtained. The wet product is dried to obtain 320kg of white solid, with a purity of 98.5%, a ...

Embodiment 3

[0034] A kind of synthetic method of vulcanizing agent 1,1-dithiodicaprolactam, the steps are as follows:

[0035] (1) After nitrogen replacement in the reaction kettle, put in 1000kg120# solvent oil, 209kg pyridine and 299kg caprolactam, after heating up to 45°C, start to drop 170kgS 2 Cl 2 After 2 hours, the dropwise addition was completed, and after the addition was completed, stirring was continued at this temperature for 2.5 hours, and the mixture was obtained after the reaction was completed;

[0036] (2) Add a sodium hydroxide solution with a mass concentration of 13% in the kettle to adjust the pH value to 7 and stir to raise the temperature to 87°C, keep it standing at 87°C for half an hour, put the water phase clean, put the solvent oil phase into the cooling kettle, Cool down to 6°C with cooling water, and the product precipitates. After filtration, the wet product dithiodicaprolactam is obtained. The wet product is dried to obtain 326 kg of white solid with a puri...

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Abstract

The invention relates to a synthetic method of a vulcanizing agent 1,1-caprolactam disulfide. The method comprises the following steps: adding solvent naphtha, caprolactam and pyridine in a reaction vessel in order, dropwise adding sulfur chloride at controlled temperature, and reacting to prepare a mixture; and neutralizing the mixture to a neutral state by adding water containing soda, heating and separating water to remove the water phase, cooling to crystallize, filtering, and drying to obtain a finished product. The method employs the 120# solvent naphtha as the solvent to achieve less volatilization of solvent in the production process; by heating water separation, the washing frequency is reduced, so as to reduce the wastewater discharge and greatly reduce the pollution to the environment. By using the solvent and the synthetic process, the product is crystallized by cooling, has improved quality of more than 98%, and increased yield of above 85%, and initial melting point of higher than 125 DEG C.

Description

technical field [0001] The invention relates to a method for synthesizing vulcanizing agent 1,1-dithiodicaprolactam, which is a synthetic rubber chemical additive to enhance the characteristics of rubber such as anti-wear, anti-aging, anti-corrosion, and durability, and belongs to the field of synthesizing rubber additives. Background technique [0002] Rubber is widely used in modern civilized society. The tires of automobiles, airplanes, bicycles, pipes and joints in various industries, and various cable rubber sleeves, rubber shoes, rubber hoses, etc. in daily life must use natural rubber or synthetic rubber. Rubber, through rubber products of various specifications, meets the needs of industrial and agricultural production and daily life. In order to enhance the service time of rubber products in hot and cold weather, appropriate rubber additives, such as rubber vulcanizing agents, accelerators, etc. must be added. Dithiodicaprolactam (DTDC) is one of the rubber vulcani...

Claims

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Application Information

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IPC IPC(8): C07D223/10
CPCC07D223/10
Inventor 王德楼孟祥克杜孟成
Owner SHANDONG YANGGU HUATAI CHEM
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