Azo allergenic disperse dye, and purifying method and application thereof

A purification method and technology for disperse dyes, applied in the field of azo sensitizing disperse dyes, can solve the problems of low purity and the like

Inactive Publication Date: 2011-04-20
SHANGHAI INST OF MEASUREMENT & TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a kind of azo allergenic disperse dyes, its purificatio

Method used

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  • Azo allergenic disperse dye, and purifying method and application thereof
  • Azo allergenic disperse dye, and purifying method and application thereof
  • Azo allergenic disperse dye, and purifying method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take Waters Xterra C 18 (5μm, 19×100mm) chromatographic column; the mobile phase is methanol: water (40:60) and linearly changes to methanol: water (95:5) in 7 minutes; the detection wavelength is 450nm; the flow rate is 15ml / min.

[0027] Dissolve 5g of Disperse Orange 1 commercial dye with 50ml of methanol: water (40:60), filter, inject 5ml each time, collect the effluent of 4.2min-4.9min, evaporate the collected solution to dryness, and obtain 100mg of solid. After analysis, the purity was 99.2%.

Embodiment 2

[0029] Take Waters Xterra C 18 (5μm, 19×100mm) chromatographic column; the mobile phase is methanol: water (40:60) and linearly changes to methanol: water (95:5) in 7 minutes; the detection wavelength is 450nm; the flow rate is 18ml / min.

[0030] Dissolve 5g of Disperse Orange 3 commercial dye with 50ml of methanol: water (40:60), filter, inject 5ml each time, collect the effluent of 3.8min-4.5min, evaporate the collected solution to dryness, and obtain 95mg of solid. After analysis, the purity was 98.2%.

Embodiment 3

[0032] Take Waters Xterra C 18 (5μm, 19×100mm) chromatographic column; the mobile phase is methanol: water (20:80) and linearly changes to methanol: water (95:5) in 7 minutes; the detection wavelength is 450nm; the flow rate is 24ml / min.

[0033]Dissolve 5g of Disperse Orange 37 commercial dye with 50ml of methanol: water (20:80), filter, inject 5ml each time, collect the effluent of 3.7min-4.8min, evaporate the collected solution to dryness, and obtain 90mg of solid. After analysis, the purity 99.8%.

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Abstract

The invention discloses a purifying method of an azo allergenic disperse dye shown as the formula I in the specification. The method comprises the following steps of: dissolving a commodity dye shown as the formula I into a polar solvent and purifying a compound I by a preparative high performance liquid chromatography, wherein the conditions of the preparative high performance liquid chromatography are that: gradient elution is performed by using an octadecyl silane bonded silica gel chromatographic column as a chromatographic column, and methanol and water as mobile phases, wherein the start gradient is the ratio of methanol to water of 20:80-40:60; the final gradient is the ratio of methanol to water of 95:5; the time of the gradient elution is over 7 minutes; the flow rate is 5 to 30ml/min; and the detection wavelength of an ultraviolet detector is 210 to 450nm. The invention also discloses the azo allergenic disperse dye produced by the purifying method, and application of the azo allergenic disperse dye serving as a standard sample for analysis. The purity of the product obtained by the purifying method reaches 97.6 to 99.8 percent.

Description

technical field [0001] The invention specifically relates to an azo allergenic disperse dye, its purification method and application. Background technique [0002] Disperse dyes can cause skin, mucous membrane or respiratory allergies in humans or animals. When people wear or use textiles containing such dyes, they may pose a potential threat to health. Therefore, some countries or international organizations have made strict restrictions on the use of such dyes through laws and regulations, standards or conformity assessment procedures. [0003] Since the German government first promulgated the prohibition of some dyes in 1994, with the continuous improvement of environmental and ecological protection requirements in various countries, the scope of banned dyes has continued to expand, and many countries and regions have successively issued regulations on banned dyes. Oeko-Tex Standard 100 (version 2006) and my country promulgated GB / T 18885-2002 "Technical Requirements for...

Claims

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Application Information

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IPC IPC(8): C09B67/54C09B67/38C09B67/36B01D15/08
Inventor 李懿睿郭卫荣
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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