Preparation method of 1-amino-anthraquinone

A technology for aminoanthraquinone and nitroanthraquinone crude products, which is applied in the field of preparation of 1-aminoanthraquinone, can solve the problems of high production cost, low yield of 1-aminoanthraquinone, environmental impact, etc., and achieve low raw material cost, The effect of high yield and strong market competitiveness

Inactive Publication Date: 2015-03-25
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology improves upon previous methods where an alkaline solution was applied during filter collection but it also causes unwanted side reactions such as diketones formation (which occurs when certain amines react) which reduces yields from desired compounds. By adding different chemicals together at once, the resulting mixture becomes clearer through chromatography techniques like liquid phase extraction. Additionally, there have been improvements made on other ways to reduce harmful substances generated while producing these valuable materials. Overall, this new approach enhance purification efficiency and quality control over existing processes.

Problems solved by technology

This patented technical problem addressed in this patents relates to producing pure or enriched 1 - aminopyrimidones (NAPs) without generating excessive amounts of unwanted materials such as dimercaptan during chemical reactions used for making them. Existing methods have limitations due to their poor yields resulting from slow addition of acids at specific points along the pathway leading to incomplete conversion of starting compounds.

Method used

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Embodiment

[0021] This embodiment provides a clean preparation method for 1-aminoanthraquinone, specifically as follows;

[0022] (1) Add 60 grams of anthraquinone, 120 milliliters of dichloroethane, and 20 grams of 98% concentrated nitric acid (molecular weight 63) into the reaction flask, and then slowly add 100% of Sulfuric acid 45 grams carries out nitration reaction, after dropwise addition, keep warm for 3 hours, take a sample and measure the end point, after the reaction ends, the material is neutralized to recover dichloroethane and then suction filtered, washed to obtain the crude product of 1-nitroanthraquinone, wherein 1-nitroanthraquinone The base anthraquinone content is 45%; the by-product content of 1.5, 1.8 and 1.6, 1.7 dinitroanthraquinone is 0.47% and 0.42% respectively, the content of 2-nitroanthraquinone is 0.38%, and the content of anthraquinone is 53.73%. The dry crude product 1-nitroanthraquinone was 66 grams.

[0023] (2) React the crude 1-nitroanthraquinone w

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Abstract

The invention relates to a preparation method of 1-amino-anthraquinone. The preparation method comprises the following steps: using anthraquinone as a raw material, generating 1-amino-anthraquinone by performing nitratlon reaction and reduction reaction in sequence, wherein a 1-amino-anthraquinone crude product obtained by nitratlon reaction is directly subjected to reduction reaction without purification, the content of the 1-amino-anthraquinone in the 1-amino-anthraquinone crude product is enabled to be 40wt%-50wt% by controlling the raw material feeding capacity and the nitration depth, and the total content of 1,5 and 1,8 binitro byproducts and the total content of 1,6 and 1,7 binitro byproducts are respectively lower than 0.5wt%; after the reduction reaction is ended, separating the 1-amino-anthraquinone crude product obtained by the reduction reaction through acid or the organic solvent, thereby obtaining 1-amino-anthraquinone fine product of which the content is more than 98wt% and anthraquinone of which the content is more than 98wt%, and recycling the anthraquinone of which the content is more than 98wt% as a raw material in next reaction. The preparation method of the 1-amino-anthraquinone is high in yield and free of solid waste residues, and is a true clean production process.

Description

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Claims

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Application Information

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Owner 苏州市罗森助剂有限公司
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