A kind of preparation method and application of synergistic oligomeric phosphate polyol
An oligomeric phosphate and polyol technology, which is applied in the field of preparation of synergistic oligomeric phosphate polyol, can solve the problem that the flame retardant ability cannot meet the requirements of use, etc., and achieves easy industrial production, mild reaction and strong practicability. Effect
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Embodiment 1
[0033] Embodiment 1 A kind of preparation method of synergistic oligomeric phosphate polyol
[0034] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 3.0g of water in 5 minutes, heat to 50°C and react for 40 minutes; add 70g of epichlorohydrin in 5 minutes, and then add 0.25g Catalyst tetraethylammonium bromide; heated to 130 ° C for 3 hours to prepare phosphate-based polyols;
[0035] 2) Cool to 50°C, add 20g of phosphorus pentoxide, and react for 20 minutes to completely dissolve;
[0036] 3) Add 100g of epichlorohydrin, add 0.8g of catalyst tetraethylammonium bromide, raise the temperature to 115°C, react for 1h, add 40g of tetrabromophthalic anhydride, react for 3h, cool, and discharge to obtain synergistic oligomerization Phosphate polyol; it is a light yellow transparent liquid with an acid value of 11.5mgKOH / g and a viscosity of 9686 mPa.s.
Embodiment 2
[0037] Example 2 A preparation method of synergistic oligomeric phosphate polyol
[0038] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 3.5g of water in 12 minutes, heat to 65°C for 50 minutes; add 90g of epichlorohydrin in 7.5 minutes, and then add 0.35g benzyltriethylammonium chloride as a catalyst; heated to 135°C for 3 hours to obtain phosphate-based polyols;
[0039] 2) Cool to 65°C, add 25g of phosphorus pentoxide, and react for 40 minutes to completely dissolve;
[0040] 3) Add 120g of epichlorohydrin, add 0.8-1.3 parts by mass of benzyltriethylammonium chloride, raise the temperature to 120°C, react for 1h, add 50g of tetrabromophthalic anhydride, react for 3h, cool, and discharge to obtain Synergistic oligomeric phosphate polyol; the synergistic oligomeric phosphate polyol is a light yellow transparent liquid with an acid value of 11.6 mgKOH / g and a viscosity of 9201 mPa.s.
Embodiment 3
[0041] Embodiment 3 A kind of preparation method of synergistic oligomeric phosphate polyol
[0042] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 4.0g of water in 10 minutes, heat to 80°C for 60 minutes; add 110 parts by mass of epichlorohydrin in 10 minutes, and then add 0.45 g of catalyst benzyltriethylammonium chloride; heated to 140 ° C for 3 hours to obtain phosphate-based polyols;
[0043] 2) Cool to -80°C, add 30 parts by mass of phosphorus pentoxide, and react for 40 minutes to completely dissolve;
[0044] 3) Add 140g of epichlorohydrin, add 1.3g of catalyst, raise the temperature to 125°C, react for 1h, add tetrabromophthalic anhydride-60g, react for 3h, cool, and discharge to prepare synergistic oligophosphate polyol; It is a light yellow transparent liquid with an acid value of 10.4mgKOH / g and a viscosity of 8974 mPa.s.
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