醇系溶剂中冠醚与碱金属离子的配位反应

The enthalpy changes, entropy changes and equilibrium constants of coordination reactions of 18-crown-6 with the alkali ions Na+ and K+ at 298.15K were measured by using RD-496 microcalorimeter with methanol, ethanol, n-propanol and n-butanol as solvents respectively. The results indicated that the enthalpy changes △rHm, entropy changes △rSm, and the stability of the complexes are closely related with the polarity of the solvents, and the order of the stability is ethanol>methanol>n-propanol>n-butanol>H2O for the same complex in the solvents investigated. The stability order was reasonably explained by relating the stability constants of the complexes with the dielectric constants of these solvents, and by using the model of solvated-desolvated ions and ion pair in the coordination reactions.     

SDS/苯甲醇/H2O体系的相行为与结构

SDS／苯甲醇／H2O体系能生成胶束、微乳液、层状液晶、六角状液晶等分子有序组合作，它们之间转换关系可以从凝聚能理论得到解释．来甲酸在O／W微乳液中的分配系数K＝168，表明绝大多数苯甲醇被增溶于SDS胶束相内．随重量比本甲醇／SDS增加，层状液晶中的do值几乎不变，溶剂渗透率略有增加，六角状液晶中圆柱缔合体的半径r值几乎不变，溶剂渗透率增加．     

孔性氧化铝模板与一维纳米新材料的制备

纳米材料尤其是以碳纳米管有序阵列为代表的一维纳米阵列材料的重要价值,促进了人们对模板合成方法的研究。本文简要回顾和总结了近年来有关孔性氧化铝模板的制备及其应用的研究进展,结合我们实验室的部分相关研究工作,揭示了孔性氧化铝模板在合成与组装一维纳米新材料方面的重要作用,以进一步活跃和促进该重要领域的研究和发展。     

低镍甲烷化催化剂中镍和氧化镧的分散研究

本文用X射线衍射法(XRD), 透射电镜(TEM), 配合电子衍射对Ni/Al2O3,Ni/γ-Al_2O_3-La_2O_3等催化剂中镍晶粒度和La_2O_3的分散状态进行了测量和讨论。用透射电镜测量了不同La_2O_3含量的催化剂中镍晶粒度分布, 其平均直径可与X射线宽化法测定值相比较。催化剂中随La_2O_3加入量的增加, Ni晶粒有细化趋势, 从而提高了甲烷化催化活性。对La_2O_3在γ-Al_2O_3表面作密置单层分散的模型提出了新的旁证, 并推断由于La_2O_3在γ-Al_2O_3表面高分散并产生较强相互作用, 使γ-Al_2O_3接近表层晶格发生畸变。     

Molecular structure and conformation of 2,3-dichloro-1-propene as determined by gas-phase electron diffraction

The molecular structure and conformation of 2,3-dichloro-1-propene have been determined by gas-phase electron diffraction at nozzle temperatures of 24, 90 and 273°C. The molecules exist as a mixture of two conformers with the chlorine atoms anti (torsion angle ∠φ = 0°) or gauche (∠φ = 109°) to each other and with the anti form the more stable. The composition (mole fraction) of the vapor with uncertainties estimated at 2σ was found to be 0.55 (0.08), 0.49 (0.08) and 0.41 (0.10) at 24, 90 and 273°, respectively. These values correspond to an energy difference with estimated standard deviation ΔE° = E°_g-E°_a = 0.7 ± 0.3 kcal mol^?1 and an entropy difference ΔS° = S°_g-S°_a = 0.6 ± 0.9 cal mol^?1 K^?1. Some of the diffraction results, together with spectroscopic observations, permit the evaluation of an approximate torsional potential function of the form 2V = V₁ (1 - cos φ) + V₂ (1 - cos 2φ) + V₃ (1 - cos 3φ); the results are V₁ = 4.4 ± 0.5, V₂ = ?2.9 ± 0.5 and V₃ = 4.8 ± 0.2, all in kcal mol^?1. The results at 24°C for the distance (r_a) and angle (∠_α) parameters, with estimated uncertainties of 2σ, are: r(C_sp²-H) = 1.098(0.020)Å, r(C_sp³-H) = 1.103(0.020)Å, r(CC) = 1.334(0.009)Å, r(C-C) = 1.504(0.013)Å, r(C_sp²-Cl) = 1.752(0.021)Å, r(C_sp³-Cl) = 1.776(0.020)Å, ∠C-CC = 127.6(1.1)°, ∠C_sp³-C_sp²-Cl = 110.2(1.0), ∠C_sp²-C_sp³-Cl = 113.1(1.2)°, ∠H-C_sp³-H = 109.5° (assumed), ∠CC-H = 120.0° (assumed) and ∠φ = 108.9(3.4)°.     

