Anthraquinone allergenic dispersed dye as well as extraction method and application thereof

A purification method and technology for disperse dyes, applied in the field of anthraquinone 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 anthraquinone allergenic disperse dyes and its purification method and application

Method used

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  • Anthraquinone allergenic dispersed dye as well as extraction method and application thereof
  • Anthraquinone allergenic dispersed dye as well as extraction method and application thereof
  • Anthraquinone allergenic dispersed dye as well as extraction method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take Waters Xterra C 18 (5μm, 19×100mm) chromatographic column; mobile phase is methanol: water (70:30) and linearly changes to methanol: water (95:5) in 8 minutes; detection wavelength is 570nm; flow rate is 12ml / min.

[0025] Dissolve 50ml with methanol: water (70:30) and dissolve 5g of Disperse Blue 1 commercial dye, filter, inject 5ml each time, collect the effluent of 4.5min-5.9min, evaporate the collected solution to dryness, and obtain 100mg of solid, after analysis, The purity is 98.9%.

Embodiment 2

[0027] Take Waters Xterra C 18 (5μm, 19×100mm) chromatographic column; the mobile phase is methanol: water (80:20) and linearly changes to methanol: water (95:5) in 8 minutes; the detection wavelength is 570nm; the flow rate is 28ml / min.

[0028] Dissolve 5g of Disperse Red 11 commercial dye with 50ml of methanol: water (80:20), filter, inject 5ml each time, collect the effluent of 4.0min-4.9min, evaporate the collected solution to dryness, and obtain 90mg of solid. After analysis, the purity 99.3%.

Embodiment 3

[0030] Take Agilent Eclipse XDB C 18 (5 μm, 21.2 × 100mm) chromatographic column; mobile phase is methanol: water (85: 15) and linearly changes to methanol: water (95: 5) in 8 minutes; detection wavelength is 570nm; flow rate is 24ml / min.

[0031] Use methanol: water (85: 15) 60ml to dissolve 5g of disperse blue 35 commercial dye, filter, inject 5ml each time, collect the effluent at 3.5min-4.5min, evaporate the collected solution to dryness, and obtain 70mg of solid. After analysis, The purity is 99.9%.

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Abstract

The invention discloses an extraction method of an anthraquinone allergenic dispersed dye shown in a formula (1) in the specification. The method comprises the following steps of: dissolving product dye corresponding to the formula (1) to a polar solvent and extracting a compound (1) by using a high-efficiency liquid-phase chromatography method under the conditions: a chromatographic column is a chromatographic column of octadecylsilyl bonded silica gel, methanol and water are used as moving phases for gradient elution, the ratio of the methanol to the water at the start gradient is 70:30 to 85:15, the ratio of the methanol to the water at the final gradient is 95 to 5, the gradient elution time is longer than 8min, the velocity of flow is 5-30ml/min, and the detection wavelength of an UV(Ultraviolet) detector is 210-570nm. The invention also discloses a product prepared by using the method and application thereof as a standard sample for analysis. The product obtained by using the extraction method of the invention reaches the purity up to 98.7-99.9 percent.

Description

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

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/54C09B67/38C09B1/54C09B1/16C09B1/515C09B1/503B01D15/08
Inventor 李懿睿郭卫荣
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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