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Method for preparing RT base through normal-pressure compression combination

A technology of base and condensation reaction, applied in the field of rubber additives, to achieve the effect of reducing three waste discharge, reducing corrosion, and avoiding disposal problems

Active Publication Date: 2021-10-22
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with tetramethylammonium hydroxide, potassium hydroxide and tetrabutylammonium bromide have strong anti-poisoning and high temperature resistance, and this method does not require the removal of a large amount of water, so it has the possibility of atmospheric pressure catalysis, but Patent CN102372640A does not involve relevant information

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of RT base:

[0028] Weigh 2.2 g of basic resin catalyst and 0.4 g of tetrabutylammonium bromide into a three-necked flask, and add 30 g of aniline. Set up a reaction device, weigh 8.0 g of nitrobenzene in a constant pressure dropping funnel, place it in the side port of a three-neck flask, set up a reflux device, heat the oil bath to 100 °C under 1 standard atmospheric pressure, stir for 1 h, and then add dropwise Nitrobenzene was reacted for 5-8 hours to obtain a condensation liquid, and the selectivity of the target product was 69.4%-84.3%.

Embodiment 2

[0030] Preparation of RT base:

[0031] Weigh 2.2 g of basic resin catalyst and 0.4 g of tetrabutylammonium bromide into a three-necked flask, and add 30 g of aniline. Set up a reaction device, weigh 8.0 g of nitrobenzene in a constant pressure dropping funnel, place it on the side of a three-necked flask, set up a reflux device, heat the oil bath to 120 °C under 1 standard atmospheric pressure, stir for 1 h, and then add dropwise Nitrobenzene was reacted for 5-8 hours to obtain a condensation liquid, and the selectivity of the target product was 67.8%-81.2%.

Embodiment 3

[0033] Preparation of RT base:

[0034] Weigh 1.5 g of basic resin catalyst and 0.4 g of sodium dodecylbenzenesulfonate into a three-necked flask, and add 30 g of aniline. Set up a reaction device, weigh 5.2 g of nitrobenzene in a constant pressure dropping funnel, place it on the side of a three-neck flask, set up a reflux device, heat the oil bath to 120 °C under 1 standard atmospheric pressure, stir for 1 h, and then add dropwise Nitrobenzene was reacted for 8-16 hours to obtain a condensation liquid, and the selectivity of the target product was 69.8%-83.6%.

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PUM

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Abstract

The invention discloses a method for preparing RT base through normal-pressure synthesis, which is mainly characterized in that a solid base catalyst is adopted, and the RT base is prepared through catalytic condensation under one standard atmospheric pressure. The method overcomes the defects in the prior art. In the production process of the RT base, a proper solid base catalyst is used; through process improvement, the reaction is carried out under a normal pressure condition, so that the use of a vacuum pump is avoided from the source; therefore, the process flow is optimized, the emission of three wastes is reduced, and the environment-friendly production of the RT base is realized.

Description

technical field [0001] The invention belongs to the field of rubber additives, and in particular relates to a process method which can be used in atmospheric compression to prepare rubber antioxidant intermediate RT base. Background technique [0002] RT base (p-aminodiphenylamine) is widely used in rubber additives, dyes, textiles, printing and pharmaceutical industries, etc. It is mainly used in rubber antioxidants 4010NA, 6PPD, etc. [0003] The total annual production capacity of domestic RT base is about 180,000 tons. Sinopec Nanhua Company currently has a 10,000-ton RT base device, which is produced by the nitrobenzene method. Tetramethylhydrogen is used for the condensation reaction in the existing nitrobenzene method. Ammonium oxide is used as a catalyst. The catalyst easily absorbs carbon dioxide in the air to form carbonate and loses its catalytic effect. Inactivate. [0004] Usually, the vacuum system is implemented by a vacuum pump, which is a kind of dynamic e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/55C07C211/56C07C209/02
CPCC07C209/02C07C209/36C07C209/38C07C211/56C07C211/55
Inventor 秦涛吕明倩张伟黄伟祝东红刘卓
Owner CHINA PETROLEUM & CHEM CORP
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