Method for preparing phosphite ester oligomer as phosphoric fire retardant
A flame retardant phosphite and oligomer technology, which is applied in the field of preparation of phosphorus-containing flame retardant phosphite oligomer, can solve the problems such as the lag in the development of phosphite oligomer, and achieve stable product quality, Environmental protection, safe and easy operation
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Embodiment 1
[0024] Add 41.2g (0.3mol) of phosphorus trichloride dropwise at 20-25°C within 0.5hr to a mixture of 22.0g (0.2mol) of hydroquinone and 46.6g (0.495mol) of monophenolic compound phenol, dropwise After completing the reaction at the same temperature for 1.5 hours, add 1.8g of aluminum trichloride, raise the reaction temperature to 80°C for 2hrs, continue to raise the temperature to 120°C for 2hrs, 160°C for 2hrs, and 170°C for 6hrs. The reaction solution was washed with hot water until neutral, and dried in vacuum for 1.5 hr to obtain 61.5 g of light yellow phosphite oligomer. Measured by infrared spectroscopy, at 1011.36cm -1 The absorption peak of the P-O-C functional group appears at , indicating that a phosphite oligomer is generated, and the GPC analysis result shows that the molecular weight is 1672.
Embodiment 2
[0026] Add 43.9g (0.32mol) of phosphorus trichloride dropwise at 20-25°C within 1hr to a mixture of 22.0g (0.2mol) of hydroquinone and 46.6g (0.495mol) of monophenolic compound phenol, and the addition is complete After reacting at the same temperature for 0.5hr, add 1.8g of aluminum trichloride, raise the reaction temperature to 80°C for 1hr, continue to raise the temperature to 120°C for 1hr, 160°C for 2hr, 170°C for 8hr, and the obtained viscous reaction The solution was washed with hot water until neutral, and dried in vacuum for 1.5 hr to obtain 65.9 g of light yellow phosphite oligomer. As a result of GPC analysis, the molecular weight was 1474.
Embodiment 3
[0028] Add 41.2g (0.3mol) of phosphorus trichloride dropwise at 20-25°C within 1hr to a mixture of 33.0g (0.3mol) of hydroquinone and 27.8g (0.295mol) of monophenolic compound phenol, and the addition is complete After reacting at the same temperature for 0.5hr, add 1.8g of aluminum trichloride, raise the reaction temperature to 80°C for 1hr, continue to raise the temperature to 100°C for 1hr, 120°C for 1hr, 160°C for 2hr, 170°C for 8hr, The obtained viscous reaction liquid was washed with hot water to neutrality, and vacuum-dried for 1.5 hr to obtain 58.6 g of light yellow phosphite oligomer. As a result of GPC analysis, the molecular weight was 3268.
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