Polyphosphinate monomer, polyphosphinate and preparation method of polyphosphinate
A technology of polyphosphinate and monomers, which is applied in the field of polymer chemistry, can solve the problems that the performance cannot meet the existing needs, and achieve the effect of easy realization and simple preparation method
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[0035] The invention also provides a preparation method for the above-mentioned polyphosphinate. The steps include: contacting phosphonyl chloride with diazomethane to obtain polyphosphinate.
[0036] Preferably, the molar ratio of phosphonyl chloride to diazomethane is 1:2-1:6, more preferably: 1:4.
[0037] Among them, the preferred temperature is -20-100°C, the contact time is 1-72 hours, and the reaction conditions are further optimized. In the present invention, there is no special limitation on the order of adding phosphonyl chloride and diazomethane. It can be prepared by adding diazomethane to phosphonyl chloride, or by gradually mixing phosphonyl chloride and diazomethane at the same time. It preferably includes slowly adding phosphonyl chloride In the solution of diazomethane, the preferred rate of addition is 1-3 mL / min, and the slow addition and reaction can be carried out under the condition of stirring to make the reaction uniform, and the rate of stirring can be...
Embodiment 1
[0053] 1. Preparation of monoethyl benzylphosphonate
[0054] Dissolve 2.28 g (10 mol) of diethyl benzylphosphonate in 50 mL of ethanol, add 0.8 g (20 mol, 2eq) of NaOH, heat and reflux for 4 hours, and the solution turns orange. Then add 1.2 g (30 mol, 3 eq) NaOH, heat and reflux for 4.5 hours, then cool to room temperature, add 3 mol / L hydrochloric acid until the solution becomes acidic, spin out part of the solvent and extract with 3×25 mL dichloromethane, take the lower layer of liquid After spin-drying the solvent, recrystallize with dichloromethane: ether: petroleum ether = 1:2:49 (V / V) to obtain 1.537 g of colorless crystal benzylphosphonic acid monoethyl ester, yield 76.9%, mp. 68- 69°C (Lit. 63-64°C).
[0055] 2. Preparation of Ethoxybenzylphosphonochloride
[0056] Dissolve 0.5 g (2.5 mmol) of monoethyl benzylphosphonate in 0.60 g (5 mmol, 2eq) of SOCl 2 , heated to reflux under nitrogen protection for 12 hours, and distilled under reduced pressure to remove exces...
Embodiment 2
[0065] 1. Preparation of Monoethyl Ethyl Phosphonate
[0066] 1.7 g (10 mmol) diethyl ethylphosphonate was mixed with 1.2 g (30 mmol) NaOH and dissolved in 100 mL ethanol solution, heated to 100 °C under electromagnetic stirring and maintained at the temperature for 4 hours. After cooling to room temperature, distill off ethanol, add 10 mL of water and 10 mL of CH 2 Cl 2 , after liquid separation, the aqueous phase was acidified with 3 mol / L hydrochloric acid to pH = 1, extracted with 3×15 mL dichloromethane, the organic phases were combined and dried over anhydrous sodium sulfate, and the solvent was distilled off to obtain a colorless liquid ethylphosphonic acid mono Ethyl ester 0.4 g, yield 29%.
[0067] 2. Preparation of Ethoxyethylphosphonyl Chloride
[0068] Add 0.69 g (5 mmol) of monoethyl ethylphosphonate dropwise into 0.78 g (6.5 mmol) of thionyl chloride, heat to reflux for 8-12 hours under nitrogen protection, cool to room temperature, and remove thionyl chloride...
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