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The method of hydrogen peroxide oxidation synthesis 2 carboxyl anthraquinone

A carboxyl anthraquinone, oxidation synthesis technology, used in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of metal equipment corrosion, waste water, high equipment price, achieve low equipment corrosion, easy industrialization , the effect of high product quality

Active Publication Date: 2017-04-05
柏盛新材料(甘肃)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] 2) Using dichloro(triphenylphosphine) palladium complex and triphenylphosphine as a catalyst, 2-chloroanthraquinone reacts with CO at 25 atmospheres, 170°C, and the yield is 92%; the method has high pressure and relatively low catalyst Expensive, CO is easily poisoned
[0006] 3) Dilute 2-methylanthraquinone in acetic acid medium with CrO 3 Oxidation; 2-methylanthraquinone is more expensive in this process, and the pollution of chromium salt wastewater is serious
[0007] 4) Oxidation of 2-methylanthraquinone with air in acetic acid medium at 200°C, 26 atmospheres, Co(OAc) 2 , Mn(OAc) 2 , NaBr catalytic oxidation to obtain 2-carboxyanthraquinone; the method acetic acid solvent and 2-methylanthraquinone are more expensive, high temperature, high pressure, high equipment price
[0008] 5) 2-Methylanthraquinone with CrO 3 、H 3 PO 4 Oxidation with a yield of 95%; this method is more expensive for 2-methylanthraquinone and phosphoric acid, and the acidic wastewater containing heavy metal chromium is difficult to treat and purify
[0009] 6) The method of synthesizing 2-carboxyanthraquinone by oxidizing 2-ethylanthraquinone with potassium dichromate. This method produces too much waste water containing heavy metal chromium, which is difficult to treat, and the heavy metal content in the product is high, which seriously affects the use of downstream customers. Sulfuric acid medium severely corrodes metal equipment

Method used

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  • The method of hydrogen peroxide oxidation synthesis 2 carboxyl anthraquinone
  • The method of hydrogen peroxide oxidation synthesis 2 carboxyl anthraquinone
  • The method of hydrogen peroxide oxidation synthesis 2 carboxyl anthraquinone

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 50g of 2-ethylanthraquinone to 150g of 35% hydrogen peroxide, then add 0.5g of surfactant sodium dodecylbenzenesulfonate and 4g of catalyst γ-aluminum oxide, the average particle size of γ-aluminum oxide at 50nm. After adding, stir, slowly heat up to 85 ° C, carry out oxidation reaction, and keep the reaction for 10 hours; when the insulation is completed, cool to normal temperature, add 200 mL of water to dilute, stir and cool to room temperature, filter, wash with water, filter, and bake the filter cake at 90 ° C Dry to obtain 2-carboxyanthraquinone with a yield of 95.1%.

Embodiment 2

[0023] Add 50g of 2-ethylanthraquinone to 250g of 27.5% hydrogen peroxide, then add 1.0g of surfactant sodium dodecylbenzenesulfonate and 5g of catalyst γ-aluminum oxide, the average particle size of γ-aluminum oxide at 20nm. After adding, stir, slowly heat up to 75 ° C, carry out oxidation reaction, and keep the reaction for 6 hours; when the insulation is completed, cool to normal temperature, add 200 mL of water to dilute, stir and cool to room temperature, filter, wash with water, filter, and bake the filter cake at 90 ° C After drying, 2-carboxyanthraquinone was obtained with a yield of 94.8%.

Embodiment 3

[0025] Add 50g of 2-ethylanthraquinone to 300g of 20% hydrogen peroxide, then add 0.5g of surfactant sodium dodecylbenzenesulfonate and 2.5g of catalyst γ-aluminum oxide, γ-aluminum oxide average particle size The diameter is 100nm. After adding, stir, slowly heat up to 95 ° C, carry out oxidation reaction, and keep the reaction for 12 hours; when the insulation is completed, cool to room temperature, add 200 mL of water to dilute, stir and cool to room temperature, filter, wash with water, filter, and bake the filter cake at 90 ° C Dry to obtain 2-carboxyanthraquinone with a yield of 94.5%.

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Abstract

The invention relates to a method for oxidative synthesis of 2-carboxyl anthraquinone through hydrogen peroxide. 2-ethylanthraquinone conducts a catalytic oxidation reaction with hydrogen peroxide under the condition that a catalyst exists, and then 2-carboxyl anthraquinone is prepared. The method has the advantages that operation is convenient, cost is low, pollution is low, and industrialization is easy; synthesized 2-carboxyl anthraquinone can serve as a new material to be widely applied to the industries such as pigments, textiles, electronics and papermaking.

Description

technical field [0001] The invention relates to a method for synthesizing 2-carboxyl anthraquinone, in particular to a hydrogen peroxide oxygen [0002] A method for the synthesis of 2-carboxyanthraquinone. Background technique [0003] The existing method for synthesizing 2-carboxyl anthraquinone mainly includes: [0004] 1) Oxidize 2-ethylanthraquinone with an aqueous nitric acid solution at 190 °C under 20 atmospheres for 1 hour, and the yield is 93%; the process temperature is high, an autoclave is required, and the acid water is seriously corroded. [0005] 2) Using dichloro(triphenylphosphorus) palladium complex and triphenylphosphorus as catalysts, 2-chloroanthraquinone reacts with CO at 25 atmospheres, 170 °C, and the yield is 92%; Expensive and easily poisoned by CO. [0006] 3) Dissolve 2-methylanthraquinone in acetic acid medium with CrO 3 Oxidation; 2-methylanthraquinone is more expensive in this process, and the chromate wastewater is seriously polluted. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C66/02C07C51/285
CPCC07C51/285C07C66/02
Inventor 张天永李彬袁仲飞黄彩红
Owner 柏盛新材料(甘肃)有限公司