牙科树脂引发剂三丁基硼的合成

Synthesis of dental resin initiator tri-n-butylborane

目的和方法：用新的改进的有机金属路线，以1-溴代正丁烷、三氯化硼乙醚溶液和镁为原料合成出一种牙科树脂聚合引发剂──三丁基硼（TBB）．详细考察了合成反应并获得最佳反应条件．研究了它做为聚甲基丙烯酸甲酯／甲基丙烯酸甲酯（PMMA／MMA）牙科树脂体系的引发剂的性能．结果：当三氟化硼乙醚在总乙醚中的浓度为0．25mol／L，滴加完1-溴代正丁烷后回流3h时。三丁基硼的产率为75％．合成的三丁基硼能引发MMA聚合而使PMMA／MMA树脂体系固化．当引发剂质量分数为12．7％和17．9％时，固化时间分别为8．1和5.6min．结论：用新的改进的有机金属路线，能合成出三丁基硼，三丁基硼能引发MMA聚合而使PMMA／MMA树脂体系固化．固化时间与三丁基硼的用量有关．

AIM and METHODS: A dental resin polymerization initiator tri-n-butylborane (TBB) was synthesized directly by using n-BuBr, BF3·Et2O and Mg as the raw materials via a novel modified organometallic route. The best synthetic condition was investigated. The properties of TBB using as a dental resin initiator were also studied. RESULTS: When the concentration of BF3·Et2O in Et2O was 0. 25 mol/L and the reflux time was 3 hours after 1-BuBr dripped in, the yield of TBB was 75%. The polymerization of MMA could be initiated by TBB and then the PMMA/MMA mixture could be solidified. When the mass fraction of the initiator was 12.7% and 17. 9 %, the solidifying time was 8. 1 and 5. 6 minutes respectively. CONCLUSION: The TBB has been synthesized via a novel modified organometallic route. The polymerization of MMA is initiated by TBB and the solidifying time of PMMA/MMA resin is related to the content of initiator.