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Method for continuously synthesizing scorch retarder CTP intermediate (dicyclohexyl disulphide)

A technology of dicyclohexyl disulfide and intermediates, which is applied in the field of raw material synthesis of anti-scorch agent, can solve the problems of large investment in tail gas recondensation, high requirements for rectification equipment, large heat consumption, etc., so as to reduce equipment investment and heat consumption. Large, energy-saving effect

Pending Publication Date: 2018-05-29
山东戴瑞克新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at the deficiencies of existing dicyclohexyl disulfide synthesis methods, high requirements for rectification equipment, large investment, large heat consumption, and large investment in tail gas recondensation during the purification process of its by-product cyclohexene, etc., and provides a A kind of anti-scorch agent CTP intermediate dicyclohexyl disulfide continuous synthesis method, the method recycles the cyclohexene crude product to the synthesis process of dicyclohexyl disulfide, without rectifying cyclohexene, saving It saves energy, reduces equipment investment, and can realize continuous production. The quality of the obtained dicyclohexyl disulfide still meets the requirements of synthetic rubber anti-scorch agent CTP, and has good practicability

Method used

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  • Method for continuously synthesizing scorch retarder CTP intermediate (dicyclohexyl disulphide)
  • Method for continuously synthesizing scorch retarder CTP intermediate (dicyclohexyl disulphide)

Examples

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Effect test

Embodiment 1

[0042] 1. Take 800kg of commercially available cyclohexene (purity ≥ 99.00%) and put it into the synthesis kettle, add 3000L of hydrochloric acid with a concentration of 28-32% into the synthesis kettle, stir and heat, raise the temperature to 95°C, react for 4 hours, and turn it on after the reaction is completed Circulating water valve cools down the synthetic kettle, stop cooling when the temperature drops below 60°C, turn off the stirring, let stand for liquid separation, the water phase obtained by liquid separation is hydrochloric acid aqueous solution, and put the separated hydrochloric acid aqueous solution into the hydrochloric acid intermediate tank for storage. The oil phase obtained by liquid separation is the crude chlorocyclohexane, which is put into the alkali washing tank and washed with a large amount of saturated sodium bicarbonate solution. Neutralize all the hydrochloric acid, then let it stand for stratification, discharge the sodium bicarbonate lotion in t...

Embodiment 2

[0046] 1. Take 800kg of commercially available cyclohexene (purity ≥ 99.00%) into the synthesis kettle, add 2900L of hydrochloric acid with a concentration of 28-32% into the synthesis kettle, stir and heat, raise the temperature to 106°C, react for 12 hours, and turn it on after the reaction is completed Circulating water valve cools down the synthetic kettle, stop cooling when the temperature drops below 60°C, turn off the stirring, let stand for liquid separation, the water phase obtained by liquid separation is hydrochloric acid aqueous solution, and put the separated hydrochloric acid aqueous solution into the hydrochloric acid intermediate tank for storage. The oil phase obtained by liquid separation is the crude chlorocyclohexane, which is put into the alkali washing tank and washed with a large amount of saturated sodium bicarbonate solution. Neutralize all the hydrochloric acid, then let it stand for stratification, discharge the sodium bicarbonate lotion in the lower ...

Embodiment 3

[0050] 1. Take 800kg of commercially available cyclohexene (purity ≥ 99.00%) into the synthesis kettle, drop 2500L of hydrochloric acid with a concentration of 28-32% into the synthesis kettle, and complete the dropwise addition in 3 hours. After the addition, stir and heat, and raise the temperature to 105 ℃, react for 10 hours, after the reaction, open the circulating water valve to cool down the synthesis kettle, stop the cooling when the temperature drops below 60°C, turn off the stirring, stand for liquid separation, the water phase obtained by liquid separation is hydrochloric acid aqueous solution, and the separated hydrochloric acid The aqueous solution enters the hydrochloric acid intermediate tank for storage for later use. The oil phase obtained by liquid separation is the crude product of chlorocyclohexane. The crude product is put into the alkali washing tank and washed with a large amount of saturated sodium bicarbonate solution. The material is recycled and washe...

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Abstract

The invention discloses a method for continuously a synthesizing scorch retarder CTP intermediate (dicyclohexyl disulphide). The method includes the steps of mixing cyclohexene and a hydrochloric acidwater solution to have an addition reaction, washing a chlorocyclohexane coarse product phase obtained through the reaction with alkali liquor to obtain chlorocyclohexane, using a hydrochloric acid water solution obtained through layering for synthesizing a next batch of chlorocyclohexane, mixing chlorocyclohexane, sulphur, sodium sulphide and water to have a vulcanization reaction, conducting standing and layering on reaction liquid obtained after the reaction, distilling an obtained oil phase, sequentially obtaining a cyclohexene coarse product and dicyclohexyl disulphide, and directly using the obtained cyclohexene coarse product for raw material reusing. The cyclohexene coarse product can be used for production, the defects that an existing dicyclohexyl disulphide synthesizing processis complex, separating and purifying operation is complicated, and yield is low are overcome, the operation environment is greatly improved, the distilling cost is reduced, production efficiency is improved, and good production advantages are achieved.

Description

technical field [0001] The invention relates to a method for synthesizing raw materials for rubber anti-scorch agent CTP, in particular to a method for continuously synthesizing dicyclohexyl disulfide, and belongs to the technical field of synthesizing anti-scorch agent raw materials. Background technique [0002] The structural formula of dicyclohexyl disulfide is , can be used as food spices, used in dyes, medicines, pesticides, organic synthesis, etc.; in the rubber additive industry, dicyclohexyl disulfide is a synthetic anti-scorch agent CTP Amine) is one of the main raw materials. The anti-scorch agent CTP was developed by Monsanto Company in the United States in the late 1960s. This product can improve the scorch time of the rubber in the rubber containing sulfenamide accelerator, and has little effect on the vulcanization speed and the performance of the vulcanized rubber. The anti-scorch time can be adjusted by changing its dosage within a wide range. The scorch...

Claims

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Application Information

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IPC IPC(8): C07C17/10C07C23/10C07C319/24C07C319/28C07C321/16
CPCC07C17/10C07C319/24C07C319/28C07C23/10C07C321/16
Inventor 许思俊李世梅李宪索郑崇纳马亚敏王兴军刘红李建民桑圣印赵丹丹
Owner 山东戴瑞克新材料有限公司
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