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Method for preparing anilines diazosalt solid powder

A technology for aniline compounds and diazonium salts, applied in the field of intermediate preparation of synthetic dyes, can solve problems such as product quality decline, decomposition and explosion, production process danger, etc., achieve good stability, avoid explosion danger, and solve product quality problems falling effect

Inactive Publication Date: 2009-12-30
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The diazonium salt of aniline compound is easily soluble in water, even in the presence of a large amount of sulfuric acid, it is difficult to separate from water, and after the diazonium salt loses water and is dried, due to its strong activity, it is easy to cause decomposition and explosion, which will affect the production process. pose a hazard or cause a decrease in product quality

Method used

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  • Method for preparing anilines diazosalt solid powder
  • Method for preparing anilines diazosalt solid powder
  • Method for preparing anilines diazosalt solid powder

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Diazotization: Take 135.3g of anhydrous sulfuric acid and slowly add dried NaNO at a temperature of 25°C 2 11.2g, reacted at 80°C for 2 hours. Cool down to below 40°C, then add 28g of 2,4-dinitroaniline with a content of 98% at 40°C, react for 6 hours, cool down to 10°C, dilute into ice-water mixture, control the temperature to ≤0°C, and obtain 2, 4-Dinitroaniline diazonium sulfuric acid aqueous solution.

[0033] (2) Crystallization: In 2,4-dinitroaniline diazonium salt sulfuric acid aqueous solution, add 50g of benzenesulfonic acid, stir and precipitate for more than 2 hours, filter to get 2,4-dinitroaniline diazonium salt filter cake , to dry.

[0034] (3) Drying: Dry the filter cake of 2,4-dinitroaniline diazonium salt at about 80°C to obtain powdery 2,4-dinitroaniline diazonium salt, that is, the weight of 2,4-dinitroaniline Nitrogen salt solid powder.

Embodiment 2

[0036] (1) Diazotization: take 93.7g of 98% sulfuric acid, and mix it with 41.6g containing SO under cooling 3 20% oleum was mixed to make 135.3g of anhydrous sulfuric acid. In the anhydrous sulfuric acid, slowly add dried NaNO at a temperature ≤30°C 2 11.2g, reacted at 60°C for 3 hours. Cool down to below 40°C, then add 32g of 6-bromo-2,4-dinitroaniline with a content of 98% at 45°C, react for 8 hours, cool down to below 15°C, dilute into ice-water mixture, control temperature ≤ 0 °C to obtain 6-bromo-2,4-dinitroaniline diazonium sulfuric acid aqueous solution.

[0037] (2) crystallization: in 6-bromo-2,4-dinitroaniline diazonium sulfuric acid aqueous solution, add 35g of 1,5-naphthalene disulfonic acid and 15g sodium dodecylsulfonate, stir and separate out 2 After more than 1 hour, filter cake of diazonium salt of 6-bromo-2,4-dinitroaniline to be dried.

[0038] (3) Drying: Dry the filter cake of 6-bromo-2,4-dinitroaniline diazonium salt at 80°C to obtain powdery 6-bromo...

Embodiment 3

[0040] (1) Diazotization: take 93.7g of 98% sulfuric acid, and mix it with 41.6g containing SO under cooling 3 20% oleum was mixed to make 135.3g of anhydrous sulfuric acid. In the anhydrous sulfuric acid, slowly add dried NaNO at a temperature ≤30°C 2 11.2g, reacted at 70°C for 2 hours. Cool down to below 40°C, then add 20g of aniline with a content of 98% at 35°C, react for 8 hours, cool down to below 15°C, dilute into ice-water mixture, and control the temperature to ≤0°C to obtain aniline diazonium sulfuric acid aqueous solution.

[0041] (2) Crystallization: Add 40 g of anthraquinone-2,5-disulfonic acid to the aqueous solution of aniline diazonium salt sulfuric acid, stir and precipitate for more than 2 hours. Filter cake of 2,4-dinitroaniline diazonium salt and wait for drying.

[0042] (3) Drying: the aniline diazonium salt filter cake is dried below 80° C. to obtain powdery aniline diazonium salt, that is, aniline diazonium salt solid powder.

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Abstract

The invention provides a method for preparing anilines diazosalt solid powder, comprising the following steps: (1) diazotization: dry NaNO2 is slowly added into anhydrous sulfuric acid, and the anilines are added into the mixture, when the reaction is completed, temperature is lowered, the obtained mixture is diluted into ice water mixture to obtain sulfuric acid solution of anilines diazosalt; (2) separation by crystallization: anion organic compounds are added into the sulfuric acid solution of anilines diazosalt and then is stirred for separation by crystallization, after being filtered, the filter cake of aniline diazosalt is obtained; and (3) drying: the filter cake of aniline diazosalt is dried to obtain powdery aniline diazosalt, namely, anilines diazosalt solid powder.

Description

technical field [0001] The invention belongs to the field of intermediate preparation of synthetic dyes, in particular to a method for preparing aniline compound diazonium salt solid powder. The diazonium salt is mainly used for synthesizing azo dyes. Background technique [0002] When synthesizing azo dyes, the problem of diazotization of aniline compounds, such as C.I. Reactive Black 52, is often encountered. The diazotization of aniline compounds is often carried out in concentrated sulfuric acid, so that after the coupling reaction, a large amount of sulfates will be produced. These sulfates will reduce the solubility of dyes, and will also affect the dyeing rate and color fastness of dyed protein fibers. And make it lower, so if most of the sulfuric acid in the aniline compound diazonium salt can be removed, it is very beneficial to the synthesis of dyes. The diazonium salt of aniline compound is easily soluble in water, even in the presence of a large amount of sulfur...

Claims

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Application Information

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IPC IPC(8): C07C245/20
Inventor 张兴华邢广文
Owner TIANJIN DEK CHEM
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