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Resource utilization method of waste residues generated by 1-nitroanthraquinone production by solvent method

A technology of nitroanthraquinone and dinitroanthraquinone is applied in the field of resource utilization of waste residue produced by solvent production of 1-nitroanthraquinone, and can solve the problem of small application value of dyes, no industrial value, poor dye performance, etc. question

Active Publication Date: 2012-01-18
YANCHENG OUHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned so-called disperse dyes, the former is actually a mixed aminoanthraquinone, and the latter is a bromide or chloride of a mixed aminoanthraquinone, the composition is not stable, the performance of the dye is poor, and the application value of the dye is small
[0005] CN 101100430A discloses a method for extracting 1-nitroanthraquinone from nitroanthraquinone waste residue, which is difficult to operate, and the obtained so-called 1-nitroanthraquinone is a substance with more complex components than "waste residue", without industrial value
[0006] CN 101591249A discloses a method for processing the "waste residue" from the production of 1-aminoanthraquinone into a raw material for the production of 1,5(1,8)-dinitroanthraquinone. Although this 1-aminoanthraquinone can be effectively used in the production "waste residue" produced, but the processed product is difficult to sell as a commodity and has low value

Method used

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  • Resource utilization method of waste residues generated by 1-nitroanthraquinone production by solvent method
  • Resource utilization method of waste residues generated by 1-nitroanthraquinone production by solvent method
  • Resource utilization method of waste residues generated by 1-nitroanthraquinone production by solvent method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Crush 200kg of "waste residue" and 2000kg of water together, add 140kg of sodium sulfite, heat to 96-100°C for 2 hours; cool down to 85°C, filter, wash the filter cake with hot water at 80°C until the filtrate is colorless, dry the filter cake, and mix Nitrate 90kg. Put the dried mixed nitric acid into 1000L of toluene, heat to 105-110°C, keep it warm for about 1 hour, and filter while it is hot. The filter cake is component B, wash off the toluene with methanol, and dry; add water to the toluene filtrate, remove the toluene by steam distillation, filter out component A, and dry. The result is as follows:

[0021]

[0022] In the table: X 1 , x 2 、X 3 for the unknown

[0023] 1,8- that is, 1,8-dinitroanthraquinone;

[0024] 1,5- that is, 1,5-dinitroanthraquinone;

[0025] 1- is 1-nitroanthraquinone;

[0026] 1,7- that is, 1,7-dinitroanthraquinone;

[0027] 1.6- namely 1,6-dinitroanthraquinone;

[0028] AQ is ant...

Embodiment 2

[0031] 200kg of "waste residue", add 1600kg of water to pulverize together, add 100kg of sodium sulfite, heat to 92-96°C for 5 hours; cool down to 85°C for filtration, wash the filter cake with hot water at 80°C until the filtrate is colorless, dry the filter cake, and obtain mixed Nitrate 100kg. Put the dried mixed nitrate into 1500L mixed xylene, heat it to 115-120°C, keep it warm for about 1 hour, and filter it while it is hot. The following operations are the same as in Example 1. The result is as follows:

[0032]

Embodiment 3

[0034] 200 kg of "waste residue", crushed together with 800 kg of water, and ammonium bisulfite solution obtained by absorbing sulfur dioxide with ammonia water, converted to 100% NH 4 HSO 3 60 kg, add 15% ammonia water to make the solution pH 7~8, heat up to 100~105°C and react for 4 hours; cool down to 85°C and filter, wash with hot water at 80°C until the filtrate is colorless, dry the filter cake to obtain mixed nitric acid 110 kg. Put the dry mixed nitric acid into 1200L o-xylene, heat to 130-135°C, keep it warm for about 1 hour, and filter while it is hot. The following operations are the same as in Example 1. The result is as follows:

[0035]

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Abstract

The invention relates to a resource utilization method of waste residues generated by 1-nitroanthraquinone production by a solvent method, which comprises the steps that: the waste residues are added with water and are crushed, sulphite or hydrosulphite is added for taking reaction for 2 to 5 hours at 96 to 105 DEG C, the mass ratio of the waste residues to the water is 1 / 3 to 10, the mass ratio of the waste residues to the sulphite (or the hydrosulphite) is 1 / 0.3 to 0.7, the temperature reduction and the filtration are carried out after the reaction completion, filter cake is washed by hot water, beta-bit nitroanthraquinone isomers are removed, the filter cake is dried to obtain mixed nitroanthraquinone (mixed nitro, for short), the dried mixed nitro and solvents are heated to 90 to 160 DEG C, the ratio of the mass to the solvent volume of the mixed nitro is 1kg / 7 to 15L, the heat is preserved for about 1 hour, the mixed materials are filtered in the hot state, the filter cake is a component B, methanol is used for washing away the solvents, the drying is carried out, the main ingredients of the component B are 1,5-dinitroanthraquinone, 1,8-dinitroanthraquinone and anthraquinone, the filter liquid solvents are added with water again, after the solvents are recovered by a water vapor distillation method, a component A is filtered out, and the main ingredient of the component A is 1-nitroanthraquinone.

Description

technical field [0001] The invention relates to a resource utilization method of "waste residue" produced by a solvent method to produce a dye intermediate 1-nitroanthraquinone. Background technique [0002] 1-Aminoanthraquinone is an important dye intermediate. At the end of the 1980s, since the successful implementation of the solvent method in my country to produce 1-nitroanthraquinone (and then reduce the production of 1-aminoanthraquinone), the production scale has continued to expand. At present, almost all 1-nitroanthraquinone and 1 -Aminoanthraquinone is produced in my country, and the annual output of 1-nitroanthraquinone has exceeded 15,000 tons. [0003] The production process of 1-nitroanthraquinone by solvent method is to carry out mononitration reaction of anthraquinone with mixed acid (composed of nitric acid and sulfuric acid) in dichloroethane medium, and obtain crude nitroanthraquinone with solvent dimethylformamide (DMF) separation to obtain high-puri...

Claims

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Application Information

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IPC IPC(8): C07C205/47C07C201/16C07C201/08
Inventor 杨思卫赵敏张劲松
Owner YANCHENG OUHUA CHEM IND
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