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Process for synthesizing azo dispersion dyes monomer compound

A technology of disperse dyes and synthesis process, which is applied in the direction of azo dyes, monoazo dyes, organic dyes, etc. It can solve the problems of increasing costs, waste of industrial resources, affecting the yield and quality of dyes, and achieves the effect of cost reduction

Inactive Publication Date: 2008-02-06
SHANGYU JINGUAN CHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Coupling is an important reaction process in the production of azo dyes. The coupling reaction is generally an exothermic reaction. Increasing the temperature can increase the coupling reaction speed, but as the temperature increases, the decomposition speed of the diazonium salt tends to be faster, and tar-like The by-products affect the yield and quality of dyes. Therefore, it has become common knowledge in the industry that the coupling is usually carried out below 10°C. description of steps
[0003] Since the coupling temperature of azo disperse dyes usually needs to be controlled at around 0°C, or below 10°C, and it is an exothermic reaction, it is customary to add a large amount of ice cubes to the coupling reactor or pass it into a freezer. Cooling media such as brine to cool down to meet the process requirements not only increases the cost, but also causes a waste of industrial resources

Method used

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  • Process for synthesizing azo dispersion dyes monomer compound
  • Process for synthesizing azo dispersion dyes monomer compound
  • Process for synthesizing azo dispersion dyes monomer compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 100g of 98% sulfuric acid and 65.4g of 40% nitrosylsulfuric acid (liquid sulfide) were dropped into the three-necked flask successively, and the temperature was lowered with stirring; After adding for 2 hours, after keeping warm for 5-10 hours, use a glass rod to dip a few drops of diazonium solution into ice water. The ice water is clear and the potassium iodide test paper is blue, depending on the end of the reaction, let it stand for later use.

[0022] Put 1000ml of water in a 2000ml beaker, control the temperature of the bottom water at 18-28°C, add 3g of Pingpingjia O-25 and 3g of sulfamic acid, and stir for 1 hour to completely dissolve the Pingpingjia O-25; control the temperature of the bottom water At 18-28°C, quickly put 46.4g of yellow palm esterification solution (N-cyanoethyl-N-acetoxyethylaniline) in a reduced amount, and then beat for about 30 minutes under the condition of 18-28°C; After coupling and beating, slowly add the diazo dilution solution into ...

Embodiment 2

[0025] Put 100g of 98% sulfuric acid and 65.4g of 40% nitrosylsulfuric acid into the three-necked flask successively, stir and cool down; slowly put in 41.4g of 2,6-dichloro-p-nitroaniline at 20-30°C, and finish adding in about 2 hours , after 5-10 hours of heat preservation, check the clarity and the end point; when the end point is reached, let it stand for later use.

[0026] Add 1000ml of bottom water to a 2000ml beaker, add 3g of Pingpingjia and 34.8g of N-ethyl-N-cyanoethylaniline, beat for about 2 hours below 15°C, add sulfamic acid, drop the temperature below 20°C and add diazonium solution , about 30 minutes or so added, the temperature of the diazo addition process need not be controlled. After reacting for 10 hours, detect the end point, filter and wash with water until neutral. The dye monomer of formula (I-2) can be prepared.

[0027]

Embodiment 3

[0029] Put 100g of 98% sulfuric acid and 65.4g of 40% nitrosylsulfuric acid into the three-necked flask successively, stir and cool down; slowly put in 59.2g of 2,6-dibromo-p-nitroaniline at 20-30°C, and finish adding in about 2 hours , after 5-10 hours of heat preservation, check the clarity and the end point; when the end point is reached, let it stand for later use.

[0030] Add 1000ml of bottom water to a 2000ml beaker, add 3g of Pingpingjia and 34.8g of N-ethyl-N-cyanoethylaniline, beat for about 2 hours below 15°C, add sulfamic acid, drop the temperature below 20°C and add diazonium solution , about 30 minutes or so added, the temperature of the diazo addition process need not be controlled. After reacting for 10 hours, detect the end point, filter and wash with water until neutral. The dye monomer of formula (I-3) can be obtained.

[0031]

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Abstract

The invention provides the synthesis process of an azo-disperse dyes monomeric compound, comprising the following steps: (1) diazotization of compound (II) and nitrosyl sulfuric acid is completed with the temperature being controlled between 1 DEG C and 25 DEG C; (2) water, emulsifying agent and compound (III) are added into a coupling reactor and stirring and pulping are completed at the temperature ranging from 10 DEG C to 25 DEG C; (3) diazonium salt is evenly added into the coupling reactor from below the slurry and is stirred till the end of the reaction, and then extraction filtration and washing are adopted till the slurry shows neutrality; finally, the azo-disperse dyes monomeric compound can be obtained after drying. Through improving preparation process, a great amount of ice or frozen salt water no longer needs to be added for cooling down during coupling reaction to meet the requirements; the temperature of coupling reaction is gradually raised to 20 DEG C to 45 DEG C by use of heat liberation of coupling reaction and diazonium salt dilution instead; thereby, under the condition of identical quality effect, cost is greatly reduced and at the same time, energy consumption during preparing cooling agent such as ice and frozen salt water is also substantially reduced.

Description

(1) Technical field [0001] The invention relates to a synthesis process of an azo disperse dye monomer compound. (2) Background technology [0002] Coupling is an important reaction process in the production of azo dyes. The coupling reaction is generally an exothermic reaction. Increasing the temperature can increase the coupling reaction rate, but as the temperature increases, the decomposition rate of the diazonium salt tends to be faster, and tar-like The by-products of dyes affect the yield and quality of dyes. Therefore, it has become common knowledge in the industry that the coupling is usually carried out below 10°C. A description of the step. [0003] Since the coupling temperature of azo disperse dyes usually needs to be controlled at about 0°C or below 10°C, and it is an exothermic reaction, the usual practice is to add a large amount of ice cubes to the coupling reaction kettle or pass it into a freezer. Cooling media such as brine to cool down to meet the proc...

Claims

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Application Information

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IPC IPC(8): C09B29/00
Inventor 阮伟祥欧其高怀庆钟玉霞
Owner SHANGYU JINGUAN CHEM IND
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