Surface organometallic chemistry (SOMC) is a recently developing research field. It is of great significance for the quantitative modification, restoration of solid surface, identification of the physical and chemical...Surface organometallic chemistry (SOMC) is a recently developing research field. It is of great significance for the quantitative modification, restoration of solid surface, identification of the physical and chemical nature of surface and the preparation of new catalyst. The production of R 3 Sn-O-MCM-41 (R 3 SnM) was obtained by heating tributyltin chloride and Al-MCM-41 mixture at 170 °C for 5 h under stirring in nitrogen atmosphere. The composition, structure and surface physical and chemical properties of the samples were characterized by inductively coupled plasma mass spectrometry (ICP-MS), 13 C, 119 Sn, 29 Si and 27 Al solid state NMR (nuclear magnetic resonance) spectra, in-situ pyridine infrared spectroscopy (Py-IR), N 2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), etc. The results of ICP and organic elemental analysis shows that the grafting yield w Sn was 6.46% for R 3 SnM. H 0 (the negative logarithm of the acid concentration)and the number of acid sites for R 3 SnM respectively were 2.77-0.99 and 4.8 mmol·g-1 by the Hammett method. N 2 adsorption-desorption, XRD, TEM analysis showed that R 3 SnM with ordered hexagonal mesopore structure, resulted in the decease of surface areas and pore size as well as the increase of mesoporous volume and surface acidity, as compared to Al-MCM-41. R 3 SnM was used in the synthesis of isoamyl acetate. The yield of isoamyl acetate was 96% when n(isoamyl alcohol)︰n(acetic acid) 1.0︰1.0, 3 R SnM w 5%, 138 °C for 5 h. The catalyst can be reused and the yield of 86% can be attained when catalyst was reused five times at the same catalytic conditions.展开更多
通过不同层次水生无脊椎动物的毒理学研究,能更好地反映有机化合物的生态效应.以氯化三丁基锡(TBTCI)为例.结果表明,TBTCI对原生动物等5种水生无脊椎动物的半致死浓度(LC_(50))为25.65—355.63ppb.有明显的种特异性;TBTCI对河口轮虫种...通过不同层次水生无脊椎动物的毒理学研究,能更好地反映有机化合物的生态效应.以氯化三丁基锡(TBTCI)为例.结果表明,TBTCI对原生动物等5种水生无脊椎动物的半致死浓度(LC_(50))为25.65—355.63ppb.有明显的种特异性;TBTCI对河口轮虫种群净生殖率的EC_(50)为10ppb,影响平均寿命EC_(50)为22ppb;根据浓度C及原生动物平衡种类数Seq进行回归,得方程Seq=11.87—1.84 In C(P<0.05).推算出TBTCI对微型生物群落的 EC_5,EC_(20).EC_(50)分别为0.29,0.98和11.14ppb.根据对不同种的急性毒性LC_(50).取AF为0.01,推算出MATC(最高毒物允许浓度)为0.26—0.67ppb,与来自群落水平的EC_5(0.29ppb)相比更具科学性和环境真实性.展开更多
基金Supported by the National Science Foundation of Heilongjiang Province (B201010)the Education Department of Heilongjiang Province (12511595)
文摘Surface organometallic chemistry (SOMC) is a recently developing research field. It is of great significance for the quantitative modification, restoration of solid surface, identification of the physical and chemical nature of surface and the preparation of new catalyst. The production of R 3 Sn-O-MCM-41 (R 3 SnM) was obtained by heating tributyltin chloride and Al-MCM-41 mixture at 170 °C for 5 h under stirring in nitrogen atmosphere. The composition, structure and surface physical and chemical properties of the samples were characterized by inductively coupled plasma mass spectrometry (ICP-MS), 13 C, 119 Sn, 29 Si and 27 Al solid state NMR (nuclear magnetic resonance) spectra, in-situ pyridine infrared spectroscopy (Py-IR), N 2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), etc. The results of ICP and organic elemental analysis shows that the grafting yield w Sn was 6.46% for R 3 SnM. H 0 (the negative logarithm of the acid concentration)and the number of acid sites for R 3 SnM respectively were 2.77-0.99 and 4.8 mmol·g-1 by the Hammett method. N 2 adsorption-desorption, XRD, TEM analysis showed that R 3 SnM with ordered hexagonal mesopore structure, resulted in the decease of surface areas and pore size as well as the increase of mesoporous volume and surface acidity, as compared to Al-MCM-41. R 3 SnM was used in the synthesis of isoamyl acetate. The yield of isoamyl acetate was 96% when n(isoamyl alcohol)︰n(acetic acid) 1.0︰1.0, 3 R SnM w 5%, 138 °C for 5 h. The catalyst can be reused and the yield of 86% can be attained when catalyst was reused five times at the same catalytic conditions.
文摘通过不同层次水生无脊椎动物的毒理学研究,能更好地反映有机化合物的生态效应.以氯化三丁基锡(TBTCI)为例.结果表明,TBTCI对原生动物等5种水生无脊椎动物的半致死浓度(LC_(50))为25.65—355.63ppb.有明显的种特异性;TBTCI对河口轮虫种群净生殖率的EC_(50)为10ppb,影响平均寿命EC_(50)为22ppb;根据浓度C及原生动物平衡种类数Seq进行回归,得方程Seq=11.87—1.84 In C(P<0.05).推算出TBTCI对微型生物群落的 EC_5,EC_(20).EC_(50)分别为0.29,0.98和11.14ppb.根据对不同种的急性毒性LC_(50).取AF为0.01,推算出MATC(最高毒物允许浓度)为0.26—0.67ppb,与来自群落水平的EC_5(0.29ppb)相比更具科学性和环境真实性.