Phosphorus-containing flame-retardant hardeners, epoxy resins, advanced epoxy resins and cured epoxy resins
a flame-retardant hardener and phosphorus technology, which is applied in the direction of printed circuits, circuit susbtrate materials, electrical equipment, etc., can solve the problems of not meeting safety requirements, generating toxic and corrosive fumes, etc., and achieves high glass transition temperature (tg), high decomposition temperature, and high elastic modulus
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preparation example 1 -
Preparation Example 1-A (P-1-A, ODOPM-BPA-A):
To an one liter four-inlet flask equipped with a thermocouple and temperature controller, a reflux condenser, a nitrogen feed and a mechanical stirrer, 1 mole (228 g) bisphenol-A (BPA) was added, heated to 170° C. and then stirred to a molten state. 0.7 g (0.3 wt %) potassium acetate was mixed with the molten BPA followed by adding slowly 1 mole (246 g) 2-(6-oxid-6H-dibenz<c,e><1,2>oxa-phosphorin-6-yl) methanol (ODOPM). The mixture was heated gradually to a temperature of 220° C. when the addition of ODOPM was completed. The substitution reaction was continued for 6 hours. The reaction product was dissolved in cyclohexanone, and washed with water several times before the solvent was evaporated under vacuum to obtain ODOPM-BPA-A (P-1-A). Yield, 98%; softening temperature, 125-132° C. Phosphorus content: 6.79%.
preparation example 1-b (
P-1-B, ODOPM-BPA-A):
To an one liter four-inlet flask equipped with a thermocouple and temperature controller, a reflux condenser, a nitrogen feed and a mechanical stirrer, 1 mole (228 9) bisphenol-A (BPA) was added, heated to 170° C. and then stirred to a molten state. 1.14 g (0.5 wt %) potassium acetate was mixed with the molten BPA followed by adding slowly 1.5 mole (369 g) ODOPM. The mixture was heated gradually to a temperature of 220° C. when the addition of ODOPM was completed. The substitution reaction was continued for 8 hours. The reaction product was dissolved in cyclohexanone, and washed with water several times before the solvent was evaporated under vacuum to obtain ODOPM-BPA-B (P-1-B). Yield, 96%; softening temperature, 136-140° C. Phosphorus content: 8.16%.
preparation example 1-c (
P-1-C, ODOPM-BPA-A):
To an one liter four-inlet flask equipped with a thermocouple and temperature controller, a reflux condenser, a nitrogen feed and a mechanical stirrer, 1 mole (228 g) bisphenol-A (BPA) was added, heated to 170° C. and then stirred to a molten state. 1.14 g (0.5 wt %) potassium acetate was mixed with the molten BPA followed by adding slowly 2 mole (492 g) ODOPM. The mixture was heated gradually to a temperature of 220° C. when the addition of ODOPM was completed. The substitution reaction was continued for 10 hours. The reaction product was dissolved in cyclohexanone, and washed with water several times before the solvent was evaporated under vacuum to obtain ODOPM-BPA-C (P-1-C). Yield, 92%; softening temperature, 143-148° C. Phosphorus content: 9.06%.
Preparation Example 2 (P-2, DPOM-BPA):
To an one liter four-inlet flask equipped with a thermocouple and temperature controller, a reflux condenser, a nitrogen feed and a mechanical stirrer, 1 mole (228 g) bisphe...
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