A kind of phosphorus-containing poss and its preparation method and application in flame retardant
A synthesis method and solvent technology are applied to phosphorus-containing POSS and its preparation, and the application field of flame retardants, which can solve the problems of low phosphorus-containing rate, high reaction temperature, poor phosphorus-silicon synergistic flame-retardant effect, etc., and the method is simple. Efficient, low cost, high practical value effect
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Embodiment 1
[0041] Such as figure 1 The preparation flow chart in is shown in: under constant temperature conditions, add 200mL of methanol, 20mL of concentrated hydrochloric acid and 5mL of deionized water to the reactor in sequence, stir mechanically and slowly add 10mL of silane coupling agent KH-590 to the mixture, heat Reflux and stir at 90°C for 30 hours, cool to room temperature to obtain a white viscous precipitate, wash the precipitate with acetone and dry it in a vacuum oven for 12 hours to obtain a white solid which is SHPOSS. At room temperature, take 1mmol SHPOSS and 8mmol vinyl diethyl phosphate and place it in 60mL of dichloromethane solvent, and add a photocatalyst DMPA with a mass fraction of 3% to the mixture, and magnetically stir it under 405nm ultraviolet light for 15min The product was obtained by removing the solvent with a rotary evaporator.
Embodiment 2
[0043] Under constant temperature conditions, add 200mL of methanol, 20mL of concentrated hydrochloric acid and 5mL of deionized water into the reactor successively, mechanically stir and slowly add 10mL of silane coupling agent KH-580 into the mixture, heat to 90°C and reflux for 30h, cool After reaching room temperature, a white viscous precipitate was obtained. The precipitate was washed with acetone and dried in a vacuum oven for 12 hours to obtain a white solid, namely SHPOSS. At room temperature, take 1mmol SHPOSS and 8mmol vinyl diethyl phosphate and place it in 60mL of dichloromethane solvent, and add a photocatalyst DMPA with a mass fraction of 3% to the mixture, and magnetically stir it under 405nm ultraviolet light for 15min The product was obtained by removing the solvent with a rotary evaporator.
Embodiment 3
[0045] Under constant temperature conditions, add 230mL of ethanol, 20mL of concentrated sulfuric acid and 5mL of deionized water to the reactor successively, mechanically stir and slowly add 10mL of silane coupling agent KH-580 to the mixture, heat to 90°C and reflux for 30h, cool After reaching room temperature, a white viscous precipitate was obtained. The precipitate was washed with acetone and dried in a vacuum oven for 12 hours to obtain a white solid, namely SHPOSS. At room temperature, take 1mmol SHPOSS and 8mmol vinyl diethyl phosphate and place it in 60mL of dichloromethane solvent, and add 3% photocatalyst benzoin ethyl ether to the mixture, and magnetically stir for 15min under 405nm ultraviolet light Afterwards, the solvent was removed with a rotary evaporator to obtain the product.
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