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Preparation process of P-tert-butylphenol disulphide vulcanilzer

A technology for the preparation of p-tert-butylphenol, which is applied in the field of preparation of rubber additives, can solve the problems of high production cost, high cost, and long reaction time, and achieve the effects of low equipment requirements, short production cycle, and simple operation

Inactive Publication Date: 2013-03-13
阳谷华泰(北京)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above process uses more toxic reagents such as acetonitrile, nitromethane, etc., the solvent cannot be recycled and reused, the reaction time is long, and the cost is high, which is not conducive to industrial production
[0008] U.S. Patent 4599451 reported that in the presence of a zirconium-containing catalyst, phenol reacted with an alkyl disulfide compound to obtain an ortho or para thiophenol product, but a relatively expensive metal catalyst was used in the preparation process and was reclaimed Reuse is very difficult and production costs are high

Method used

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  • Preparation process of P-tert-butylphenol disulphide vulcanilzer

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Effect test

Embodiment 1

[0018] The preparation method of p-tert-butylphenol disulfide (TB710) adopts the following steps:

[0019] Add 15 g of p-tert-butylphenol and 2 ml of petroleum ether into a 100 ml four-neck glass flask equipped with a stirring, thermometer and constant pressure dropping funnel, and stir to raise the temperature until the solid is completely dissolved. Add 13.5g of sulfur monochloride dropwise through the dropping funnel, control the drop rate, drop it in about 30 minutes, absorb the tail gas with dilute lye, continue the reaction until the reaction has no gas release and reach the end of the reaction, the reaction temperature is 100-140°C , from the initial dissolution to the completion of the reaction, the temperature gradually increased in this range. The alkane solvent was recovered by distillation under reduced pressure in the system, and the next mother liquor was used mechanically. The remaining brown viscous liquid after distillation was granulated to obtain a brown sol...

Embodiment 2

[0021] The preparation method of rubber vulcanizing agent (TB710) adopts the following steps:

[0022] Add 300 g of p-tert-butylphenol and 400 ml of petroleum ether into a 1000 ml four-neck glass flask equipped with a stirring, thermometer and constant pressure dropping funnel, stir and heat up until the solid is completely dissolved. Add 297g of sulfur chloride dropwise through the dropping funnel, and control the dropping rate. After about 2.0 hours, the tail gas is absorbed with dilute lye. After the dropwise addition, continue the reaction until the reaction has no gas release and reaches the end of the reaction. The reaction temperature is 100-140°C. From the initial dissolution to the completion of the reaction, the temperature gradually increases in this range. The linear alkane solvent was recovered by distillation under reduced pressure for the next mother liquor to be used mechanically to obtain a brown viscous liquid, which was released while hot and granulated to o...

Embodiment 3

[0024] The preparation method of rubber vulcanizing agent (TB710) adopts the following steps:

[0025] Add 150 g of p-tert-butylphenol and 150 ml of petroleum ether into a 500 ml four-neck glass flask equipped with a stirring, thermometer and constant pressure dropping funnel, stir and heat up until the solid is completely dissolved. Add 162g of sulfur chloride dropwise through the dropping funnel, control the drop rate, drop it in about 1.5 hours, absorb the tail gas with dilute lye, continue the reaction until the reaction has no gas release, and then reach the end of the reaction. From the initial dissolution to the completion of the reaction, the temperature gradually increases within this range. , Distilled under reduced pressure to recover the linear alkane solvent for the next mother liquor to be applied mechanically to obtain a brown viscous liquid and release it while hot for granulation to obtain a brown solid with a yield ≥ 98%, a softening point of 90°C, and a sulf...

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Abstract

The invention relates to a preparation process of P-tert-butylphenol disulphide vulcanilzer and belongs to the technical field of preparation methods of rubber auxiliary. The P-tert-butylphenol disulphide vulcanilzer is synthesized by reaction of P-tert-butylphenol and sulphur chloride in liquid phase alkane solvent, the P-tert-butylphenol disulphide vulcanilzer is heated in the solvent until solid is completely dissolved, sulphur chloride is dropwise added into a system, reduced pressure distillation is directly carried out after reaction is completely finished, and the solid after distillation is directly subjected to pelleting, so that the target product is obtained. The preparation process provided by the invention is easy to operate, equipment requirement is low, production cycle is short, and the alkane is used for substituting trichloro ethylene to be taken as reaction solvent, so that the preparation process provided by the invention is environment-friendly, safe and applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of rubber additives, in particular to a new preparation process of rubber vulcanizing agent p-tert-butylphenol disulfide (TB710). Background technique [0002] Natural rubber (NR) has excellent physical and mechanical properties, elasticity and processing properties, so it is widely used. However, the long-term use temperature of NR is generally not higher than 70°C, because at higher temperatures, the main chain and crosslinking structure of rubber molecules in vulcanized NR will change, resulting in a decrease in mechanical properties and ultimately affecting the performance of the product. In order to improve the performance of rubber, vulcanization is an essential process in the production process of rubber products. In this process, the rubber undergoes a series of complex chemical reactions, changing from a linear structure to a spatial network structure, losing the plasticity of the compounded rubbe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/20C07C319/22
Inventor 董瑞国王艳峰
Owner 阳谷华泰(北京)新材料科技有限公司
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