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Synthetic method for precursor of anthraquinone reactive disperse dye used in supercritical CO2

A technology of reactive disperse dyes and synthesis methods, which is applied in the field of synthesis of anthraquinone-type reactive disperse dye precursors for supercritical CO2, and can solve the problems of poor applicability and few types of reactive disperse dyes

Active Publication Date: 2016-05-04
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, how to diversify the synthesis methods of reactive disperse dyes, and solve the problems of few types of reactive disperse dyes and poor applicability, has become the key to breaking through the bottleneck, and it can be used for supercritical CO 2 Water-free dyeing of natural fibers in fluids offers broader prospects

Method used

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  • Synthetic method for precursor of anthraquinone reactive disperse dye used in supercritical CO2
  • Synthetic method for precursor of anthraquinone reactive disperse dye used in supercritical CO2
  • Synthetic method for precursor of anthraquinone reactive disperse dye used in supercritical CO2

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Embodiment 1

[0022] Supercritical CO 2 With the synthetic method of anthraquinone type reactive disperse dye precursor, comprise the steps:

[0023] (1) Add 0.005mol2,5-diaminotoluene sulfate and 0.0075molK 2 CO 3 , into the nitrogen, and quickly added 0.556mmolCuI. Weigh 0.005mol of 1-chloroanthraquinone, add 30mL of N,N-dimethylformamide to dissolve (if there is a small amount of insoluble solid, use ultrasonic vibration until it becomes yellow and transparent), and quickly add it to the dropping funnel, start stirring and Slowly add dropwise (dropping is completed in about 10 minutes), start timing when the temperature rises to 100°C, and reflux for 12 hours.

[0024] (2) After the reaction, the reaction solution was naturally cooled to 35°C, water and dichloromethane (volume ratio: 2:1) were added, and neutral silica gel was used as a filter aid to filter under pressure to remove the mixed solution. The black flocculent precipitate was then subjected to operations such as extractio...

Embodiment 2

[0034] This embodiment provides a supercritical CO 2 Use the synthetic method of anthraquinone type active disperse dye precursor, other steps of this method are the same as embodiment 1. Wherein the reaction medium in the step (1) is 30 mL dimethyl sulfoxide; the yield of the dye precursor in the step (2) is 37.03%.

Embodiment 3

[0036] This embodiment provides a supercritical CO 2 Use the synthetic method of anthraquinone type active disperse dye precursor, other steps of this method are the same as embodiment 1. Wherein in step (1), 2,5-diaminotoluene sulfate and K 2 CO 3 The dosages are respectively 0.0075 mol and 0.015 mol, the reaction temperature is 110° C., and the reaction time is 6 h; the yield of the dye precursor in the step (2) is 38.79%.

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Abstract

The invention specifically relates to a synthetic method for a precursor of an anthraquinone reactive disperse dye used in supercritical CO2, which belongs to the technical field of dyes. According to the method, 1-chloroanthraquinone and 2,5-diaminotoluene sulfate are used as raw materials, K2CO3 is used as an acid-binding agent, and CuI is used as a reaction catalyst, a heating reflux reaction is carried out at 80 to 140 DEG C for 6 to 14 h under the protection of nitrogen; and after completion of the reaction, post-treatment is carried out so as to obtain solid powder of the dye precursor. The method has the advantages of a low usage amount of the catalyst, mild reaction conditions, high yield and low cost, and the obtained precursor has good applicability; and the method is applicable to synthesis of the anthraquinone reactive disperse dye used in supercritical CO2 and to synthesis of reactive disperse dyes used in conventional water-bath dyeing.

Description

technical field [0001] The invention belongs to the technical field of dyes, in particular to a supercritical CO 2 Synthetic method of anthraquinone reactive disperse dye precursor. Background technique [0002] The emergence and development of reactive disperse dyes can be traced back to the 1950s and 1960s. However, due to its great influence on the use conditions, it is difficult to achieve uniform dyeing when dyeing polyester / cotton blended fabrics, and its applicability is poor. Therefore, a bottleneck has been encountered in the development process (reference: Reactive dyes landmark progress and basic theoretical research results in fifty years [J]. Dyestuffs and Dyeing, 2008, 2: 1-9, 44.). While using supercritical CO 2 Fluid dyeing technology can realize the dyeing of polyester / cotton blended fabrics and natural fibers with reactive disperse dyes, which has injected new vitality into its development (references: One-bathdyeingofpolyester / cottonblendswithreactivedis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C221/00C07C225/34
CPCC07C221/00C07C225/34Y02P20/54
Inventor 龙家杰章燕琴於琴
Owner SUZHOU UNIV
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