Preparation method for (para, para)-diisopropylphenyl diphenylamine product

A technology of propylphenyl diphenylamine and diphenylamine, which is applied in the field of organic compound synthesis, can solve the problems of long reaction time, poor reactivity, and impossibility, and achieve the effect of short reaction time, high reactivity, and bright color

Inactive Publication Date: 2016-07-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] The technical solution of the present invention is to overcome the problem of discharge and pollution in the preparation method of p-, p-dicumyl diphenylamine products, and reaction problems existing in the prior art because the catalyst cannot be completely recycled. The activity is poor, the reaction time is long, and after the catalyst is recycled each time, it is necessary to further add some new catalysts to continue to recycle. A kind of p-, p-dicumyl diphenylamine product preparation method is proposed, The invention is montmorillonite loaded silica prepared by means of activ

Method used

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  • Preparation method for (para, para)-diisopropylphenyl diphenylamine product
  • Preparation method for (para, para)-diisopropylphenyl diphenylamine product
  • Preparation method for (para, para)-diisopropylphenyl diphenylamine product

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Embodiment 1

[0070] Add 50.7 g of diphenylamine and 30.8 g of α-olefin in a 500 ml glass container equipped with a stirrer, a thermometer, a heating mantle, a reflux condenser, a water separator, and a nitrogen pipeline, pass into nitrogen protection, stir with a magnetic stirrer, and After melting at 85°C, add 5g of montmorillonite-type supported catalyst, gradually increase the temperature to 145°C, add 60g of α-olefin within 5 hours, control the reflux speed and heating temperature, so that the temperature of the reactant is not lower than 120°C, and the reaction time for 8 hours. According to the TLC tracking reaction until the DPA has completely disappeared, remove the olefins, add organic co-solvent and stabilizer A to completely dissolve after cooling properly, heat filter at 45 ° C ~ 140 ° C, and distribute and purify the crystals to obtain the final product and recover olefins and catalysts , the product is a white powdery crystal. The purity is higher than 99%, and the base numb...

Embodiment 2

[0072] Add 50.7g of diphenylamine into a 500ml glass container equipped with a stirrer, thermometer, heating mantle, reflux condenser, water separator, and nitrogen pipeline, pass in nitrogen protection, stir with a magnetic stirrer, and melt at 85°C Add 5g of montmorillonite-type supported catalyst, gradually increase the temperature to 145°C, add 90.8g of α-olefin within 5 hours, control the reflux rate and heating temperature, so that the temperature of the reactant is not lower than 120°C, and the reaction time is 8 hours. According to the TLC tracking reaction until the DPA has completely disappeared, remove the olefins, add organic co-solvent and stabilizer B after proper cooling until completely dissolved, heat filter at 45°C to 140°C and distribute and purify crystals to obtain the final product and recover olefins and catalysts , the product is a white powdery crystal. The purity is higher than 99%, and the base number is 144.

[0073] The invention relates to the pr...

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Abstract

The invention belong to the technical field of organic compound synthesis and provides a preparation method for a (para, para)-diisopropylphenyl diphenylamine product. The method includes the steps of: (A) in the presence of a montmorillonite-type supported catalyst and under the protection of nitrogen gas, mixing a polymerization inhibitor with [alpha]-olefin and diphenylamine to perform an alkylation reaction at 75-175 DEG C for 4-16 h; and (B) reducing the temperature to 45-140 DEG C, and adding an organic cosolvent and a stabilizer with stirring, and filtering the reaction liquid while hot, and performing stepwise crystallization and purification, wherein a mother liquid can be recycled. The (para, para)-diisopropylphenyl diphenylamine crystal product has stable performance and high base number, is free of the problems such as yellowing, performance reduction and the like even after long-time storage, has uniform granular size and is less than 0.2% in residual diphenylamine content. In the production process, the olefin and the catalyst can be recycled and no waste water and waste gas emission exists, so that the process is environment-friendly. The product can be widely applied in various elastomers, foam plastics and lubricant oil for achieving the effects of resisting oxidization and aging.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and relates to a preparation method of p-, p-dicumyl diphenylamine product. Background technique [0002] At present, there are many kinds of antioxidants that can be used in the fields of lubricating oil blending plastic rubber products technology, medicine, dyes, etc. The typical ones are amine-type and phenol-type antioxidants. Among the amine-type antioxidants, alkylated di Aniline and alkylated naphthalene amines have been widely used, but the application of amine antioxidants in the food field is relatively seldom, because aromatic amines used as raw materials for production have strong carcinogenicity, and many widely used None of the amine-type antioxidants can reduce the remaining diphenylamine content in the product to a range that is completely non-toxic to the human body, while p-, p-dicumyl diphenylamine can reduce the content of dicumyl diphenylamine to The raw m...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/68C07C209/90
CPCY02P20/584
Inventor 火鹏飞徐小红张杰周旭光李建明薛卫国
Owner PETROCHINA CO LTD
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