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Method for preparing tire antioxidant 3100

An anti-aging agent and tire technology, which is applied in the preparation of organic compounds, amino compounds, chemical instruments and methods, etc., can solve the problems of restricting the process of industrialization, complex catalyst preparation process, and little significance of industrialization.

Inactive Publication Date: 2019-08-23
扬州市业昌助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of the catalyst is very complicated, and the industrialization is of little significance; the route of process 3 conforms to the concept of atom economy, and the reaction conditions are mild and green, but because 1,4-cyclohexanedione itself is difficult to obtain and expensive, it is limited The process of industrialization of the route

Method used

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  • Method for preparing tire antioxidant 3100
  • Method for preparing tire antioxidant 3100
  • Method for preparing tire antioxidant 3100

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 184g p-aminodiphenylamine and 5.5g CuCl 2 Put it into the reactor, start stirring and mixing, raise the temperature to above 110°C, then turn on the vacuum to keep the vacuum degree at -0.06MPa, then add the mixture of 33g phenol and 72g o-cresol in 3 batches, and control the addition within 2h, Keeping the temperature within 110-140°C, the reaction is dehydrated, and when the temperature reaches 130°C and no water is released, the reaction is completed. The reaction solution was cooled to 90-100°C, and the catalyst was filtered off while hot to obtain 276 g of finished product, the reaction yield was 96.2%, and the melting point was 92.5°C.

Embodiment 2

[0028] 184g p-aminodiphenylamine and 6g CuCl 2 Put it into the reactor, start stirring and mixing, raise the temperature to above 110°C, then turn on the vacuum to keep the vacuum degree at -0.06MPa, then add the mixture of 47g phenol and 54g o-cresol in 5 batches, and control the addition within 2h, Keeping the temperature within 110-140°C, the reaction is dehydrated, and when the temperature reaches 130°C and no water is released, the reaction is completed. The reaction solution was cooled to 90-100°C, and the catalyst was filtered off while hot to obtain 280 g of finished product, the reaction yield was 98.2%, and the melting point was 92°C.

Embodiment 3

[0030] 184g p-aminodiphenylamine and 6g NiCl 2 Put it into the reactor, start stirring and mixing, raise the temperature to above 110 ℃, then turn on the vacuum to keep the vacuum degree at -0.06MPa, then add the mixture of 61g phenol and 38g o-cresol in 4 batches, and control the addition within 2h, Keeping the temperature within 110-140°C, the reaction is dehydrated, and when the temperature reaches 130°C and no water is released, the reaction is completed. The reaction solution was cooled to 90-100 DEG C, and the catalyst was filtered off while hot to obtain 270 g of finished product with a reaction yield of 95.7% and a melting point of 91.4 DEG C.

[0031] The finished products obtained in the above three cases were respectively tested by GC, and they were all tire anti-aging agent 3100.

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Abstract

The invention discloses a method for preparing a tire antioxidant 3100, belongs to the field of fine chemical synthesis, and concretely relates to a production technology for the tire antioxidant 3100. The production technology comprises the following steps: p-aminodiphenylamine and a catalyst are placed in a reaction vessel, and are heated to 110-140 DEG C, the temperature is kept, vacuumizing iscarried out to -0.06 MPa, a mixture of phenol and o-cresol is added under a stirring condition, the obtained mixture is reacted until no water is evaporated, the temperature is reduced to 90-100 DEGC, and the catalyst is filtered out to obtain the tire antioxidant 3100. The technology has the advantages of easily available raw materials, simple reaction process, mild conditions, low and controlled energy consumption, few generated wastes, and suitableness for large-scale production.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis, and specifically relates to the production technology of anti-aging agent 3100 for tires. Background technique [0002] The active ingredients of antioxidant 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, and its resistance to flexing and cracking is similar to that of anti-aging agents 4010NA and 6PPD, and far better than that of anti-aging agents A and D. Antioxidant 3100 has good long-term performance, especially when used together with anti-aging agent 6PPD or 4010NA 1:1, it is the best anti-ozone system to improve the service life of tires. The reason is that the two types of p-phenylenediamine have a synergistic effect. 4010NA provides the necessary short-term protection in the early stages, while the antioxidant 3100 provides long-ter...

Claims

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Application Information

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IPC IPC(8): C07C209/18C07C209/68C07C211/55C08K5/18
CPCC07C209/18C07C209/68C08K5/18C07C211/55
Inventor 朱运昇李辉宁张才山朱平太
Owner 扬州市业昌助剂有限公司
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