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Preparation method of yellow complex dye

A complexing and dyeing technology, which is applied in the field of preparation of yellow complexing dyes, can solve problems such as poor solubility, difficult to handle organic matter, and difficult to control the end point, so as to save production costs, reduce environmental burdens, and improve separation effects.

Inactive Publication Date: 2017-06-09
HENGSHENG CHEM QIDONG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although relatively cheap chromium formate or chromium acetate is used in the production process of this process, such complexing agents must be under acidic conditions for further complexation reactions. At the same time, the product shown in formula I has no hydrophilicity in the structural formula group, the final product generated under acidic conditions has poor solubility in the water phase, and it is also easy to wrap a small amount of compound of formula II, the end point is not easy to control, the performance and conversion rate of the product are unstable, and the final commercial product has a solubility of 5~ 25g / L(90℃)
Due to the relatively poor solubility, a large amount of dispersant is required to improve the solubility, which further makes it difficult to provide high-quality products
Moreover, since the complexing agent uses formic acid or acetic acid as a carrier, a large amount of untreatable organic matter will remain in the filtrate after separation, which brings serious problems to the subsequent sewage treatment.

Method used

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  • Preparation method of yellow complex dye

Examples

Experimental program
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Effect test

Embodiment 1

[0017] (1) In the diazo reactor, add 28kg 2-aminobenzoic acid, 60kg hydrochloric acid, 500kg ice water and stir evenly, then add dropwise 55kg of sodium nitrite aqueous solution with a mass concentration of 27%, and react at 10~15°C to obtain a weight Nitrogen solution;

[0018] (2) Add 2000kg of ice water, 37kg of 1-phenyl-3-methyl-5-pyrazolone into the coupling reaction kettle, add 58kg of liquid caustic soda, stir and dissolve completely, and slowly add the above-mentioned Diazo solution, at the same time use liquid caustic soda, control pH = 5.5~6.0, after the reaction reaches the end point, raise the temperature to 70~75°C for crystallization, after the coupling system has gone through the process of changing from thick to thin, keep it warm for another 2 hours, cool down and press the material, Squeeze dry to get coupling filter cake;

[0019] (3) In the chromium salicylate reaction kettle, add 180kg water, 53kg chromium alum, 32kg salicylic acid, after heating up, add ...

Embodiment 2

[0023] (1) In the diazo reactor, add 28kg 2-aminobenzoic acid, 60kg hydrochloric acid, 500kg ice water and stir evenly, then add dropwise 55kg of sodium nitrite aqueous solution with a mass concentration of 27%, and react at 10~15°C to obtain a weight Nitrogen solution;

[0024] (2) Add the above-mentioned diazonium salt into the coupling reaction kettle, add 500kg of ice, and slowly add 1000kg of water, 37kg of 1-phenyl-3-methyl-5-pyrazolone, 58kg of liquid caustic soda Use liquid caustic soda to control the pH=6.0~6.5 of the prepared solution. After the reaction reaches the end point, raise the temperature to 70~75°C for crystallization. Dry to obtain a coupling filter cake;

[0025] (3) In the chromium salicylate reaction kettle, add 180kg water, 53kg chromium alum, 32kg salicylic acid, after heating up, add 75kg liquid caustic soda, filter to obtain chromium salicylate aqueous solution for subsequent use;

[0026] (4) Add the above-mentioned chromium salicylate aqueous s...

Embodiment 3

[0029] (1) In the diazo reactor, add 28kg 2-aminobenzoic acid, 60kg hydrochloric acid, 500kg ice water and stir evenly, then add dropwise 55kg of sodium nitrite aqueous solution with a mass concentration of 27%, and react at 10~15°C to obtain a weight Nitrogen solution;

[0030] (2) Add 2000kg of ice water, 37kg of 1-phenyl-3-methyl-5-pyrazolone into the coupling reaction kettle, add 58kg of liquid caustic soda, stir and dissolve completely, and slowly add the above-mentioned Diazo solution, at the same time use liquid caustic soda, control pH = 5.5~6.0, after the reaction reaches the end point, raise the temperature to 70~75°C for crystallization, after the coupling system has gone through the process of changing from thick to thin, keep it warm for another 2 hours, cool down and press the material, Squeeze dry to get coupling filter cake;

[0031] (3) In the chromium salicylate reaction kettle, add 150kg water, 53kg chromium alum, 4kg salicylic acid, a batch of recycled sal...

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Abstract

The invention discloses a preparation method of yellow complex dye shown by formula I. The preparation method comprises the following steps: (1) reacting a diazonium salt aqueous solution of 2-aminobenzoic acid with an aqueous solution of 1-phenyl-3-methyl-5-pyrazolone for 1-3 hours when a pH is 5.5-6.5; and transforming crystal and filtering to obtain a coupled filter cake of a compound shown by formula II; (2) adding the coupled filter cake of the compound shown by formula II into an aqueous solution of chromium salicylate, controlling the pH to 7.0-9.0, and reacting for 24-72 hours at 110-130 DEG C; and when the reaction ends, cooling and filtering to obtain a wet material of a compound shown by formula I; and (3) adding water into the wet material of the compound shown by formula I, dispersing at a high speed by an emulsifying machine, and performing fine grinding by a ball mill; and adding a dispersing agent, dispersing uniformly and drying to obtain a finished product of the compound shown by formula I. The preparation method is economical and feasible, the application performance is similar, and the finished product has more stable dissolubility and higher quality.

Description

technical field [0001] The invention relates to the technical field of dye preparation, in particular to a preparation method of a yellow complex dye. Background technique [0002] The traditional preparation method of the yellow complex dye shown in formula I is that the compound of formula II carries out complex reaction with chromium formate or chromium acetate in aqueous phase, then mixes with MF dispersant and sand grinding beads, and sands for 24 hours. After settling, take the upper dispersion liquid, dry it, and standardize to obtain the corresponding dye product. Although relatively cheap chromium formate or chromium acetate is used in the production process of this process, such complexing agents must be under acidic conditions for further complexation reactions. At the same time, the product shown in formula I has no hydrophilicity in the structural formula group, the final product generated under acidic conditions has poor solubility in the water phase, and it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B45/01C09B45/22C09B67/36
CPCC09B45/01C09B67/0079C09B67/0084
Inventor 谢迎伟陈爱巍马徐阳
Owner HENGSHENG CHEM QIDONG
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