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Method for preparing 4,4'-bis(phenyl isopropyl)diphenylamine

A technology of phenylisopropyl and diphenylamine, which is applied in the field of chemical synthesis of antioxidants, can solve the problems of poor catalytic effect of catalysts, achieve the effects of reducing the content of impurities, improving utilization rate, and low price

Inactive Publication Date: 2016-06-08
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problem of poor catalytic effect of the catalyst in the preparation process of 4,4'-bis(phenylisopropyl)diphenylamine existing in the prior art, the present invention provides a method for preparing 4,4'-bis(phenylisopropyl)diphenylamine Propyl) diphenylamine method

Method used

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  • Method for preparing 4,4'-bis(phenyl isopropyl)diphenylamine
  • Method for preparing 4,4'-bis(phenyl isopropyl)diphenylamine

Examples

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Embodiment 1

[0029] Refer to the process figure 1 , this specific embodiment discloses a method for preparing 4,4'-bis(phenylisopropyl)diphenylamine, specifically a laboratory preparation of 4,4'-bis(phenylisopropyl)diphenylamine Methods.

[0030] In this embodiment, the weight percentage of activated clay and diphenylamine is 12%, and the molar ratio of diphenylamine to α-methylstyrene is 1:2.0.

[0031] Selection of raw materials and preparation equipment, including diphenylamine (purity ≥ 99.5%), α-methylstyrene (purity ≥ 99%), petroleum ether (analytical pure), activated clay, constant temperature magnetic stirrer, vacuum pump, reflux condensation Device, feeding device, nitrogen protection device, 1L round bottom three-neck reaction flask, thermometer, iron stand, vacuum glass stopper, electric heating mantle, Buchner funnel and other glass instruments.

[0032] Measure 16.9g of diphenylamine and add it to a 1L round-bottomed three-neck reaction flask, weigh 2g of activated clay and...

Embodiment 2

[0037] Refer to the process figure 1 , this specific embodiment discloses a method for preparing 4,4'-bis(phenylisopropyl)diphenylamine, specifically a laboratory preparation of 4,4'-bis(phenylisopropyl)diphenylamine Methods.

[0038] The difference from Example 1 is that the weight percent of activated clay and diphenylamine in this example is 14%, and the molar ratio of diphenylamine to α-methylstyrene is 1:2.4.

[0039] The reaction time for preparing 4,4'-bis(phenylisopropyl)diphenylamine in this example is 0.3 hours shorter than the reaction time for preparing 4,4'-bis(phenylisopropyl)diphenylamine in Example 1.

Embodiment 3

[0041] Refer to the process figure 1 , this specific embodiment discloses a method for preparing 4,4'-bis(phenylisopropyl)diphenylamine, specifically a laboratory preparation of 4,4'-bis(phenylisopropyl)diphenylamine Methods.

[0042] The difference from Example 1 is that the weight percent of activated clay and diphenylamine in this example is 20%, and the molar ratio of diphenylamine to α-methylstyrene is 1:2.6.

[0043] The reaction time for preparing 4,4'-bis(phenylisopropyl)diphenylamine in this example is comparable to the reaction time for preparing 4,4'-bis(phenylisopropyl)diphenylamine in Example 1.

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Abstract

The invention provides a method for preparing 4,4'-bis(phenyl isopropyl)diphenylamine. Under the action of catalyst activated clay, diphenylamine and alpha-methyl styrene react at the temperature of 105 DEG C-165 DEG C to generate a crude product 4,4'-bis(phenyl isopropyl)diphenylamine, 4,4'-bis(phenyl isopropyl)diphenylamine is filtered, then recrystallized with solvent, and then subjected to centrifugal baking smashing or pelleting to obtain high-purity 4,4'-bis(phenyl isopropyl)diphenylamine, the activated clay and diphenylamine are prepared into jelly mixed liquor, and alpha-methyl styrene is uniformly added into the mixed liquor of the activated clay and diphenylamine in a fractionated mode. Compared with the prior art, reaction speed is high, efficiency is high, three wastes are not generated, and 4,4'-bis(phenyl isopropyl)diphenylamine is high in purity and good in color.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis of antioxidants, in particular to a method for preparing 4,4'-bis(phenylisopropyl)diphenylamine. Background technique [0002] 4,4'-bis(phenylisopropyl)diphenylamine can be used to protect natural rubber and synthetic rubber such as styrene-butadiene, isoprene, chloroprene and butyl from aging caused by heat, light and ozone. It has a good synergistic effect with sulfur-containing antioxidants. Suitable for light-colored and bright-colored rubber products. It can also be used as an antioxidant for polyurethane foam, polyolefin, carbon black-filled polyolefin, rubber and plastic wire and cable, food packaging materials and adhesives, especially in neoprene colored cable sheaths. . It is usually prepared by the reaction of diphenylamine and α-methylstyrene in the presence of activated clay catalyst. At present, there are many kinds of antioxidants used in the technical field of plasti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C209/84C07C211/55
CPCC07C209/68C07C209/84C07C211/55
Inventor 曹宏生王宇吴开运王忠冬
Owner JIANGSU FEIYA CHEM IND
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