Small-scale suspension polymerisation procedure. Aqueous polyvinyl
alcohol (PVA) solution (20 ml, 1% wt/wt, 87–89% hydrolyzed PVA,
average MW 85000–146000) was prepared and transferred to the reaction
vessel (screw cap boiling tube attached to a N2/vacuum manifold system)
and degassed with N2 for 20 minutes. A monomer mixture—styrene (10
mmol), divinylbenzene and quantum dots (Table 1)—was prepared and
stirred for 5 minutes. AIBN (76 mmol) was added to the monomer mixture
then the resultant mixture was stirred for a further 15 minutes with N2
degassing. The dark orange monomer solution (colour due to the quantum
dots) was added to the PVA solution while rapidly stirring with a crossshaped
magnetic stirrer. A two phase system resulted with orange droplets
being suspended in the uncoloured aqueous PVA solution. The suspension
was stirred at room temperature for 30 minutes before the temperature was
increased to 70 °C and stirring was continued for a further 4 hours. The resin
beads were then collected over a 38 mm sieve and washed in situ with
copious amounts of water. The damp beads were then transferred to a
sintered funnel and washed with methanol (100 cm3), MeOH/THF, 1/1 (100
cm3), THF (100 cm3), CH2Cl2 (100 cm3) and acetone (100 cm3).
Small-scale suspension polymerisation procedure. Aqueous polyvinylalcohol (PVA) solution (20 ml, 1% wt/wt, 87–89% hydrolyzed PVA,average MW 85000–146000) was prepared and transferred to the reactionvessel (screw cap boiling tube attached to a N2/vacuum manifold system)and degassed with N2 for 20 minutes. A monomer mixture—styrene (10mmol), divinylbenzene and quantum dots (Table 1)—was prepared andstirred for 5 minutes. AIBN (76 mmol) was added to the monomer mixturethen the resultant mixture was stirred for a further 15 minutes with N2degassing. The dark orange monomer solution (colour due to the quantumdots) was added to the PVA solution while rapidly stirring with a crossshapedmagnetic stirrer. A two phase system resulted with orange dropletsbeing suspended in the uncoloured aqueous PVA solution. The suspensionwas stirred at room temperature for 30 minutes before the temperature wasincreased to 70 °C and stirring was continued for a further 4 hours. The resinbeads were then collected over a 38 mm sieve and washed in situ withcopious amounts of water. The damp beads were then transferred to asintered funnel and washed with methanol (100 cm3), MeOH/THF, 1/1 (100cm3), THF (100 cm3), CH2Cl2 (100 cm3) and acetone (100 cm3).
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Small-scale suspension polymerisation procedure. Aqueous polyvinyl
alcohol (PVA) solution (20 ml, 1% wt/wt, 87–89% hydrolyzed PVA,
average MW 85000–146000) was prepared and transferred to the reaction
vessel (screw cap boiling tube attached to a N2/vacuum manifold system)
and degassed with N2 for 20 minutes. A monomer mixture—styrene (10
mmol), divinylbenzene and quantum dots (Table 1)—was prepared and
stirred for 5 minutes. AIBN (76 mmol) was added to the monomer mixture
then the resultant mixture was stirred for a further 15 minutes with N2
degassing. The dark orange monomer solution (colour due to the quantum
dots) was added to the PVA solution while rapidly stirring with a crossshaped
magnetic stirrer. A two phase system resulted with orange droplets
being suspended in the uncoloured aqueous PVA solution. The suspension
was stirred at room temperature for 30 minutes before the temperature was
increased to 70 °C and stirring was continued for a further 4 hours. The resin
beads were then collected over a 38 mm sieve and washed in situ with
copious amounts of water. The damp beads were then transferred to a
sintered funnel and washed with methanol (100 cm3), MeOH/THF, 1/1 (100
cm3), THF (100 cm3), CH2Cl2 (100 cm3) and acetone (100 cm3).
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