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Preparation method of composite reactive black dye

A technology of reactive black and dyes, which is applied in the field of preparation of composite reactive black dyes, can solve the problems of increasing the difficulty of color matching, low solid content of slurry, and high energy consumption, so as to save reaction time, dye shade and The effect of increasing yield and improving liquidity

Inactive Publication Date: 2019-04-19
ZHEJIANG JINGGUANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesizing monochromatic dyes separately not only takes up a lot of equipment and man-hours, but also has a relatively low solid content in the slurry, which requires a lot of energy consumption during spray drying, and increases the difficulty of color mixing when compounding into black dyes

Method used

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  • Preparation method of composite reactive black dye
  • Preparation method of composite reactive black dye
  • Preparation method of composite reactive black dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: preparation of raw material sulfomethyl J acid

[0042] Add 23.93g of 100% J acid into a 500mL four-necked flask, add 140mL of water to disperse evenly, raise the temperature to 40°C, adjust the pH to 6.3-6.5 with 30wt% liquid caustic soda until dissolved, continue to add 16g of sodium hydroxymethanesulfonate solid, mix After homogeneity, use soda ash dry powder to maintain pH 6-6.5, keep warm at 40°C and react for 4-5 hours until the acid reaction is completed. The reaction solution was concentrated and crystallized under reduced pressure, and dried to obtain a solid of sulfomethyl J acid with a yield of over 95%.

Embodiment 2

[0043] Embodiment 2: preparation of composite reactive black

[0044] (1) One condensation

[0045] Weigh 3.73g of cyanuric chloride and place it in a 500mL beaker in an ice bath at 0-3°C for beating for 30min. After the beating is completed, add 7.39g of sulfomethyl J acid dry powder and continue beating for 1h. Use a mixed alkali solution of soda ash and baking soda (soda ash The mass ratio to baking soda is 2:3), adjust and maintain the pH at 3.5-4, control the temperature at 3-8°C, and react for 2-3 hours until the end point is reached.

[0046] (2) para-ester diazo

[0047] Take by weighing 28.29g of para-ester percent (the mol ratio of para-ester and H acid is 1:0.385, and the mol ratio of para-ester and sulfomethyl J acid is 1:0.2) in a 1000mL beaker for beating in an ice bath, After beating, add technical amount of hydrochloric acid, stir for 5 minutes, continue to add technical amount of sodium nitrite, after 10-15 minutes, the pH is 1-1.3, keep warm at 2-5°C, and r...

Embodiment 3

[0052] Embodiment 3: preparation of composite reactive black

[0053] (1) One condensation

[0054] Weigh 2.8g of cyanuric chloride, place it in a 500mL beaker in an ice bath at 0-3°C for beating for 30min, and after the beating is completed, add 5.54g of sulfomethyl J acid dry powder to continue beating for 1h, using a mixed alkali solution of soda ash and baking soda (soda ash The mass ratio to baking soda is 2:3), adjust and maintain the pH at 3.5-4, control the temperature at 3-8°C, and react for 2-3 hours until the end point is reached.

[0055] (2) para-ester diazo

[0056] Take by weighing 28.02g of the para-ester equivalent (the mol ratio of the para-ester to the H acid is 1:0.413, and the mol ratio of the para-ester to the sulfomethyl acid is 1:0.147) and make a slurry in an ice bath in a 1000mL beaker, After beating, add technical amount of hydrochloric acid, stir for 5 minutes, continue to add technical amount of sodium nitrite, after 10-15 minutes, the pH is 1-1.3,...

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Abstract

The invention relates to a preparation method of a composite reactive black dye. The method comprises the steps that 1), 4-hydroxy-7-methylamino-2-naphthalenesulfonic acid is added to a cyanuric chloride beating solution, a mixed alkaline solution is added after beating, the solution is adjusted, the pH is maintained to be 3.5-4, and condensation reaction is conducted to obtain a first condensatesolution; 2), hydrochloric acid and a sodium nitrite solution is added to a para-ester beating solution to perform diazotization reaction to obtain a para-ester diazo solution; the mole ratio of the para-ester to H acid is 1:0.365-0.413, the mole ratio of the para-ester to the 4-hydroxy-7-methylamino-2-naphthalenesulfonic acid is 1:0.147-0.246, and the mole of the para-ester is higher than or equal to the total mole of two times of the H acid and one time of the 4-hydroxy-7-methylamino-2-naphthalenesulfonic acid; 3), the H acid is added to the para-ester diazo solution to perform acid coupledreaction to obtain an acid coupled solution; 4), the first condensate solution is added to the acid coupled reaction in step 3), sodium bicarbonate is added to adjust the pH to be 6-7 to perform alkaline coupled reaction to obtain the composite reactive black dye. The method has the advantages that the method is convenient, the occupied resource is less, the synthesis cost is low, and dye physicochemical parameters and application performance parameters are significantly improved.

Description

technical field [0001] The invention relates to the field of reactive dye preparation, in particular to a preparation method of composite reactive black dye. Background technique [0002] Reactive dyes are famous for their bright color, complete chromatogram, easy application, relatively low price, strong adaptability, and excellent fastness. Now they have developed into the most important dye category in cotton dyes, and have become a kind of dye that has been developed and paid attention to in the world. . Such dye molecules contain groups that can chemically react with cellulose fibers. When dyeing, the dyes react with cellulose fibers, and form a covalent bond between the two to fix them on the fabric, making the washing and rubbing fastness excellent. for other dyes. [0003] Because the orange component is bright and bright, the composite reactive black obtained after mixing with the navy blue component has excellent blackness, the dyeing temperature only needs to be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/513
Inventor 王国林赵强韩东
Owner ZHEJIANG JINGGUANG IND
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