Preparation methods of anthracene, phenanthrene and carbazole
Application number: CN99122301.2
Application date: 19991029
Disclosure/announcement No.: CN1250768
Publication/Announcement Date: 20000419
Application/Patentee: Zheng Jinan
Inventor/Designer: Zheng Jinan
International main classification number: C07C15/28
International classification number: C07C15/28;C07C15/30;C07C5/22;C07C7/148;C07D209/82
Address: 032100 Shanxi Province Jinfeng Chemical Factory, Xicheng Village, Wenshui County
Patent agency: Shanxi Patent Service Center
Agent: Wang Jinsuo
Category classification number: 18D
p>Country and Province Code: Shanxi (14)
Number of pages of instructions: 8
Basic legal status: 20020320 Valid patent
Other legal status: 20091223 Rights transfer
Patent life cycle: 0
Instruction CD volume:
Abstract: The present invention relates to a preparation method of anthracene, phenanthrene and carbazole, Add raw material crude anthracene into the reaction kettle of xylene solvent to obtain anthracene and carbazole mixture; add anthracene and carbazole mixture into potassium soluble kettle, further add anthracene, phenanthrene and carbazole; anthracene and phenanthrene are then added to normal pressure In the evaporation kettle, a white anthracene and phenanthrene mixture is obtained; the white anthracene and phenanthrene mixture is put into a xylene solvent kettle to obtain anthracene and phenanthrene products; carbazole is added to a water-filled reaction kettle to obtain a filter cake carbazole; the filter cake is Add carbazole to the distillation kettle to obtain crude carbazole; add crude carbazole to the xylene solvent kettle and react to obtain carbazole. Anthracene, phenanthrene and carbazole are simultaneously obtained using a set of processes, with low cost and high purity.
Sovereign Item: Claim 1. A method for preparing anthracene, phenanthrene and carbazole, which includes the following steps: (1) Add raw material crude anthracene into a reaction kettle filled with xylene solvent , the ratio of crude anthracene to solvent is 1:1.2. When heated to 90-100°C, all will dissolve. The dissolved mixture is discharged into a crystallization pot with a filter cartridge. The filtrate is cooled and crystallized to 28-32°C, and then Centrifuge to obtain a mixture of anthracene and carbazole; (2) Add the anthracene and carbazole mixture into a potassium kettle containing potassium hydroxide at a ratio of 3:1, heat the reaction to 200-220°C, and keep it warm for 2 hours. After the reaction is completed, discharge the reaction material into a sealed container and cool it to 30°C. Open the sealed tank and take out the anthracene and phenanthrene in the upper layer and the carbazole in the lower layer respectively; (3) Add the anthracene and phenanthrene mixture in the upper layer to normal pressure and evaporate. In the kettle, keep the temperature at 250-270°C, and the anthracene and phenanthrene begin to float into the receiving tank to obtain a white anthracene and phenanthrene mixture; (4) Add the white anthracene and phenanthrene mixture into the reaction kettle filled with xylene solvent , the ratio is 1:2, keep it at 90-100°C, keep it warm for 1 hour, then cool to 30°C, put it into a centrifuge for separation, and get the finished product anthracene; after separation, the filtrate is put into a distillation kettle for distillation, the temperature is 150- 170°C, all the solvent is evaporated, and the finished phenanthrene is at the bottom of the kettle; (5) Crush the lower carbazole and add it to the reaction kettle with water. The ratio of water to carbazole is 3:1, and steam directly for 3 hours. , the temperature is maintained at 80-100°C, and then separated to obtain the filter cake carbazole; (6) Add the filter cake carbazole to the steaming kettle, keep the temperature at 250-270°C, and the carbazole begins to float