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Grinding coupling method for preparing disperse dye

A technology of disperse dyes and dispersants, which is applied in the coupling reaction of azo dyes, azo dyes, organic dyes, etc., and can solve the problems of high energy consumption for low-temperature coupling, high acid or alkali consumption for dissolution, and high water consumption for dye synthesis, etc. problems, to achieve the effect of increasing output, saving grinding time, and saving material consumption

Active Publication Date: 2015-07-01
HANGZHOU FLARIANT SPECIALTY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the coupling of disperse dyes, the dissolution of insoluble coupling components consumes a large amount of acid or alkali, the water consumption of dye synthesis is large, the energy consumption of low-temperature coupling is large, and the insoluble coupling components are wrapped by dyes during the coupling process. The invention provides A kind of coupling of disperse dyes under the condition of proper temperature and proper pH, under the condition that the grinding medium is mixed into the material, and the material is controlled to be in a proper grinding state by adjusting the speed and stirring

Method used

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  • Grinding coupling method for preparing disperse dye
  • Grinding coupling method for preparing disperse dye
  • Grinding coupling method for preparing disperse dye

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 68.0 g of industrial product nitrosyl sulfuric acid with a content of 40% in a 250 ml three-necked flask. Control the temperature in the bottle at 35°C-45°C and gradually add 28.2g of p-nitroaniline (98.0% content, 0.2mol), after the addition, keep stirring at 35°C-45°C for 3 hours and let it stand for 6 hours. Use a glass rod to dip a few drops of diazonium solution into ice water, and the ice water is clear; detect it with potassium iodide test paper, it turns blue, and the diazotization reaction is completed, and a diazonium salt solution is obtained. In a 2000ml beaker, set it up and stir, add 400.0g of glass beads with a particle size of 1mm and 200.0g of sea sand with a particle size of 1mm into the beaker, add 500.0g of water, add 1.0g of flat plus emulsifier and 2.0 gMF dispersant, then add 47.7g (content 99.0%, 0.2mol) of coupling component N-cyanoethyl-N-benzylaniline, start stirring, control pH=1-2, start stirring, and keep grinding for 1.5 hours , so th...

Embodiment 2

[0031] Change the amount of the coupling component to 45.3g (content 99.0%, 0.19mol), the grinding medium to 906.0g of glass beads with a particle size of 2.0mm, the amount of water added to 679.5g, and the emulsifier to 0.453g of OP -10, the dispersant is changed into the dispersant Reax 85A of 2.25g, and other operating methods are with embodiment 1, obtain disperse orange 288 filter cake 71.9g, purity 96.4% (HPLC), molar yield is 94.7% (with coupling component count).

Embodiment 3

[0037] Change the amount of coupling components to 50.1g (content 99.0%, 0.21mol), the grinding medium to 906.0g zirconia beads with a particle size of 0.5mm, the amount of water added to 679.5g, and the emulsifier to 2.5g NP-30, the dispersant is changed into dispersant Reax 85A of 0.453g, and other operating methods are the same as embodiment 1, obtain disperse orange 288 filter cake 78.5g, purity 95.7% (HPLC), molar yield is 92.8% (with coupling component count).

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Abstract

The invention relates to the field of dye preparation, particularly a grinding coupling method for preparing a disperse dye. According to the grinding coupling method for preparing a disperse dye, a coupling component and a diazonium salt are subjected to coupling reaction in the presence of a grinding medium to obtain the disperse dye. The method provided by the invention obviously reduces the discharge of acidic wastewater, enhances the unit volume yield, lowers the consumption of the cold source, saves the subsequent commercial grinding time due to the pre-ground crude dye, and synthesizes the dye on the basis of the insoluble coupling component, thereby providing a practical method capable of saving the material consumption and energy consumption and obtaining a high-quality dye filter cake without coupling component residues. The obtained crude dye is equivalently subjected to pre-dispersion grinding treatment, and about 10-20% of milling time can be saved when the crude dye is sent to the subsequent procedure for commercial processing. The energy-saving coupling of the disperse dye is implemented through the control on optimized technological conditions.

Description

technical field [0001] The invention relates to the field of dye preparation, in particular to a grinding coupling method for preparing disperse dyes. Background technique [0002] The production of azo-type disperse dyes mainly includes three processes. The first is diazotization, that is, the diazotization reaction between the diazo component and nitrous acid in an acid solvent generates a diazonium salt solution. The second is coupling. Usually, the coupling components are dissolved or dispersed in an appropriate solvent to form a coupling solution, and then the diazonium salt is added to the coupling solution at low temperature to undergo a coupling reaction to generate the original dye. The third is to obtain standardized commercial disperse dyes through commercial processing such as grinding operations on the original dyes. [0003] In the second process, the solvent in which the coupling components are dissolved is usually hydrochloric or sulfuric acid or caustic so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B41/00C09B29/085C09B29/42C09B29/26
Inventor 李百春
Owner HANGZHOU FLARIANT SPECIALTY
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