共查询到17条相似文献,搜索用时 78 毫秒
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室温和低热温度固-固相反应合成化学 总被引:23,自引:0,他引:23
概要地综述了室温和低热温度固相反应在配合物合成中的应用,包括新的原子簇化合物、多酸化合物,以及简单配合物、混配化合物、长链配合物、固配化合物、中间化合物等的合成。 相似文献
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三核钼-硫簇合物的低热固相合成及其晶体结构 总被引:1,自引:0,他引:1
三核钼-硫配合物Mo_3S_7(dtc)_3I·S_8·2CH_2Cl_2(dtc=C_4H_8NCS_2~-)是由低热固相合成得到的。晶体属单斜晶系,M_r=1500.19,空间群P2_1/n,a=11.881(3),b=15.559(4),c=26.197(7),β=98.53(2)°,V=4789A~3,Z=4,D_c=2.08g/cm~3,F(000)=2920,μ(MoKα)=25.24cm~(-1),对于2397个I≥3σ(I)的独立衍射点,最终偏离因子R=0.060,R=0.066。该配合物的基本骨架是[Mo_3S_7(dtc)_3]~+,其簇芯为[Mo_3S_7]~(4+)单元,3中Mo原子组成正三角形平面,Mo-Mo的平均键长力2.723,Mo原子平面上的硫原子形成盖帽的μ_3-S,其Mo-S平均键长为2.383A,3个S_2基团分别位于三角形3个棱的外侧,并分别与邻近的两个Mo原子结合形成12中Mo-S键。与μ_3-S相对而位于平面另一侧的Ⅰ原子与3个μ_2-S连结,平均距离为3.257A,成键作用较弱。 相似文献
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三核钼-硫配合物Mo_3S_7(dtc)_3I·S_8·2CH_2Cl_2(dtc=C_4H_8NCS_2~-)是由低热固相合成得到的。晶体属单斜晶系,M_r=1500.19,空间群P2_1/n,a=11.881(3),b=15.559(4),c=26.197(7),β=98.53(2)°,V=4789A~3,Z=4,D_c=2.08g/cm~3,F(000)=2920,μ(MoKα)=25.24cm~(-1),对于2397个I≥3σ(I)的独立衍射点,最终偏离因子R=0.060,R=0.066。该配合物的基本骨架是[Mo_3S_7(dtc)_3]~+,其簇芯为[Mo_3S_7]~(4+)单元,3中Mo原子组成正三角形平面,Mo-Mo的平均键长力2.723,Mo原子平面上的硫原子形成盖帽的μ_3-S,其Mo-S平均键长为2.383A,3个S_2基团分别位于三角形3个棱的外侧,并分别与邻近的两个Mo原子结合形成12中Mo-S键。与μ_3-S相对而位于平面另一侧的Ⅰ原子与3个μ_2-S连结,平均距离为3.257A,成键作用较弱。 相似文献
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本文报道室温固-固相化学反应一步法合成氨基酸铜配合物.trans-Cu(Gly)_2·H_2O、cis-Cu(Gly)_2·H_2O、trans-Cu(DL-Ala)_2、trans-Cu(DL-Ala)_2·H_2O、trans-Cu(DL-Val)和trans-Cu(DL-Leu)_2,经元素分析、IR、XRD、DTA测定,确定了配合物的组成及几何构型.并初步讨论了室温固相反应合成机理. 相似文献
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固相配位化学反应研究(LXVII):—固—固相反应合成混配… 总被引:5,自引:0,他引:5
室温或近室温条件下,Co(acac)2(H2O)2与第二配体2,2'-联吡啶、1,10-啡罗啉、8-羟基喹啉、水杨醛肟固相反应得到4个混配化合物,经XRD、IR、UV及元素分析表征了这些产物。 相似文献
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The layered nanocrystalline sodium manganese phosphate was synthesized by low‐heating solid state reaction using MnSO4·H2O and Na3PO4·12H2O as raw materials. The resulting sodium manganese phosphate and its calcined products were characterized using element analysis, thermogravimetry and differential thermal analyses (TG/DTA), Fourier transform IR (FT‐IR), X‐ray powder diffraction (XRD), scanning electron microscopy (SEM), ultraviolet‐visible (UV‐Vis) absorption spectroscopy, and magnetic susceptibility. The results showed that the product obtained at 70°C for 3 h, NaMnPO4·3H2O, was a layered compound, and its crystallite size and interlayer distance were 27 nm and 1.124 nm, respectively. The thermal process of NaMnPO4·3H2O between room temperature and 700°C experienced three steps, the dehydration of the one adsorption water at first, and then dehydration of the two crystal waters, at last crystallization of NaMnPO4. Magnetic susceptibility measurements of NaMnPO4· 3H2O from room temperature to 2.5 K point to ferrimagnetic ordering at TN‐35 K. 相似文献
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“凝聚态化学”是化学学科一个新的发展领域,其基本思想是超越分子和理想晶体的界限,多层次地研究物质的组成、结构、性质、制备以及它们之间的关系。本文简要回顾了从固体物理到凝聚态物理的历史以及固体化学的发展历史,分析了固体化学的学科特点,指出固体化学的发展必然孕育着“凝聚态化学”的形成,同时指出,化学学科中的多个领域也都会将“凝聚态化学”作为自己的发展方向。建议了从固体化学向“凝聚态化学”发展的途径:完善固体化学学科的知识体系,拓展固体化学的知识范围,创造“凝聚态化学”的标志性成果。最后强调,与凝聚态物理学家密切合作,共建“凝聚态科学”大厦。 相似文献
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Ammonium cerium phosphate was prepared with (NH4)3PO4·3H2O and Ce(SO4)2·4H2O as raw materials and PEG‐400 as surfactant via a solid state reaction at low‐heating temperature. The characterization result of XRD indicates that the molecular formula of the product was (NH4)2Ce(PO4)2·H2O. The synthesis of benzyl acetate was carried out with H2SO4/ammonium cerium phosphate as catalyst, and uniform experimental design as well as data mining technology was applied to the experiments, in which the effect of the reaction time, the molar ratio of acid to alcohol and the amount of catalyst on the conversion yield of acetic acid were studied. When benzalcohol was 0.10 mol, under the optimal reaction conditions, i.e. reaction time of 174 min, 2.02 of molar ratio of acid to alcohol and 0.5 g of catalyst, the esterification rate of acetic acid was 97.9%. The ammonium cerium phosphate had potential for industry application since it not only was feasible and simple in synthesis technics, but also had good catalysis activity for the synthesis of benzyl acetate. 相似文献
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Kazuo EdaSatoshi Fukiharu Takashi SuzukiNoriyuki Sotani 《Journal of solid state chemistry》2002,164(1):157-162
An interesting structural transformation from a two dimensional (2d) covalent oxide network with a layered structure to a three-dimensional (3d) network with a tunnel structure was found at room temperature in the mixture of hydrated alkali-metal molybdenum bronze and amorphous alkali-metal molybdate. From various experimental results it was concluded that the transformation was due to a room temperature solid state reaction. 相似文献