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Method for refining 1-nitroanthraquinone by using mixed nitroanthraquinone

A technology of nitroanthraquinone and dimethylformamide, applied in the direction of nitro/nitroso dyes, chemical instruments and methods, azo dyes, etc., can solve the problem of reducing the yield of 1-nitroanthraquinone and operating costs Increased height, high production cost and other problems, to achieve the effect of suitable refining yield, improved solubility and low production cost

Active Publication Date: 2005-03-16
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mostly adopt the method of solvent crystallization in actual production at present, used solvent is dimethylformamide (hereinafter referred to as DMF), this method does not produce waste water, also can obtain high-purity 1-nitroanthraquinone, but, because DMF is mixed The solubility of 1,5-dinitroanthraquinone and 1,6-dinitroanthraquinone in nitroanthraquinone is very small. In order to obtain high-purity 1-nitroanthraquinone, it must undergo multiple recrystallizations
Like this, not only operating cost increases, also reduced the yield of 1-nitroanthraquinone simultaneously
In order to improve the refining effect, someone has adopted the method of adding additives during refining, such as Japanese Patent No. 1974-55655, which uses the method of treating the mixed nitroanthraquinone in the organic solvent with alkali in the presence of a catalyst. The catalyst used has sub- Nitrate, thiocyanate, iodide, bromide and fluoride etc., used auxiliary agent is triethylamine; Japanese patent 1974-76853 adopts the situation of adding initiator in solvent refining process with one or two A refining method in which more than one carbonyl compound is used as an auxiliary agent. The initiator includes sodium nitrite or sodium thiocyanate. ester, diethyl malonate, butanone, acetophenone, 3-methyl-1-phenylpyrazolone, benzoylphenone, pentanone, pentanedione, etc.; The method of refining by adding additives such as primary amine, secondary amine or a mixture of the two. The selected additives include morpholine, diethanolamine, etc.; but the amount of additives added by the above refining methods is too large, generally 10-25 %, the prices of the additives used are relatively high, making the production cost high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 500ml three-necked flask, add 80% 1-nitroanthraquinone, 5% 2-nitroanthraquinone, 2% anthraquinone, 1,5-dinitroanthraquinone 3%, and 1,8-dinitro 150g mixed nitroanthraquinone 2%, 1,6-dinitroanthraquinone 4%, 1,7-dinitroanthraquinone 4%, add 200g of solvent dimethylformamide (DMF), help 2g of sodium nitrite, heated to 140°C and kept stirring for 3 hours, cooled to 50°C and filtered, and the filter cake was washed with DMF to obtain 103g of 1-nitroanthraquinone, the content of which was 98.5%, and the refined yield was 84.55%. The amount of auxiliary agent is 1.33% of the mixed nitroanthraquinone.

Embodiment 2

[0016] In a 500ml three-necked flask, add 80% 1-nitroanthraquinone, 5% 2-nitroanthraquinone, 2% anthraquinone, 1,5-dinitroanthraquinone 3%, and 1,8-dinitro 150g mixed nitroanthraquinone 2%, 1,6-dinitroanthraquinone 4%, 1,7-dinitroanthraquinone 4%, add 200g of solvent dimethylformamide (DMF), help 3g of urea and 1g of sulfur, heated to 140°C and kept stirring for 3 hours, cooled to 50°C, filtered, and the filter cake was washed with DMF to obtain 108g of 1-nitroanthraquinone, the content of which was 97.8%, and the refined yield was 88.02%. , The amount of auxiliary agent is 2.67% of the mixed nitroanthraquinone.

Embodiment 3

[0018] In a 500ml three-necked flask, add 83% of 1-nitroanthraquinone, 5% of 2-nitroanthraquinone, 1.5% of anthraquinone, 2.5% of 1,5-dinitroanthraquinone, and 1,8-dinitro 150g of mixed nitroanthraquinone 2%, 1,6-dinitroanthraquinone 3%, 1,7-dinitroanthraquinone 3%, add 100g of solvent dimethylformamide (DMF) and chlorine 150g of benzene, 2.5g of sodium nitrite as auxiliary agent, heat up to 140°C and keep stirring for 3 hours, cool down to 50°C and filter, and then wash the filter cake with DMF to obtain 102g of 1-nitroanthraquinone, the content of which is 99%, refined The yield is 81.10%, and the amount of auxiliary agent is 2.0% of the mixed nitroanthraquinone.

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PUM

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Abstract

The invention provides a resin composition for laminated material comprising at least 10 wt% of vinyl compound having chemical formula (1), the pre-impregnated product and metal cover laminated material employing the resin.

Description

Technical field [0001] The invention relates to a method for refining 1-nitroanthraquinone by using mixed nitroanthraquinone. Background technique [0002] 1-Nitroanthraquinone is a heavy dye intermediate. The 1-aminoanthraquinone produced with it can be used to manufacture vat dyes, disperse dyes, reactive dyes and acid dyes, and can also be used to synthesize dye intermediates. At the same time, 1-nitroanthraquinone can also be used directly in the production of dyes. At present, anthraquinone is commonly used as raw material, and 1-nitroanthraquinone is prepared by nitration with mixed acid (nitric acid and sulfuric acid) in a solvent medium. In the obtained mixed nitroanthraquinone, the content of 1-nitroanthraquinone is generally Around 80%. Therefore, it is necessary to increase the content of 1-nitroanthraquinone in the mixed nitroanthraquinone and prepare high-purity 1-nitroanthraquinone. At present, most of the actual production adopts the method of solvent crystallizati...

Claims

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Application Information

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IPC IPC(8): C09B51/00
Inventor 尹云李少文
Owner JIANGSU YABANG DYE
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