(1) Put in a 1000ml four-necked flask into a phenylmagnesium chloride solution as an initiator. 60g of magnesium chips were put in. Warm to reflux. 300 g of tetrahydrofuran, 420 g of toluene, and 240 g of chlorobenzene were mixed well in advance. Control the dropwise addition under reflux. Finished dripping in 3 hours. After dripping, the reflux reaction was continued for 1 hour; (2) be cooled to 80 ℃, drip the mixture of 96g phosphorus trichloride and 96g toluene, control at 80～85 ℃ 4 hours drip off, continue to react for 2 hours after dripping; (3) Cool to room temperature, and dropwise add 600 g of 10-15% dilute sulfuric acid. After dropping, continue stirring for 10 minutes. Let stand for 30 minutes. Separate the lower layer of acid water. Then wash with 600g of clean water. Finally, wash with 100 g of 30% liquid caustic soda. Fully separate the lower water phase; (4) Take the upper organic phase, heat up and distill. Steam to 120°C with no fractions, then distill under reduced pressure until the solvent is completely evaporated to dryness; (5) Cool to 60° C. or lower, add 600 g of methanol, and stir for 1 hour. Great to space temperature as well as allow mean 1 hour. Aspirate the supernatant. The temperature is increased for distillation, and the methanol is completely evaporated to dryness; (6) Transfer the remaining feed liquid to a rectifying flask for rectification. The front fraction is removed during rectification, and the main fraction is collected to obtain high-purity triphenylphosphine; (7) triphenylphosphine is heated and melted, put into the slicer to cool and slice; its concrete process is: pass chilled water into the slicer jacket, connect the power supply to rotate the slicer hub. Put the melted triphenylphosphine into the material liquid tank of the slicer, and the material liquid in the tank is driven by the rotating hub. The feed liquid is driven by the rotating hub and frozen by the freezing water to form a sheet-like solid, and then the solid is scraped off from the rotating hub with a scraper to obtain a regular sheet-like triphenylphosphine; (8) Final analysis and packaging. Experimental results: The appearance of the obtained sheet-like triphenylphosphine is: 10.2mm×8.0mm×1.1mm (length×width×thickness) The dissolving speed of the obtained sheet-like triphenylphosphine is 1 minute and 18 seconds, the specific surface area is 70.048 m2/g, the purity is 99.8%, no residual solvent, and the chromaticity is less than or equal to 10.
