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采用水热法,在DMF-水溶剂中合成出一种新型的电荷转移配合物(C2H8N)3(PW12O40).2H2O.利用红外光谱和差热热重对其进行结构表征和热稳定分析,并通过X-射线单晶衍射对其结构进行确证.结果表明,配合物属于三方晶系,R3 m空间群,晶胞参数为a=1.626 82(12)nm,b=1.626 82(12)nm,c=2.481 9(4)nm,α=90°,β=90°,γ=120°,V=5.688 4(11)nm3,Z=6,R1=0.057 7,wR2=0.144 4,S=1.006.配合物对甲醇具有较好的催化活性,175℃时,当甲醇初始浓度为5.37g.m-3,流速为4.51mL·min-1,0.20g催化剂对甲醇的消除率达到59%.
A new type of charge-transfer complex (C2H8N) 3 (PW12O40) .2H2O was synthesized by hydrothermal method in DMF-water solvent. Structural characterization and thermal stability analysis were carried out by infrared spectroscopy and differential thermal analysis Its structure was confirmed by X-ray single crystal diffraction. The results showed that the complex belongs to the trigonal system with space group R3m, a = 1.626 82 (12) nm and b = 1.626 82 (12) nm, C = 2.481 9 (4) nm α = 90 ° β = 90 ° γ = 120 ° V = 5.688 4 (11) nm3 Z = 6 R1 = 0.057 7 wR2 = 0.144 4 S = 1.006 The complex has good catalytic activity to methanol, and the methanol elimination rate reaches 59% at 175 ℃ when the initial concentration of methanol is 5.37gm-3 and the flow rate is 4.51mL · min-1 and 2.0g.