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Supercritical CO2 dyeing special-purpose azo-type active disperse dye

A reactive disperse dye, azo-type technology, applied in the direction of reactive dyes, azo dyes, monoazo dyes, etc., can solve the problem of loss

Inactive Publication Date: 2016-03-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods require pretreatment of the fiber, and a relatively high concentration of modifying agent needs to be added during the dyeing process to obtain a higher dyeing depth. Sometimes the fiber needs to be cleaned after dyeing, thus losing the supercritical CO 2 The unique advantages of dyeing (references: the past, present and future of supercritical fluid dyeing technology (two) [J]. Printing and Dyeing, 2003, 4: 37-45; Application of supercritical carbon dioxide in finishing processes [J]. Journal of the Textile institute, 1993, 84 (4): 534-552; Dyeing of cotton in supercritical carbondioxide [J]. Dyes and Pigments, 1998, 39 (4): 335-340; Mordant dyeing of wool by super critical processing [J]. 2 [C] / / 4thInternationalSymposiumExtractionforSamplePreparation-SFE-(X)SE-SPME-Bookofabstracts.1999:29-30;Dyeingofcottonfiberswithdispersedyesinsupercriticalcarbondioxide[J].DyesandPigments,1998,36(2):103-110;Thedyeingofnaturalfiberswithreactivedispersedyesinsupercriticalcarbondioxide[J].DyesandPigments,2003 , 56(1):27-35.)

Method used

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  • Supercritical CO2 dyeing special-purpose azo-type active disperse dye
  • Supercritical CO2 dyeing special-purpose azo-type active disperse dye
  • Supercritical CO2 dyeing special-purpose azo-type active disperse dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Weigh 0.002mol 2-chloro-4-nitroaniline, add 50mL polyethylene glycol 200 and 50mL deionized water, place it in an ultrasonic cleaner to shake and dissolve, then add 0.02mol concentrated hydrochloric acid to the solution And transfer it to a three-necked flask equipped with a magnetic stirring bar and a thermometer, in an ice-water bath, and control the temperature at 0-5°C. After stirring evenly, slowly add 0.0022mol of sodium nitrite (dissolved in 5mL of deionized water) to the reaction solution dropwise. After 2.5 hours of reaction, add 0.0002mol of urea (dissolved in 5mL of deionized water), and stir for 15 minutes to obtain a yellow , Clear diazonium salt solution.

[0019] (2) Measure 0.0022mol m-toluidine (add 5mL polyethylene glycol 200 to dilute as a diluent), slowly drop it into the above-mentioned diazonium salt solution, and adjust the pH value to about 6 with 30% NaOH aqueous solution , keep the temperature at 0-5°C, and finish the reaction after 4h. T...

Embodiment 2

[0028] The supercritical CO provided by this embodiment 2 Dyeing special-purpose azo-type reactive disperse dyes, the steps of its synthetic method are the same as in Example 1, wherein m-toluidine in step (2) is changed to 3-methoxyaniline, and the yield of the product obtained is 97.55%. In step (3), weigh 0.001 mol of the product in step (2), add 50 mL of 1,4-dioxane and 50 mL of deionized water, and finally obtain a crude reactive disperse dye with a yield of 94.73%. In the step (4), the crude product of the reactive disperse dye obtained in the step (3) is purified.

[0029] Using Fourier transform infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy (400MHz, DMSO-d 6 ) and UV-visible absorption spectroscopy and other testing techniques to characterize the structure of the purified product obtained in this example, the results are as follows figure 2 , 4 , 5 shown.

[0030] figure 2 shows that at 3299.09cm -1 There is N-H stretching vibration pe...

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Abstract

The invention belongs to the technical field of dye synthesis, and especially relates to a supercritical CO2 dyeing special-purpose azo-type active disperse dye. The supercritical CO2 dyeing special-purpose azo-type active disperse dye is a dichlorotriazine dye. In a preparation method, 2-chloro-4-nitroaniline and an aniline derivative are taken as raw materials to synthesize a dye precursor; the dye precursor and cyanuric chloride are subjected to nucleophilic substitution so as to obtain the supercritical CO2 dyeing special-purpose azo-type active disperse dye finally. The supercritical CO2 dyeing special-purpose azo-type active disperse dye possesses relatively high reaction activity, and low dyeing temperature, is suitable for supercritical CO2 fluid dyeing of natural fiber, and is green and friendly to the environment; the synthesis technology is simple; operation is convenient; and yield is relatively high.

Description

technical field [0001] The present invention relates to azo dyes, in particular to a supercritical CO 2 Special azo reactive disperse dyes for dyeing. Background technique [0002] Supercritical CO 2 Waterless dyeing technology was proposed by Schonmeyer et al. in 1988, and then further developed by Knittel (references: the past, present and future of supercritical fluid dyeing technology (1) [J]. Printing and Dyeing, 2003, 29 (3): 42 -45; Dyeing of natural fibers with reactive disperse dyes in supercritical carbon dioxide [J]. Foreign Textile Technology: Dyeing and Finishing of Chemical Fibers for Textile Knitwear, 2003, 9: 22-27.). At present, the supercritical CO of synthetic fibers (such as polyester, nylon, etc.) 2 Fluid dyeing technology is relatively mature, and some applicable dyes can be screened from existing disperse dyes, with excellent fastness properties. [0003] However, in natural fibers supercritical CO 2 There are many problems in anhydrous dyeing, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/08C09B62/085D06P1/18D06P1/382D06P3/66D06P3/68
CPCC09B29/0832C09B62/085D06P1/18D06P1/382D06P3/6033D06P3/66D06P3/68Y02P20/54
Inventor 龙家杰章燕琴魏晓晨
Owner SUZHOU UNIV
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