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Method for synthesizing reactive yellow DF 3RS

A technology of DF-3RS and synthesis method, which is applied in the field of chemical synthesis of dyes, can solve problems such as increasing costs, achieve the effects of reducing raw material costs, eliminating sewage discharge, and improving product yield

Inactive Publication Date: 2007-05-09
泰州市姜堰区东风染料化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the existing active yellow DF-3RS synthesis method, it is very easy to generate waste water, especially in the salting out step, it is necessary to add a large amount of chloride to the reaction, which not only increases the cost, but also discharges a large amount of sewage into the environment

Method used

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  • Method for synthesizing reactive yellow DF 3RS
  • Method for synthesizing reactive yellow DF 3RS
  • Method for synthesizing reactive yellow DF 3RS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The synthetic method of reactive yellow DF-3RS of the present invention operates as follows:

[0054] A. Diazo:

[0055] Put 2000L of bottom water, weigh 299kg of 2-naphthylamine-3,6,8-trisulfonic acid, put into beating for 1.5h, add ice, add HCl 28.5kg, temperature T=5℃, add NaNO 2 After adding the solution, keep the KI test paper microscopic blue, and react for 2 hours.

[0056] B. Coupling:

[0057] Put 400L of ice water, throw in 117.8kg of ureidoaniline, beat for 1 hour, add 80kg of NaCO 3 Stir for 10 minutes, put the diazonium solution in step A into the coupling barrel, keep the pH=4, the temperature is 6°C, react for 3h, then adjust the pH=9.5 with soda water, and react for 1.2h to reach the end point.

[0058] C. One condensation:

[0059] Put 200L of bottom water, add ice and put 150kg of cyanuric chloride into ice grinder for beating for 1 hour at 0°C, add the coupling liquid in Step B that has reached the end point into the cyanuric chloride suspe...

Embodiment 2

[0067] A. Diazo:

[0068] Put 2000L of bottom water, weigh 284.1kg of 2-naphthylamine-3,6,8-trisulfonic acid, put it into beating for 2h, add ice, add HCl 29.9kg, temperature T=5℃, add NaNO 2solution, equivalent to NaNO 2 56.5kg, after adding, keep the KI test paper micro-blue, and react for 1h.

[0069] B. Coupling:

[0070] Put 400L of bottom water, throw in 123.7kg of ureidoaniline, beat for 1 hour, add 80kg of NaCO 3 Stir for 10 minutes, put the diazonium solution in step A into the coupling barrel, keep the pH=4, temperature 6°C, react for 1h, then adjust the pH=9 with aqueous sodium carbonate solution, and react for 1h to reach the end point.

[0071] C. One condensation:

[0072] Put 200L of bottom water, add ice and put 156.4kg of cyanuric chloride into ice grinder for beating at 0°C for 1 hour, add the coupling solution in Step B that has reached the end point into the cyanuric chloride suspension within 1 hour, and use soda ash after the addition is completed. A...

Embodiment 3

[0080] A. Diazo:

[0081] Put 2000L of bottom water, weigh 314.0kg of 2-naphthylamine-3,6,8-trisulfonic acid, put it into beating for 1.5h, add ice, add HCl27.1kg, temperature T=5℃, add NaNO 2 solution, equivalent to NaNO 2 51.1kg, after adding, keep KI test paper microscopic blue, and react for 4h.

[0082] B. Coupling:

[0083] Put 400L of bottom water, throw in 111.9kg of ureidoaniline, beat for 1 hour, add 80kg of NaCO 3 Stir for 10 minutes, put the diazonium solution in step A into the coupling barrel, keep the pH=4.5, temperature 7°C, react for 5h, then adjust the pH=10 with aqueous sodium carbonate solution, and react for 1.5h to reach the end point.

[0084] C. One condensation:

[0085] Put 200L of bottom water, add appropriate amount of ice, put 142.0kg of cyanuric chloride into ice grinder for beating at 0°C for 1 hour, add the coupling solution in Step B that has reached the end point into the cyanuric chloride suspension within 1 hour, and add it in about 1 ho...

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Abstract

This invention discloses a method for synthesizing active yellow DF-3RS. The method comprises: (1) pulping 2-naphthylamine-3,6,8-trisulfonic acid, adding HCl and NaNO2, and reacting to obtain diazo salt; (2) pulping m-ureido-naphthylamine, adding NaHCO3 and the above diazo salt, and reacting to obtain a coupling compound; (3) adding the coupling compound into pulped cyanuric chloride suspension, and reacting to obtain a first condensate; (4) adding sulfate ethylsulfone naphthylamine, reacting, removing inorganic salts with an ionic membrane, and spray-drying to obtain yellow DF-3RS. The method can reduce the deterioration of the environment, and raise the product yield.

Description

technical field [0001] The invention relates to a chemical synthesis method of a dye, in particular to a preparation method of reactive yellow DF-3RS. Background technique [0002] The synthesized DF-3RS of the present invention has the following characteristics: [0003] 1. Excellent reactivity, energy saving; [0004] 2. Excellent cleanliness and good color fastness; [0005] 3. Excellent solubility, level dyeing property and excellent dyeing depth; [0006] 4. Good stability, excellent performance in pad dyeing and printing; [0007] 5. High dye uptake rate and fixation rate, bright color and excellent performance. [0008] In the existing active yellow DF-3RS synthesis method, waste water is easily generated, especially in the salting out step, a large amount of chloride needs to be added to the reaction, which not only increases the cost, but also discharges a large amount of sewage into the environment. [0009] The invention focuses on improving the yield of the ...

Claims

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Application Information

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IPC IPC(8): C07D251/50
Inventor 陈才美李兴喜
Owner 泰州市姜堰区东风染料化工厂
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