Method for manufacturing yellow dye by utilizing 1-amino anthraquinone production waste residues

An aminoanthraquinone and waste residue technology, applied in anthracene dyes, organic dyes, chemical instruments and methods, etc., can solve the problems of waste of organic components, inability to fully utilize waste residues, generation of waste residues, etc., and achieve improved utilization, obvious economic benefits, The effect of price reduction

Active Publication Date: 2011-04-20
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This treatment method not only wastes a large amount of organic components in vain, but also pollutes the environment; now some domestic manufacturers have proposed some methods of using this kind of production waste residue
However, in the process of utilizing waste residue, it is necessary to carry out chemical refining treatme

Method used

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  • Method for manufacturing yellow dye by utilizing 1-amino anthraquinone production waste residues
  • Method for manufacturing yellow dye by utilizing 1-amino anthraquinone production waste residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] ① Preparation of reducing agent sodium hydrosulfide aqueous solution

[0042] In a 500ml beaker, add 200ml of hot water above 85°C and 20g of sodium hydrosulfide, stir until completely dissolved, filter, collect the filtrate sodium hydrosulfide aqueous solution, and set aside;

[0043] ② reduction

[0044] In a 500ml four-neck flask, add the sodium hydrosulfide aqueous solution prepared in step ①, add 60g of dried 1-aminoanthraquinone production waste residue under stirring, heat to 95°C for reduction reaction, and keep it warm under stirring at this temperature After 5 hours to reduce the various nitroanthraquinones contained in the production waste residue to the corresponding aminoanthraquinones, lower the temperature to 60 ° C and filter, wash the filter cake to neutrality, and then dry it to obtain the reduced raw material aminoanthraquinone mixture (34-36g ), the weight ratio of production waste residue and sodium hydrosulfide used for the reduction reaction is 6...

Embodiment 2

[0050] Step 1. sodium hydrosulfide consumption is 50g, step 2. the weight ratio of production waste residue and sodium hydrosulfide is 60: 50 (1: 0.83), and all the other are identical with embodiment 1;

[0051] ③Condensation

[0052] In a 250ml four-neck flask, add 180g of medium-chlorobenzene and 20g of the reducing material obtained in step ② under stirring, and after stirring for 0.5 hours, add 4g of halogenated heterocyclic compound cyanuric fluoride and heat it up to 55°C, add Sodium bicarbonate 2g, heat preservation at 95~98°C for 4 hours to conduct condensation reaction, measure the amino value of the material at 23wt%, the condensation reaction can be completed, cool down to 80°C, add hot water to carry out steam distillation of the material, collect and condense The distilled product is to be treated, the remaining material is suction filtered, the obtained filter cake is washed with hot water until neutral, and dried to obtain a yellow primary dye (22g). The appear...

Embodiment 3

[0055] Step 1. sodium hydrosulfide consumption is 40g, step 2. the weight ratio of production waste residue and sodium hydrosulfide is 60: 40 (1: 0.67), and all the other are identical with embodiment 1;

[0056] ③Condensation

[0057] In a 250ml four-neck flask, add 200g of o-dichlorobenzene as a medium and 20g of the reducing material obtained in step ② under stirring. After stirring for 0.5 hours, add 7g of halogenated heterocyclic compound cyanuric chloride and heat it up to 55°C. Sodium bicarbonate 3g, heat preservation at 98~100°C for 4 hours to carry out condensation reaction, measure the amino value of the material at 28wt%, the condensation reaction can be completed, lower the temperature to 80°C, add hot water to carry out steam distillation of the material, collect and condense The distilled product is to be treated, the remaining material is suction filtered, the obtained filter cake is washed with hot water until neutral, and dried to obtain a yellow primary dye (...

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Abstract

The invention relates to a method for manufacturing a yellow dye by utilizing 1-amino anthraquinone production waste residues, which is characterized by comprising the following steps of: performing reduction reaction on the 1-amino anthraquinone production waste residues to obtain a reduction product, namely amino anthraquinone mixture, performing condensation reaction on the reduced material amino anthraquinone mixture and a halogenated heterocyclic compound at 90 to 100 DEG C in the presence of sodium bicarbonate in a medium chlorobenzene to prepare a crude yellow dye in form of yellow powder and with colored light approximate to C.I. vat yellow 1, and performing commercial processing to obtain a commercial yellow dye. The crude yellow dye manufactured by the method has performance capable of reaching the level of an ordinary vat dye, can be applied to combination dyeing and the like completely or partially instead of the C.I. vat yellow 1 and also can be used independently as a single species. In the method, a new approach to the utilization of the 1-amino anthraquinone production waste residues is developed, the waste residues can be converted into available commodities with low cost without producing new wastes, and the requirements of environmental protection are met.

Description

technical field [0001] The invention relates to a method for producing yellow dye by using 1-aminoanthraquinone production waste residue. Background technique [0002] In the process of producing 1-aminoanthraquinone by solvent method, in order to make the obtained 1-aminoanthraquinone more pure, all domestic manufacturers are currently refining the nitrates, during which a large number of by-products are dissolved in the refined mother liquor is separated, and the mother liquor is distilled to form a waste residue. The chromatographic analysis results of this 1-aminoanthraquinone production waste residue are: the chromatographic content of 1-nitroanthraquinone is 20-30wt%, and the chromatographic content of 1,5 or 1,8-dinitroanthraquinone is 35-40wt% %, the chromatographic content of 1,6 or 1,7-dinitroanthraquinone is 30-35 wt%, and the rest are unknown miscellaneous peaks. The current widely used treatment method for this production waste residue is incineration. This t...

Claims

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Application Information

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IPC IPC(8): C09B1/20
Inventor 王继昌郑冬松
Owner JIANGSU YABANG DYE
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