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Method for extracting refined phenazine from RT base wastes

A waste and phenazine technology, which is applied in the field of extracting and refining phenazine, can solve the problems of low purity of phenazine products, high recycling cost, and long operation cycle, and achieve the effects of strong continuity, good product crystal form, and reduced recycling cost

Active Publication Date: 2013-08-07
张国柱
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the process of producing RT base with nitrobenzene and aniline as raw materials, the by-product phenazine is difficult to be effectively separated by the current production process, and it is mixed with a small amount of aniline, 4-aminodiphenylamine, and azobenzene to form Waste, direct discharge or incineration not only pollutes the environment, but also causes a great waste of resources
The existing method for extracting phenazine from RT waste is as described in the patent (CN200810099916.1), which adopts the processes of dissolution extraction, solid-liquid separation, recrystallization, drying, distillation, and rectification, but the purity of the obtained phenazine product is Low, and the rectification method is used to recover the distillation residue aniline, 4-aminodiphenylamine, azobenzene, etc., the operation cycle is long and the recovery cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for extracting refined phenazine from RT base waste material is carried out according to the following steps:

[0029] The first step, an extraction

[0030] Add the RT base waste material to the secondary extraction mother liquor, the ratio of the RT base waste material to the secondary extraction mother liquor is 1:5 (g:mL), heat up and reflux for 60min, then cool to 25°C and centrifuge to obtain a filter cake and one extraction mother liquor;

[0031] The second step, melt crystallization

[0032] The primary extraction mother liquor is distilled at 80°C, and the 77-80°C fraction is collected to recover ethanol. After the distillation, the raffinate is kept at 80°C for 30 minutes, and then poured into a suction filter funnel and a suction filter bottle preheated to 80°C Rapid filtration obtains thick phenazine and molten crystallization mother liquor;

[0033] The third step, secondary extraction

[0034] Add the filter cake into the primary crystallizat...

Embodiment 2

[0041] Solvent extraction process: Add 100g RT base waste material to 700mL secondary extraction mother liquor, heat up and reflux for 1h, then place in cold water to cool down for about 1h, suction filter when cooled to 25°C, and fully filter dry to obtain a wet weight of about 70g once Extract the filter cake, and extract about 700mL of the mother liquor once. Add the primary coarse filter cake to 700mL primary crystallization mother liquor, raise the temperature and reflux for 1 hour, then place it in cold water to cool down for about 1 hour, suction filter when cooled to 25°C, and fully filter dry to obtain a secondary extraction filter cake with a wet weight of about 62g , about 700mL of the mother liquor was extracted twice.

[0042] Recrystallization process: Add the secondary extraction filter cake to 800mL secondary crystallization mother liquor, raise the temperature and reflux for 30 minutes, and then let it stand for 3 minutes, pour about 2 / 3 of the supernatant int...

Embodiment 3

[0046] A method for extracting refined phenazine from RT base waste material is carried out according to the following steps:

[0047] The first step, an extraction

[0048] Add the RT base waste material to the secondary extraction mother liquor, the ratio of the RT base waste material to the secondary extraction mother liquor is 1:9 (g:mL), heat up and reflux for 60min, then cool to 25°C and centrifuge to obtain a filter cake and one extraction mother liquor;

[0049] The second step, melt crystallization

[0050] The primary extraction mother liquor is distilled at 80°C, and the 77-80°C fraction is collected to recover ethanol. After the distillation, the raffinate is kept at 80°C for 30 minutes, and then poured into a suction filter funnel and a suction filter bottle preheated to 80°C Rapid filtration obtains thick phenazine and molten crystallization mother liquor;

[0051] The third step, secondary extraction

[0052] Add the filter cake into the primary crystallizat...

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PUM

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Abstract

The invention provides a method for extracting refined phenazine from RT base wastes, belonging to the technical field of phenazine refining. The method provided by the invention has the advantages that high-purity phenazine crystals can be obtained, used solvents are all recovered and repeatedly-used solvents, and no waste liquid pollution exists. The adopted technical scheme is as follows: the refined phenazine is obtained in a manner that the RT base wastes are subjected to extraction twice, recrystallization twice, drying, solvent recovery and melting crystallization. According to the phenazine produced by the method, the purity can be stabilized over 99.8%, is much higher than the requirements of a pharmaceutical grade and can fully meet the market demand. The method is widely applied to the field of extracting the refined phenazine from the RT base wastes.

Description

technical field [0001] The invention discloses a method for extracting and refining phenazine from RT base waste, belonging to the technical field of phenazine refining. Background technique [0002] In the process of producing RT base by the nitrobenzene method, aniline undergoes a nucleophilic addition reaction with nitrobenzene under the catalysis of basic tetramethylammonium hydroxide, and the nucleophile attacks the para-position of nitrobenzene. The reduction finally produces the main reaction product RT base, and the attack on the ortho position of nitrobenzene produces phenazine, the by-product of the reaction. From the reaction mechanism, we can see that phenazine is an inevitable by-product in the production process of RT base, so its comprehensive utilization is an important issue for RT production enterprises. [0003] However, in the process of producing RT base with nitrobenzene and aniline as raw materials, the by-product phenazine is difficult to be effectiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/46
Inventor 吴永廷刘云龙张兴会
Owner 张国柱
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