(浙江師范大學(xué)化學(xué)系，金華321004)
摘 要: 用流變相-前驅(qū)物反應(yīng)法合成了水楊酸錳配合物。通過元素分析和TG分析確定該配合物的組成為Mn(HSal)2·2.5H2O（HSal=o-OHC6H4COO）；XRD確定該配合物為單斜晶系，晶胞參數(shù)為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與Mn2+以雙齒螯合方式配位。樣品在氮?dú)庵薪?jīng)330 ℃熱分解的最終產(chǎn)物是MnO和有機(jī)化合物，在空氣中經(jīng)800 ℃熱分解的最終產(chǎn)物為Mn3O4。TEM觀察表明，MnO和Mn3O4均為球形粒子, 平均粒徑分別約為25和28 nm；激光粒度分析儀測定MnO和Mn3O4的平均粒徑約為45.6和69.1 nm。
關(guān)鍵字: 水楊酸錳；流變相； 熱分解； 納米氧化錳
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
