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Treatment method of RT base production waste

A technology for production waste and treatment methods, which is applied in the field of rubber anti-aging agents, and can solve problems that affect the stable operation of the production system, cumbersome processes, and high energy consumption.

Active Publication Date: 2017-03-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of combining melt separation and solvent separation is cumbersome
[0005] The process of separating and purifying phenazine waste residue with ethanol as a solvent can obtain 99.5% of phenazine, such as CN101580494A and CN103232402A, but adopting this process not only uses a large amount of ethanol as a solvent, but the ratio of solvent to phenazine waste residue reaches or even exceeds 6 : 1. The process of recovering solvent ethanol consumes a lot of energy, and the recovery rate of ethanol is only about 95%. During the recovery process of RT base, a large amount of ethanol will enter the rectification system with the recovery of RT base. Affect the stable operation of RT base production system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Mix 100g of aniline with 100g of RT base distillation waste containing 35% phenazine and 58% RT base, heat to 60°C, after completely dissolving, cool down to 25°C, and after 2 hours, separate the solid and liquid to obtain the solid phase 36.7 g, the solid phase contained 69.3% phenazine, 11.3% RT base, and the yield of crude phenazine was 72.7%; the liquid phase was 163.3 g, the liquid phase contained 33.0% RT base, and the recovery rate of RT base was 92.8%.

Embodiment 2

[0019] Mix 150g of aniline with 100g of RT base distillation waste containing 27% phenazine and 60% RT base, heat to 55°C, after completely dissolving, cool down to 20°C, and after 4 hours, separate the solid and liquid to obtain the solid phase 24.7 g, containing 73.5% of phenazine in the solid phase, 10.2% of RT base, and 67.2% yield of crude phenazine; 225.3 g of liquid phase was obtained, containing 25.5% of RT base and 3.9% of phenazine in the liquid phase, and RT base was recovered The rate is 95.8%.

Embodiment 3

[0021] Mix 90g of aniline with 100g of RT base distillation waste containing 56% phenazine and 35% RT base, heat to 70°C, after completely dissolving, cool down to 35°C, and after 4 hours, separate the solid and liquid to obtain the solid phase 66.4 g, containing 73.5% of phenazine in the solid phase, 11.7% of RT base, and 87.2% of crude phenazine yield; 123.6g of liquid phase was obtained, containing 22.0% of RT base and 5.8% of phenazine in the liquid phase, and RT base was recovered The rate is 77.8%.

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Abstract

The invention provides a treatment method of RT base production waste. According to the treatment method, aniline is taken as a solvent, at 30 to 180 DEG C, waste, with a phenazine content higher than 10%, generated in RT base production process is dissolved; a liquid phase obtained via dissolving is subjected to crystallization separation at 10 to 50 DEG C so as to obtain a solid phase product and a liquid phase product; wherein the solid phase product can be taken as a raw material of phenazine refining, and the liquid phase product can be delivered into a RT base distillation system for recycling of RT base, aniline, and azobenzene.

Description

technical field [0001] The invention belongs to the technical field of rubber antioxidants, and relates to a method for treating RT base production waste. Background technique [0002] It has been more than 100 years since RT base (p-aminodiphenylamine) was first synthesized. With the increase in the amount of RT base and the improvement of product quality requirements, its synthesis route is constantly innovating. Although there are more than a dozen synthetic routes, there are three main ones used for industrialization: diphenylamine method, aniline method and nitrobenzene method. The nitrobenzene method is currently the most widely used industrial synthetic RT base process in the world. It is a clean and green process that has developed rapidly in recent years. While the nitrobenzene method has become the main process for producing RT base in China, phenazine is the main by-product in the RT base production process of the nitrobenzene method. Since the phenazine waste r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/51C07C211/46C07C209/86C07C245/08
Inventor 陈永平金汉强吴其建何育苗金玉存周亚岺
Owner CHINA PETROLEUM & CHEM CORP
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