Preparation method of blue dye

A blue dye and product technology, applied in the direction of azo dyes, organic dyes, complex metal compounds of azo dyes, etc., can solve the problems of low coupling yield, large waste water, high COD waste water, etc., to reduce the content of COD , reduce environmental pollution, and stabilize the diazo product

Active Publication Date: 2012-06-27
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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AI Technical Summary

Problems solved by technology

[0007] However, the two-step complexation method in the prior art still has certain problems: the primary diazo protective agent uses naphthalenesulfonic acid, the coupling yield is low, and wastewater with higher COD is produced after pressure filtration
The first-stage complexation did not detect the first-stage coupling yield, and added a chromating agent that greatly exceeded the theoretical amount, resulting in a large waste of raw materials; after press filtration, waste water with high chromium content was produced, causing environmental pollution
In order to ensure product quality, the existing technology adopts multi-step filter press, which on the one hand produces a large amount of waste water with high salt content; on the other hand increases the intensity of manual labor and energy consumption

Method used

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preparation example Construction

[0042] The invention provides a kind of preparation method of the blue dye shown in formula I, comprising:

[0043] a) Mix 2-amino-5-nitrophenol, hydrochloric acid and nitrous solution in ice water, and carry out the first diazotization reaction to obtain the first diazonium product;

[0044] b) performing the first coupling reaction on the first diazonium product obtained in step a), butanone, and 1-naphthol-5-sulfonic acid solution to obtain the first coupling product;

[0045] c) mixing 2-amino-5-nitrophenol, hydrochloric acid, and sodium nitrite in an ice-water bath, using potassium iodide for color development, and performing a second diazotization reaction to obtain a second diazonium product;

[0046] d) mixing the alkaline solution of N,N-diethyl-m-hydroxyaniline with the second diazonium product, and performing the second coupling reaction to obtain the second coupling product;

[0047] e) mixing the first coupling product with basic chromium sulfate, salicylic acid, a...

Embodiment 1

[0090] a. Dissolution suction filtration of 1-naphthol-5-sulfonic acid and N,N-diethyl-m-hydroxyaniline

[0091] Add 2040L of water into the reaction kettle, adjust the temperature to 25°C, add 352.2Kg of 1-naphthol-5-sulfonic acid while stirring, stir for 40min until complete dissolution and suction filtration, and the filtrate drops to 10-15°C for later use.

[0092] Add water into the dissolving pot, start stirring, add 117Kg of liquid caustic soda, adjust the temperature to 65-70°C, turn on the vacuum to inhale the melted N,N-diethyl-m-hydroxyaniline, keep stirring for one hour, and suction and filter the whole solution . The filtrate will be stored at 10°C for later use.

[0093] b. Once diazotization

[0094] Add 680L water, 235.62Kg 2-amino-5-nitrophenol into the L reactor, adjust pH=12.5-13 with liquid caustic soda, stir to dissolve completely, add 153Kg hydrochloric acid, cool down to 0-5°C, at this temperature, It takes 30 minutes to add 105.4Kg of nitrous solutio...

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Abstract

The invention relates to a preparation method of a blue dye. The preparation method provided by the invention comprises two times of diazotization reactions; a first diazotization product is mixed with a 1-naphthol-5-sulfonic acid solution and butanone, such that first coupling is carried out; a second diazotization product is subject to a reaction with N,N-diethyl-m-aminophenol, such that a second coupling product is obtained; the first coupling product is subject to a complexation reaction with a chromising reagent, such that a first complexation product is obtained; the first complexation product is mixed with the second coupling product, such that a second complexation reaction is carried out, and the asymmetric 1:2 blue dye represented by a formula I is obtained. According to the preparation method provided by the invention, butanone is used as a protecting agent for the diazotization product in the first coupling reaction, such that the diazotization product is more stable, the reaction between the diazotization product and 1-naphthol-5-sulfonic acid is more sufficient, the yield of the first coupling product is improved, and COD content in sewage is reduced. The formula I is presented below.

Description

technical field [0001] The invention relates to the technical field of fabric dyeing and finishing, in particular to a preparation method of blue dye. Background technique [0002] Acid Dyes are a class of dyes that are dyed in acidic medium. Most acid dyes are soluble in water, bright in color and complete in color spectrum. It is mainly used for dyeing wool, silk and nylon, and can also be used for leather, paper, ink, etc. Generally, it has no coloring power to cellulose fibers. Among acid dyes, acid complex dyes have the most excellent properties and are widely used. Acid complex dyes are formed by complexing acid dyes with metals such as chromium and cobalt. Soluble in water, its dyed products are light-fast and light-fast. Its dye matrix is ​​similar to acid mordant dyes, but metal atoms have been introduced into azo dye molecules during the preparation of dyes. The ratio of metal atoms to dye molecules is 1:1, so it is also called 1:1 metal complex dyes. There i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B45/00
Inventor 杨伦花逄环民刘方先
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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