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Method for separating, desalting and recycling recovered quaternary ammonium base

A quaternary ammonium base, separation technology, applied in chemical instruments and methods, purification/separation of amino compounds, preparation of organic compounds, etc., can solve the problem that the quality of recovered quaternary ammonium base cannot meet the requirements of production and operation, and the recovery of quaternary ammonium base Unable to dehydrate and desalt normally, affect condensation reaction and reduction reaction, etc., to achieve the effect of reducing viscosity, enhancing fluidity, and promoting normal progress

Active Publication Date: 2018-12-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existence of organic impurities in the reclaimed quaternary ammonium base, especially the existence of p-aminodiphenylamine and macromolecular viscous organic substances, makes the reclaimed quaternary ammonium base thicken, and the reclaimed quaternary ammonium base cannot be dehydrated and desalted normally, resulting in the recovery of the quaternary ammonium base. The quality of the ammonium base does not meet the requirements of production and operation, thus affecting the normal progress of the subsequent condensation reaction and reduction reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The recovered quaternary ammonium base is the same as Comparative Example 1. Take 200.0g of the recovered quaternary ammonium base, centrifuge at 20℃ and rotate speed 8000r / min, and separate for 3 minutes, and separate the p-aminodiphenylamine and macromolecular viscosity in the recovered quaternary ammonium base. Analyze the organic matter in the recovered quaternary ammonium base after centrifugal separation: 1.00% aniline, 0.27% p-aminodiphenylamine, 0.05% of viscous macromolecular organic matter, 141.5g of recovered quaternary ammonium base and 150.0g of aniline , Nitrobenzene 40.0g, condensation reaction 5h, sample and analyze the condensation liquid, the remaining amount of nitrobenzene in the condensation liquid is 0.19%, the obtained condensation liquid is hydrogenated and reduced, and the reduction conditions: condensation liquid 200.0g, hydrogenation catalyst 5.0g, reduction reaction At 38 minutes, the remaining amount of p-(nitroso) diphenylamine in the reducin...

Embodiment 2

[0024] The recovered quaternary ammonium base is the same as in Comparative Example 1. Take 200.0g of the recovered quaternary ammonium base, centrifuge at 20℃ and rotate speed 5000r / min, and the separation time is 8 min. The p-aminodiphenylamine and macromolecular viscosity in the recovered quaternary ammonium base are separated Analyze the organic matter in the recovered quaternary ammonium base after centrifugal separation: 0.99% of aniline, 0.23% of p-aminodiphenylamine, 0.03% of viscous macromolecular organic matter, 141.5g of recovered quaternary ammonium base and 150.0g of aniline , Nitrobenzene 40.0g, condensation reaction 5h, sample and analyze the condensation liquid, the remaining nitrobenzene in the condensation liquid is 0.17%, the obtained condensation liquid is hydrogenated and reduced, and the reduction conditions: 200.0g condensation liquid, 5.0g hydrogenation catalyst, reduction reaction At 36 minutes, the remaining amount of p-(nitroso) diphenylamine in the re...

Embodiment 3

[0026] The recovered quaternary ammonium base is the same as in Comparative Example 1. Take 200.0g of recovered quaternary ammonium base, centrifuge at 20℃ and rotate speed 3000r / min for 15 minutes, and separate the p-aminodiphenylamine and macromolecular viscosity in the recovered quaternary ammonium base. Analyze the organic matter in the recovered quaternary ammonium base after centrifugal separation: 0.99% of aniline, 0.10% of p-aminodiphenylamine, viscous macromolecular organic matter was not detected, take 141.5g of recovered quaternary ammonium base and 150.0 of aniline g. Nitrobenzene 40.0g, condensation reaction 5h, sample and analyze the condensation liquid, the remaining nitrobenzene in the condensation liquid is 0.13%, the obtained condensation liquid is hydrogenated and reduced, and the reduction conditions: 200.0g condensation liquid, 5.0g hydrogenation catalyst, reduction After 33 minutes of reaction, the remaining amount of p-(nitroso) diphenylamine in the reduci...

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Abstract

The invention discloses a method for separating, desalting and recycling recovered quaternary ammonium base. The method for separating, desalting and recycling the recovered quaternary ammonium base,disclosed by the invention, has the advantages that shortcomings in the prior art of recovering the quaternary ammonium base during using a nitrobenzene method to prepare p-aminodiphenyl amine are eliminated; a procedure of centrifugally separating p-aminodiphenyl amine and macromolecular viscous organic substances in the recovered quaternary ammonium base is increased to reduce the contents of the p-aminodiphenyl amine and macromolecular viscous organic substances in the recovered quaternary ammonium base, reduce the viscosity of the recovered quaternary ammonium base, reduce the desalting and filtering difficulty of the recovered quaternary ammonium base, improve the desalting effect of the recovered quaternary ammonium base and promote normal implementations of follow-up condensation reaction and reduction reaction.

Description

Technical field [0001] The invention belongs to the technical field of fine chemicals, and more specifically relates to a method for reducing the content of organic substances in the quaternary ammonium base, reducing the content of carbonate, and improving the quality of the quaternary ammonium base. Background technique [0002] In the process of preparing p-aminodiphenylamine by nitrobenzene method, nitrobenzene and aniline undergo condensation reaction under the catalysis of quaternary ammonium base to produce p-(nitroso) diphenylamine, and the condensation liquid containing quaternary ammonium base is hydrogenated and reduced to produce p-aminodiphenylamine. Amino diphenylamine, the reducing solution is filtered and the hydrogenation catalyst is added with water for extraction, the quaternary ammonium base is extracted into the water phase, and the water phase is processed to recover the quaternary ammonium base. The recovered quaternary ammonium base is used in the condensat...

Claims

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Application Information

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IPC IPC(8): C07C209/60C07C211/56C07C209/86C07C209/36C07C211/55
CPCC07C209/36C07C209/60C07C209/86C07C211/56C07C211/55
Inventor 吴其建陈永平金汉强刘卓陈永乐
Owner CHINA PETROLEUM & CHEM CORP
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