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A kind of precursor of blue anthraquinone reactive disperse dye and preparation method thereof

A technology of reactive disperse dyes and precursors, applied in the preparation of anthracene dyes, organic compounds, organic dyes, etc., can solve the problems of unsatisfactory natural fiber dyeing, low manufacturing cost, and single structure, and achieve good application prospects and low manufacturing costs. Low, good dyeing quality

Active Publication Date: 2020-04-03
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 A reactive disperse dye precursor with an anthraquinone structure for fluid dyeing and a preparation method thereof. The precursor can be prepared into a dye, which can solve the problems that the current anthraquinone reactive disperse dye has a single structure and few varieties, and cannot meet the needs of natural fiber dyeing; Apply the dye prepared from the precursor provided by the invention to supercritical CO 2 In anhydrous 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 dyes quickly, the dyeing quality is good, and the manufacturing cost is low.

Method used

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  • A kind of precursor of blue anthraquinone reactive disperse dye and preparation method thereof
  • A kind of precursor of blue anthraquinone reactive disperse dye and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In this embodiment, taking the reaction with ethylenediamine as an example, the structural formula of the product is:

[0025] ,

[0026] Among them, n=2.

[0027] The specific method is: 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 1ml of ethyl Dissolve diamine 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 catalyst copper acetate and piperidine , the molar ratio of 1,4-dihydroxyanthraquinone to copper acetate is 1:1.5, and an appropriate amount of piperidine is heated to 108°C for boiling for 3 hours; filled with oxygen for 3 hours; cooled to room temperature, and the reaction is complete. Using petroleum ether and dichloromethane (1:3, v / v) as eluents for...

Embodiment 2

[0031] 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:

[0032] 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...

Embodiment 3

[0036] In this example, the reaction with 1,6-hexanediamine is taken as an example to prepare the blue anthraquinone reactive disperse dye precursor. The specific steps are as follows:

[0037] 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 3.3 ml of 1,6- Dissolve hexamethylenediamine 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 1:5, appropriate amount of piperidine, heat up to 108°C and boil for 3 hours; fill with oxygen for 3 hours; cool to room temperature, the reaction is complete. Using petroleum ether and dichloromethane (1:3, v / v) as the eluent for chromato...

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Abstract

The invention discloses a precursor of blue anthraquinone active disperse dye and a preparing method thereof. A parent body structure of the precursor is of an anthraquinone structure, has amidogen capable of being reacted with an active group, and can be used for preparing the anthraquinone active disperse dye; the synthetic technology is simple, operation is easy, and the preparing cost is low;the anthraquinone active disperse dye prepared with the method can be applied to dyeing of natural fibers in supercritical CO2 fluid dyeing and dyeing processing of blended fabrics of the natural fibers, particularly, has good dyeing effect on natural fibers such as cotton, wool and silk.

Description

technical field [0001] The invention relates to a method for supercritical CO 2 The precursor of dyed anthraquinone active disperse dye and its synthesis 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C221/00C07C225/34C09B1/32
CPCC07C221/00C07C225/34C09B1/325Y02P20/54
Inventor 龙家杰樊月
Owner SUZHOU UNIV