新型P^N^O配体过渡金属烯烃聚合催化剂的合成及其催化性能研究
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摘要
本论文合成并表征了两个2-氨基苯基三苯基膦的水杨醛类配体(P^N^O配体)L1、L2及相应的镍、钴金属配合物,研究了配合物催化烯烃聚合的活性及影响因素。同时,论文还合成并表征了三个新型的联苯甲酰类配体(N^O配体)L3、L4、L5。主要研究成果如下:
1.合成了以2-氨基苯基三苯基膦和水杨醛为基本骨架的(P^N^O)配体L1、L2及镍金属配合物cat1、cat2、cat3、cat4、cat5、cat6和钴金属配合物cat7、cat8。通过元素分析和红外光谱对其组成和结构进行表征,并通过单品X-ray衍射测定了配合物cat1、cat2、cat3、cat5的分子结构,确定了目标产物;在助催化剂甲基铝氧烷(MAO)的活化下,镍金属配合物对催化降冰片烯聚合均显示出很高的催化活性。研究表明,和中心金属Ni配位的卤素的变化对催化剂的催化活性有一定的影响,但配体的空间位阻对催化活性有明显的影响。各种聚合参数(催化剂种类、Al/Ni摩尔比、聚合温度、聚合时间、溶剂种类、单体浓度和催化剂浓度)明显影响催化剂的活性及产物聚降冰片烯(PNB)的粘均分子量。对PNB进行表征分析发现,聚合物是通过乙烯型加成聚合得到,热稳定性很高,且为非晶态。另外,研究还发现镍金属配合物和钴金属配合物对催化乙烯齐聚、苯乙烯聚合具有一定的催化活性,但总体活性不高。
2.合成了三个新型的联苯甲酰类配体(N^O配体)L3、L4、L5。通过元素分析和红外光谱对其组成和结构进行确定和表征;通过单晶X-ray衍射测定了配体L3和L4的晶体结构;对其配合物的生长条件进行了探索。
In this thesis, the two P^N^O ligands (L1 and L2) , and their corresponding nickel and cobalt complexes cat1、cat2、cat3、cat4、cat5、cat6 and cat7、cat8 were successfully synthesized and characterized by IR and element analysis. The X-ray single crystal diffraction was used to determine the molecular structure of cat1、cat2、cat3、cat5. Nickel complexes were used to catalyse norbornene polymerization under methylaluminoxane (MAO) activation, showing high acitivities. The research was showed the variety of halogens which connect with center metal has not greatly influence on the catalyst activities but the big groups of ligands do so. It was showed that the polymerization conditions, such as different catalysts, Al/Ni ratio, reaction temperature, reaction time, different solvents, monomer concentration and catalyst concentration, had great effects on the catalytic activities and the viscid average molecular weight of polynorbornene (PNB). The characterization of the polymers showed PNB was formed by vinyl-type polymerization, with high thermal stability and none-crystalline structure. The research also showed nickel complexes can catalyse ethylene oligomerization, styrene polymerization, but the polymerization activities were low. And cobalt complexes were used to catalyse ethylene oligomerization, styrene and norbornene polymerization under methylaluminoxane (MAO) activation , showing low acitivities.
In addition, the three N^O ligands L3、L4 and L5 were also synthesized and characterized by IR and element analysis. The X-ray single crystal diffraction was used to determine their molecular structures, and we try to synthesize their relative complexes.
1.合成了以2-氨基苯基三苯基膦和水杨醛为基本骨架的(P^N^O)配体L1、L2及镍金属配合物cat1、cat2、cat3、cat4、cat5、cat6和钴金属配合物cat7、cat8。通过元素分析和红外光谱对其组成和结构进行表征,并通过单品X-ray衍射测定了配合物cat1、cat2、cat3、cat5的分子结构,确定了目标产物;在助催化剂甲基铝氧烷(MAO)的活化下,镍金属配合物对催化降冰片烯聚合均显示出很高的催化活性。研究表明,和中心金属Ni配位的卤素的变化对催化剂的催化活性有一定的影响,但配体的空间位阻对催化活性有明显的影响。各种聚合参数(催化剂种类、Al/Ni摩尔比、聚合温度、聚合时间、溶剂种类、单体浓度和催化剂浓度)明显影响催化剂的活性及产物聚降冰片烯(PNB)的粘均分子量。对PNB进行表征分析发现,聚合物是通过乙烯型加成聚合得到,热稳定性很高,且为非晶态。另外,研究还发现镍金属配合物和钴金属配合物对催化乙烯齐聚、苯乙烯聚合具有一定的催化活性,但总体活性不高。
2.合成了三个新型的联苯甲酰类配体(N^O配体)L3、L4、L5。通过元素分析和红外光谱对其组成和结构进行确定和表征;通过单晶X-ray衍射测定了配体L3和L4的晶体结构;对其配合物的生长条件进行了探索。
In this thesis, the two P^N^O ligands (L1 and L2) , and their corresponding nickel and cobalt complexes cat1、cat2、cat3、cat4、cat5、cat6 and cat7、cat8 were successfully synthesized and characterized by IR and element analysis. The X-ray single crystal diffraction was used to determine the molecular structure of cat1、cat2、cat3、cat5. Nickel complexes were used to catalyse norbornene polymerization under methylaluminoxane (MAO) activation, showing high acitivities. The research was showed the variety of halogens which connect with center metal has not greatly influence on the catalyst activities but the big groups of ligands do so. It was showed that the polymerization conditions, such as different catalysts, Al/Ni ratio, reaction temperature, reaction time, different solvents, monomer concentration and catalyst concentration, had great effects on the catalytic activities and the viscid average molecular weight of polynorbornene (PNB). The characterization of the polymers showed PNB was formed by vinyl-type polymerization, with high thermal stability and none-crystalline structure. The research also showed nickel complexes can catalyse ethylene oligomerization, styrene polymerization, but the polymerization activities were low. And cobalt complexes were used to catalyse ethylene oligomerization, styrene and norbornene polymerization under methylaluminoxane (MAO) activation , showing low acitivities.
In addition, the three N^O ligands L3、L4 and L5 were also synthesized and characterized by IR and element analysis. The X-ray single crystal diffraction was used to determine their molecular structures, and we try to synthesize their relative complexes.
引文
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