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Method for continuously preparing N, N'-bis(1,4-dimethylpentyl)-p-phenylenediamine

A technology of dimethylpentyl and p-phenylenediamine is applied in the field of energy-saving and high-efficiency preparation technology, which can solve the problems of difficulty in recycling and high cost, and achieve the effects of saving labor costs, reducing costs and reducing labor intensity.

Inactive Publication Date: 2013-12-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses precious metals such as palladium or platinum as a catalyst, which is costly and difficult to recycle.

Method used

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  • Method for continuously preparing N, N'-bis(1,4-dimethylpentyl)-p-phenylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 1382.0 grams of p-nitroaniline and 5710.4 grams of 5-methyl-2-hexanone into the raw material mixer. After mixing well, use the delivery pump to drive the mixed raw materials into the preheater at a speed of 20ml / h to keep the preheater. The temperature of the heater is 145~150°C. At the same time, hydrogen gas is passed into the reactor filled with palladium catalyst and replaced with nitrogen, and the reactor temperature is kept at 190~200°C, and the hydrogen pressure is kept at 0.7Mpa. After 24 hours, the Let off the liquid sample from the liquid separator, and after another 24 hours, collect the reaction solution, distill under 20mmHg vacuum, stop when the kettle temperature is 240°C, cool down and vent the vacuum, and obtain 178g of finished product. After testing, p-nitroaniline is not detected, N, The content of N'-bis(1,4-dimethylpentyl)-p-phenylenediamine is 96.31%.

Embodiment 2

[0021] The operating conditions are the same as in Example 1, the catalyst used is a platinum catalyst, and 189 grams of finished product are obtained. After testing, p-nitroaniline is not detected, and N,N'-bis(1,4-dimethylpentyl)-p-phenylenediamine The content is 97.06%.

Embodiment 3

[0023] Operating condition is the same as embodiment 1, and catalyzer used is the copper series catalyst that has reduced (CuO39W%, Cr 2 o 3 7W%, Al 2 o 3 ,54W%) the flow rate of the delivery pump was increased to 30ml / h, and 274g of finished product was obtained. After testing, p-nitroaniline was not detected, containing N,N'-bis(1,4-dimethylpentyl)terephthalene The amine content is 97.54%.

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Abstract

The invention belongs to the technical field of fine chemical engineering, and relates to a method for continuously preparing N, N'-bis(1,4-dimethylpentyl)-p-phenylenediamine, and the method helps to realize continuous and low-pressure production of N'-bis(1,4-dimethylpentyl)-p-phenylenediamine, so that cost is saved and economical benefit is raised. The method comprises: mixing p-phenylenediamine (or p-nitroaniline ) and 5-methyl-2-hexanone according to a certain ratio, continuously conveying to a preheater, keeping the preheater at 110-150 DEG C, then enabling preheated materials to enter into a narrow and long reactor loaded with a solid catalyst via a pipeline, and keeping the reactor at 150-200 DEG C, at the same time continuously introducing hydrogen with a pressure of 0.5-2.5 MPa into the reactor, after the materials are reacted, collecting the product into a gas-liquid separator via a cooler, moving out the reaction solution and performing reduced pressure distillation to obtain N, N'-bis(1,4-dimethylpentyl)-p-phenylenediamine. The conversion rate of p-nitroaniline is 99% or more and selectivity is 95% or more.

Description

technical field [0001] The invention belongs to the field of fine chemicals, relates to a method for continuously preparing N,N'-bis(1,4-dimethylpentyl)-p-phenylenediamine under low pressure conditions, and is an energy-saving and efficient preparation process. Background technique [0002] N,N'-bis(1,4-dimethylpentyl)-p-phenylenediamine is commonly known as anti-aging agent 4030. It is a high-efficiency anti-ozone anti-aging agent. It is mainly used in rubber materials that work under static conditions for a long time. Such as aviation tires, engineering tires, agricultural equipment tires and vehicle structural supports, fixed hoses, sealing strips, etc.; due to its excellent anti-ozone function, it is widely used as a stabilizer for colored solution-polymerized and emulsion-polymerized elastomers, such as some synthetic rubbers and elastomer stabilizers. In addition, this product is a liquid product, which is easy to disperse and facilitate rubber processing. It has a go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/26
Inventor 韦志强郁铭付春黄伟孙阿沁张萍
Owner CHINA PETROLEUM & CHEM CORP
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