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Preparation method of liquid-state aromatic amine antioxidant 5057

The technology of aromatic amines and antioxidants is applied in the field of preparation of polymers and oil antioxidants, and achieves the effects of simple operation, easy separation and purification, and long catalytic life.

Active Publication Date: 2013-11-27
RIANLON +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no process for applying perfluorosulfonic acid tree as a catalyst to the preparation of antioxidant 5057

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 1690g of diphenylamine and 340g of perfluorosulfonic acid resin Nafion-H into the reactor, then heat it up to 180°C under stirring, then add 1500g of diisobutylene dropwise into the reactor within 60 minutes, and continue After stirring and reacting at 180°C for 6 hours, the perfluorosulfonic acid resin was recovered by filtration, and the filtrate was distilled under reduced pressure to remove unreacted diphenylamine (about 5%), and then decolorized with 30g of activated carbon to obtain a light yellow liquid aromatic amine antibiotic. Oxygen agent, productive rate 93%, liquid phase mass spectrometry analysis shows that butyl diphenylamine derivative accounts for about 22%, octyl diphenylamine derivative accounts for about 38%, and butyl octyl diphenylamine derivative accounts for about 24%, Dioctyl dianiline derivatives accounted for about 12%, and other unknown substances accounted for about 4%.

Embodiment 2

[0015] Add 1690g of diphenylamine and 500g of perfluorosulfonic acid resin Nafion-H into the reactor, then heat it to 165°C under stirring, then add 1400g of diisobutylene dropwise into the reactor within 120 minutes, and continue After stirring and reacting at 150°C for 8 hours, the perfluorosulfonic acid resin was recovered by filtration. After the filtrate was distilled under reduced pressure to remove unreacted diphenylamine (about 4%), it was decolorized with 30g of activated carbon to obtain a light yellow liquid aromatic amine antibiotic. Oxygen agent, yield 95%, liquid phase mass spectrometry analysis shows that butyl diphenylamine derivatives account for about 28%, octyl diphenylamine derivatives account for about 35%, butyl octyl diphenylamine derivatives account for about 22%, Dioctyl dianiline derivatives account for about 10%, and other unknown substances account for about 5%.

Embodiment 3

[0017] Add 1690g of diphenylamine and 845g of perfluorosulfonic acid resin PFSA into the reactor, then heat it to 150°C under stirring, then add 1500g of diisobutylene dropwise into the reactor within 120 minutes, and continue at 150 After stirring and reacting at ℃ for 10 hours, the perfluorosulfonic acid resin was recovered by filtration, and the filtrate was distilled under reduced pressure to remove unreacted diphenylamine (about 6%), and decolorized with 30g of activated carbon to obtain a light yellow liquid aromatic amine antioxidant , the yield is 92%, liquid phase mass spectrometry analysis shows that butyl diphenylamine derivatives account for about 27%, octyl dianiline derivatives account for about 39%, butyl octyl dianiline derivatives account for about 20%, and dioctyl diphenylamine derivatives account for about 20%. Diphenylamine derivatives accounted for about 9%, and other unknown substances accounted for about 5%.

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PUM

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Abstract

The invention discloses a p reparation method of a liquid-state aromatic amine antioxidant 5057. The preparation method comprises the following steps of: by utilizing perfluorinated sulfonic acid resin as a solid acid catalyst, adding diphenylamine and perfluorinated sulfonic acid resin into a reaction kettle at a mass ratio of 1:(0.2-0.5), then heating to 150-180DEG C while stirring, and dropwise adding diisobutylene into the reaction kettle within 60-120 minutes, wherein the mole ratio of diisobutylene and diphenylamine is (1.2-1.4):1; stirring and reacting for 6-10 hours at 150-180DEG C, then filtering and recovering the perfluorinated sulfonic acid resin, removing unreacted diphenylamine from the filtrate through reduced pressure distillation, and performing decoloration through activated carbon to obtain the liquid-state aromatic amine antioxidant. Compared with the existing synthetic method, the preparation method has the advantages of being simple to operate, easy for the liquid-state aromatic amine antioxidant to separate and purify, long in one-way catalytic life of the catalyst, and capable of being repeatedly utilized, and the like, and is suitable for industrial clean production.

Description

technical field [0001] The invention belongs to the preparation method of polymer and oil product antioxidant, in particular to a preparation method of liquid aromatic amine antioxidant. Background technique [0002] Antioxidant 5057, as a liquid aromatic amine antioxidant, is the reaction product of N-phenylaniline (diphenylamine) and diisobutylene, with a CAS number of 68411-46-1, easily soluble in toluene and petroleum ether, etc. Organic solvents. Antioxidant 5057 is composed of butyl dianiline derivatives, octyl dianiline derivatives, butyl octyl dianiline derivatives, dioctyl dianiline derivatives, and other small amounts of unknown substances. It is analyzed by liquid chromatography mass spectrometry. Among them, butyl diphenylamine derivatives accounted for 22-28%, octyl diphenylamine derivatives accounted for 35-39%, butyl octyl diphenylamine derivatives accounted for 20-24%, and dioctyl diphenylamine derivatives accounted for 9-12%. %, other small amount of unkno...

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C211/55
CPCY02P20/584
Inventor 范小鹏李海平孙春光汤翠祥
Owner RIANLON
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