A kind of preparation method of phosphorus-containing flame-retardant polyethylene cable material
A flame retardant polyethylene and cable material technology, applied in chemical instruments and methods, circuits, electrical components, etc., can solve problems such as difficulty in ensuring flame retardant effects
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[0024] The invention is a preparation method of phosphorus-containing flame-retardant polyethylene cable material, the steps of which are as follows:
[0025] (1) The steps to synthesize DHPP are:
[0026] Add 4,4'-dihydroxybenzophenone, solvent, and acid-binding agent into a reaction vessel equipped with a stirring device and a temperature control device; under inert gas protection conditions, stir at 20~-30°C for 30 minutes, then add chlorophosphoric acid Diphenyl ester, stirred at 20-30°C for 1 hour after the addition, the system changed from cloudy to clear, quenched the reaction with water, extracted 3 times with dichloromethane, washed the organic phase with deionized water 3 times, evaporated the dichloromethane to dryness under reduced pressure, A colorless liquid was obtained, and the product was separated and purified by column chromatography, and the column chromatography was petroleum ether:ethyl acetate=5:1 according to V / V, and a white solid 4,4'-diphenyl phospha...
Embodiment 1
[0047] Add 12 parts of 4,4'-dihydroxybenzophenone, 120 parts of solvent and 5 parts of triethylamine into the reaction vessel equipped with mechanical stirring and temperature control device. Blow nitrogen, stir at 20-30°C for 30 minutes, then add 30 parts of diphenyl chlorophosphate, stir at 20-30°C for 1 hour after the addition, the system turns from cloudy to clear, add water to quench the reaction, evaporate the solvent under reduced pressure, and use dichloromethane Extracted 3 times, the organic phase was washed 3 times with deionized water, dichloromethane was evaporated to dryness under reduced pressure to obtain a colorless liquid, and the product was separated and purified by column chromatography (petroleum ether: ethyl acetate=5:1, V / V). DHPP was obtained as a white solid.
Embodiment 2
[0049] Add 80 parts of DHPP, 100 parts of ethanol, and 8 parts of sodium borohydride into a reaction vessel equipped with a mechanical stirring and temperature control device. Stir at 20-30°C for 6 hours after the addition, the system turns from turbid to clear, add 15 parts of sodium hydroxide (5%wt) solution, the system becomes turbid, stir for 5 minutes, the system turns from turbid to clear. The solvent was evaporated to dryness under reduced pressure to obtain a milky white liquid, which was then extracted 3 times with dichloromethane, the organic phase was washed 3 times with deionized water, and the dichloromethane was evaporated to dryness under reduced pressure to obtain a colorless liquid. : 1, V / V) separation and purification product, obtains colorless transparent liquid DHPP-OH.
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