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室温固相法合成稀土三元配合物
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摘要：以稀土氯化物、丙烯酸、8-羟基喹啉为原料，利用室温固相合成法合成了丙烯酸-8-羟基喹啉合铕(III)和丙烯酸-8-羟基喹啉合镧(III)，并进行了元素分析、红外光谱和综合热分析(TG-DTG-DSC-DTA)等表征。通过红外光谱测定，丙烯酸-8-羟基喹啉合铕(III)红外光谱中的8-羟基喹啉配体的特种吸收峰νC=N和νC=C(1480cm-1)分别位移至1572.85cm-1，1499.28cm-1，1466.87cm-1处。配体中羟基伸缩振动吸收峰νOH移至1069.38cm-1，弯曲振动吸收峰δO-H（1223cm-1）移至1205.53cm-1，以及在902.49cm-1处增加了C=C的单取代吸收峰。通过热分析(TG-DTG-DSC-DTA)，两种稀土元素的三元配合物在120-150℃左右开始失结晶水，在420℃的时候配合物剧烈分解，在600℃之后生成稀土氧化物。根据热分解动力学研究测得反应的活化能,得出丙烯酸-8-羟基喹啉合铕(镧)三元配合物的热分解反应为0级反应，丙烯酸-8-羟基喹啉合铕(III)配合物的活化能Ea=92.96kJ/mol，丙烯酸-8-羟基喹啉合镧(III)配合物的活化能为Ea=107.7kJ/mol。当温度在400℃以下，配合物的热稳定性良好。稀土丙烯酸-8-羟基喹啉三元配合物以其刚性大及吸光系数大而被广泛用于制备稀土有机配合物发光材料,为合成稀土高分子功能材料的研究奠定了基础。
关键词： 丙烯酸；8-羟基喹啉；铕；镧；三元配合物
Rare earth ternary complexes of solid-phase synthesis in room temperature
Abstract：Take rare earth chloride, acrylic acid, eight - hydroxyquinoline as raw material, we can synthesis the acrylates-8 - hydroxyquinoline europium (III) and acrylates-8 - quinolinolato lanthanum (III) by the method of solid-phase synthesis in room temperature, and elemental analysis, infrared spectroscopy and thermal analysis (TG-DTG-DSC-DTA) were characterized. By infrared spectroscopy, acrylates, 8 - hydroxyquinoline europium (III) IR spectrum 8 - hydroxyquinoline ligands special absorption νC = N and νC = C (1480cm-1) are shifted to 1572.85cm-1,1499.28 cm-1, 1466.87cm-1 . In ligand the stretching vibration absorption peak of OH moves 1069.38cm-1, bending vibration absorption peak δO-H (1223cm-1) move to 1205.53cm-1, and added a 902.49cm-1 mono-substituted absorption peak of the C = C, By thermal analysis (TG-DTG-DSC-DTA), we can know two kinds of rare earth ternary complexes start to lose crystal water around 120-150 ℃ and at 420 ℃ the complexes decompose violently,about at 600 ℃ rare earth oxides generated after . According to the measured thermal decomposition kinetics of activation energy, the level of derived acrylates- 8 - hydroxyquinoline europium (La) ternary complex thermal decomposition reaction is 0, the activation energy of acrylates-8- hydroxyquinoline europium (III) complexes is Ea = 92.96kJ/mol, and the acrylates-8- quinolinolato lanthanum (III) complexes is Ea = 107.7kJ/mol. When the temperature is below 400 ℃, the thermal stability of the complexes is good. Rare acrylates, 8 - hydroxyquinoline ternary complexes with its good rigidity and high light absorption coefficient is widely used in the preparation of organic complexes of rare earth luminescent materials,and also lay a foundation for the synthesis of rare earth functional polymeric materials research .
Key words : Acrylic acid；8-hydroxyquinoline；Eu；La；ternary complexes
目录
1引言 - 1 -
1.1 固相合成法 - 1 -
1.1.1 固相化学反应 - 1 -
1.1.2 固相反应机理 - 1 -
1.1.3低热固相化学反应的特有规律 - 2 -
1.1.4固相反应与液相反应的差别 - 3 -
1.1.5低热固相反应在合成化学中的应用 - 3 -
1.1.6其他合成方法 - 3 -
1.2 低热固相合成 - 4 -