Method for refining 4-amino diphenylamine

A technology of aminodiphenylamine and aniline, which is applied in the field of refining 4-aminodiphenylamine, and can solve the problems of difficult separation by distillation, waste of resources, and aniline being mechanically returned.

Inactive Publication Date: 2004-01-28
JIANGSU SINORGCHEM TECH CO LTD
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Problems solved by technology

If a simple distillation method is adopted, it is difficult to separate the above-mentioned components by distillation; if a two-tower distillation is adopted, the three materials of aniline, phenazine and azobenzene are discharged from the top of the front fraction tower, and 4-aminodiphenylamine is discharged from the top of the front fraction tower. The tower kettle is discharged, and then 4-aminodiphenylamine is continuously fed to the product tower, and the 4-aminodiphenylamine is discharged at the top of the tower, and the remaining materials are discharged at the tower kettle. The aniline in the raw material contains two substances, phenazine and azobenzene, and a large amount of aniline in the top of the product tower cannot be used mechanically back to the previous process, so the aniline cannot be recycled and used mechanically, resulting in waste of resources and increased production costs

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  • Method for refining 4-amino diphenylamine

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Embodiment Construction

[0015] The crude product containing 4-aminodiphenylamine (containing 4-aminodiphenylamine 78.1%, aniline 20.1%, azobenzene 1.1%, phenazine 0.7%) was continuously fed into No. 1 rectification through a gear pump at a flow rate of 120 kg / hour tower. The temperature of the tower kettle was controlled at 270°C, the temperature at the top of the tower was controlled at 110°C, the degree of vacuum was 0.094MPa, the reflux ratio was 5:1, and three substances, aniline, azobenzene, and phenazine, were extracted from the top of the tower, and the flow rate was 26.2 kg. About / hour, enter No. 3 rectifying tower, No. 3 rectifying tower tower still temperature 150 ℃, tower top temperature 90 ℃, vacuum degree 0.094MPa, reflux ratio 1: 1, tower top distills out aniline with flow rate 24 kg / hour , what is left in the tower still is azobenzene, phenazine, 1 rectifying tower tower still liquid enters No. 2 rectifying tower, keeps tower still temperature 280 ℃, vacuum degree 0.097MPa, tower top ...

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Abstract

The present invention relates to a method for refining 4-aminodiphenylamine by adopting three-column continuous rectification and intermittent distillation. The crude product of 4-aminodiphenylamine can be obtained by rectification in the column No.1, and the substances of phenylamine, phenazine and azobenzene can be obtained at the top of column, said crude product can be purified in column No.2, in the column No.3 the phenylamine is separated, and the intermittent column can be used for making batch distillation of 4-aminophenylamine made up by using column bottoms of column No.2 and returning it into column No.2 for refining it. The yield rate of its whole process can be raised to 99% from 94%, and the content of 4-aminodiphenylamine in the finished product is greater than 99 wt%, at the same time the phenylamine can be recovered, and can be used.

Description

technical field [0001] The invention relates to a method for purifying 4-aminodiphenylamine, in particular to a method for purifying 4-aminodiphenylamine by three-column rectification and batch distillation. Background technique [0002] 4-Aminodiphenylamine is an important intermediate compound of rubber antioxidants, and its quality directly affects the quality of downstream products. The existing method of distilling 4-aminodiphenylamine generally adopts simple distillation, its vacuum degree is 0.095MPa, the kettle temperature is 280℃-330℃, the top temperature is 220℃-240℃, and the heating adopts flue gas heating or far-infrared heating. Heating, using this method in the later stage of simple distillation, the kettle temperature is as high as 300 ℃ or more, and a large amount of coking is formed in the kettle at the same time, resulting in a decrease in the product yield and quality of 4-aminodiphenylamine; at the same time, simple distillation is used. The number of pl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/86C07C211/55
Inventor 冯晓根
Owner JIANGSU SINORGCHEM TECH CO LTD
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