A kind of phosphorus-containing halogen-free epoxy resin and its preparation method and composite flame-retardant material
A technology based on epoxy resin and epoxy resin, which is applied in the field of epoxy resin flame retardancy, can solve the problems of high phosphorus leaching, poor water decomposition resistance and chemical resistance, and affect the performance and appearance of the insulating layer of the board. Excellent flame retardancy and chemical resistance
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[0033] The invention provides a preparation method of phosphorus-containing halogen-free epoxy resin, which comprises the following steps:
[0034] 1) Provide melting of novolac polyglycidyl ether, o-cresol epoxy resin, tetrafunctional epoxy resin and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide mixture;
[0035] 2) The molten mixture obtained in step 1) is subjected to a first catalytic reaction under the action of a triphenylphosphine catalyst to obtain an intermediate product;
[0036] 3) Mix the intermediate product obtained in step 2) with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and perform the second catalysis under the action of a triphenylphosphine catalyst Through the reaction, a phosphorus-containing halogen-free epoxy resin is obtained.
[0037] In the present invention, the epoxy equivalent of the novolac polyglycidyl ether is preferably 170-200 g / eq, more preferably 175-185 g / eq; the epoxy equivalent of the o-cresol novolac epoxy resin is preferably 200...
Embodiment 1
[0061] 220g novolac polyglycidyl ether, 230g o-cresol epoxy resin, 51g tetrafunctional epoxy resin and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 47.2g Mix, heat up to 120°C and melt for 30 minutes. During the temperature up process, the solvent acetone in the tetrafunctional epoxy resin volatilizes in the form of steam.
[0062] To the above molten mixture, 0.12 g of the catalyst triphenylphosphine was added, and the reaction was carried out at 160°C for 2 hours. Then, 70 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added to the reaction vessel, and the reaction was continued at 160° C. for 4 hours to obtain a phosphorus-containing halogen-free epoxy resin.
[0063] The present invention monitors the molecular weight distribution of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in real time by GPC method, and it can be known that the 9,10-dihydro-9-oxa -10-Phenanthroline-10-oxide content. When the content of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-1...
Embodiment 2
[0068] 211g novolac polyglycidyl ether, 232g o-cresol epoxy resin, 50g tetrafunctional epoxy resin and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 47.2g Mix, heat up to 117°C, melt for 45 minutes, and evaporate the solvent acetone in the tetrafunctional epoxy resin during the heating process.
[0069] To the above molten mixture, 0.15 g of the catalyst triphenylphosphine was added, and the reaction was carried out at 165°C for 1 hour. Then, 71 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added to the reaction vessel, and the reaction was continued at 165° C. for 4 hours to obtain a phosphorus-containing halogen-free epoxy resin.
[0070] Take 600g of the phosphorus-containing halogen-free epoxy resin prepared above, add 67g of bisphenol A epoxy resin with a molecular weight of 4500-5500 and 25g of bisphenol A epoxy resin with a molecular weight of 800-1000, at 160℃ , Heat preservation for 45 minutes to obtain a composite flame retardant material.
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