Preparation method of energy-efficient and environmentally-friendly disperse dye

A technology of disperse dyes, energy saving and environmental protection, applied in the direction of azo dyes, organic dyes, monoazo dyes, etc., can solve the problems of increasing the difficulty of wastewater treatment, economic loss, and difficulty in transferring dyes, to reduce the difficulty of treatment and improve the The effect of transferring crystal quality and reducing energy consumption

Active Publication Date: 2016-03-30
ZHEJIANG DIBANG CHEM
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  • Claims
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Problems solved by technology

[0004] In the above-mentioned technical process, especially in the dissolving process of diazotization and coupling components, sulfuric acid with higher concentration and more quantity needs to be used as solvent, and the sulfuric acid content of the filter cake mother liquor is usually up to 10% (mass fraction) after the reaction finishes. ), under such strong acid conditions, it is difficult for the dye to undergo crystal transformation. Sometimes, although the crystal transformation is achieved at high temperature, under high temperature, the solubility of the dye in the acid solution increases, so that it is discharged together with the mother liquor , which not only caused economic losses, but also greatly increased the difficulty of wastewater treatment

Method used

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  • Preparation method of energy-efficient and environmentally-friendly disperse dye

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Effect test

Embodiment 1

[0031] In the diazo kettle, 2000 kg of 98% sulfuric acid (mass percentage concentration) and 1972 kg of 28% nitrosyl sulfuric acid (mass percentage concentration, solvent is sulfuric acid) were successively dropped into the diazo kettle, stirred and cooled, and slowly dropped into 2,6-dibromo-p-nitro 1250kg of aniline, after adding, keep warm until the reaction is complete, and set aside;

[0032]Add 16,000kg of bottom water to the coupling kettle, add 30kg of Pingpingjia and 735kg of N-ethyl-N-cyanoethylaniline, after beating for 2 hours, dig out crushed ice to cool down, then add the above-mentioned diazonium solution, keep warm for 6 hours after adding, and detect the end point After qualified, start to add ammonia solution (mass percentage concentration is 10%) to adjust the pH value of the system to 4.5-5.5, then raise the temperature to 60-65 °C, stir for 1 hour, and after the dye is crystallized, enter the filter press to filter, Wash with water until neutral to obtain ...

Embodiment 2

[0035] In the diazo kettle, 1000kg of 98% sulfuric acid and 3150kg of nitrosylsulfuric acid of 28% are successively dropped into, stirred and lowered in temperature, slowly dropped into 900kg of p-nitroaniline, after adding, keep warm until the reaction is complete, and set aside;

[0036] Add 15,000kg of bottom water to the coupling kettle, add 25kg of Pingpingjia and 735kg of N, N-diacetoxyethyl-m-acetaniline, after beating for 2 hours, dig out crushed ice to cool down, then add the above-mentioned diazo solution, and keep warm for 6 hours after adding , after the detection end point is qualified, start to add ammonia solution (18% by mass percentage concentration) to adjust the pH value of the system to 6.0-7.0, then heat up to 65-70°C, stir and turn the crystal for 1 hour, and then enter the filter press after the dye turns crystal. Filter and wash with water until neutral to obtain 74 scarlet disperse dye filter cake, the mother liquor water is collected and used for the p...

Embodiment 3

[0039] Put 550kg of 98% sulfuric acid and 2100kg of 28% nitrosylsulfuric acid into the diazo kettle successively, stir and cool down, slowly put in 1200kg of 2,4-dinitro-6-bromoaniline, after adding, keep warm until the reaction is complete, and set aside ;

[0040] Add 20,000kg of bottom water to the coupling kettle, add 30kg of Pingpingjia and 945kg of N, N-diethyl-3-acetamidoaniline, after beating for 1 hour, dig out crushed ice to cool down, then add the above-mentioned diazonium solution, and keep warm for 7 hours after adding. After the detection end point is qualified, start to add sodium hydroxide solution (mass percentage concentration is 20%) to adjust the pH value of the system to 5.0-6.0, then raise the temperature to 60-65°C, stir for 1 hour and wait for the dye to crystallize before entering the filter press Press filter and wash with water until neutral to obtain 93 violet disperse dye filter cake, the mother liquor is collected and used for the preparation of s...

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Abstract

The invention discloses a preparation method of an energy-efficient and environmentally-friendly disperse dye. The method comprises the following steps: carrying out a coupling reaction on a diazo salt and a coupling component to obtain a corresponding azo compound, adding an alkali to to adjust the pH value of the obtained system to 2-7.5, carrying out heating crystal transformation to obtain a stable crystal form, press-filtering obtained crystals, and washing the press-filtered crystals with water to obtain a dye filter cake. The method mainly has the following advantages: 1, the pH value of the system is improved, so obtaining of the stable crystal form through dye crystal transformation is facilitated, and electricity and time are saved in the sand milling process; 2, parts of the disperse dye dissolved in a mother liquor can be recovered, so the content of organic matters in the mother liquor is greatly reduced, and the wastewater treatment difficulty is reduced; 3, the filter cake mother liquor is rich in ammonium sulfate (or sodium sulfate), and can be used to prepare ammonium sulfate (or sodium sulfate), so wastewater recycling is realized; and 4, the amount of water for washing is greatly reduced, so the wastewater discharge is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of disperse dyes, and in particular relates to a preparation method of energy-saving and environment-friendly disperse dyes. Background technique [0002] Disperse dyes are a kind of special materials used in polyester fiber dyeing. In terms of their chemical structures, they mainly include azos, anthraquinones, nitrodiphenylamines, methines and non-azoheterocyclics. Among them, azo and anthraquinones are the majority, and azo dyes occupy an extremely important position in disperse dyes. Among the disperse dyes that have been industrially produced, the dye varieties with azo structure account for 50%, and the output accounts for more than 70%. , the dye has a wide chromatographic coverage, good application performance, simple production process and low cost. [0003] As we all know, the production method of azo-type disperse dyes mainly includes three processes: 1, diazotization, that is, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/36C09B67/48C09B29/085
Inventor 徐万福傅伟松陈华祥唐智勇徐斌丁亚刚
Owner ZHEJIANG DIBANG CHEM
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