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Method for preparing age inhibitor 3100

A technology for anti-aging agent and solvent, applied in the field of preparing anti-aging agent 3100, can solve the problems of large market price fluctuation of hydroquinone, large amount of waste water in the washing process, and high production cost of anti-aging agent, and achieves low cost, simplified operation, and avoidance of materials. The effect of coking

Active Publication Date: 2012-07-18
宜兴市聚金信科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, due to the large fluctuations in the market price of raw material hydroquinone, the production cost of anti-aging agent 3100 is too high, which greatly limits the field and scope of its application
Moreover, the existing process uses alkali neutralization and water washing to achieve the purpose of removing the inorganic catalyst. The water washing process has a large amount of wastewater, serious pollution, and is difficult to operate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 100 grams of aniline and 200 grams of o-toluidine into the reactor, start stirring and mixing, raise the temperature to 60-70°C, add 109 grams of p-aminophenol, 5 grams of benzenesulfonic acid and 5 grams of toluene into the reactor in turn, The temperature is continuously raised to about 220°C within 30 minutes to carry out the condensation reaction, and the water and ammonia generated by the reaction are continuously exported by the solvent toluene. After about 5 hours, when the reaction no longer produces water, the reaction reaches the end, and the temperature of the reaction solution is lowered to 100-110°C , filtered while hot to remove the catalyst, and then the filtrate was distilled to remove toluene, aniline, o-toluidine and intermediates to obtain 228 grams of finished product with an active ingredient content of 93.5% and a melting point of 92°C.

Embodiment 2

[0017] Add 100 grams of aniline and 220 grams of o-toluidine into the reactor, start stirring and mixing, raise the temperature to 60-70°C, add 109 grams of p-aminophenol, 10 grams of benzenesulfonic acid and 7 grams of toluene into the reactor in turn, The temperature is continuously raised to about 210°C within ~30 minutes to carry out the condensation reaction. The water and ammonia produced by the reaction are continuously exported by the solvent toluene for about 5 hours. ℃, filtered while hot to remove the catalyst, and then the filtrate was distilled to remove toluene, aniline, o-toluidine and intermediate products to obtain 227 grams of finished product with an active ingredient content of 92.8% and a melting point of 92.5°C.

Embodiment 3

[0019] The operating conditions were the same as in Example 1, but 5 grams of p-toluenesulfonic acid was used as the catalyst to obtain 208 grams of finished product with an active ingredient content of 91% and a melting point of 93.5°C.

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Abstract

The invention discloses a method for preparing an age inhibitor 3100. In the method, paraaminophenol, aniline and o-nitrotoluene are taken as raw material for condensation reaction under the effect of organic sulfonic acid catalyst, the reaction temperature is 110 to 220 DEG C, water and ammonia produced by the reaction can be led out through azeotropic solvent continuously, after the reaction reaches an end point, the temperature is lowered to 100 to 140 DEG C, filtering is performed while hot, and filter liquor is distilled for removing impurities. The method provided by the invention has a high raw material conversion rate, the contents of the obtained effective components are high, the cost is low, the three wastes are less, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a low-cost, energy-saving and high-efficiency method for preparing anti-aging agent 3100. Background technique [0002] The active ingredients of anti-aging agent 3100 are N-phenyl-N'-o-tolyl-p-phenylenediamine, N,N'-diphenyl-p-phenylenediamine, N,N'-di-o-tolyl-p-phenylenediamine The mixture is a p-phenylenediamine anti-aging agent, which can prevent ozone, flex and crack resistance, which is similar to anti-aging agent 4010NA and 6PPD, far better than anti-aging agent A and D. The anti-aging agent 3100 has good long-term performance, especially when used together with the anti-aging agent 6PPD or 4010NA 1:1, it is the best anti-ozone system to improve the service life of the tire. Provides the necessary short-term protection in the early stage, while Antioxidant 3100 provides long-term protection. Since one or two solubilizing genes are induced on the benzene rings on both sides of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/18C07C211/55
Inventor 储云仙俞大伟
Owner 宜兴市聚金信科技有限公司
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