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Preparation method of anti-aging agent

A technology of anti-aging agent and reagent, which is applied in the field of anti-aging agent preparation, and can solve the problems of complex preparation process and low production efficiency of anti-aging agent

Inactive Publication Date: 2017-01-11
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to provide a preparation method of anti-aging agent to solve the problems of complex preparation process and low production efficiency of anti-aging agent 616 in the prior art

Method used

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  • Preparation method of anti-aging agent
  • Preparation method of anti-aging agent
  • Preparation method of anti-aging agent

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preparation example Construction

[0019] As described in the background technology section, the existing preparation process of anti-aging agent 616 requires the use of two different catalyst systems, and requires high acid resistance of equipment, resulting in high production costs, complicated post-processing, and low production efficiency. In order to solve this problem, the present invention provides a preparation method of anti-aging agent, which comprises the following steps: taking p-cresol, dicyclopentadiene and tert-butylating reagent as raw materials, under the catalysis of sulfonic acid catalyst Reaction, obtain antiaging agent 616, or obtain antiaging agent 616 and antiaging agent 264 simultaneously.

[0020] In the above method provided by the present invention, using p-cresol, dicyclopentadiene and tert-butylating reagent as raw materials, only sulfonic acid catalysts can be used to prepare anti-aging agent 616, or anti-aging agent 616 and anti-aging agent Agent 264. Specifically, when p-cresol ...

Embodiment 1

[0035] Add 200g p-cresol (1.85mol molar weight) and 0.60g catalyst trifluoromethanesulfonic acid (accounting for 3.0% by mass of p-cresol) in a 1000mL four-necked reaction flask, start stirring, and heat up to 70°C , began to dropwise add 120 g of dicyclopentadiene (the molar weight is 0.91 mol), and after the dropwise addition was completed, the temperature was raised to 120° C. to continue the reaction for 1-2 h. After the reaction is completed, add 400g of toluene, 180g of isobutylene is introduced at 75°C for about 3-6 hours, after the reaction is completed, add 4g of calcium hydroxide to neutralize for 2 hours, then filter and rectify, recover toluene, rectify anti-aging agent 264, the yield is 98% , with a purity of 91%. Finally, the bottom of the kettle is anti-aging agent 616, the yield is 99%, and the purity is 98.85%.

Embodiment 2 to 13

[0037] Adopt the processing steps of preparing anti-aging agent 616 and anti-aging agent 264 described in embodiment 1, by changing the catalyst in the reaction, the obtained experimental result data is as follows:

[0038]

[0039] It should be noted that the anti-aging agent 616 is a polymer, essentially a mixture of products with different degrees of polymerization of p-cresol and dicyclopentadiene. The purity of the above antiaging agent 616 represents the percentage of the mixture of different degrees of polymerization in the total amount of the antiaging agent 616 product. (the same below)

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Abstract

The invention discloses a preparation method of an anti-aging agent. The preparation method comprises the following steps: allowing p-cresol, dicyclopentadiene and t-butylation reagent as raw materials to react under the catalysis of a sulfonic acid catalyst to obtain the anti-aging agent 616 or simultaneously obtain the anti-aging agent 616 and the anti-aging agent 264. The sulfonic acid catalyst is relatively low in equipment requirement, simple in later separation and less in three wastes, facilitates the simplification of the preparation process of the anti-aging agent 616, the cost is reduced, and the production efficiency is improved. In addition, the sulfonic acid catalyst is adopted to catalyze the reaction among the p-cresol, the dicyclopentadiene and the t-butylation reagent, the catalytic activity is also relatively high, and the yield and purity of the target product anti-aging agent 616 are improved on the basis of simplifying the process and reducing the cost. Meanwhile, the preparation of the anti-aging agent 264 by using the sulfonic acid catalyst is low in acid resistance requirement on equipment, the amount of generated wastewater is less, and the post-treatment step of excessive p-cresol in the crude product of the anti-aging agent 616 can be avoided.

Description

technical field [0001] The invention relates to the field of preparation of anti-aging agents, in particular to a preparation method of anti-aging agents. Background technique [0002] The properties of rubber, plastic and their products tend to gradually decline with aging, or even completely lose their use value. In order to prolong the service life of rubber and plastic products, it is usually necessary to add substances that inhibit aging, which are called anti-aging agents. [0003] Antiager 616 is a polymeric hindered phenol with excellent properties such as large molecular weight, wash-out resistance, extraction resistance, volatility resistance, small migration, excellent oxidation resistance, discoloration resistance, and non-toxicity. It is widely used in light-colored or Colored rubber, latex products, polyurethane, film plastics and other industries. [0004] In the prior art, p-cresol and dicyclopentadiene are usually used as raw materials, and a two-step meth...

Claims

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Application Information

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IPC IPC(8): C08G61/02C07C39/06C07C37/16C08L65/00C08K5/13
Inventor 李庆华周肖寅陈新民缪振敢徐传兴
Owner JIANGSU SINORGCHEM TECH CO LTD