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The preparation method of disperse blue 60 and/or its homologue

A technology for dispersing blue and homologues, applied in chemical instruments and methods, organic dyes, anthracene dyes, etc., can solve problems such as consumption, potential safety hazards, incomplete reactions, etc., to reduce environmental pollution, improve lifting power, and increase yield and quality effects

Active Publication Date: 2015-10-14
JIANGSU HELIRUI TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In above-mentioned existing method, adopt the disperse blue 60 that absolute ethanol solvent method reacts to obtain, because the existence of solvent, yield is lower, and take away ethanol and γ-methoxypropylamine in the disperse blue filter cake, cause consumption partial High, 1,4-diamino-2,3-dicarboximide anthraquinone needs to be dried, consumes a certain amount of steam and has physical losses during the reaction process, resulting in high production costs
The use of ethanol in the reaction process also brings certain potential safety hazards
In addition, pressurized reaction in aqueous solution can avoid some of the above problems, but because it is a pressurized reaction, the ammonia gas generated by the reaction cannot be taken away in time, which will slow down the reaction speed and increase the pressure of the reaction system, resulting in long reaction time , incomplete response and other results, will also bring certain security risks

Method used

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  • The preparation method of disperse blue 60 and/or its homologue

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method of embodiment 1, disperse blue 60, its steps are as follows:

[0031] Add 2000kg of water into the 5000L reactor, start stirring, put in the wet product of 1,4-diamino-2,3-dicarboximide anthraquinone (500kg on a dry basis), raise the temperature to 95°C, turn on the vacuum, and keep the pressure at 0.90 x 10 5 At about Pa, start to add 300kg of γ-methoxypropylamine dropwise, and finish dropping in 1 hour, keep the temperature at 85°C to 95°C, carry out vacuum distillation and condensation reaction to obtain fractions; after the fractions are separated from gas and liquid, the liquid fractions are collected and returned In the reaction system, the gas is absorbed by water to make ammonia water. After half an hour, 120 kg of remaining γ-methoxypropylamine was added dropwise to the reaction system, and the drop was completed in 20 minutes. After completion, the reaction was kept for 1 hour. During the reaction, if the volume of the material in the ...

Embodiment 2

[0032] Embodiment 2, the preparation method of disperse blue 60 homologue, its steps are as follows:

[0033] Add 2000kg of water into the 5000L reactor, start stirring, put in the wet product of 1,4-diamino-2,3-dicarboximide anthraquinone (500kg on a dry basis), raise the temperature to 100°C, turn on the vacuum, and maintain the pressure at 0.85 x 10 5 At about Pa, start to add 350kg of γ-ethoxypropylamine dropwise, and finish dropping in 1 hour, keep the temperature at 90°C-100°C, carry out vacuum distillation and condensation reaction to obtain fractions; after the fractions are separated by gas and liquid, the liquid fractions are collected and returned In the reaction system, the gas is absorbed by water to make ammonia water. After half an hour, 150 kg of remaining γ-ethoxypropylamine was added dropwise to the reaction system, and the drop was completed in 20 minutes. After completion, the reaction was kept for 1 hour. During the reaction, if the volume of the materia...

Embodiment 3

[0034] Embodiment 3, the preparation method of disperse blue 60 and its homologue, its steps are as follows:

[0035] Add 2000kg of water into the 5000L reactor, start stirring, put in the wet product of 1,4-diamino-2,3-dicarboximide anthraquinone (500kg on a dry basis), raise the temperature to 95°C, turn on the vacuum, and keep the pressure at 0.90 x 10 5 At about Pa, start to drop 350kg of the mixture of γ-methoxypropylamine and γ-ethoxypropylamine (γ-methoxypropylamine:γ-ethoxypropylamine weight ratio=50%:50%), drop it in 1 hour, The temperature is kept at 90°C to 95°C, and the vacuum distillation condensation reaction is carried out to obtain fractions; after the fractions undergo gas-liquid separation, the liquid fractions are collected and returned to the reaction system, and the gas is absorbed by water to make ammonia water. After half an hour, 110 kg of the remaining γ-methoxypropylamine and γ-ethoxypropylamine mixture were added dropwise to the reaction system, and...

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Abstract

The invention discloses a preparation method of disperse blue 60 and / or homolog thereof, which is characterized in that a condensation reaction is carried out through normal pressure or reduced pressure distillation, in the condensation reaction process, 1,4-diamido-2,3-dicarboximide anthraquinone is unnecessary to dry, no other solvent is used, water is used as the solvent, gamma-alkoxy propylamine is dropwise added in batches, gas-liquid separation is carried out on fractions, liquid fractions are collected, and the rest fractions return to the reaction system, a gas is absorbed by water and is prepared into ammonia water, and mother liquor obtained after the reaction can return to the process to replace all or a part of water in the next batch of reactions. The process of the method disclosed by the invention is more reasonable and the mother liquor can be recycled, thereby effectively improving the product yield, improving the product quality (elevating power), lowering the production cost and reducing the emission of wastewater (ammonia nitrogen).

Description

technical field [0001] The present invention relates to the preparation method of disperse blue 60 and / or its homologue. Background technique [0002] The existing production method of disperse blue 60 mainly uses 1,4-diaminoanthraquinone leuco as raw material, and reacts with chlorosulfonic acid in o-dichlorobenzene solvent to prepare 1,4-diamino-2,3-di Anthraquinone sulfonate, followed by cyanation in aqueous solution. Also in the patent ZL200610156081.X, cyanide was carried out using dimethylformamide as a solvent to obtain 1,4-diamino-2,3-dicyanoanthraquinone; then hydrolyzed under the action of sulfuric acid to obtain 1,4-dicyanoanthraquinone Amino-2,3-dicarboximide anthraquinone was removed by activated carbon and dried, and refluxed with γ-methoxypropylamine in anhydrous ethanol solvent to obtain Disperse Blue 60. In addition, in the publication number CN101817989A, 1,4-diamino-2,3-dicarboximide anthraquinone does not need to be dried, and can be obtained by pressur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/58C09B5/24
CPCC09B5/2472
Inventor 方标钱吉荣丁利江
Owner JIANGSU HELIRUI TECH DEV CO LTD