反应详情

温度

30 °C

To a 2-liter 4-neck flask equipped with a -10° C. Friedrichs condenser, thermometer, mechanical stirrer, and 0.16 centimeter in diameter dip tube are added 180 grams (0.79 moles) of bisphenol-A and 880 mL of methanol containing 4 wt. % water. Bromine (513 grams, 3.2 moles) was fed with a peristaltic pump to a 1.8 meter, 0.63 centimeter outside diameter teflon tube held in hot water which was maintained at a temperature of >80° C. Bromine vapor thus generated was fed to the reaction flask over a 52 minute period and the temperature was maintained during the ({reaction at 28-32° C. by use of an ice bath. When all of the bromine had been added, additional methanol (175 mL) containing 4 wt. % water was added to the reaction flask and the mixture was stirred at 30° C. The overall methanol to bisphenol-A ratio was 32 moles of methanol per mole of bisphenol-A. A first sample of the homogenous mixture was taken 60 minutes after the bromine was added. The first sample was analyzed and indicated the presence of 0.03% yield of dibromophenol, 0.03% hydrolyzable impurities, 2.79% tribromobisphenol-A, and 97.18% tetrabromobisphenol-A. After an additional 30 minutes, a sample of liquid portion of the heterogenous mixture was analyzed and contained 2.17% tribromobisphenol-A. Water (700 mL) addition was begun immediately after taking the second sample and was complete in 20 minutes. The resulting orange mixture was filtered and the tetrabromobisphenol-A product was washed with 500 mL of deionized water. The product, thus isolated, was placed in a crystallizing dish and 1 mL of 56 wt % HBr was added. The product was then oven dried at 130° C for four hours. The dried product was analyzed as in Example 2 and indicated 99.24 wt. % tetrabromobisphenol-A, an acetone color of 10 APHA, a TOHTO color of 20 APHA, an ionic bromide content of 0 ppm, and a hydrolyzable bromide content of 21 ppm.

1. customTo a 2-liter 4-neck flask equipped with a -10° C
2. temperaturewas maintained at a temperature of >80° C
3. temperaturethe temperature was maintained during the (
4. custom{reaction at 28-32° C. by use of an ice bath
5. additionwas added to the reaction flask