A kind of preparation method of 9,9-bis[(4-hydroxyethoxy)phenyl]fluorene
A technology of hydroxyethoxy and phenyl, applied in the field of compound synthesis, can solve the problems of large amount of waste water, high raw material cost, low product content, etc., and achieve the effects of improving product and content, simplifying operation process and simple process route
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Embodiment 1
[0022] Add 35KG bisphenol fluorene, 11.2KG potassium hydroxide, and 140KG toluene to the high-pressure reactor, replace the air in the reactor with nitrogen, and add 9.0KG of liquid ethylene oxide under the protection of nitrogen, seal the reactor, and slowly Raise the temperature to 100°C, and keep it warm at 100°C for 6 hours. After the reaction, cool down to 20-30°C, then remove the pressure in the reactor, and then heat up to 90-100°C for hot filtration to obtain a filter cake For the next batch of application, the filtrate is added to the reaction kettle, under stirring, slowly lower the temperature to 5-10°C, and stir at 5-10°C for 2 hours, use toluene in the system as a recrystallization solvent to fully crystallize the reaction product, filter , 37.5KG was obtained after drying, the HPLC normalized content was 99.3%, and the yield was 85.6%.
Embodiment 2
[0024] Add 105KG bisphenol fluorene, 25.2KG sodium hydroxide and 315KG xylene to the high-pressure reactor, replace the air in the reactor with argon, and add 21.1KG of liquid ethylene oxide under the protection of argon, and seal the reaction Slowly raise the temperature to 110°C, and keep it warm at 110°C for 4 hours. After the reaction, cool down to 20-30°C, then remove the pressure in the reactor, and then heat up to 100-110°C for hot filtration. Add the filtrate to the reaction kettle, slowly lower the temperature to 10-15°C, stir at 10-15°C for 4 hours, use xylene in the system as a recrystallization solvent to fully crystallize the reaction product, filter, and dry to obtain 104.5KG, HPLC The normalized content is 99.4%, and the yield is 79.5%.
Embodiment 3
[0026] In the autoclave, add 35KG bisphenol fluorene, 11.5KG potassium hydroxide (the filter cake that reclaims in embodiment 1) and 175KG toluene, replace the air in the autoclave with nitrogen, and under nitrogen protection, add liquid ring Oxygen 10.6KG, seal the reactor, slowly heat up to 100°C, and keep warm at 100°C for 8 hours, after the reaction, cool down to 20-30°C, then remove the pressure in the reactor, and then raise the temperature to 90 Heat filtration at ~100°C to obtain a filter cake for the next batch of mechanized use. The filtrate is added to the reaction kettle, and the temperature is slowly lowered to 5-10°C under stirring, and stirred for 3 hours at 5-10°C. Using the toluene in the system As a recrystallization solvent, the reaction product was fully crystallized, filtered, and dried to obtain 34.5KG, with an HPLC normalized content of 99.7% and a yield of 78.8%.
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