Process for purifying dialkyl diphenylamine

A technology of dialkyldiphenylamine and dialkyldiphenylamine crystal is applied in the field of material antioxidant purification, can solve the problems of low output, low product yield and high distillation temperature, and achieves good environmental protection and product yield High, easy-to-use effects

Inactive Publication Date: 2012-10-03
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dialkyldiphenylamine is a kind of alkylated diphenylamine antioxidant. Due to its high purity, high melting point and excellent oxidation resistance, it is widely used in many high-grade rubber products and high-grade oil products. However, due to its production The process is complex, especially the purification process is cumbersome, resulting in low yield and high price
[0004] Dialkyl diphenylamine antioxidants often produce equivalent monoalkyl diphenylamines during the preparation process, and even contain incompletely reacted olefins and diphenylamines, and these monoalkyl diphenylamines, olefins, and diphenylamines are what we call Undesirable, if these impurities are not removed, the final product may be in a liquid state, and may also lead to a very low melting point of the final product, which does not meet the requirements of high-purity anti-oxidant
[0006] 1. The distillation temperature is too high, as high as 250°C, and octylated diphenylamine itself is a heat-sensitive material, which will be partially cracked at high temperature, and the product wil

Method used

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Examples

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Embodiment Construction

[0022] One, prepare the crude product of dioctyl diphenylamine

[0023] Put 100kg of diphenylamine and 20kg of catalyst activated clay into a reactor equipped with a stirrer and a dropping device, then add 268kg of diisobutylene dropwise for alkylation reaction, and filter to remove the catalyst to obtain the crude product of dioctyldiphenylamine.

[0024] The above diisobutylene can be replaced by α-methylstyrene or tetrapropylene.

[0025] After analysis, the mass percentage of dioctyl dianiline in the crude product of dioctyl dianiline is 61%, and the rest is diisobutylene, monooctyl dianiline, etc.

[0026] 2. Purification

[0027] Put the crude product into the crystallizer, heat and melt it all, then slowly lower the temperature at a rate of 1.0-4.0°C / h (preferably 4.0°C / h), cool to 60-75°C and keep it for 5-10h (preferably 7h), discharge after crystallization mother liquor to obtain dioctyl dianiline crystal layer.

[0028] The dioctyl diphenylamine crystal layer is ...

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Abstract

The invention relates to a process for purifying dialkyl diphenylamine and belongs to the field of purification of material antioxidants. The process comprises: firstly heating dialkyl diphenylamine crude products to be melt, slowly cooling to the temperature of 60-75 DEG C, keeping the temperature of 60-75 DEG C for 5-10 hours, and discharging mother liquid after melt dialkyl diphenylamine crude products are crystallized to obtain a dialkyl diphenylamine crystal layer; heating the dialkyl diphenylamine crystal layer through a method of gradient increased temperature until the temperature rises to be close to a melting point of the dialkyl diphenylamine, and discharging liquid phase to obtain the purified dialkyl diphenylamine. The quality of the dialkyl diphenylamine purified through the process can meet quality requirements of high-purity-level products, and high-quality dialkyl diphenylamine can be obtained through the process while only a distillation process or a solvent crystallization process can not obtain the high-quality dialkyl diphenylamine. The process is simple in operation, free of consumption of any solvent, high in product yield, good in environmental friendliness and capable of causing no waste water or waste gas.

Description

technical field [0001] The invention relates to a purification process of dialkyl diphenylamine, in particular to a method for preparing high-content dialkyl diphenylamine, which belongs to the field of material antioxidant purification. Background technique [0002] With the development of rubber, plastics, and oil industries, the research and production of antioxidants have attracted more and more attention. At present, whether it is ordinary rubber products, high-grade aerospace lubricants, engine lubricants, etc., there are requirements for high-performance antioxidants, and this requirement is becoming more and more stringent. Therefore, high-performance, high-purity antioxidants are required to meet these requirements. [0003] The above needs can be met by the antioxidant dialkyl diphenylamine. Dialkyldiphenylamine is a kind of alkylated diphenylamine antioxidant. Due to its high purity, high melting point and excellent oxidation resistance, it is widely used in man...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/84
Inventor 曹宏生徐志华吴开赟王忠冬
Owner JIANGSU FEIYA CHEM IND
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