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A kind of continuous preparation method of 1-aminoanthraquinone

A technology of aminoanthraquinone and nitroanthraquinone, applied in chemical instruments and methods, preparation of organic compounds, chemical recovery, etc., can solve problems such as environmental pollution and restricted applications, achieve precise control of reaction conditions, high conversion rate, The effect of efficient production

Active Publication Date: 2017-10-17
YANGZHOU RIXING BIO TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional processes for the production of 1-aminoanthraquinone mainly include sulfonated ammonolysis method and soda sulfide method, but the "three wastes" produced in the production process have caused serious pollution to the environment and have gradually withdrawn from the historical stage
In addition, the ammonolysis method and the catalytic hydrogenation reduction method have less pollution to the environment and have attracted people's attention. However, due to the high pressure, high temperature and other conditions that are not conducive to safe production in the production process, the application in the industrial production process is greatly limited. At the same time, how to improve the utilization rate of atoms and increase the yield is also a problem that needs to be solved at present.

Method used

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  • A kind of continuous preparation method of 1-aminoanthraquinone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Palladium carbon with a mass percentage of Pd of 5% is first filled inside the fixed bed.

[0015] Mix and stir 100 g of 1-nitroanthraquinone with a purity of 99% and 2 L of toluene to form a 1-nitroanthraquinone-toluene mixture, and output it at a flow rate of 0.2 mL / min and a flow rate of 2.66 mL / min. Hydrogen is mixed, then the temperature is raised to 50°C, and the mixed raw materials enter the fixed bed (and the volume ratio of the total volume to the Pd / C catalyst after mixing 1-nitroanthraquinone and toluene is 100:5) for hydrogenation reaction, hydrogenation The response time is 100s.

[0016] The reaction liquid flowing out after the hydrogenation reaction is mixed with ammonia water (introduction rate is 0.05ml / min), and the excess H in the hydrogenation reaction is released at the same time. 2 , and then mixed with oxygen (flow rate 1.8mL / min), the residence time in the oxidation reaction module after mixing was 100s, and the oxidation reaction temperature w...

Embodiment 2

[0020] Palladium carbon with a mass percentage of Pd of 5% is first filled inside the fixed bed.

[0021] Mix and stir 100 g of 1-nitroanthraquinone with a purity of 99% and 2 L of toluene to form a 1-nitroanthraquinone-toluene mixture, and output it at a flow rate of 0.2 mL / min, and a flow rate of 2.66 mL / min The hydrogen gas is mixed, and then the temperature is raised to 80°C. The mixed raw materials enter the fixed bed (and the volume ratio of the total volume of 1-nitroanthraquinone and toluene to the Pd / C catalyst is 100:5) for hydrogenation reaction. The hydrogenation reaction time is 80s.

[0022] The reaction liquid flowing out after the hydrogenation reaction is mixed with ammonia water (0.05ml / min), and the excess H in the hydrogenation reaction is released at the same time. 2 , and then mixed with oxygen (flow rate 1.8 mL / min). After mixing, the residence time in the oxidation reaction module was 80s, and the oxidation reaction temperature was controlled at 80°C. ...

Embodiment 3

[0026] Palladium carbon with a mass percentage of Pd of 5% is first filled inside the fixed bed.

[0027] Mix and stir 100 g of 1-nitroanthraquinone with a purity of 99% and 2 L of toluene to form a 1-nitroanthraquinone-toluene mixture, and output it at a flow rate of 0.2 mL / min and a flow rate of 2.66 mL / min. Hydrogen is mixed, and then the temperature is raised to 100°C. The mixed raw materials enter the fixed bed (and the volume ratio of the total volume to the Pd / C catalyst after mixing 1-nitroanthraquinone and toluene is 100:5) for hydrogenation reaction, hydrogenation The response time is 50s.

[0028] The reaction liquid flowing out after the hydrogenation reaction is mixed with ammonia water (0.05ml / min), and the excess H in the hydrogenation reaction is released at the same time. 2 , and then mixed with oxygen (flow rate 1.8mL / min), the residence time in the oxidation reaction module after mixing is 50s, and the oxidation reaction temperature is controlled at 100°C. ...

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Abstract

A continuous preparation method for 1-aminoanthraquinone belongs to the field of organic synthesis application technology. After mixing 1-nitroanthraquinone and toluene, they are mixed with hydrogen, preheated, and then passed into a fixed catalyst filled with Pd / C The hydrogenation reaction is carried out in the bed; the reaction solution after the hydrogenation reaction is mixed with the lye, and at the same time, the excess H2 of the hydrogenation reaction is released, and then mixed with oxygen to carry out the oxidation reaction, and the oxidized reaction solution is cooled to obtain crystallized 1-aminoanthraquinone . The invention has the characteristics of high conversion rate, continuous safety, precise control of reaction conditions, reusable waste liquid and catalyst, etc., can produce 1-aminoanthraquinone in a safe, environmentally friendly and efficient manner, and the mother liquor after filtering 1-aminoanthraquinone can be Direct recycling.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and specifically relates to a production process of anthraquinone series intermediates. Background technique [0002] 1-Aminoanthraquinone is an important intermediate for the synthesis of anthraquinone dyes. It has a wide range of uses and a large consumption, and occupies an extremely important position in the dye industry. The traditional processes for the production of 1-aminoanthraquinone mainly include sulfonated ammonolysis method and soda sulfide method, but the "three wastes" produced in the production process have caused serious pollution to the environment and have gradually withdrawn from the historical stage. In addition, the ammonolysis method and the catalytic hydrogenation reduction method have less pollution to the environment and have attracted people's attention. However, due to the high pressure, high temperature and other conditions that are not conduciv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C221/00C07C225/34
CPCY02P20/584
Inventor 王文龙张超丁振中冯柏年史劲松朱萌张海东孔庆年方祥赵耀徐俊山郑莉
Owner YANGZHOU RIXING BIO TECH