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

A technology of dimethylbenzyl and diphenylamine, which is applied in the field of preparation of alkylated diphenylamine, can solve problems such as equipment corrosion and high labor intensity, and achieve the effects of no three wastes, reduced costs, and mild reaction conditions

Active Publication Date: 2009-09-23
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 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. Prepare 26g of α-methylstyrene at the same time, and slowly add it to the reactor through the feeding device. After all the α-methylstyrene is added, the reaction mixture is kept for about 4 hours, and the temperature is controlled at 125-145°C, and then Cool down to below 120°C and perform hot filtration. After filtering out the catalyst, the filtrate was poured into a four-necked flask equipped with a thermometer, a bubbling device and a condenser tube, distilled under negative pressure (2.66k Pa), steamed to 245-250°C to stop distillation, cooled, and collected the still liquid to obtain 36.5g Product, yield 85.1%.

Embodiment 2

[0025] In a 1L reactor equipped with a stirrer, a reflux condenser, a feeding device and a nitrogen protection device, add 169g of diphenylamine (purity 99.8%) and 25g of activated clay for heating (heating and dehydration 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 253g of α-methylstyrene and slowly add it to the reactor through the feeding device. After all the α-methylstyrene is added, the reaction mixture is kept for about 4-6 hours, and the temperature is controlled at 125-155°C. , and then lower the temperature to below 120°C for hot filtration. After filtering out the catalyst, pour the filtrate into a four-neck flask equipped with a thermometer, a bubbling device and a condenser tube, distill under negative pressure (13.30k Pa), steam to 200-245°C to stop distillation, cool, and collect the still liquid to obtain 358g of product , The yie...

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Abstract

The invention discloses a method for preparing mixture of 4-(alpha, alpha-dimethylbenzyl) diphenylamine and 4,4-bis(alpha, alpha-dimethylbenzyl) diphenylamine, relating to a preparation method of alkylated diphenylamine. The method comprises the following steps: diphenylamine and excessive a-methyl styrene carry out alkylate reaction at 120-175 DEG C in the presence of catalyst of activated clay to produce a coarse product, i.e. a mixture of 4-(alpha, alpha-dimethylbenzyl) diphenylamine and 4,4-bis(alpha, alpha-dimethylbenzyl) diphenylamine, and the mixture is filtered, distilled in decompression condition, prilled or crushed to produce mixture of 4-(alpha, alpha-dimethylbenzyl) diphenylamine and 4,4-bis(alpha, alpha-dimethylbenzyl) diphenylamine. The invention is a high-efficiency and clean synthetic process and has the advantages of long-term oxidization resistance, heat resistance, disturbance resistance and favorable stability.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a preparation method of alkylated diphenylamine, to be precise, it is a diphenylamine synthetic antioxidant 4-(α,α-dimethylbenzyl)diphenylamine and 4,4' - Improved process for bis(α,α-dimethylbenzyl)diphenylamine mixtures. Background technique [0002] At present, there are many kinds of anti-aging agents used in the technical field of plastics and rubber products, and the typical ones are amine and phenolic anti-aging agents. [0003] The antioxidant product is usually synthesized from diphenylamine and α-methylstyrene. Diphenylamine is an important fine organic chemical raw material with a wide range of uses. It is mainly used in industries such as rubber additives, explosive stabilizers, medicines, and dyes. The main synthetic raw material for many amine antioxidants. Many documents on diphenylamine antioxidants have now been published. For example: CN1195661A disc...

Claims

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Application Information

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IPC IPC(8): C07C211/54C07C209/60C08K5/18
Inventor 徐志华曹宏生王宇吴开运花月明
Owner JIANGSU FEIYA CHEM IND
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