Composite structural phosphorus fire retardant containing poly-DOPO cyclic phosphate and preparation method thereof
A technology of cyclic phosphate ester and composite structure, which is applied in the field of flame retardants, can solve the problems that affect the wide use, difficult to disperse uniformly, poor compatibility, etc., and achieve the effects of good flame retardant effect, convenient use, and high flame retardant efficiency
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[0031] Example 1
[0032] A 3-liter four-necked flask was equipped with a mechanical stirrer, an H-type oil-water separator, a reflux condenser, a dropping funnel and a nitrogen inlet. Add 253.3 grams (1.172mol) DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), 100.6 grams of p-xylene, 800 grams of PXE (1,1-double (3,4-Dimethylphenyl)ethane) solvent and 56.45 grams of glycerol solution (53.9 grams (0.586 mol) of glycerol dissolved 2.55 grams of sodium iodide). After the oil-water separator is filled with p-xylene, the reaction mixture is heated to 200°C for 14 hours under the protection of nitrogen flow, and the water produced is continuously discharged through the oil-water separator during the reaction. In the later stage of the reaction, less water is generated, so increase the reaction temperature to 205°C and react for 2 hours. After the reaction, when the temperature of the system drops to room temperature, 29.94 grams (0.195 mol) of phosphorus oxychloride is add...
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[0033] Example 2
[0034] According to the procedure of Example 1, only the reactant 56.45g glycerol solution was replaced with 64.67g butanetriol solution (62.12g 1.2.4-butanetriol dissolved 2.55g sodium iodide), and the amount of other reactants and solvents was not change. And after the reaction mixture is cooled to room temperature, before the dropwise addition of phosphorus oxychloride, 150 ml of pyridine is added to the reaction flask. The reaction product is a pale yellow syrupy liquid, labeled as P2, the yield is about 81%, and the phosphorus content is 13.98%. 1HNMR: 7.13-7.95 ppm, m, 16H (H-Ar); 2.60-2.88-ppm, m, 6H (CH2); 3.54 ppm, m, 1H (CH). 13CNMR: 119.9-150.2 ppm (C-Ar); 38.8-39.3 ppm (CH2); 50.1 ppm (CH). 31PNMR: 37.12-37.34ppm (DOPO structural chiral isomer mixture); -5.8ppm ((-O-)3P(O)).
Example Embodiment
[0035] Example 3
[0036] 53.13 g (0.391 mol) of pentaerythritol was dissolved in 160 ml of ethanol, 2.55 g of sodium iodide was added thereto, the mixture was heated to reflux for 2 hours, and then the ethanol was gradually evaporated to prepare a reaction mixture of pentaerythritol and sodium iodide. This mixture was substituted for the glycerol solution in Example 1 as the reactant, and the amount of other reactants and solvents remained unchanged, and the reaction was carried out according to the procedure of Example 1. And after the reaction mixture is cooled to room temperature, before the dropwise addition of phosphorus oxychloride, 150 ml of pyridine is added to the reaction flask. The product is a white solid, labeled as P3, with a yield of 86% and a phosphorus content of 13.84%. 1HNMR: 7.29-8.02 ppm, m, 24H (H-Ar); 2.42 ppm, s, 6H (P-CH2-C); 3.89 ppm, s, 2H (C-CH2-O). 13CNMR: 119.9-150.2 ppm (C-Ar); 39.7 ppm (CH2); 69.0 ppm (CH2), -4.8 ppm (tert-C). 31PNMR: 37.12-37....
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