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Solvent-free coupling synthesis process of disperse blue 360

A synthesis process, disperse blue technology, applied in the direction of azo dyes, monoazo dyes, organic dyes, etc., can solve the problems that acid waste liquid cannot be recycled, acetone and organic acid cannot be recovered separately, and the yield is only low, etc., to achieve Reduce the production of waste solvents and impurity components, facilitate recycling and improve yield

Active Publication Date: 2020-12-18
JIANGSU HANSYN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although using an organic acid as a medium can achieve exothermic controllability, the yield is only 53%, and acetone and organic acid cannot be recovered separately (acetone is heated under concentrated sulfuric acid to generate mesityl oxide, and its boiling point is close to that of organic acid). A large amount of acidic waste liquid cannot be recycled

Method used

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  • Solvent-free coupling synthesis process of disperse blue 360
  • Solvent-free coupling synthesis process of disperse blue 360

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Put 200g (1.378mol, 1.0eq) of 2-amino-5-nitrothiazole and 2L organic acid into a 3L reaction flask with mechanical stirring (the volume ratio of acetic acid: propionic acid is 1:1.0), and then cool down to - 5°C, control the temperature at -5°C and slowly add 460g (1.447mol, 1.05eq) of 40% nitrosyl sulfuric acid dropwise, the system gradually changes from milky white to orange-yellow turbid liquid, the reaction is stirred for 3 hours, and the TLC plate (EA :PE=1:2), ultraviolet color development shows that the conversion of 2-amino-5-nitrothiazole is complete, add 14g (0.14mol, 0.1eq) sulfamic acid to quench the diazotization reagent, and prepare the diazonium solution for use ; Prepare another 3L reaction bottle with mechanical stirring, put 270g (1.654mol, 1.2eq) of N,N-diethyl-m-methylaniline, cool down to -5°C, and control the temperature at -5~5°C The above diazo solution was added dropwise to N,N-diethyl-m-methylaniline for coupling reaction, and the temperature w...

Embodiment 2

[0039] Put 200g (1.378mol, 1.0eq) of 2-amino-5-nitrothiazole and 2L organic acid into a 3L reaction flask with mechanical stirring (the volume ratio of acetic acid: propionic acid is 1:1.5), and then cool down to - 5°C, control the temperature at -5°C and slowly add 460g (1.447mol, 1.05eq) of 40% nitrosyl sulfuric acid dropwise, the system gradually changes from milky white to orange-yellow turbid liquid, the reaction is stirred for 3 hours, and the TLC plate (EA :PE=1:2), ultraviolet color development shows that the conversion of 2-amino-5-nitrothiazole is complete, add 14g (0.14mol, 0.1eq) sulfamic acid to quench the diazotization reagent, and prepare the diazonium solution for use ; Prepare another 3L reaction bottle with mechanical stirring, put 270g (1.654mol, 1.2eq) of N,N-diethyl-m-methylaniline, cool down to -5°C, and control the temperature at -5~5°C The above diazo solution was added dropwise to N,N-diethyl-m-methylaniline for coupling reaction, and the temperature w...

experiment example 3

[0043] Put 200g (1.378mol, 1.0eq) of 2-amino-5-nitrothiazole and 2L organic acid into a 3L reaction flask with mechanical stirring (the volume ratio of acetic acid: propionic acid is 1:2.0), and then cool down to - 5°C, control the temperature at -5°C and slowly add 460g (1.447mol, 1.05eq) of 40% nitrosyl sulfuric acid dropwise, the system gradually changes from milky white to orange-yellow turbid liquid, the reaction is stirred for 3 hours, and the TLC plate (EA :PE=1:2), ultraviolet color development shows that the conversion of 2-amino-5-nitrothiazole is complete, add 14g (0.14mol, 0.1eq) sulfamic acid to quench the diazotization reagent, and prepare the diazonium solution for use ; Prepare another 3L reaction bottle with mechanical stirring, put 270g (1.654mol, 1.2eq) of N,N-diethyl-m-methylaniline, cool down to -5°C, and control the temperature at -5~5°C The above diazo solution was added dropwise to N,N-diethyl-m-methylaniline for coupling reaction, and the temperature w...

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Abstract

The invention discloses a solvent-free coupling synthesis process of disperse blue 360. The process comprises the following steps: adding 2-amino-5-nitrothiazole into an organic acid medium, controlling the temperature, dropwise adding nitroso-sulfuric acid and carrying out a diazotization reaction to obtain a diazonium solution; adding N, N-diethyl m-methylaniline into a coupling reactor to carryout solventless reaction, cooling to -10 to 10 DEG C, adding the diazonium solution to carry out coupling reaction until the coupling is finished, filtering and washing to obtain a crude product; andobtaining a high-purity fine blue crystal, namely the disperse blue 360 through a crystal transformation process. According to the solvent-free coupling synthesis process of disperse blue 360, pure disperse blue 360 crystals can be obtained, the yield is high, the produced organic acid and crystal transformation solvent can be completely recycled, energy is saved, waste is reduced, the productioncost is greatly reduced, multiple purposes are achieved, and the process has good practical significance for achieving large-scale clean production.

Description

technical field [0001] The invention belongs to the field of manufacturing chemical dyes and chemicals, and relates to a preparation method of known disperse dyes with high dyeing strength. Specifically, it discloses an energy-saving and waste-reducing, solvent-free coupling synthesis process of disperse blue 360. Background technique [0002] Since the 20th century, with the successful application of many new chemical fibers, disperse dyes have also been developed rapidly. According to the molecular structure, disperse dyes are mainly divided into two types: azo type and anthraquinone type. Among them, anthraquinone type disperse dyes have bright color and high light fastness, but low color fastness and expensive price; azo type disperse dyes It contains various colors, complete chromatogram, simple synthesis process and low cost. It is the main body in the modern dye industry, especially the heterocyclic azos characterized by high molar extinction coefficient, high color, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/042C09B29/09
CPCC09B29/0085C09B29/0844
Inventor 赵建邹泽锦胡振宇杨多
Owner JIANGSU HANSYN PHARMA
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