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Solvothermal Synthesis Of Organic-Inorganic Hybrid Sulfide

Posted on:2007-03-25Degree:MasterType:Thesis
Country:ChinaCandidate:X M GuFull Text:PDF
GTID:2121360185478084Subject:Inorganic Chemistry
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A two-steps solvothermal synthetic procedure was used for the preparation of two one-dimensional thiostannates:[{Mn(en)2}2(μ-en)(μ-Sn2S6)]∞and [Mn(en)3(Sn2S4)]∞. A clear solution was obtained under mild solvothermal condition by reacting SnCl4·5H2O with S8 in en (ethyldiamine) at 150 oC, in which the [Sn2S6]4- dimeric anoin was the main product of the reaction system. Using this mother solution as starting material, second step solvothermal reaction was carried out by adding metal salts as connecting ions to synthesize new polymeric thiostannates. In [{Mn(en)2}2(μ-en)(μ-Sn2S6)]∞, the [Mn(en)2]2+ ions is bridged by [Sn2S6]4- anions and linear coordinated en molecules forming a one dimensional structure.Compound [Mn(en)3(Sn2S4)]∞contains the discrete [Mn(en)3]2+ ions and [Sn2S42-]∞chains. The Crystal structures were characterized by CCD X-ray determination.Crystal structure data: [{Mn(en)2}2(μ-en) (μ-Sn2S6)]∞: Mw = 840.14 (C10H40Mn2N10S6Sn2), triclinic, space group P-1 (No.2) with a = 9.0097(8), b = 9.7735(5), c = 10.8421(2) ?, a = 60.379(14)?,β= 67.235(16)?, r = 70.250(18)?, V = 752.38(8) ?3. T = 193 K, Z = 1; [Mn(en)3(Sn2S4)]∞: Mw = 600.87 (C6H24MnN6S4Sn2), orthorhombic, space group Pbcn with a = 9.664(2), b = 15.117(4), c = 12.821(3) ?, a =β=r = 90?, V = 1873.1(7) ?3. T = 193 K, Z = 4. The results of this work show that in the two-steps reaction, the thiometalates tend to form polymeric structures.A new inorganic-organic hybrid compound, [(ZnS)3(NH2CH2CH2NHCH2)2]∞, was synthesized by solvothermal technique from elemental sulfur and zinc (Ⅱ) salt in triethylenetetramine. Its structure was characterized by IR, XRD and TEM, etc. The compound is an stable polymer and has little solubility in water, ethanol, acetone and chloroform. The compound has good photocatalytic activity for degradation of dyestuff X-2R and keep nearly same activity after recycling experiments.
Keywords/Search Tags:thiostannate, solvothermal synthesis, crystal structure, photocatalytic activity
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