Preparation method of 1-aminoanthraquinone
A technology of aminoanthraquinone and nitroanthraquinone, applied in the field of organic chemical synthesis, can solve the problems of retention, high production cost, and no industrialization, and achieve the effects of low temperature and pressure, good product quality, and no three-waste pollution
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Embodiment 1
[0019] Embodiment 1: take 100 kilograms of 1-nitroanthraquinones to produce 1-aminoanthraquinones as an example, the catalyst used is the precious metal rhodium / carbon of loading 0.5wt%, and the total amount of catalyst used in the production process is 1% (0.1 kilogram), solvent DMF, chloroform total amount are 10 times (100 kilograms) of raw material, and concrete process is as follows:
[0020] In this embodiment, the reduction reaction occurs while maintaining the hydrogen pressure at 0.8-1 Mpa. Heat is released during the hydrogenation reaction, and the temperature of the reactor is adjusted by cooling water so that the temperature of the reactor is always controlled between 60-80°C. The reaction lasts for 60-90 minutes. After the reducing solution enters the oxidation tank, start stirring, open the oxygen valve, and let in oxygen , the oxidation reaction temperature is 20°C to 30°C, after the oxidation is completed, the filter cake is filtered to obtain the target produc...
Embodiment 2
[0022] Embodiment 2: take 200 kilograms of 1-nitroanthraquinones to produce 1-aminoanthraquinones as example, used catalyst is noble metal platinum, palladium / carbon of loading 1wt%, uses the total amount of catalyst in the production process to be 1% of raw material ( 2 kilograms), the solvent DMF total amount is 10 times (2000 kilograms) of raw material, and concrete process is as follows:
[0023] In this embodiment, the hydrogen pressure is kept at 0.8-1Mpa to generate the reduction reaction. Heat is released during the hydrogenation reaction, and the temperature of the reactor is adjusted by cooling water so that the temperature of the reactor is always controlled between 60-80°C. The reaction lasts for 60-90 minutes. After the reducing solution enters the oxidation tank, start stirring, open the oxygen valve, and feed Oxygen, the oxidation reaction temperature is 20°C to 30°C, after the oxidation is completed, the filter cake is filtered to obtain the target product 1-am...
Embodiment 3
[0025] Embodiment 3: take 1 ton of 1-nitroanthraquinone to produce 1-aminoanthraquinone as an example, the catalyst used is the precious metal platinum / carbon of loading 0.85wt%, and the total amount of catalyst used in the production process is 1% (10% of the raw material) kilogram), the solvent DMF total amount is 10 times (10 tons) of raw material, and concrete process is as follows:
[0026] In this embodiment, the hydrogen pressure is kept at 0.8-1 Mpa to generate the reduction reaction. Heat is released during the hydrogenation reaction, and the temperature of the reactor is adjusted by cooling water so that the temperature of the reactor is always controlled between 60-80°C. The reaction lasts for 60-90 minutes. After the reducing solution enters the oxidation tank, start stirring, open the oxygen valve, and feed Oxygen, the oxidation reaction temperature is 20°C to 30°C, after the oxidation is completed, the filter cake is filtered to obtain the target product 1-aminoa...
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