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Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof

A technology of benzisothiazopyrazolone and disperse dyes, which is applied in azo dyes, monoazo dyes, dyeing methods, etc., and can solve the problems of counterfeit and inferior products, complex components, and agglomeration

Inactive Publication Date: 2013-02-13
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Known coloring agents with certain applications are composed of a variety of dyes, complex components
Especially when anionic dyes are mixed with cationic dyes, different degrees of aggregation are prone to occur during preparation, storage, and use, which is not stable enough.
Moreover, the disperse dye components have coloring ability on synthetic fibers and semi-synthetic fibers, and the color difference of the colorant composed of mixed dyes is not obvious on different fibers. For example, the HI-1 fiber identification colorant is jade on polyester. Red, orange for acetate, sauce red for nylon, peach red for acrylic fiber, red lotus for wool, etc. are all red tones. If the operation is not done properly or the dyeing is insufficient, it is still easy to confuse
[0006] Consumers of clothing fabrics are often troubled by counterfeit and shoddy products. They need to quickly and easily identify the types and approximate contents of common fibers at home, which is currently difficult to achieve.

Method used

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  • Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof
  • Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof
  • Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Weigh 0.227g (3.3mmol) NaNO 2 , add 2.5ml (39.6mmol, 1:12) concentrated sulfuric acid, stir quickly, when heated to 65-70°C (the temperature should not exceed 80°C), stop heating, and cool down naturally, if there is salt precipitation, heat it slightly to dissolve it , to obtain nitrosylsulfuric acid. Weigh 0.585g (3mmol) of 3-amino-5-nitro-2,1-benzisothiazole, dissolve it in the above solution, and then add 2ml of concentrated sulfuric acid to obtain a dark brown solution in which all solids are dissolved.

[0058] Take 5ml of concentrated sulfuric acid and 7.5ml of glacial acetic acid, mix it into a 40% sulfuric acid / acetic acid solution in a 250ml three-necked bottle, add a little ice cubes, and put it in an ice-salt bath. Add the above-prepared dark brown solution dropwise into the sulfuric acid solution, and stir rapidly. After the dropwise addition, react for 10-15 minutes.

[0059] Weigh 0.523g (3mmol) 1-phenyl-3-methyl-5-pyrazolone, put it into a 250ml three...

Embodiment 2

[0063] Weigh 0.227g (3.3mmol) NaNO 2 , add 2.5ml (39.6mmol, 1:12) concentrated sulfuric acid, stir quickly, when heated to 65-70°C (the temperature should not exceed 80°C), stop heating, and cool down naturally, if there is salt precipitation, heat it slightly to dissolve it , to obtain nitrosylsulfuric acid. Weigh 0.585g (3mmol) of 3-amino-5-nitro-2,1-benzisothiazole, dissolve it in the above solution, and then add 2ml of concentrated sulfuric acid to obtain a dark brown solution in which all solids are dissolved.

[0064] Take 5ml of concentrated sulfuric acid and 7.5ml of glacial acetic acid, mix it into a 40% sulfuric acid / acetic acid solution in a 250ml three-necked bottle, add a little ice cubes, and put it in an ice-salt bath. Add the above-prepared dark brown solution dropwise into the sulfuric acid solution, and stir rapidly. After the dropwise addition, react for 10-15 minutes.

[0065] Weigh 3mmol 1-phenyl-3-methoxycarbonyl-5-pyrazolone, put it into a 250ml three...

Embodiment 3

[0068] Weigh 0.227g (3.3mmol) NaNO 2, add 2.5ml (39.6mmol, 1:12) concentrated sulfuric acid, stir quickly, when heated to 65-70°C (the temperature should not exceed 80°C), stop heating, and cool down naturally, if there is salt precipitation, heat it slightly to dissolve it , to obtain nitrosylsulfuric acid. Weigh 0.585g (3mmol) of 3-amino-5-nitro-2,1-benzisothiazole, dissolve it in the above solution, and then add 2ml of concentrated sulfuric acid to obtain a dark brown solution in which all solids are dissolved.

[0069] Take 5ml of concentrated sulfuric acid and 7.5ml of glacial acetic acid, mix it into a 40% sulfuric acid / acetic acid solution in a 250ml three-necked bottle, add a little ice cubes, and put it in an ice-salt bath. Add the above-prepared dark brown solution dropwise into the sulfuric acid solution, and stir rapidly. After the dropwise addition, react for 10-15 minutes.

[0070] Weigh 3mmol 1-(2-chlorophenyl)-3-methyl-5-pyrazolone, put it into a 250ml three...

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Abstract

The invention discloses a benzo isothiazole azo pyrazolone disperse dye. The benzo isothiazole azo pyrazolone disperse dye is a compound having the structure shown in a formula (I) in the specification. Conjugate migration of hydrogen connected with a heteroatom in the benzo isothiazole azo pyrazolone heterocyclic ring disperse dyes is performed among benzo isothiazole ring, azo and pyrazolone to display bright-colored yellow, red and blue; and moreover, the dye is large in hue span and rich in colors; and therefore, the benzo isothiazole azo pyrazolone disperse dye can be used for preparing a fiber identification coloring agent. The invention discloses a preparation method of the benzo isothiazole azo pyrazolone disperse dye.

Description

technical field [0001] The invention relates to a benzisothiazole azopyrazolone disperse dye and its application in common textile fiber identification. Background technique [0002] Fiber identification is extremely important for quality acceptance and production control in fiber processing, textile, printing and dyeing, etc. Many people have conducted research, so many identification methods have been produced, such as birefringence, fluorescence, X-ray diffraction, and infrared absorption. Spectrometry, rotational linear polarization detection method, terahertz time-domain spectroscopy, density gradient method and thermogravimetric method, etc., have high accuracy of analysis results, but the equipment is expensive and requires specialized experimenters. Usually laboratories use microscope observation, combustion , chemical test, coloring test and other simple methods. [0003] For natural fibers - cotton, wool, silk, linen, a small amount of samples can be distinguished...

Claims

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Application Information

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IPC IPC(8): C09B29/50C09B67/38D06P1/18G01N21/25
Inventor 黄伟陈晓春王银歌
Owner NANJING UNIV
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