Silicon-phosphorus hybrid flame retardant, preparation method thereof and silicon-phosphorus hybrid emulsion
A flame retardant and hybridization technology, applied in the field of flame retardants, can solve the problems of limited research and achieve the effect of simple preparation method, few steps and easy operation
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[0050] The present invention provides a method for preparing a silicon-phosphorus hybrid flame retardant described in the above scheme, comprising the following steps:
[0051] Carrying out nucleophilic addition reaction of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and p-hydroxybenzaldehyde in a benzene solvent to obtain a compound having the structure shown in formula a;
[0052]
[0053] Under the action of an acidic catalyst, the compound having the structure shown in formula a and γ-glycidyl etheroxypropyl trimethoxysilane are subjected to ring-opening addition reaction in an organic solvent to obtain the silicon compound having the structure shown in formula I Phosphorized flame retardants.
[0054]In the present invention, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and p-hydroxybenzaldehyde (HBA) are subjected to nucleophilic addition reaction in a benzene solvent to obtain A compound (DOPO-HBA) having the structure shown in formula a. In the...
Embodiment 1
[0099] Using xylene as a solvent, 0.02mol of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and 0.22mol of p-hydroxybenzaldehyde (HBA) were heated and refluxed at 125°C After 5 hours of reaction, the product was filtered with suction, washed with absolute ethanol three times, and dried in a vacuum oven at 80° C. for 60 minutes to obtain DOPO-HBA as a white solid.
[0100] Dissolve 0.02 mol of dehydrated γ-glycidyl etheroxypropyl trimethoxysilane (GPTMS) in DMF as a solvent, then add DOPO-HBA0.048 mol and catalyst triphenylphosphine (the addition amount is GPTMS) dropwise to the system at 130°C 0.8% of the total mass of DOPO-HBA), heated up to 150 ° C for 4 hours, and after the reaction was completed, the product was distilled under reduced pressure to obtain a flame retardant (DDPSi-FR) with a structure shown in Formula I, which was a brownish-yellow liquid.
[0101] Use infrared spectrometer to detect gained DOPO, HBA and DOPO-HBA, gained infrared spectrum is as fo...
Embodiment 2
[0104] With toluene as solvent, 0.01mol of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and 0.01mol of p-hydroxybenzaldehyde (HBA) were heated and refluxed at 130°C for 4.5 h. After the reaction was completed, the product was filtered with suction, washed with absolute ethanol three times, and dried in a vacuum oven at 85° C. for 50 min to obtain DOPO-HBA as a white solid.
[0105] Dissolve 0.02mol of dehydrated γ-glycidyl etheroxypropyltrimethoxysilane (GPTMS) with carbon tetrachloride as a solvent, then add DOPO-HBA0.045mol and catalyst triphenylphosphine dropwise to the system at 130°C (add The amount is 1% of the total mass of GPTMS and DOPO-HBA), and the temperature is raised to 160° C. for 3.5 hours. After the reaction is completed, the product is distilled under reduced pressure to obtain a flame retardant (DDPSi-FR) having a structure shown in formula I, which is brown yellow liquid.
[0106] The obtained DOPO-HBA and DDPSi-FR were detected by infrared sp...
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