(浙江师范大学化学系,金华321004)
摘 要: 用流变相-前驱物反应法合成了水杨酸锰配合物。通过元素分析和TG分析确定该配合物的组成为Mn(HSal)2·2.5H2O(HSal=o-OHC6H4COO);XRD确定该配合物为单斜晶系,晶胞参数为a=1.893 5(4) nm,b=0.617 9(0) nm,c=1.732 5(6) nm,β=114.93(1)°,V=1.838 2(3) nm3,Z=6,ρcal=1.775 kg/dm3,ρexp=1.769 kg/dm3;IR研究表明配合物中羧酸根与Mn2+以双齿螯合方式配位。样品在氮气中经330 ℃热分解的最终产物是MnO和有机化合物,在空气中经800 ℃热分解的最终产物为Mn3O4。TEM观察表明,MnO和Mn3O4均为球形粒子, 平均粒径分别约为25和28 nm;激光粒度分析仪测定MnO和Mn3O4的平均粒径约为45.6和69.1 nm。
关键字: 水杨酸锰;流变相; 热分解; 纳米氧化锰
manganese salicylate and shape of
nanometric manganese oxide
( Department of Chemistry, Zhejiang Normal University,
Jinhua 321004, China)
Abstract: Manganese salicylate was synthesized with the rheological phase reaction method. The composition is Mn(HSal)2·2.5 H2O(HSal=o-OHC6H4COO) through elemental and TG analysis. This complex belongs to monoclinic system with cell dimension: a=1.893 5(4) nm,b=6.179 0(2) nm,c=17.325 6(1) nm,β=114.93(1)°,V=1.838 2(3) nm3,Z=6,ρcal=1.775 kg/dm3,ρexp=1.769 kg/dm3 through powder X-ray diffraction. IR spectrum of sample shows that there is an asymmetric bidentate bridging coordination between the COO- and the Mn2+ of manganese salicylate. Final products of sample thermal decomposition are MnO powder and organic compounds in N2 at 330 ℃ and Mn3O4 in air at 800 ℃. TEM measurement indicates that both MnO and Mn3O4 are spherical particles. The average diameter of the MnO and Mn3O4 particles are 25 nm and 28 nm through TEM and 45.6 nm and 69.1 nm through laser particles size analyzer.
Key words: manganese salicylate; rheological phase; thermal decomposition; nano-manganese oxide