Preparation method for producing disperse orange by salt-free diazotization method and high-temperature coupling method

A diazo method and disperse orange technology, applied in chemical instruments and methods, azo dyes, monoazo dyes, etc., can solve problems such as inability to divert waste water, backward dye production technology, and failure to recycle waste water. Achieve the effect of reducing the amount of ice, reducing labor intensity and improving the reaction conversion rate

Inactive Publication Date: 2013-05-01
JIANGSU YUANZHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The defect of this method is: original production process, product intensity is low, yield is low, the waste water discharge (COD) of unit commodity is high; Waste water treatment is simpler, waste water fails to recycle, also can not accomplish waste water diversion; Dyestuff synthetic adopts manual Control, visually observe the reaction end point, there are batch-to-batch quality differences and yield fluctuations; the dye production process is backward, the diazo reagent uses sodium nitrite, and the coupling must be reacted below 2°C, so that the salt concentration of the dye wastewater is very high, and the coupling refrigeration energy consumes a lot

Method used

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  • Preparation method for producing disperse orange by salt-free diazotization method and high-temperature coupling method
  • Preparation method for producing disperse orange by salt-free diazotization method and high-temperature coupling method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1, a kind of preparation method of salt-free diazonium method and high temperature coupling method produces disperse orange, and its steps are as follows:

[0028] (1) Diazotization: Put nitrosyl sulfuric acid in the reaction pot, wait until the temperature drops to 20°C, start to add 2,6-dichloro-4-nitroaniline, control the feeding temperature at 25°C, and add naturally Raise the temperature to 30°C, maintain the reaction at this temperature for 5 hours, check whether the diazotization is complete (diazo solution and freezing point test), and wait for coupling after the heat preservation; the nitrosyl sulfuric acid (100%), 2,6 - The weight ratio of dichloro-4-nitroaniline is 0.59:1, and the mass content of nitrosyl sulfuric acid is 25%.

[0029] (2) Coupling: Add 5 tons of mother liquor water, pour in diazonium solution under stirring, 1.0 hour, after finishing, control the temperature at -5°C, add esterification solution (N-cyanoethyl-N-acetoxyethyl) dropwi...

Embodiment 2

[0030] Embodiment 2, a kind of preparation method of salt-free diazonium method and high-temperature coupling method producing disperse orange, its steps are as follows:

[0031] (1) Diazotization: Put nitrosyl sulfuric acid in the reaction pot, wait until the temperature drops to 15°C, start to add 2,6-dichloro-4-nitroaniline, control the feeding temperature at 15°C, and add naturally Raise the temperature to 35°C, maintain the reaction at this temperature for 7 hours, check whether the diazotization is complete (diazo solution and freezing point test), and wait for coupling after the heat preservation is completed. The weight ratio of the nitrosyl sulfuric acid (100%) to 2,6-dichloro-4-nitroaniline is 0.64:1, and the mass content of the nitrosyl sulfuric acid is 40%.

[0032] (2) Coupling: Pour in 15 tons of mother liquor water, pour in diazonium solution under stirring, about 2.5 hours, after finishing, control the temperature at 5°C, add esterification solution (N-cyanoeth...

Embodiment 3

[0033] Embodiment 3, a kind of preparation method of salt-free diazonium method and high-temperature coupling method producing disperse orange, its steps are as follows:

[0034] (1) Diazotization: Put nitrosyl sulfuric acid in the reaction pot, wait until the temperature drops to 30°C, start to add 2,6-dichloro-4-nitroaniline, control the feeding temperature at 30°C, and add naturally Raise the temperature to 35°C, maintain the reaction at this temperature for 6 hours, check whether the diazotization is complete (diazo solution and freezing point test), and wait for coupling after the heat preservation is completed. The weight ratio of the nitrosyl sulfuric acid (100%) to 2,6-dichloro-4-nitroaniline is 0.62:1, and the mass content of the nitrosyl sulfuric acid is 30%;

[0035] (2) Coupling: Pour in 10 tons of mother liquor water, pour in diazonium solution under stirring, about 1.5 hours, after finishing, control the temperature at 0°C, add esterification solution (N-cyanoeth...

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Abstract

The invention relates to a preparation method for producing disperse orange by a salt-free diazotization method and a high-temperature coupling method, which includes the steps of diazotization, coupling and the like. In the step of diazotization, nitrosylsulfuric acid is utilized, and the salt-free diazotization method and a high-temperature diazotization method are adopted; in the step of coupling, mother liquor with certain acidity is adopted as diazo thinner, the solid content is increased by esterifying liquid, acetic acid is recovered, a stage-by-stage dripping method is adopted, washing water is utilized for material precipitation, and after filter pressing, washing and drying, the finished disperse orange is obtained. The process of the method is more reasonable, the mother liquor can be recycled, the product yield is effectively increased, the production cost is reduced, and the discharge of waste water (COD) is reduced.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to a preparation method for producing disperse orange by a salt-free diazonium method and a high-temperature coupling method. Background technique [0002] Disperse Orange 30 is a dye with a relatively large variety in the disperse dye orange series, and it can match colors with Disperse Ruby 2GFL and Disperse Navy Blue S-2GL (or Disperse Blue BGL). Light fastness, sweat resistance, rubbing (color) fastness is good, soap fastness is average. It is mainly used in the printing and dyeing of polyester and its blended fabrics, and also in the dyeing of acetate fibers. Its traditional process route is obtained by diazotizing 2,6-dichloro-4-nitroaniline with sodium nitrite and coupling reaction with N-cyanoethyl-N-acetoxyethylaniline. [0003] The defect of this method is: original production process, product intensity is low, yield is low, the waste water discharge (COD) of unit commod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/085C09B29/01
Inventor 王海民韩军彭炫杨洋
Owner JIANGSU YUANZHENG CHEM
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