Gray reactive dye and preparation method thereof

A gray and dye technology, applied in the field of reactive dye preparation, can solve the problems of insufficient Integ value, poor improvement performance, and insufficient solubility, and achieve the effects of good printing reproducibility, improved performance, and high color fixation rate.

Active Publication Date: 2016-05-18
ZHEJIANG JINGGUANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the product still has poor lifting performance, the Integ value is not deep enough, and Cr remains in textile fabrics. 6+ Exceeding the standard up to dozens of times, the solubility is still not up to 200g / L of other dyes and chemicals, and many other problems

Method used

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  • Gray reactive dye and preparation method thereof
  • Gray reactive dye and preparation method thereof
  • Gray reactive dye and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 1500L in the diazo kettle, heat up to 40°C, add 158 kg of 30% hydrochloric acid and 154 kg of 4-nitro-2-aminophenol, stir for 30 minutes to dissolve, then start to drop 230 kg of 30% sodium nitrite solution, Both the dropping temperature and the reaction temperature are controlled below 25°C, the reaction time is 60-90 minutes, and excess sodium nitrite is eliminated with sulfamic acid;

[0044]Add 1700L of bottom water to the coupling kettle, add 341 kg of H acid, and dissolve the H acid with 20% lithium hydroxide after stirring for 20 minutes. The pH value is controlled at 7.0-7.5. After a while, slowly add the diazonium salt prepared in step (1), the pH value is always greater than 6.5, and the temperature is 0-5°C for more than 10 hours;

[0045] After the end point of the coupling is reached, the temperature is raised to 60°C, and the pH is adjusted to 4.5-5.0 with 30% hydrochloric acid, and 10 kg of salicylic acid is added, and the temperature is continued to ...

Embodiment 2

[0049] Add 1500L in the diazo kettle, heat up to 40°C, add 158 kg of 30% hydrochloric acid and 154 kg of 4-nitro-2-aminophenol, stir for 30 minutes to dissolve, then start to drop 230 kg of 30% sodium nitrite solution, Both the dropping temperature and the reaction temperature are controlled below 25°C, the reaction time is 60-90 minutes, and excess sodium nitrite is eliminated with sulfamic acid;

[0050] Add 1700L of bottom water to the coupling kettle, add 341 kg of H acid, and dissolve the H acid with 20% lithium hydroxide after stirring for 20 minutes. The pH value is controlled at 7.0-7.5. After a while, slowly add the diazonium salt prepared in step (1), the pH value is always greater than 6.5, and the temperature is 0-5°C for more than 10 hours;

[0051] After the end point of the coupling is reached, heat up to 60°C, adjust the pH to 4.5-5.0 with 30% hydrochloric acid, add 12.5 kg of phthalic anhydride, continue to heat up to 100°C, add 125 kg of chromium trichloride ...

Embodiment 3

[0055] Add 1500L in the diazo kettle, heat up to 40°C, add 158 kg of 30% hydrochloric acid and 154 kg of 4-nitro-2-aminophenol, stir for 30 minutes to dissolve, then start to drop 230 kg of 30% sodium nitrite solution, Both the dropping temperature and the reaction temperature are controlled below 25°C, the reaction time is 60-90 minutes, and excess sodium nitrite is eliminated with sulfamic acid;

[0056] Add 1700L of bottom water to the coupling kettle, add 341 kg of H acid, and dissolve the H acid with 20% lithium hydroxide after stirring for 20 minutes. The pH value is controlled at 7.0-7.5. After a while, slowly add the diazonium salt prepared in step (1), the pH value is always greater than 6.5, and the temperature is 0-5°C for more than 10 hours;

[0057] After the end point of the coupling is reached, heat up to 60°C, adjust the pH to 4.5-5.0 with 30% hydrochloric acid, add 5 kg of salicylic acid and 5 kg of phthalic anhydride, continue to heat up to 100°C, and add 115...

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Abstract

The invention discloses a preparation method of gray reactive dye. 4-nitro-2-aminophenol diazonium and H acid have an alkaline coupling reaction, the pH value is controlled to be larger than 6.5, and the mixture reacts for 10 h at the temperature of 0-5 DEG C; a coupling body and chromium trichloride have a metal complex reaction under the action of a catalyst at the temperature of 95-100 DEG C, and the residual amount of free chromium metal is controlled; tricyanogen chloride and 3 times of ammonia water have a primary condensation reaction, ice water is added to a condensation product, washing is performed twice, and ammonium chloride is removed; the primary condensation product and a complexing solution have a secondary condensation reaction; finally, a dispersant NNO and a dispersant MF are added for standardization, and a gray reactive dye product is obtained through filtering, impurity removal and spray drying.

Description

technical field [0001] The invention belongs to the field of preparation of reactive dyes, in particular to a method for preparing metal complex reactive gray dyes. Background technique [0002] C.I.ReactiveBlack8 belongs to metal complex dyes. The dyes contain metal chromium, or metal cobalt, or a mixture of metal chromium and cobalt. It is gray after dyeing on cellulose fabrics, and it turns black when the dosage reaches 80-100g / L. It is mostly used for fabrics. It has good compatibility with different dyes and chemicals, and is widely used in various color toning components. Most of the products on the market are compounded with a mixture containing metallic chromium and cobalt, or compounded with a certain ratio of metallic chromium dyes and red dyes to standard product shades. [0003] The traditional synthesis process is alkaline coupling of 4-nitro-2-aminophenol diazonium salt with H acid solution, chromogen salting out and refining, and metal complexation with chrom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/095
CPCC09B62/095
Inventor 王国林单国静
Owner ZHEJIANG JINGGUANG IND
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