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Black reactive dyestuff and preparation method thereof

A reactive dye and black technology, which is applied in the field of black reactive dye and its preparation, can solve the problems that the blackness and fastness cannot reach the same level, and cannot really replace medium black PV, etc., and achieve the effect of improving color fixation rate and fastness

Active Publication Date: 2012-12-19
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Some products have been launched at home and abroad as substitutes for acid medium black PV, but the blackness and fastness cannot reach the same level, and cannot really replace medium black PV

Method used

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  • Black reactive dyestuff and preparation method thereof
  • Black reactive dyestuff and preparation method thereof
  • Black reactive dyestuff and preparation method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0057] A kind of preparation method of black reactive dye, comprises the steps:

[0058] a. Preparation of condensate diazonium salt: Add 2.4-sodium diaminobenzenesulfonate to water, control the temperature at 2-8°C with ice, add 2.3-dibromopropionyl chloride, and control with 10--20% sodium carbonate solution pH = 6-8, react for 3-6 hours, and the reaction temperature is always controlled at 2-8°C to obtain a condensate suspension; add hydrochloric acid and ice to the condensate suspension, cool down to 0-5°C, add sub Sodium nitrate, react at 7-14°C for 1-2 hours, keep a slight excess of sodium nitrite throughout the reaction, add sulfamic acid H 2 NSO 3 H removes excess sodium nitrite;

[0059] b. Preparation of dinitroaniline diazonium salt: add sodium nitrite to 98% sulfuric acid, control the temperature below 30°C, heat up to 65--70°C after adding, keep warm for 2-3 hours; cool down to 30°C Next, add dinitroaniline, control the temperature below 40°C, keep warm at 40±3...

Embodiment 1

[0098] Structure 1

[0099]

[0100] 1. Preparation of Condensate

[0101] Add 420kg of sodium 2.4-diaminobenzenesulfonate to 7500L of water, control the temperature at 2-8°C with ice, add 515kg of 2.3-dibromopropionyl chloride, control the pH=6-8 with 10--20% sodium carbonate solution, and react 3--6 hours, the reaction temperature is always controlled at 2--8 °C. The condensate suspension was obtained and set aside.

[0102] 2. Preparation of condensate diazonium salt

[0103] Add 560 kg of 30% hydrochloric acid to the condensate suspension in step 1, add ice and cool down to 0-5°C. Add a solution containing 138kg of sodium nitrite, the concentration of the solution is 30-40%, and react at 7-14°C for 1-2 hours. After the reaction is complete, add H 2 NSO 3 H (sulfamic acid) removes excess sodium nitrite.

[0104] 3. Preparation of p-nitroaniline diazonium salt

[0105] Add 12kg of Brigade-12 surfactant, 238.6kg of p-nitroaniline, and 543kg of 30% hydrochloric acid...

Embodiment 2

[0115] Structure 2

[0116]

[0117] 1. Preparation of p-nitroaniline diazonium salt

[0118] Add 12kg of Brigade-12 surfactant, 238.6kg of p-nitroaniline, and 543kg of 30% hydrochloric acid in 7500L of water, beat for one hour, add ice to cool to 0--5°C, add 138kg of sodium nitrite solution, the solution concentration is 30 -40%, react at 0-5°C for 2-3 hours, add sulfamic acid after the reaction, and remove excess nitrous acid.

[0119] 2. Preparation of sulfonated meta-ester diazonium salt

[0120] Add 722kg of sulfonated meta-ester and 317kg of 30% hydrochloric acid to 7500L water, add ice to cool down to 0--5°C, add 138kg of sodium nitrite solution, the solution concentration is 30-40%, and react at 0--5°C for 4- -6 hours, after the reaction is complete, add sulfamic acid to remove excess nitrous acid. .

[0121] 3. One-step coupling

[0122] In the diazonium salt in step 2, add H acid directly, control the temperature at 10--15°C, and react for more than 6 hours. ...

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Abstract

The present invention relates to black active dyes and the preparation of the same, and 2,4-biaminobenzene sulfonic acid sodium, H acid, 2,3-bibromopropionyl chloride and dinitroaniline are used as the prime starting materials. Through the process of condensation reaction, diazo-reaction, coupling reaction and post treatment. When adding appropriate of red compositions or orange compositons, hight jet black active black product can be obtained, when using it can stain without adding any heave metals as the addtivites, it can replace the acid mordant black PV used for staining the cashmere and other worsted fabric, it also can be used for staining the fiber, such as cotton, silk, polyamide and so on. The method avoid the product of printing and dyeing wastewater containing heavy metal Cr6 + , and promote technological progress of printing and dyeing fields.

Description

technical field [0001] The invention relates to a reactive dye and a preparation method thereof, in particular to a black reactive dye used for dyeing fibers such as wool, cotton, silk and polyamide and a preparation method thereof. Background technique [0002] Acid dyes, acid mordant dyes, and metal complex dyes are generally used for dyeing wool textiles. Acid dyes have average dyeing fastness and damage to wool fibers, so they cannot be used for dyeing worsted wool fabrics. Although the fastness of acid mordant dyes and metal complex dyes has been improved, the shade is dull, and there is heavy metal Cr in dyeing. 6+ Existence, causing dyeing wastewater is difficult to treat. [0003] With the continuous development of the wool spinning industry, people have higher and higher requirements for the quality of wool textiles, and the comfort and safety of wool fabrics has become a new focus. Dark dyes, especially black dyes, have always been the bulk products of wool spin...

Claims

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Application Information

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IPC IPC(8): C07C245/08
CPCC07C309/50C09B62/513C09B67/004C09B33/10D06P1/382D06P3/148C09B62/475
Inventor 张克栋张兴华邢广文
Owner TIANJIN DEK CHEM
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