溶液还原法制备球形超细镍粉

超细镍粉由于表面活性高、导电性和导热性好而被广泛应用于化学催化剂、烧结活化剂、导电浆料门等方面．目前，制备超细镍粉的方法主要有问：真空蒸馏冷凝法、机械粉碎法、电解法、羰基镍热分解法、浆化氢还原法和溶液还原法等．在这些方法中，溶液还原法的工艺简单，所得粉末纯度高，颗粒尺寸小且分布均匀[3]．法国的Figlarz等[4]用弱有机还原剂乙二醇还原粒径小干0．1μm的Ni（OH）2。超细粉末，引入AgNO3。作为成核剂后，制得了粒径＜1μm的超细镍粉，但这种方法需长时间高温回流反应，对原料要求苛刻，且采用有机分散介质成本较高，…     

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．     

Growth and Spectral Properties of Yb^3＋-doped Ba3Gd（BO3）3 Crystal

Crystal of Yb3+-doped Ba3Gd(BO3)3 has been grown by the Czochralski method. The spectroscopic characterizations have been investigated at room temperature. The Yb3+:Ba3Gd(BO3)3 crystal exhibits broad absorption at 976nm with FWHM of 7nm and large overall spitting of 2F7/2 manifold (823cm-1). The absorption and emission cross sections are 5.09×10-21cm2 at 976nm and 0.97×10-21cm2 at 1040nm,respectively. The fluorescence lifetime is 2.84 ms.     

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。     

三氯化铁掺杂稀土聚乙炔的电性能

自从1981年A.Prón等人用三氯化铁掺杂钛系聚乙炔而得到高电导率掺杂聚乙炔以来,对此掺杂聚乙炔的低温电性能已作了一定的研究。不同作者所报道结果可分为两类:一类报道各种掺杂量聚乙炔的电导率均随温度降低而单调减少;另一类则观察到随温度的降低电导率约在200K时出现最大值(增加5%),接着电导率降低。新近我们报导了三氯化铁掺杂的稀土聚乙炔的基本特性。本文进一步对此掺杂稀土聚乙炔的低温电性能作了研究,观察到与上述两种情况相似但不完全相同的结果。     

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)°.     

CHARACTERIZATION OF RADICAL ADDUCTS FORMED DURING PHOTOCHEMICAL SPIN TRAPPING IN LIPOSOMES

There exists an urgent need to monitor radical reactions in biological membranes. With the exception of a few studies in model and natural membranes, most biological spin trapping reactions have been confined to homogeneous media. In the present work we have devised a methodology by which spin trapping reactions can be investigated in liposomes composed of a fully-saturated phospholipid, dimyristoylphosphatidylcholine. Using photochemical spin trapping, we have detected and characterized the formation and partitioning of spin adducts in liposomes. Benzophenone (a lipid-soluble photosensitizer) and benzoyl peroxide (a lipid-soluble radical initiator) have been used to generate free radicals from hydrogen donors during photolysis in liposomes. Both water-soluble and lipid-soluble spin traps have been used to trap the radicals.     

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.     

Syntheses and characterizations of poly[2‐(dimethylamino)ethyl methacrylate]–poly(propylene oxide)–poly[2‐(dimethylamino)ethyl methacrylate] ABA triblock copolymers

A novel, near‐monodisperse, well‐defined ABA triblock copolymer, poly[2‐(dimethylamino)ethyl methacrylate]‐b‐poly(propylene oxide)‐b‐poly[2‐(dimethylamino)ethyl methacrylate], was synthesized via oxyanion‐initiated polymerization. The initiator was a telechelic‐type potassium alcoholate prepared from poly(propylene glycol) and KH in dry tetrahydrofuran. The copolymers produced were characterized by Fourier transform infrared, ¹H NMR, and gel permeation chromatography (GPC). GPC and ¹H NMR analyses showed that the products obtained were the desired copolymers, with narrow molecular weight distributions (ca. 1.09–1.11) very close to that of the original poly(propylene glycol). ¹H NMR, surface tension measurements, and dynamic light scattering all indicated that the triblock copolymer led to interesting aqueous solution behaviors, including temperature‐induced micellization and very high surface activity. © 2002 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 40: 624–631, 2002; DOI 10.1002/pola.10144