Mixed glycol polyphosphonate compounds
A phosphonate, reaction mixture technology, applied in the field of new polyphosphonate compounds, can solve problems such as limitations
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Embodiment 1
[0060] Preparation of polyphosphonate oligomers from diethylene glycol and bisphenol A (6:1 molar ratio)
[0061] Diethylene glycol (31.8 g, 0.3 mol), bisphenol A (11.4 g, 0.05 mol) and trimethyl phosphite (49.6 g, 0.4 mol) were added to the reaction vessel. The mixture was heated to 150°C in air. A total of 20.7 g of methanol was distilled off from the reaction mixture. The temperature was lowered to 100°C and trimethyl phosphite (5.5 g) was added. After heating at 150°C for 5 hours, 31 The P NMR spectrum shows that the phosphite has been fully converted to the phosphonate. There is no need to add catalysts for Arbuzov-type rearrangement reactions. The reaction mixture was subjected to a vacuum of 5 mm Hg at 120°C for 1 hour to remove volatile components. The residual product was a colorless liquid with an acid number of 0.7 and a hydroxyl number of 12.4.
Embodiment 2
[0063] Preparation of polyphosphonate oligomers from diethylene glycol and bisphenol A (6:1 molar ratio)
[0064] In the scale-up test of Example 1, diethylene glycol (572.4 g; 5.4 mol), bisphenol A (205.2 g; 0.9 mol) and trimethyl phosphite (892.8 g; 7.2 mol) were added to the reaction vessel. The mixture was heated and maintained at 150°C for 7 hours under air. A total of 399.1 grams of methanol was distilled from the reaction mixture. 31 The P NMR spectrum shows that the phosphite has been fully converted to the phosphonate. The condition of this reaction vessel is at 150 DEG C, under the vacuum degree of 2mm mercury column vacuum distillation 1 hour, blow nitrogen 30 minutes, obtain the colorless viscous liquid that acid value is 1.0 and hydroxyl number is 40. The product had a viscosity of 9500 cps.
Embodiment 3
[0066] Preparation of polyphosphonate oligomers from diethylene glycol and bisphenol A (molar ratio 5.8:0.2)
[0067] Diethylene glycol (30.7 g; 0.29 mol), bisphenol A (2.3 g; 0.01 mol) and trimethyl phosphite (43.4 g; 0.35 mol) were charged to the reaction vessel. The mixture was heated at 110°C for 1 hour, the temperature was brought to 90°C and trimethyl phosphite (3.1 g) was added. The mixture was reheated to 120°C for 1 hour. 19.2 g of methanol were collected. Chlorinated toluene (12.1 g, 0.1 mol) was added to the mixture, the temperature was maintained at 120°C for 1 hour, and the temperature was gradually lowered to 60°C after 2 hours of continuous heating at 120°C. After that, methyl iodide (0.5 mL) was added, and the temperature was continued to 120° C. for 3 hours. 31 The P NMR spectrum shows that the phosphite has been fully converted to the phosphonate. At 120° C. and a vacuum of 5 mm Hg, heat to 120° C. for 1 hour to obtain a colorless liquid with an acid va...
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