Study On The Synthesis And Purification Process Of Phenylcarbazole Based On High Gravity Technology

OLED,also known as Organic Light Emitting Diode,stands out in the display industry with its various advantages and is a new type of display technology with great potential for development.Carbazole materials have shown excellent photoelectric properties due to their special molecular structure,and have been widely used in the field of OLED.In recent years,carbazole derivatives with various structures have emerged in endlessly,but the relevant research usually focuses on the high performance brought by molecular structure design,and less attention is paid to the research of material purification and synthesis process technology for large-scale product application.In this paper,phenylcarbazole,a commonly used carbazole material,is selected as the research object.Based on the principles and methods of molecular chemical engineering,a new process of preparing phenylcarbazole by high gravity enhanced Ullmann reaction is proposed.Through solubility measurement and modeling,the solubility database of intermediate materials for OLED has been enriched and improved,and a new method of purifying phenylcarbazole materials by high gravity solvent antisolvent method is developed.The main research contents are as follows:(1)The Ullmann reaction in the preparation of phenylcarbazole materials was enhanced by high gravity technology,and the effects of various factors on the experiment were studied.The results showed that using a high gravity reactor can increase the yield of the reaction compared to traditional stirred reactors at the same temperature and environment.The use of a high gravity reactor combined with a traditional reactor,using CuI as a catalyst,and in an alkaline environment can increase the 24 hours reaction yield from 68.36% to72.82%.(2)The solubility data of phenylcarbazole in twelve solvents at 278.15K-313.15 K under standard atmospheric pressure were measured.The results showed that the solubility of phenylcarbazole increased with the increase of temperature.The modified Apelblat equation was used to correlate the solubility data,and the correlation results were good.The obtained data provides support for the design and optimization of the recrystallization and purification process of phenylcarbazole.(3)Based on the data of solubility,the purification experiment of phenylcarbazole was guided,and the micro mixing and mass transfer between solvent and antisolvent were enhanced by high gravity.The research results showed that when acetonitrile was used as the solvent and methanol as the antisolvent,and the solution volume ratio was 1:10,the purity of the sample obtained from single purification in the high gravity reactor was 98.54%.Compared with the ordinary beaker experiment,the purification efficiency was significantly improved,it can provide scientific guidance for process optimization in the production process.