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Allergenic disperse dye as well as purification method and application thereof

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

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 allergenic disperse dyes, its purification method and application

Method used

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  • Allergenic disperse dye as well as purification method and application thereof
  • Allergenic disperse dye as well as purification method and application thereof
  • Allergenic disperse dye as well as purification 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 (65:35) and linearly changes to methanol: water (95:5) in 6 minutes; the detection wavelength is 420nm; the flow rate is 18ml / min.

[0027] Dissolve 5g of Disperse Yellow 1 commercial dye with 50ml of methanol: water (65:35), filter, inject 5ml each time, collect the effluent of 3.2min-4.5min, evaporate the collected solution to dryness, and obtain 100mg of solid. After analysis, the purity 99.1%.

Embodiment 2

[0029] Take Agilent Eclipse XDB C 18 (5 μm, 21.2 × 100mm) chromatographic column; mobile phase is methanol: water (75: 25) and linearly changes to methanol: water (95: 5) in 6 minutes; detection wavelength is 420nm; flow rate is 28ml / min.

[0030] Dissolve 6g of Disperse Yellow 9 commercial dye with 50ml of methanol: water (75:25), filter, inject 5ml each time, collect the effluent of 3.0min-3.9min, evaporate the collected solution to dryness, and obtain 90mg of solid. After analysis, the purity 99.5%.

Embodiment 3

[0032] Take Waters Xbridge OBD-C 18 (5μm, 30×100mm) chromatographic column; the mobile phase is methanol: water (75:25) and linearly changes to methanol: water (95:5) in 6 minutes; the detection wavelength is 420nm; the flow rate is 30ml / min.

[0033] Dissolve 6g of Disperse Yellow 9 commercial dye with 50ml of methanol: water (75:25), filter, inject 5ml each time, collect the effluent of 3.1min-4.0min, evaporate the collected solution to dryness, and obtain 100mg of solid. After analysis, the purity 99.6%.

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Abstract

The invention discloses a purification method of an allergenic disperse dye as shown in formula I, which comprises the following steps: dissolving a commodity dye corresponding to formula I in a polar solvent; and purifying a compound I by the preparative high-performance liquid chromatography, wherein the conditions of the preparative high-performance liquid chromatography are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, methanol and water are used as flowing phases for gradient elution, the start gradient for the ratio of the methanol to the water is 65:35 to 75:25, the final gradient for the ratio of the methanol to the water is 95:5, the time for gradient elution is more than 6 minutes, and the flow rate is 5-30 ml / min; the detection wavelength of an ultraviolet detector is 210-420 nm; and R is a hydroxyl group or an amino group. The invention also discloses a product prepared by the method and application of the product as a standard sample for an analysis. By using the purification method, the purity of the obtained product can be up to 99.1-99.5%.

Description

technical field [0001] The present invention specifically relates to an 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...

Claims

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Application Information

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IPC IPC(8): C09B67/54C09B67/38C09B51/00B01D15/08
Inventor 李懿睿郭卫荣
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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