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Method for synthesizing 2-carboxyl anthraquinone by using dichromic acid to oxidize 2-ethyl anthraquinone

A technology of ethyl anthraquinone and carboxy anthraquinone, which is applied in the field of synthesizing 2-carboxy anthraquinone, can solve the problems of chromium salt wastewater pollution and expensive phosphoric acid, and achieve the effects of convenient operation, less pollution and low cost

Active Publication Date: 2010-09-08
柏盛新材料(甘肃)有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

2-Methylanthraquinone is more expensive, chromium salt wastewater pollution
2-Methylanthraquinone and phosphoric acid are more expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 15.95g of finely ground 2-ethylanthraquinone to 625g of sulfuric acid with a content of 60-70% (eg 60%, 65%, 70%), and stir for 0.5h after the addition. Then add 50g of potassium dichromate at room temperature, stir for 10 minutes, raise the temperature to 110°C, and keep it at 110-120°C (for example, 110°C, 115°C, 120°C) for 2 hours. After the heat preservation is over, cool to 60°C and add 450g of water , stirred and cooled to room temperature, filtered, washed with water until neutral, and dried at 90°C to obtain 2-carboxyanthraquinone with a yield of ≥92% and a purity (HPLC) of ≥99%.

Embodiment 2

[0020] The weight ratio of 2-ethylanthraquinone, potassium dichromate, sulfuric acid, and water was adjusted to 1:3.8:36:33, and the rest were the same as in Example 1.

[0021] Example 2:

[0022] The weight ratio of 2-ethylanthraquinone, potassium dichromate, sulfuric acid, and water was adjusted to 1:3.5:45:25, and the rest were the same as in Example 1.

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PUM

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Abstract

The invention discloses a method for synthesizing 2-carboxyl anthraquinone by using dichromic acid to oxidize 2-ethyl anthraquinone, comprising the steps of: leading the 2-ethyl anthraquinone and potassium dichromate to have reaction under the condition of existence of sulphuric acid, and preparing the 2-carboxyl anthraquinone. The method has convenient operation, low cost and little pollution, and can be taken as new material to be applied in the industries such as pigment, spinning, electronics, paper making and the like on a large scale.

Description

Technical field: [0001] The invention relates to a method for synthesizing 2-carboxyanthraquinone. Background technique: [0002] The method of existing synthetic 2-carboxyanthraquinone mainly contains: [0003] 1) 2-Ethylanthraquinone was oxidized with aqueous nitric acid at 190°C and 20 atmospheres for 1 hour, and the yield was 93%. The temperature is high, an autoclave is required, and the corrosion is severe. [0004] 2) Reaction of 2-chloroanthraquinone with CO, using dichloro(triphenylphosphine) palladium complex and triphenylphosphine as catalysts, 25 atmospheres, 170°C, yield 92%. The pressure is high, the catalyst is expensive, and CO is easily poisoned. [0005] 3) 2-methylanthraquinone in acetic acid medium, with CrO 3 oxidation. 2-Methylanthraquinone is more expensive and pollutes chromium salt wastewater. [0006] 4) 2-Methylanthraquinone (2.61 grams) is oxidized with air in acetic acid medium, 200 ° C, 26 atmospheric pressure, Co(OAc) 2 , Mn(OAc) 2 0.24...

Claims

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Application Information

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IPC IPC(8): C07C66/02C07C51/16
Inventor 袁仲飞许庆丰黄春燕
Owner 柏盛新材料(甘肃)有限公司
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