[2-[2-(2-乙酰氧基苯基)乙基]苯基] 乙酸甲酯

反应条件: temp:245.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A charge consisting of 167 parts of isophthalic acid and 298 parts of 1,2-bis(acetoxyphenyl)ethane and 0.005 mols potassium carbonate per mol of 1,2-bis(acetoxyphenyl)ethane is placed in a reaction vessel equipped with a stirrer, condenser and receiver. The vessel is evacuated and purged with nitrogen three times. During the reaction a nitrogen blanket is maintained in the reactor. The temperature is raised to about 245° C. and acetic acid distills. The rate of distillation during the initial 67 percent of reaction is 1.82 ml mol-1 min.-1. The distillation rate tapers after 87 parts of acetic acid have distilled in 55 minutes. The temperature rises slowly to 270° C. during the initial stage. Thereupon the vessel is evacuated to a pressure of about 200 torr for about 5 minutes and the pressure is then slowly reduced to about 1 torr while the temperature is increased to about 290° C. When the amperage on the stirrer motor increases by 0.02 to 0.04 amps, the stirrer motor is switched off and the vacuum is released with nitrogen. A total of 112 parts of acetic acid (98 percent of theoretical) is collected. The rate of evolution of acetic acid during the vacuum stage is 1.67 ml mol-1 min.-1. The prepolymer is extruded from the vessel under slight nitrogen pressure and is reduced in a mill to a powder of particle size in the range of from 0.1 to 0.25 mm. The inherent viscosity of the prepolymer is 0.28. The prepolymer is off white in color. is placed in a reaction vessel equipped with a stirrer, condenser The vessel is evacuated purged with nitrogen three times During the reaction a nitrogen blanket is maintained in the reactor acetic acid distills The rate of distillation during the initial 67 percent of reaction The distillation rate tapers after 87 parts of acetic acid have distilled in 55 minutes rises slowly to 270° C. Thereupon the vessel is evacuated to a pressure of about 200 torr for about 5 minutes is increased to about 290° C When the amperage on the stirrer motor increases by 0.02 to 0.04 amps A total of 112 parts of acetic acid (98 percent of theoretical) is collected

反应条件: temp:245.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A charge consisting of 167 parts of isophthalic acid and 298 parts of 1,2-bis(acetoxyphenyl)ethane and 0.005 mols potassium carbonate per mol of 1,2-bis(acetoxyphenyl)ethane is placed in a reaction vessel equipped with a stirrer, condenser and receiver. The vessel is evacuated and purged with nitrogen three times. During the reaction a nitrogen blanket is maintained in the reactor. The temperature is raised to about 245° C. and acetic acid distills. The rate of distillation during the initial 67 percent of reaction is 1.82 ml mol-1 min.-1. The distillation rate tapers after 87 parts of acetic acid have distilled in 55 minutes. The temperature rises slowly to 270° C. during the initial stage. Thereupon the vessel is evacuated to a pressure of about 200 torr for about 5 minutes and the pressure is then slowly reduced to about 1 torr while the temperature is increased to about 290° C. When the amperage on the stirrer motor increases by 0.02 to 0.04 amps, the stirrer motor is switched off and the vacuum is released with nitrogen. A total of 112 parts of acetic acid (98 percent of theoretical) is collected. The rate of evolution of acetic acid during the vacuum stage is 1.67 ml mol-1 min.-1. The prepolymer is extruded from the vessel under slight nitrogen pressure and is reduced in a mill to a powder of particle size in the range of from 0.1 to 0.25 mm. The inherent viscosity of the prepolymer is 0.28. The prepolymer is off white in color. is placed in a reaction vessel equipped with a stirrer, condenser The vessel is evacuated purged with nitrogen three times During the reaction a nitrogen blanket is maintained in the reactor acetic acid distills The rate of distillation during the initial 67 percent of reaction The distillation rate tapers after 87 parts of acetic acid have distilled in 55 minutes rises slowly to 270° C. Thereupon the vessel is evacuated to a pressure of about 200 torr for about 5 minutes is increased to about 290° C When the amperage on the stirrer motor increases by 0.02 to 0.04 amps A total of 112 parts of acetic acid (98 percent of theoretical) is collected