Monoazo lake pigment and preparation method thereof

A technology of lake pigments and monoazo, applied in the directions of monoazo dyes, azo dyes, lakes, etc., can solve the problem of no economical method, and achieve the effect of reducing residual amount, reducing treatment difficulty and economic cost.

Active Publication Date: 2021-02-05
瑞素士化学(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of reaction solution containing sodium chloride or sodium bisulfat

Method used

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  • Monoazo lake pigment and preparation method thereof
  • Monoazo lake pigment and preparation method thereof
  • Monoazo lake pigment and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0044] Example 1

[0045] The first step, the diazotization reaction of aromatic primary amine sulfonic acid

[0046] P-aminobenzenesulfonic acid (industrial product, Hebei Jianxin Chemical Co., Ltd., 17.4g, 0.1mol) was mixed with water (800ml) and stirred until the solid was completely dissolved to obtain an aqueous solution of p-aminobenzenesulfonic acid (pH=1-2 ) and cooled with an ice / water bath to reduce the temperature of the solution to <10°C. Under stirring, slowly add 40% nitrosyl sulfuric acid (industrial product, 40% sulfuric acid solution, Zhejiang Sanmen Jieshi Chemical Co., Ltd., 33g, 0.105mol) into the above solution, about 30min, during which the temperature is controlled <10°C, After adding, continue stirring for 20min to obtain a water turbid solution of p-aminobenzenesulfonic acid diazonium salt, pH=1, and the starch-potassium iodide test paper detects a slight excess of nitrous acid.

[0047] The second step, the preparation of barbituric acid coupling so...

Example Embodiment

[0055] Example 2

[0056] The first to third steps are the same as those in Example 1.

[0057] The fourth step, lake reaction

[0058] After the third step of the reaction, directly heat the reactant to 60°C and keep it for 1 hour to obtain a transparent and clear solution, adjust pH=5-6 with 10% KOH, and add CaCl dropwise. 2 (industrial product, 11.3 g, 0.1 mol) aqueous solution, after the dropwise addition was completed, the heating was stopped, naturally cooled, and allowed to stand overnight. The precipitated filter cake was filtered, washed with water until neutral, and dried at 120° C. to obtain 33.2 g of a bright bright yellow solid, which was the monoazo lake pigment I-1-1.

Example Embodiment

[0059] Example 3

[0060] The first step, the diazotization reaction of aromatic primary amine sulfonic acid

[0061] Tosate's acid (industrial product, Inner Mongolia Xinya Chemical Co., Ltd., 22.7g, 0.1mol) was mixed with water (600ml), heated to 50° C. under stirring, and 10% KOH solution was added dropwise until the solid was completely dissolved to obtain toss acid. The aqueous solution of potassium salt is naturally cooled to room temperature, adjusted to pH=1-2 with sulfuric acid, and the turbid acid is precipitated from the water to form a cloudy liquid, and the temperature of the cloudy liquid is reduced to <10°C with an ice / water bath. Under stirring, slowly dropwise add 40% nitrosyl sulfuric acid (industrial product, 40% sulfuric acid solution, 33 g, 0.105 mol) into the above solution, about 30 min, during which the temperature is controlled <10 ° C, and after the addition, continue to stir for 20 min to obtain a spit. Diazonium salt of uric acid (turbid liquid, li...

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Abstract

The invention discloses a monoazo lake pigment. The structural general formula of the monoazo lake pigment is one of the structures described in the description: M is one of Ca, Ba and Sr; R is H, OH,NO2, Cl, Br or C1 to C4 alkyl, and n is a positive integer from 1 to 3; and Ar is described in the description. According to the preparation method of the monoazo lake pigment, sodium chloride or sodium hydrogen sulfate/sodium sulfate can be prevented from being generated in the process of preparing the aromatic primary amine diazonium salt. Meanwhile, in the coupling reaction process, alkali containing a sodium element is not adopted, generation of inorganic sodium salt can be avoided in the manufacturing process of the monoazo lake pigment, and conditions are provided for clean treatment and comprehensive utilization of coupling reaction liquid.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a structure of a monoazo lake pigment and a preparation method thereof. Background technique [0002] The precursor of monoazo lake pigment is monoazo acid dye, which contains at least one sulfonic acid or sodium sulfonate group in its molecule, so it is water-soluble. The monoazo lake pigment is insoluble in water because it converts the sulfonic acid or sodium sulfonate group in the monoazo acid dye into a group such as calcium sulfonate or barium sulfonate. [0003] The coupling components used in existing monoazoic acid dyes are mainly aromatic amines, phenols, pyrazolones or pyridones. They are coupled with the diazonium salts of various aromatic primary amines, and the obtained reaction products are water-soluble. In order to obtain solid state dyes, the method of salting out is often used. Restricted by solubility, some dyes must not be precipitated fr...

Claims

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Application Information

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IPC IPC(8): C09B63/00C09B29/00C07D239/62
CPCC09B63/00C09B29/0007C07D239/62
Inventor 沈永嘉沈珺沈倩
Owner 瑞素士化学(上海)有限公司
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