Method for extracting high-purity phenazine from RT base (4-Aminodiphenylamine) byproduct waste material

A high-purity, phenazine technology, applied in the field of phenazine refining, can solve the problems of dull product color, high consumption, disturbing RT production system, etc., and achieve the effect of bright appearance, increased burden, and stable purity

Active Publication Date: 2014-08-20
张国柱
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The existing method of extracting phenazine from RT base waste is as described in the patent (CN201310217173.4). Through the processes of extraction, crystallization, drying, solvent recovery and melt crystallization of RT base waste, the purity > 99.8% phenazine, but it has the following defects: a. The color of the product is dull due to the small amount of dye intermediate 4-aminodiphenylamine; b. The extraction process includes two extractions and two crystallizations, and the purified mother liquor is repeatedly circulated in the system. higher consumption
c. The ethanol recovery rate in the solvent recovery process is only 95%, and the remaining 5% ethanol will be brought into the RT production system, and long-term operation will inevitably disturb the RT production system

Method used

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  • Method for extracting high-purity phenazine from RT base (4-Aminodiphenylamine) byproduct waste material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for extracting high-purity phenazine from RT base by-product waste, comprising the steps of:,

[0032] (1), heating separation

[0033] Heat 120g of RT base by-product waste 1 in a water bath to 85°C, filter and separate to obtain liquid phase 2 and crude phenazine 3;

[0034] (2), extraction

[0035] Add all the heated and separated crude phenazine 3 into the primary crystallization mother liquor 7, heat up and reflux for 60 minutes, cool to 25°C, pour into a funnel for filtration, and obtain the extraction mother liquor 5 and the extraction phenazine 4;

[0036] (3), primary crystallization

[0037] Add all the extracted phenazine 6 to the secondary decolorization crystallization mother liquor 10, heat up and reflux for 50 minutes, cool to 25°C, pour into a funnel for filtration, and obtain the primary crystallization mother liquor 7 and the primary crystallization phenazine 6;

[0038] (4), secondary decolorization crystallization

[0039] The primary cr...

Embodiment 2

[0048] A method for extracting high-purity phenazine from RT base by-product waste, comprising the steps of:,

[0049] (1), heating separation

[0050] The crude phenazine 14 obtained in Example 1 was heated and melted together with 120 g of RT base by-product waste at 100° C., and the liquid phase and solid-phase crude phenazine with higher phenazine content were separated;

[0051] (2), extraction

[0052] Add the solid-phase crude phenazine obtained by heating and separating in step (1) to the primary crystallization mother liquor 7 obtained in Example 1, heat up and reflux for 30-60 minutes, and cool to 20°C-30°C for solid-liquid separation to obtain the extract mother liquor and extract phenazine;

[0053] (3), primary crystallization

[0054] Add the extracted phenazine obtained in step (2) to the secondary decolorization crystallization mother liquor 10 obtained in Example 1, stir and raise the temperature and reflux for 40-70 minutes, then cool to 20°C-30°C for soli...

Embodiment 3

[0065] A method for extracting high-purity phenazine from RT base by-product waste, comprising the steps of:,

[0066] (1), heating separation

[0067] The crude phenazine 14 obtained in Example 2 was heated and melted together with 120 g of RT base by-product waste at 100° C., and the liquid phase and solid phase crude phenazine with higher phenazine content were separated;

[0068] (2), extraction

[0069] Add the solid-phase crude phenazine obtained by heating and separating in step (1) to the primary crystallization mother liquor obtained in Example 2, heat up and reflux for 30-60 minutes, cool to 20°C-30°C for solid-liquid separation, and obtain the extract mother liquor and extract phenazine Zinc;

[0070] (3), primary crystallization

[0071] Add the extracted phenazine obtained in step (2) to the secondary decolorization crystallization mother liquor obtained in Example 2, stir and raise the temperature and reflux for 40-70 minutes, then cool to 20°C-30°C for solid-...

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Abstract

The invention discloses a method for extracting high-purity phenazine from an RT base byproduct waste material, belonging to the technical field of refining of the phenazine. The technical problem to be solved is to provide a method for extracting the phenazine from the RT base byproduct waste material, wherein the product is high in purity and bright in color and gloss, the amount of used solvents is small and the recycle rate of the solvents is high. The method comprises the following steps: separation by heating, extraction, primary crystallization, secondary decoloration and crystallization, drying, primary distillation and crystallization and secondary solvent distillation, wherein due to the step of the separation by heating, the amount of the used solvents in the extraction step and the crystallization step is reduced, and an active carbon decoloration step is added, so the product purity is stable and not lower than 99.8% and the product is also brighter in color and gloss and totally meets the requirements of all markets including a pharmaceutical-grade market; due to the addition of the secondary distillation, the recycle rate of the solvents is as high as 99.5%, the consumption of purifying solvents is reduced, and the amount of the solvents introduced to an RT production system causes no burthen to an existing RT production system.

Description

technical field [0001] The invention discloses a method for extracting high-purity phenazine from by-product waste of RT base, belonging to the technical field of phenazine refining. Background technique [0002] The nitrobenzene method is used to synthesize RT base, the product quality is high, and the reaction conditions are mild, but the by-product phenazine residue will be produced during its production process, which contains about 80% of phenazine and a small amount of aniline and 4-aminodi Aniline, direct discharge will cause environmental pollution, and incineration treatment will cause a lot of waste. And phenazine itself is an important organic intermediate, which is widely used in the fields of medicine, pesticide, conductor and battery material. Therefore, the comprehensive recycling of phenazine residues, a by-product of RT base, is an urgent issue in the production of RT base by the nitrobenzene method. [0003] The existing method of extracting phenazine fro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/46
CPCC07D241/46
Inventor 张彩凤吴永廷刘云龙
Owner 张国柱
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