A kind of trioctyl phosphine oxide compound and preparation method thereof
A technology of trioctyl phosphine oxide and dioctyl phosphine chloride is applied in the field of trioctyl phosphine oxide compound and preparation thereof, can solve the problems of unfavorable industrial application, low yield, high toxicity and the like, achieves easy control, The effect of convenient purification and enhanced safety
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Embodiment 1
[0051] The synthesis of trioctylphosphine oxide, taking n-octene as an example, comprises the following steps:
[0052]1) Octene addition:
[0053] Add 10g (0.114mol) of sodium hypophosphite into 50ml of acetic acid, heat to 120°C, slowly drop in 30g (0.268mol) of n-octene, continue heating to 135°C for 4 hours, and use 31 PNMR detects the end point of the reaction. After the reaction is completed, cool, add water and chloroform to remove the acid, distill under reduced pressure (400Pa, 35°C) to remove the organic solvent, and vacuum dry (120Pa, 25°C) to obtain a white solid dioctylphosphine Sodium phosphate 30.8g (0.106mol). Yield 93.2%.
[0054] 2) Trichlorosilane reduction
[0055] Put 2g (0.007mol) of sodium dioctylphosphinate obtained in Step 1 into a 50ml airtight reaction kettle, add 30ml of chloroform (water has been removed) as a solvent, add 2g (0.015mol) of trichlorosilane, 80°C 16 hours of reaction, 31 The end point of the reaction was detected by PNMR. After ...
Embodiment 2
[0061] The difference with embodiment 2 lies in the processes after step 2.
[0062] 1) Hydrolysis: Dissolve 2 g (0.007 mol) of dioctylphosphine chloride obtained in step 2 in Example 1 in 20 ml of chloroform, add distilled water for hydrolysis, 31 The end point of the reaction was detected by PNMR. After the reaction was completed, lye was added to separate the liquid, the water layer was removed, chloroform (400 Pa, 35° C.) was distilled off under reduced pressure, and 1.73 g (0.006 mol) of white solid dioctylphosphine oxide was obtained by vacuum drying. Yield 92.9%.
[0063] 2) Addition of octene again: put 2g of dioctylphosphine oxide (0.007mol) into 20ml of acetic acid, after heating to 120°C, slowly drop in 2.2 (0.020mol)g of octene, continue heating to 135°C for 8 hours , 31 PNMR detects the end point of the reaction. After the reaction is completed, add chloroform and distilled water, remove acetic acid, remove chloroform (400Pa, 35°C) by distillation under reduced ...
Embodiment 3
[0065] Dissolve 2 g (0.007 mol) of dioctylphosphine chloride obtained in step 2 in Example 1 in 20 ml of chloroform, add 1 g (0.0077 mol) of n-octanol, and react at 50 ° C for 2 hours. 31 PNMR detects the end point of the reaction. After the reaction is completed, water is added, and chloroform (400Pa, 35° C.) and excess n-octanol (400 Pa, 65° C.) are removed by distillation under reduced pressure to obtain 2.57 g of white solid trioctylphosphine oxide (0.0067 mol). Yield 95.1%
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