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Preparation method of rubber antioxidant N,N'-di-sec-butyl-1,4-phenylenediamine

A technology of di-sec-butyl-p-phenylenediamine and rubber antioxidant is applied in the field of preparation of rubber antioxidant, which can solve the problems of high price, dependence on imports and the like, and achieves good effect, high product yield and simple process. Effect

Inactive Publication Date: 2015-05-06
QINGDAO WANGYU RUBBER
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Problems solved by technology

At present, the demand in the domestic market is very large, but it mainly depends on imports, and the price is very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0015] 1. Add p-phenylenediamine and methyl ethyl ketone with a mass ratio of 1:6 into the autoclave, and pass nitrogen to replace the air in the autoclave for 4 times. Heat to 160°C and react under the conditions of 3.3MPa-5.6MPa. 10h;

[0016] 2. After the reaction is completed, cool, filter, and distill to remove excess methyl ethyl ketone and produced sec-butanol to obtain N,N'-di-sec-butyl-p-phenylenediamine.

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Abstract

The invention discloses a preparation method of rubber antioxidant N,N'-di-sec-butyl-1,4-phenylenediamine. The preparation method comprises following steps: step 1, p-phenylenediamine, butanone, and a catalyst are delivered into a high-pressure autoclave, air in the high-pressure autoclave is replaced with nitrogen, and an obtained mixture is heated to 160 DEG C, and is reacted for 10h under 3.3 to 5.6MPa, wherein mass ratio of p-phenylenediamine to butanone is 1:6; and step 2, after reaction, an obtained product is subjected to cooling, filtering, and distilling so as to remove excess butanone and obtained sec-butyl alcohol so as to obtain N,N'-di-sec-butyl-1,4-phenylenediamine. According to the preparation method, catalytic hydrogenation effect is excellent in presence of the catalyst, the preparation method is simple, and product yield is high.

Description

[0001] Technical field [0002] The invention relates to a preparation method of a rubber antioxidant, in particular to a preparation method of N,N`-di-sec-butyl p-phenylenediamine. [0003] Background technique [0004] N,N`-Di-sec-butyl p-phenylenediamine is a good anti-oxidant and anti-glue agent for gasoline, and can also be used as a general anti-ozonant for natural rubber and synthetic rubber. At present, the domestic market demand is very large, but it mainly depends on imports and the price is very high. [0005] Summary of the invention [0006] The purpose of the present invention is to provide a method for preparing rubber antioxidant N,N'-di-sec-butyl-p-phenylenediamine, which has simple process and high product yield. [0007] The preparation method of the rubber antioxidant N,N'-di-sec-butyl-p-phenylenediamine includes the following steps: [0008] 1. Add p-phenylenediamine and methyl ethyl ketone with a mass ratio of 1:6 into the autoclave, introduce nitrogen to replace ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C209/68
Inventor 梁松杰
Owner QINGDAO WANGYU RUBBER
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