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Comprehensive utilization method of waste residues generated in refining 1-aminoanthraquinone

A technology of aminoanthraquinone and nitroanthraquinone, applied in the direction of organic dyes, etc., can solve the problem of difficulty in selling separately, and achieve the effects of considerable economic value, large output and reduction of processing costs

Active Publication Date: 2014-01-29
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These varieties are difficult to sell separately due to the difference in color and shade from the existing varieties on the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1, the preparation of disperse red brown E-2B

[0037] Add 300g of 98% concentrated sulfuric acid and 150g of industrial concentrated nitric acid into a 500ml flask, stir evenly and cool down to below 50°C, slowly add 120g of waste residue within 2~3 hours, slowly raise the temperature to 70~80°C and Insulate and react for 3 hours. After the reaction reaches the end point, cool down to below 40°C. Transfer the material to a sand core funnel for suction filtration. After fully draining, the filter cake is evenly washed with a small amount of 50-60% sulfuric acid and fully drained again. Finally, use Wash the filter cake with clear water, take out the filter cake and dry to obtain 105 g of dinitroanthraquinone mixture.

[0038] In the autoclave of 500ml, add above-mentioned bisnitroanthraquinone mixture 100g, calcium oxide 35g, urea 40g, dimethylbenzene 150g, content is 25% methylamine aqueous solution 100g, cover still cover and seal rapidly after feeding fini...

Embodiment 2

[0040] Embodiment 2, the preparation of disperse violet E-2R

[0041] The dinitroanthraquinone mixture obtained by double-nitrating the waste residue according to the aforementioned method, add 30 g of the above-mentioned dinitroanthraquinone mixture, 150 ml of nitrobenzene (or chlorobenzene), and 25% ammonia solution in a 500 ml autoclave 100ml, cover the kettle lid and seal it quickly after feeding, raise the temperature to 130-140°C and keep it warm for 10 hours. After the reaction, transfer the material into a 1000ml flask, evaporate the solvent and filter while it is hot. After washing and drying, take 20g of the dry product and add it to a 250ml flask, then 150g of 95% sulfuric acid, heat up and dissolve under stirring, then add 15g of bromine dropwise at 60-80°C, and keep it warm for 3 hours after the addition is completed. Then remove the remaining bromine under reduced pressure, add 200g of 20% fuming sulfuric acid and 6g of boric acid after the material drops to norm...

Embodiment 3

[0043] Embodiment 3, the preparation of disperse blue E-3R

[0044] The dinitroanthraquinone mixture obtained by carrying out double nitration of waste residue according to the aforementioned method, add 500ml of water and 150g of industrial sodium sulfide to a 1000ml beaker, stir and dissolve, then filter, add the filtrate to a 1000ml flask, and add the above dinitroanthraquinone mixture Dry 60g, heat up to reflux and keep it warm for 4 hours, filter, wash and dry to obtain a mixture of diaminoanthraquinone, add 150g of 95% sulfuric acid to a 250ml flask, reduce 20g of raw materials, heat up and dissolve under stirring, and then dissolve in 60-80 Add 30g of bromine dropwise at ℃ for about 2 hours. After the dropwise addition, keep warm at 80-90℃, 90-100℃, and 100-110℃ for 2 hours respectively, then reduce the pressure or use air bubbles to remove the remaining bromine and control the temperature. Slowly add 100ml of water below 80°C for isolation, filter and wash, and then d...

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Abstract

The invention provides a comprehensive utilization method of waste residues generated in refining 1-aminoanthraquinone. The dye varieties such as disperse reddish brown, disperse yellow, disperse blue and the like are directly prepared without separating and purifying by taking waste resides generated in the production process of 1-aminoanthraquinone as raw materials, and dye varieties equivalent with the existing commodity dyes such as the traditional products disperse ash, disperse black and the like are prepared after the dye varieties are mixed according to different proportions. The waste residues obtained by using the method are not needed to be treated by processes such as refining, purification and the like, and all components in the waste residues can be utilized, so that not only are the economic values of the waste residues increased, but also the secondary pollution caused by refining and purifying are avoided, and the environmental pollution problem is effectively solved; the comprehensive utilization method has high economic and environment-friendly values.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a comprehensive utilization method of 1-aminoanthraquinone refining waste residue. [0002] Background technique [0003] 1-Aminoanthraquinone is one of the most important varieties of anthraquinone series intermediates. At present, the annual domestic output is about 20,000 tons, and a large amount of waste residue is produced in the production process. The composition of the waste residue is complex, mainly containing 1-nitro Anthraquinone, 2-nitroanthraquinone, 1,5-dinitroanthraquinone, 1,6-dinitroanthraquinone, 1,7-dinitroanthraquinone, 1,8-dinitroanthraquinone, A small amount of unreacted anthraquinone and impurities such as tar produced during the refining process, because the content of each component in the waste residue is not high, it is difficult to separate and purify. It caused secondary pollution and caused a lot of waste of resources. [0004] M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/38
Inventor 李少文马红燕牟忠丽
Owner JIANGSU YABANG DYE
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