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Method for preparing 4,4-bis (alpha, alpha-dimethylbenzyl) diphenylamine

A technology of dimethylbenzyl and diphenylamine is applied in the field of chemical synthesis of diphenylamine to synthesize antioxidant KY-405, which can solve the problems of high labor intensity, poor product color, equipment corrosion, etc., and achieve good color and anti-aging performance. Significant, high-purity effects

Active Publication Date: 2013-02-13
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses a large amount of solvent in the reaction process, and acidifies with hydrochloric acid in the post-treatment, and then washes with water after neutralization with alkali, which is labor-intensive and severely corrodes the equipment, and the color of the product is poor

Method used

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  • Method for preparing 4,4-bis (alpha, alpha-dimethylbenzyl) diphenylamine

Examples

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Effect test

Embodiment 1

[0019] In a 1L reactor equipped with a stirrer, reflux condenser, feeding device and nitrogen protection device, add 16.9g of diphenylamine (99.8% purity) and 2g of activated clay, heat to 60-80°C, and wait until the diphenylamine is completely melted , start stirring and heat up to 120-135°C. At the same time, 30 g of α-methylstyrene was prepared and slowly added to the reactor through the feeding device. After all the α-methylstyrene is added, the reaction mixture is kept for about 4 hours, the temperature is controlled at 120-145°C, and then the temperature is lowered to below 120°C for hot filtration. After filtering out the catalyst, the filtrate was poured into a four-necked flask equipped with a thermometer, a stirring device and a condenser, recrystallized with petroleum ether, then filtered, and the solid was collected and dried to obtain 38g of product with a yield of 81% and a melting point of 97.5 ℃.

Embodiment 2

[0021] In a 1L reactor equipped with a stirrer, reflux condenser, feeding device and nitrogen protection device, add 169g of diphenylamine (purity 99.8%), 25g of activated clay (heated and dehydrated for two hours before use), and heat to 60-80 °C, after the diphenylamine is completely melted, start stirring and raise the temperature to 120-135 °C. At the same time, prepare 295g of α-methylstyrene, and slowly add it into the reactor through the feeding device. After completion, keep it warm for about 4-6 hours, control the temperature at 120-145°C, then cool it down to below 120°C, and perform hot filtration. After filtering out the catalyst, filter at lower temperature, pour the filtrate into a four-necked flask equipped with a thermometer, a stirring device and a condenser, recrystallize with petroleum ether, then filter, collect the solid and dry it to obtain 380g of the product, with a yield of 82% , melting point 97°C.

[0022] The mother liquor obtained by centrifugal f...

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Abstract

The invention discloses a method for preparing 4,4-bis (alpha, alpha-dimethylbenzyl) diphenylamine, relating to the technical field of chemical synthesis of antioxidant KY-405 using diphenylamine. The method comprises the following steps: diphenylamine reacts with a-methyl styrene at 105-175 DEG C in the presence of catalyst of activated clay to produce a coarse product, i.e. 4,4-bis(alpha,alpha-dimethylbenzyl) diphenylamine, and the coarse product is filtered, recrystallized using solvent, and centrifugally dried and crushed or prilled to produce highly purified 4-(alpha, alpha-dimethylbenzyl) diphenylamine and 4,4-bis(alpha,alpha-dimethylbenzyl) diphenylamine. The product produced by the method has the advantages of no toxicity, no odor, light color and the like, and is one of countable antioxidants with no toxicity, no odor and light color in the amine antioxidants, can be utilized in various elastomers and plastic color masterbatches, such as polyethylene, polypropylene and polyvinyl chloride widely.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis of diphenylamine synthetic antioxidant KY-405. Background technique [0002] At present, there are many kinds of antioxidants used in the technical field of plastics and rubber products, and the typical ones are amine and phenolic antioxidants. [0003] 4,4'-bis(α,α-dimethylbenzyl)diphenylamine, trade name antioxidant KY-405, is usually synthesized from diphenylamine and α-methylstyrene, diphenylamine is an important fine Organic chemical raw materials, widely used, mainly used in rubber additives, explosive stabilizers, medicine, dyes and other industries, and is the main synthetic raw material for many amine antioxidants. Many literatures have been published on diphenylamine antioxidants. For example: CN1195661A discloses a kind of preparation antioxidant 4 by diphenylamine and 2-methylstyrene, the method of 4 '-2 cumyl-4 "-cumyl diphenylamine. This method adopts in the reaction pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/54C07C209/60C08K5/18
Inventor 王宇曹宏生徐志华吴开运花月明
Owner JIANGSU FEIYA CHEM IND