Microwave assisted hydrothermal synthesis of tin niobates nanosheets with high cycle stability as lithium-ion battery anodes

SnNb₂O₆ and Sn₂Nb₂O₇ nanosheets were synthetized via microwave assisted hydrothermal method, and innovatively employed as anode materials for lithium-ion battery. Compared with Sn₂Nb₂O₇ and the previously reported pure Sn-based anode materials, the SnNb₂O₆ electrode exhibited outstanding cycling performance.     

Hydrothermal synthesis and intercalation behavior of a layered titanium phosphate Ti2(H2PO4)(HPO4)(PO4)2 · 0.5C6N2H16, with an extended γ-phase intercalated into organic amine

With a hydrothermal technique, a layered titanium phosphate with the formula Ti₂(H₂PO₄)(HPO₄)(PO₄)₂ · 0.5C₆N₂H₁₆ (denoted TP-J2) has been prepared by treating the Ti/H₃PO₄/H₂O/1-methylpiperazine system directly. The as-synthesized products were characterized by powder X-ray diffraction, CP-MAS solid-state ³¹P NMR spectroscopy, thermogravimetric and differential thermal analyses (TG-DTA). The structure was solved by single-crystal X-ray diffraction analysis and it presents an extended γ-phase intercalated with organic amine. Crystal data: triclinic, , a = 8.106 (2) Å, b = 8.197 (2) Å, c = 11.658 (2) Å.  = 78.32 (3)°, β = 80.85 (3)°, γ = 77.90 (3)°, Z = 2. Additionally, the intercalation behavior of TP-J2 with n-alkyl monoamine (n = 2, 3, 4, 6, 8, 10 and 12) was investigated. Owing to the strong brønsted base, N,N′-dimethylpiperazine, resides in the interlayer, it presented unusual features of TP-J2 in contrast with that of γ-Tip.     

Growth of Sb(2)E(3) (E = S, Se) polygonal tubular crystals via a novel solvent-relief-self-seeding process

A novel solvent-relief-self-seeding (SRSS) process was applied to grow bulk polygonal tubular single crystals of Sb(2)E(3) (E = S, Se), using SbCl(3) and chalcogen elements E (E = S, Se) as the raw materials at 180 degrees C for 7 days in ethanol solution. The products were characterized by various techniques, including X-ray powder diffraction (XRD), scanning electronic microscope (SEM), transmission electronic microscope (TEM), electronic diffraction (ED), and X-ray photoelectron spectra (XPS). The calculated electrical resistivities of the tubular single crystals in the range 20-320 K were of the order of 10(5)-10(6) Omega cm for Sb(2)S(3) and 10(3)-10(4) Omega cm for Sb(2)Se(3), respectively. The studies of the optical properties revealed that the materials formed had a band gap of 1.72 eV for Sb(2)S(3) and 1.82 eV for Sb(2)Se(3), respectively. The optimal reaction conditions for the growth of bulk tubular single crystals were that the temperature was not lower than 180 degrees C and the reaction time was not shorter than 7 days. The possible growth mechanism of tubular crystals was also discussed.     

离子交换法从发酵液中提取谷氨酰胺工艺研究

本文系统地研究了７３２树脂和Ｄ３０１树脂对发酵液中谷氨酰胺的静态和动态吸附性能及影响因素，并对洗脱条件进行了研究。实验结果表明，在阳离子交换柱上有效地降低了谷氨酰胺向谷氨酸的转化，在阴离子交换柱上谷氨酰胺和谷氨酸实现彻底分离，谷氨酰胺的总收率达５６．６％。     

胆甾-4α-甲基-8-烯-3β，7α-二醇二乙酸酯的结构与性质研究

Lophenol, cholest-4α-methyl-7-en-3β-ol (1), obtained from Dracaena cochinchinensis (Lour.) S. C. Chen, was structurally modified. It was acetylated to protect 3β-hydroxyl group, and then oxidised by selenium dioxide in acetic acid to give cholest-4a-methyl-8-en-3β, Ta-diol diacetate (3). This compound 3 is unstable in chloroform solution or when heated and easily converted to a diene compound, cholest-4a-methyl-7,14-dien-3β-ol acetate (4). The structures of 3 and 4 were elucidated by means of IR, ^1H NMR, ^13C NMR and MS, and the absolute configuration of 3 was established by X-ray crystallography. The property of 3 was also discussed in this paper. Both 3 and 4 are new compounds and were reported for the first time.