【作者】 刘娜；

【导师】 吴芹；

【作者基本信息】 北京理工大学 ， 制药工程， 2015， 硕士

【摘要】 双(2,4,6-三甲基苯甲酰基)苯基氧化膦是一种高效的紫外光引发剂,在紫外光的照射下引发单体聚合。相比较很多传统光引发剂,双(2,4,6-三甲基苯甲酰基)苯基氧化膦的激发态寿命很短,在引发过程中,很难被其它物质淬灭而导致活性消失;光固化速度快,在紫外光条件下,产生大量的自由基,具有高的引发效率;光固化后的体系中,引发剂剩余量几乎为零等优点。本文以苯基二氯化膦为初始原料,采用金属钠还原法,在金属钠作用下将苯基二氯化膦还原成苯基膦氢,苯基膦氢和2,4,6-三甲基苯甲酰氯反应生成双(2,4,6-三甲基苯甲酰基)苯基膦,双氧水氧化双(2,4,6-三甲基苯甲酰基)苯基膦得到双(2,4,6-三甲基苯甲酰基)苯基氧化膦。采用红外光谱(FT-IR)、核磁共振波谱(1H NMR)、质谱(ESI-MS)对双(2,4,6-三甲基苯甲酰基)苯基氧化膦进行结构表征。结果表明成功合成了双(2,4,6-三甲基苯甲酰基)苯基氧化膦。对合成双(2,4,6-三甲基苯甲酰基)苯基氧化膦的工艺条件进行了优化,探究了反应过程中原料苯基二氯化膦及金属钠的摩尔配比、金属钠取代步骤的反应时间、质子化过程质子源以及反应时间、酰化过程的反应温度及时间、氧化过程中催化剂种类的选择等对反应产物产率的影响,确定了最佳反应条件。以季戊四醇、2,2-羟甲基丙酸和顺丁烯二酸酐为原料合成了超支化顺丁烯聚酯预聚物单体。采用红外光谱(FT-IR)、核磁共振波谱(13C NMR)、热重分析仪(TG)、X-射线衍射(XRD)对其进行结构表征,结果表明成功合成了HBPE2与HBPE2-MA。并且对其涂膜性能进行了测试。其次,探究了不同浓度二苯甲酮、α,α二甲基-α羟乙基苯乙酮、双(2,4,6-三甲基苯甲酰基)苯基氧化膦光引发剂对光固化时间的影响,发现随着光引发剂浓度的增大,光固化时间呈现先减小后增大的趋势;引发剂浓度相同时,双(2,4,6-三甲基苯甲酰基)苯基氧化膦为光引发剂时光固化时间最短,具有高的引发效率。最后,对其进行合成经济成本核算。更多还原

【Abstract】 Bis(2,4,6-trimethylbenzoyl) phenyl phosphine oxide as an effective UV photoinitiator can initiate monomers polymerization. Compared to many traditional photoinitiators, bis-(2,4,6-trimethylbenzoyl)phenylphosphine oxide`s reaction time is very short and its reaction activity is excellent in the initiation process. Its curing speed is fast, it can produce large amounts of free radicals in the UV-curing process, so it has a high efficiency in UV-cured systems, the amount of free radicals is almost zero when the reaction is over.In this thesis, bis(2,4,6-trimethylbenzoyl)phenyl phosphine oxide was prepared by metal Na reduction method and it was characterized by spectroscopy(FT-IR), nuclear magnetic resonance(1H NMR) and mass spectrometry(ESI-MS), it was found that its structure was consistent with the designed structure.Conditions of bis(2,4,6-trimethylbenzoyl)phenyl phosphine oxide’s synthesis process were optimized. Study the molar ratio of phenyl phosphonic dichloride and sodium metal, the reaction time in sodium metal substitution, different proton source, the reaction time and temperature in acylation and the different oxidation catalyst of the reaction. Optimized the reaction conditions.Hyperbranched maleic polyester prepolymer monomers was prepared by pentaerythritol, 2,2-dimethylol propionic acid and maleic anhydride, then it was characterized by spectroscopy(FT-IR), nuclear magnetic resonance(13C NMR), thermal gravimetric(TG) and X- ray diffraction(XRD), the results showed that its structure was consistent with the designed structure. Then test its film properties. Study the influence of concentration of benzophenone, Darocure1173, bis(2,4,6-trimethylbenzoyl) phenyl phosphine oxide to UV-curing time. Compared to benzophenone and α,α-dimethyl-acetophenone-α-hydroxyethy, bis(2,4,6-trimethylbenzoyl) phenyl phosphine oxide has a high efficiency of chemical reactivity. Made a synthesis economic costs accounting.更多还原