Process for preparing high-purity auramine O

A process method and high-purity technology, applied in the field of auramine O, can solve the problems of increasing product composition complexity, many by-products, difficulties, etc., and achieve the effect of novel process, simple operation and high product purity

Active Publication Date: 2014-04-30
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to high temperature reaction conditions, there are many by-products, which increases the complexity of product composition
The current purification methods generally use solvents such as alcohols for crystallization and purification. Auramine O is soluble in cold water, easily soluble in hot water and turns bright yellow, and decomposes when boiled. Therefore, there are still great difficulties in obtaining high-purity auramine O.
Reagent service providers, including Sigma-Aldrich, can only provide auramine O products with a purity of up to about 85% at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A process for preparing high-purity auramine O, the steps are as follows:

[0019] (1) Put 50g of crude auramine O with a purity of 80% into 350ml of dichloromethane at a temperature of 30°C, stir and keep warm for 6h.

[0020] (2) After the stirring is stopped, the above mixture is suction filtered, and the filter cake is pressed dry. The mother liquor is distilled under reduced pressure, and the organic solvent is recovered for recycling.

[0021] (3) A total of 31 g of solids obtained by vacuum distillation of the above mother liquor were put into 100 ml of methyl tert-butyl ether, and stirred at room temperature for 2 h.

[0022] (4) After the stirring was stopped, the above mixture was suction-filtered, and the filter cake was washed twice with 20 ml of methyl tert-butyl ether, and the filter cake was drained and dried to obtain 29 g of high-purity auramine O. The mother liquor is distilled under reduced pressure, and the organic solvent can be recovered for recy...

Embodiment 2

[0024] A process for preparing high-purity auramine O, the steps are as follows:

[0025] (1) Put 120g of crude auramine O with a purity of 80% into 800ml of dichloromethane at a temperature of 35°C, stir and keep warm for 8h.

[0026] (2) After the stirring is stopped, the above mixture is suction filtered, and the filter cake is pressed dry. The mother liquor is distilled under reduced pressure, and the organic solvent is recovered for recycling. (3) A total of 77 g of solids obtained by vacuum distillation of the above mother liquor were put into 200 ml of isopropyl ether and stirred at room temperature for 2 h.

[0027] (4) After the stirring was stopped, the above mixture was filtered with suction, and the filter cake was washed twice with 50 ml of isopropyl ether, and the filter cake was drained and dried to obtain 73 g of high-purity auramine O. The mother liquor is distilled under reduced pressure, and the organic solvent can be recovered for recycling. The purity d...

Embodiment 3

[0029] A process for preparing high-purity auramine O, the steps are as follows:

[0030] (1) Put 100g of crude auramine O with a purity of 80% into 550ml of chloroform at a temperature of 30°C, stir and keep warm for 8h.

[0031] (2) After the stirring is stopped, the above mixture is suction filtered, and the filter cake is pressed dry. The mother liquor is distilled under reduced pressure, and the organic solvent is recovered for recycling. (3) A total of 63 g of solids obtained by vacuum distillation of the above mother liquor were put into 150 ml of isopropyl ether and stirred at room temperature for 2 h.

[0032] (4) After the stirring was stopped, the above mixture was filtered with suction, and the filter cake was washed twice with 40ml of isopropyl ether, and the filter cake was drained and dried to obtain 60g of high-purity auramine O. The mother liquor is distilled under reduced pressure, and the organic solvent can be recovered for recycling. The purity detected...

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PUM

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Abstract

The invention discloses a process for preparing high-purity auramine O. The process is characterized in that the process concretely comprises the following steps: 1, adding a crude auramine O raw material to an organic solvent at 20-40DEG C, uniformly stirring, and maintaining the temperature for 2-8h, wherein the weight of the organic solvent is 5-10 times the mass of auramine O; 2, carrying out reduced pressure suction filtration of the obtained mixture, pressing the obtained filter cake to dryness, carrying out reduced pressure distillation of the obtained mother solution, and recovering the organic solvent which can be recycled; 3, adding a solid obtained after the reduced distillation concentration of the mother solution to an another organic solvent, and stirring for 1-2h, wherein the weight of the another organic solvent is 1-3 times the weight of the solid; and 4, carrying out reduced pressure suction filtration of a mixture obtained in step 3, washing the obtained filter cake with the another organic solvent 1-3 times, carrying out suction drying of the filter cake, and drying to obtain the high-purity auramine O, wherein the weight of the another organic solvent is 0.5-1 times the weight of the solid. The process successfully solves the high purity auramine O preparation problem.

Description

technical field [0001] The invention belongs to the technical field of chemical reagents and relates to auramine O, i.e. C 17 h 22 ClN 3 separation and purification process. Background technique [0002] Auramine O (Auramin O), also known as Basic Bright Yellow O, Basic Light Yellow O, Basic Fluorescent Yellow GR, also known as Auramin O, yellow uniform powder. Widely used in dyeing of leather, paper, hemp and viscose. Alkaline products can be used for coloring oil, fat, paint, etc. Auramine O emits light in the visible light region, and the aromatic group in the molecule is connected to the central carbon by a single bond, which is easy to rotate, and its fluorescence quantum efficiency changes significantly with the viscosity of the environment. Due to this special property, auramine O It is not only widely used in clinical medical tests such as tuberculosis bacteriology (Journal of Modern Clinical Medicine Bioengineering 2007, 13 (1) 41; Acta Polymer Sinica 1990, 3 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B11/02
Inventor 杨永磊凌青
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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