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Blue anthraquinone active disperse dye and preparation method thereof

A technology of reactive disperse dyes and anthraquinones, applied in reactive dyes, dyeing methods, azo dyes, etc., can solve the problems of unsatisfactory natural fiber dyeing, good dyeing quality, and low manufacturing cost, and achieve good application prospects and high dyeing quality Good, low manufacturing cost effect

Active Publication Date: 2018-09-07
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the deficiencies in the prior art, and provides a supercritical CO 2 The reactive disperse dye with anthraquinone structure for fluid dyeing and its preparation method can solve the problems that the current anthraquinone reactive disperse dye has a single structure and few varieties and cannot meet the dyeing of natural fibers; the reactive disperse dye is applied to supercritical CO 2 Waterless dyeing or traditional printing and dyeing processing, it has good dyeing performance on cotton, wool, silk and other natural fibers and their blended textiles, the dye diffuses into the fiber and the dyeing speed is fast, the dyeing quality is good, and the manufacturing cost is low

Method used

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  • Blue anthraquinone active disperse dye and preparation method thereof
  • Blue anthraquinone active disperse dye and preparation method thereof
  • Blue anthraquinone active disperse dye and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This embodiment takes the reaction with ethylenediamine as an example to prepare the precursor of the blue anthraquinone reactive disperse dye, and its reaction formula is:

[0023] .

[0024] The specific steps are:

[0025] Take 0.24g of 1,4-dihydroxyanthraquinone and its leuco 1,4-diaminoanthraquinone 0.619g and 0.462ml of isobutanol in a three-necked flask, and dissolve 6.840mL of aniline and 1ml of ethylenediamine in In 15ml of 20% isobutanol solution, keep stirring at 60°C for 2 hours under nitrogen protection; heat for 2 hours and then raise the temperature to 108°C and boil at this temperature for 3 hours; cool down to 95°C and add copper acetate and piperidine catalysts, 1,4 - The molar ratio of dihydroxyanthraquinone to copper acetate is 1:1.5, and an appropriate amount of piperidine is heated to 108°C for boiling for 3 hours; charged with oxygen for 3 hours; cooled to room temperature, and the reaction is complete. Using petroleum ether and dichlorometha...

Embodiment 2

[0037] The precursor provided in Example 1 of the present invention is used to prepare anthraquinone reactive disperse dyes with α-bromoacrylamide as the active group, and the reaction formula is:

[0038] .

[0039] Specific steps are as follows:

[0040] Take 1 mmol (0.357 g) of the dye precursor provided in Example 1 and dissolve it in 15 mL of dichloromethane, and control the temperature within the range of 0-5 °C. Take 0.0015mol of 2,3-dibromopropionyl chloride, dilute it in 5mL of dichloromethane, and slowly add it dropwise, raise the temperature to 35°C, stir for 1h, add 1mL of triethylamine, and stir for 3h. After the reaction, add water (about 350 mL) to dilute, precipitate flocculent precipitate, filter with suction, wash with water, and dry in vacuum to obtain a blue solid. Then use petroleum ether and dichloromethane (1:2, v / v) as the eluent for chromatographic column separation and purification to obtain a blue solid, which is anthraquinone reactive disperse d...

Embodiment 3

[0045] In this example, 1,4-butylene diamine is used as a reactant to prepare a blue anthraquinone reactive disperse dye precursor. The specific steps are as follows:

[0046] Take 0.24g of 1,4-dihydroxyanthraquinone and its leuco 1,4-diaminoanthraquinone 0.619g and 0.462ml of isobutanol in a three-necked flask, and simultaneously put 6.840mL of aniline and 1.5ml of 1,4- Dissolve butanediamine in 15ml of 20% isobutanol solution, heat and stir at 60°C for 2 hours under nitrogen protection; heat for 2 hours and then raise the temperature to 108°C and boil at this temperature for 3 hours; cool down to 95°C and add copper acetate and piperidine Catalyst, the molar ratio of 1,4-dihydroxyanthraquinone to copper acetate is 1:3, appropriate amount of piperidine, the temperature is raised to 108°C and boiled for 3 hours; filled with oxygen for 3 hours; cooled to room temperature, the reaction is completed. Using petroleum ether and dichloromethane (1:3, v / v) as the eluent for chromatog...

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Abstract

The invention discloses a blue strontium active disperse dye and a preparation method thereof. The dye is suitable for a supercritical CO2 fluid dyeing process. A parent structure of the active disperse dye is an anthracene structure, the active disperse dye has an amino group reactive with active groups, the active groups include groups such as dichlorotriazine, monochlorotriazine, alpha-bromoacrylamide, vinyl sulfone and the like which can react with fibers, and the shortcomings that structure of existing active disperse dyes is single, and the variety of the active disperse dyes is insufficient are overcome. The anthraquinone active disperse dye can be used for dyeing of natural fibers and dyeing processing of blended fabrics in the supercritical CO2 fluid dyeing, and have good dyeing effect especially for fibers such as cotton, wool, silk and the like. The fastness indexes of the dyed fabrics are good. The dye synthesis process is simple, the reaction conditions are mild, the manufacturing cost is low, and the applicability is strong.

Description

technical field [0001] The invention relates to a method for supercritical CO 2 The dyed anthraquinone reactive disperse dye and its preparation method belong to the technical field of dye synthesis. Background technique [0002] Supercritical CO 2 The dyeing technique is based on supercritical CO 2 The new dyeing and finishing technology of dyeing and finishing textiles with fluid as the dyeing medium began in the 1980s. It is characterized by no need to add auxiliaries and no waste water. Textiles in supercritical CO 2 The dyeing technology in the fluid has entered the pilot scale research in the laboratory and is expected to replace the traditional water bath process in the future. It greatly alleviates the demand for water, and at the same time greatly reduces the discharge of sewage, and fundamentally solves the problem of environmental pollution caused by the dyeing process. in supercritical CO 2 The dyed product obtained in the body has good levelness and can ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/06C09B62/467D06P1/382D06P1/384D06P3/66D06P3/14D06P3/10
CPCC09B62/06C09B62/467D06P1/382D06P1/384D06P3/10D06P3/148D06P3/663D06P3/666Y02P20/54
Inventor 龙家杰樊月
Owner SUZHOU UNIV
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