A kind of polysiloxane flame retardant containing hybrid structure and preparation method thereof
A technology of polysiloxane and hybrid structure, which is applied in the field of polysiloxane flame retardants and their preparation, can solve the problems of limited flame retardant elements and limited flame retardant effect of flame retardants, and achieve good flame retardant effect, Improved compatibility and high flame retardant efficiency
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Embodiment 1
[0055] 6 parts of poly(methylhydrogensiloxane-dimethylsiloxane copolymer), 6*10 -5 Parts of Karstdet catalyst and 70 parts of isopropanol were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere, and the temperature was raised to 60°C and then stirred at a constant temperature for 30 minutes; after the temperature was raised to 100°C, the 10 parts CH in a press funnel 2 =CH-NH-Si-(OCH 2 CH 3 ) 3 , 30 parts of allyl glycidyl ether and 30 parts of isopropanol were added dropwise in a four-necked flask, and the constant temperature was reacted for 24 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain a flame retardant intermediate I; The flame retardant intermediate I obtained in the step, 50 parts of phosphorus-containing active substance diphenylphosphine oxide, 0.18 parts of triethanolamine and 100 parts of isopropanol are added to a four-necked flask,...
Embodiment 2
[0061] Mix 5 parts of poly(methylhydrogensiloxane-dimethylsiloxane copolymer), 8*10 -5 Speier catalyst and 50 parts of benzene were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere. After the temperature was raised to 80°C, it was stirred at a constant temperature for 10 minutes; after the temperature was raised to 95°C, within 3 hours, the 10 copies of CH 2 =CH-COO(CH 2 ) 3 -(H 3 C)Si-(OCH 3 ) 3, 50 parts of allyl glycidyl ether, and 50 parts of benzene solution were added dropwise in a four-necked flask, and reacted at a constant temperature for 18 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain a flame retardant intermediate I; the previous step Obtained flame retardant intermediate I, 20 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and phosphorous acid (the molar ratio of the two is 1:1), 0.2 parts Triphenylphosphine and 100...
Embodiment 3
[0063] 9 parts of 1,3,5,7-tetramethylcyclotetrasiloxane, 5*10 -5 Add the Karstdet catalyst and 50 parts of toluene solvent into a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere. After heating up to 70°C, stir at a constant temperature for 25 minutes; 15 copies of CH 2 =CH-Si-(OCH 3 ) 3 , 40 parts of allyl glycidyl ether, and 40 parts of toluene solution were added dropwise in a four-necked flask, and the constant temperature was reacted for 10 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain the flame retardant intermediate I; the previous step The obtained flame retardant intermediate I, 50 parts of diphenylphosphine oxide, 0.125 parts of triphenylphosphine and 80 parts of toluene were added to a four-necked flask, equipped with a reflux condenser, a thermometer and a magnetic stirrer, and nitrogen gas was introduced, and the temperature was raised to 100 ...
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