Preparation method of water-soluble blue printing dye

A water-soluble, blue technology, which is applied in the direction of anthracene dyes, organic dyes, chemical instruments and methods, etc., can solve the problems of reduced performance of dye application, influence of dye application, difficulty of bromidine, etc., and achieve improvement of dye application performance and increase Catalyst efficiency, the effect of reducing the amount of catalyst

Active Publication Date: 2018-05-11
ZHEJIANG JINGGUANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The blue series of printing dyes are favored by the printing and dyeing industry because of their bright color and excellent color fastness. However, anthraquinone dyes have low solubility, and the synthetic shade is not bright enough. Heavy metals are needed as catalysts to promote the reaction in the color base preparation process. , and bromonic acid is difficult to react completely, and salting-out treatment is required for purification after synthesis, otherwise it will lead to reddish and darker shade, which will affect the application of dyes. Earth limit
[0003] Chinese invention patent application (CN 104559309 A) discloses a method for preparing blue reactive dyes. The chromophore preparation process uses copper sulfate and cuprous chloride as catalysts. The synthesized chromophore needs to be refined by salting out. After refining, a large amount of Hazardous wastewater containing heavy metals will cause great harm to water bodies and the atmosphere
A blue reactive dye prepared by Chinese invention patent application (CN 103602099A), using copper powder, copper sulfate and cuprous chloride as catalysts, the resulting chromogen is salted out, and finally mixed with cyanuric chloride and sulfamic acid ethanolamine The condensate of the ester is subjected to secondary condensation to obtain a reactive blue dye. Due to its strong activity, ethanolamine sulfamate is easily hydrolyzed into a hydroxyl structure or into an ethyl sulfone structure, which affects the color fixation rate and solubility of the dye, making the application performance of the dye reduce

Method used

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  • Preparation method of water-soluble blue printing dye
  • Preparation method of water-soluble blue printing dye
  • Preparation method of water-soluble blue printing dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of solid-supported copper catalyst (copper / hollow ceramic ball)

[0034] The hollow ceramic ball was immersed in a hydrochloric acid solution, magnetically stirred at room temperature for 11 hours, washed with deionized water to pH 7 several times, filtered with suction, dried at 155°C, and placed in a desiccator for activation. Put the hollow ceramic ball into a muffle furnace at 300°C for thermal activation for 2.5 hours, and put it in a desiccator to cool for use. Mix a certain amount of copper powder with acrylic acid, stir at 4°C for 8 hours, and finally add a certain amount of activated hollow ceramic balls, raise the temperature to 70°C, continue to stir for 10 hours, and finally put it into a muffle furnace for 300°C calcination 2 Within hours, the copper / hollow ceramic ball catalyst is obtained.

Embodiment 2

[0035] Example 2: Preparation of solid-supported cuprous chloride catalyst (cuprous chloride / hollow ceramic balls)

[0036] The hollow ceramic ball was immersed in a hydrochloric acid solution, magnetically stirred at room temperature for 11 hours, washed with deionized water to pH 7 several times, filtered with suction, dried at 155°C, and placed in a desiccator for activation. Put the hollow ceramic ball into a muffle furnace at 300°C for thermal activation for 2.5 hours, and put it in a desiccator to cool for use. Mix a certain amount of cuprous chloride with anhydrous methanol, add a certain amount of activated hollow ceramic balls, raise the temperature to about 50°C, stir for 5.5 hours, distill under reduced pressure to remove excess methanol, and finally put the catalyst in a muffle furnace at 210°C Calcined for 5 hours, the cuprous chloride / hollow ceramic ball catalyst is obtained.

Embodiment 3

[0038] 1) Blue base intermediate liquid

[0039] Add 100mL of water to a 500mL four-necked flask, add 45.86 grams of M acid, heat up to 60°C, add 30% of the process mass fraction of liquid caustic soda, adjust pH 9.0, M acid is completely dissolved; 38.2 grams of bromamine acid, stir evenly, add the technological amount of baking soda, control the pH to 8.0, heat up to 75°C, add 0.5 grams of solid-supported copper catalyst, and then divide into 4 times and add 0.5 grams of solid-loaded chlorine every 30 minutes. Cuprous oxide catalyst 2.0g, keep for 13 hours, make up 100mL of water, add diatomaceous earth and stir for 20 minutes, filter, continue to use hydrochloric acid to adjust the pH of the filtrate to 1.7, filter and recover M acid for the next batch of blue base synthesis, filtrate Adjust the pH to neutral with soda ash powder and set aside.

[0040] 2) Secondary condensation

[0041] Weigh 18.45 grams of cyanuric chloride and 0.2 grams of dispersant MF in a 1000mL beaker for...

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Abstract

The invention relates to a preparation method of a water-soluble blue printing dye. The method includes the following steps of 1, dissolving M acid in water, adding bromamine acid, controlling pH to main within 8.0-8.5, raising the temperature to 70-80 DEG C for conducting a first condensation reaction, and adding a solid-supported catalyst in batches during the condensation reaction, wherein themolar ratio of M acid to bromamine acid is (1.8-2.2):1; 2, after the first condensation reaction is completed, adding water and diatomaceous earth and conducting stirring and filtering, adjusting thepH of the filtrate to 1.5-2.0, conducting filtering again, and adjusting the pH of the filtrate to neutrality to obtain a blue-based intermediate liquid; 3, after cyanuric chloride is subjected to icebath, beating and dispersion, adding the blue-based intermediate liquid, controlling the temperature to main within 3-8 DEG C and the pH to more than 6.0, and conducting a second condensation reaction; 4, after the second condensation reaction is completed, adding a mixture of m-aminobenzenesulfonic acid and p-aminobenzenesulfonic acid, raising the temperature to 40-45 DEG C, maintaining the pH within 6.0-7.0, and conducting a third condensation reaction to obtain raw pulp of the blue dye. The method can solve the problem that a large amount of high-COD high-salt colored wastewater is produced by traditional salting-out refining methods.

Description

Technical field [0001] The invention belongs to the field of reactive dye synthesis, and specifically relates to a preparation method of water-soluble blue printing dye. Background technique [0002] There are many kinds of reactive printing dyes, complete chromatogram, simple printing process, convenient color paste preparation, and good printing effect. It is one of the most widely used dye categories. The blue series of printing dyes are favored by the printing and dyeing industry because of their bright color and excellent color fastness. However, the anthraquinone dyes have low solubility and the synthetic shades are not bright enough. Heavy metals are needed as catalysts to promote the reaction during the preparation of the color base. , And the bromamine acid is difficult to completely react. It needs to be purified by salting out after the synthesis is completed. Otherwise, the color light will become reddish and dark, which will affect the application of dyes. At the sam...

Claims

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Application Information

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IPC IPC(8): C09B1/48B01J27/122B01J35/10
CPCC09B1/48B01J27/122B01J35/61
Inventor 王国林赵强
Owner ZHEJIANG JINGGUANG IND
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