HRID1020519

反应详情

EQUATION

反应方程式

HRID 1020519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In a round bottom flask 0.9 grams of dicobalt octacarbonyl salt was dissolved in 30 grams of toluene. To this solution, treated nanosilica in methyl ethyl ketone (0.9 grams, containing 15 weight percent of nanosilica; the nanosilica was treated with methacryloxy propyl trimethoxy silane in presence of triethyl amine at 80° C. was added and mechanically stirred (600-900 rpm) at room temperature for 10 minutes. The resultant solution was then added to a glass tube reactor containing bisphenol-A (24 g) and BMSC (35.78 g) to form a reactant mixture. 400 microliters of a solution containing TMAH (2.6 mg) and NaOH (9.58 mg) were added as a catalyst to the reactant mixture and the resultant mixture was purged with nitrogen and heated to a temperature of 50° C. under stirring at a speed of 90 rpm for 20 minutes. The temperature was then maintained at 120° C. for 20 minutes at 910 millibar in nitrogen gas and stirring at 90 rpm. After 20 minutes the temperature was increased to 180° C. inside the tube reactor and maintained for 15 minutes. The temperature was then increased to 220° C. The pressure was slowly reduced from 910 millibar to 100 millibar over a period of 4 to 5 minutes at a rate of 75 to 100 millibar per 30 seconds. After being maintained at 100 millibar and 220° C. for 10 minutes, the temperature was increased to 280° C. The reaction mixture was then maintained at 280° C. and 0 millibar for 10 minutes to provide a bisphenol-A polycarbonate nanocomposite comprising 1.2 wt % cobalt nanoparticles.

WORKUP

后处理

  1. additioncontaining 15 weight percent of nanosilica
  2. additionwas added
  3. customto form a reactant mixture
  4. additionwere added as a catalyst to the reactant mixture
  5. customthe resultant mixture was purged with nitrogen
  6. temperatureheated to a temperature of 50° C.
  7. stirringunder stirring at a speed of 90 rpm for 20 minutes
  8. temperatureThe temperature was then maintained at 120° C. for 20 minutes at 910 millibar in nitrogen gas
  9. stirringstirring at 90 rpm
  10. temperatureAfter 20 minutes the temperature was increased to 180° C. inside the tube reactor
  11. temperaturemaintained for 15 minutes
  12. temperatureThe temperature was then increased to 220° C
  13. waitThe pressure was slowly reduced from 910 millibar to 100 millibar over a period of 4 to 5 minutes at a rate of 75 to 100 millibar per 30 seconds
  14. temperatureAfter being maintained at 100 millibar and 220° C. for 10 minutes
  15. temperaturethe temperature was increased to 280° C
  16. temperatureThe reaction mixture was then maintained at 280° C.