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Synthesis method of black active dyestuff compound

A technology for reactive dyes and a synthesis method, which is applied in the synthesis field of black reactive dye compounds, can solve the problems of difficult removal of by-products, high preparation cost, low yield and the like, and achieves the elimination of processes and equipment, reduction of reaction equipment occupancy rate, less time effect

Inactive Publication Date: 2017-12-22
SHANGHAI WANDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0025] But above-mentioned scheme by-product is difficult to remove, yield is not high, and preparation cost is also high

Method used

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  • Synthesis method of black active dyestuff compound
  • Synthesis method of black active dyestuff compound
  • Synthesis method of black active dyestuff compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] 1. Diazonium salt①

[0067] With the p-(β-sulfate ethyl sulfone) aniline of 2.51mol parts (being commonly called as p-position ester, R in formula (1) 1 =-H,Z 1 =-SO 2 CH 2 CH 2 OSO 3 H) Make a slurry in an appropriate amount of water, add hydrochloric acid and stir evenly, then cool down to 0-5°C, then add 30% sodium nitrite solution for diazotization reaction, keep T=3-10°C throughout the diazotization process , and keep both hydrochloric acid and sodium nitrite in excess. After 1 hour of heat preservation reaction, use sulfamic acid to balance the excess sodium nitrite, diazonium salt ① for later use, reaction time: 2.5 hours;

[0068] 2. Diazonium salt②

[0069] The 4-(beta-hydroxyethylsulfone-sulfate) aniline-2-sulfonic acid of 0.425mol part (being commonly called as sulfonated p-position ester, R in formula (2) 2 =-SO 3 H, Z 2 =-CH 2 CH 2 OSO 3 H) Make a slurry in an appropriate amount of water, add hydrochloric acid and stir evenly, then cool down t...

Embodiment 2

[0079] 1. Diazonium salt①

[0080] The p-(beta-sulfate ethyl sulfone) aniline (being commonly called as p-position ester of 2.63mol parts, R in formula (1) 1 =-H,Z 1 =-SO 2 CH 2 CH 2 OSO 3 H) Make a slurry in an appropriate amount of water, add hydrochloric acid and stir evenly, then cool down to 0-5°C, then add 30% sodium nitrite solution for diazotization reaction, keep T=3-10°C throughout the diazotization process , and keep both hydrochloric acid and sodium nitrite in excess, after heat preservation reaction for 1 hour, balance the excess sodium nitrite with sulfamic acid, diazonium salt ① Standby, reaction time: 2.5 hours;

[0081] 2. Diazonium salt②

[0082] With the 4-(β-hydroxyethylsulfone-sulfate) aniline-2-sulfonic acid of 0.43mol part (being commonly called as sulfonated p-position ester, R in formula (2) 2 =-SO 3 H, Z 2 =-CH 2 CH 2 OSO 3 H) and 0.17 parts of anthranilic acid (R in formula (2) 2 =-SO 3 H, without Z 2 substituent) in an appropriate am...

Embodiment ３

[0091] 1. Diazonium salt①

[0092] The p-(beta-sulfate ethyl sulfone) aniline of 2.65mol parts (being commonly called as p-position ester, R in formula 1 1 =-H,Z 1 =-SO 2 CH 2 CH 2 OSO 3 H,) in an appropriate amount of water to beat evenly, add hydrochloric acid and stir evenly, then cool down to 0~5°C, then add 30% sodium nitrite solution to carry out diazotization reaction, and keep T=3~10 throughout the diazotization process ℃, and keep both hydrochloric acid and sodium nitrite in excess. After 1 hour of heat preservation reaction, use sulfamic acid to balance the excess sodium nitrite, diazonium salt ① for later use, reaction time: 2.5 hours;

[0093] 2. Diazonium salt②

[0094]With 0.05mol part of 4-(β-hydroxyethylsulfone-sulfate) aniline-2-sulfonic acid (commonly known as sulfonated para-ester, R in formula 2 2 =-SO 3 H, Z 2 =-CH 2 CH 2 OSO 3 H,) and 0.26mol parts of anthranilic acid (R in formula (2) 2 =-SO 3 H, no Z 2 substituent) in an appropriate amo...

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Abstract

The invention relates to a synthesis method of a black active dyestuff compound and belongs to the field of dyestuff chemistry. The synthesis method comprises the following steps: preparing a raw material A shown as a formula 1 into a first coupling solution; preparing a raw material B shown as a formula 2 into second diazonium salt and preparing the second diazonium salt, a raw material C shown as a formula 3 and a raw material D shown as a formula 4 into a second coupling solution under the condition that baking soda is added; mixing the first coupling solution and the second coupling solution; carrying out third coupling reaction and drying to obtain the black active dyestuff compound. The synthesis method of the black active dyestuff compound, provided by the invention has comprehensive advantages in the aspects of equipment, manpower, reaction time, product quality and the like when being compared with a former technology; the reaction time is greatly shortened to 8h to 14h; a synthesized black dyestuff has stable quality and good reproducibility; the yield of a product is 2 percent to 3 percent higher than that of a former mixture technology; reaction steps are reduced so that the occupied rate of reaction equipment is low; meanwhile, post-treatment procedures and equipment are saved, so that the defects of more mixture reaction equipment and great blending working amount are overcome.

Description

technical field [0001] The invention relates to a synthesis method of a black reactive dye compound, which belongs to the field of dye chemistry. Background technique [0002] Application number: 200580008899.0 discloses a kind of formula (I) reactive dyestuff is suitable for dyeing cellulose or containing amide base fiber material, [0003] [0004] Among them, Q 1 and Q 2 independently of each other is hydrogen or substituted or unsubstituted C 1 -C 4 Alkyl, D 1 is a diazo component group which is itself a mono- or disazo dye or contains such a dye, D 2 have with D 1 same definition, [0005] Or a group of formula (II): [0006] [0007] Among them, (Q 3 ) 0-3 Represents 0-3 selected from halogen, C 1 -C 4 Alkyl, C 1 -C 4 The same or different substituents of alkoxy, carboxyl and sulfo, [0008] Z 1 For the formula: [0009] -SO 2 -Y(3A), [0010] -NH-CO-(CH 2 ) M -SO 2 -Y(3B), [0011] -CONH-(CH 2 ) N -SO 2 -Y(3C), [0012] -NH-CO-CH(HAL)-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/513
CPCC09B62/513
Inventor 俞玉萍董振堂吴晓明商友芬施美莉季成忠
Owner SHANGHAI WANDE CHEM
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