两相体系中胰酶拆分DL-苯丙氨酸

将DL-苯丙氨酸与甲醇酯化得DL-苯丙氨酸甲酯盐酸盐,在甲苯/水两相体系中用碳酸氢钠中和DL-苯丙氨酸甲酯盐酸盐得游离DL-苯丙氨酸甲酯,在甲苯/水两相体系中用胰酶拆分DL-苯丙氨酸甲酯得到L-苯丙氨酸和D-苯丙氨酸甲酯,取得了各步反应的最优条件,并将D-苯丙氨酸甲酯外消旋得到DL-苯丙氨酸甲酯继续用于拆分。拆分摩尔收率为61.4%,所得L-苯丙氨酸粗品纯度为92.2%,重结晶后为98.6%,［α］     

高效毛细管电泳法分析苯丙氨酸苯丙酮酸和亚苄基海因

用高效毛细管电泳法同时分析了工业生产过程中的苯丙氨酸、苯丙酮酸和亚苄基海因。该方法简便、高效、快速,并对其分离条件的优化等方面进行了探讨。     

新生儿血液中的多种氨基酸及尿液中的苯丙酮酸和对羟基苯乙酸的GC/MS分析

将新生儿血液中的氨基酸及尿液中的苯丙酮酸和对羟基苯乙酸采用不同的方法提取后，分别探讨两种衍生化技术在氨基酸代谢遗传算病筛查中的应用，即新生儿血样中的氨基酸经甲醇提取后用正丁醇和三氟乙酸酐和其衍生化，或者尿样加入乙腈心除蛋白后用乙酸乙酯提取，双（三甲基硅烷）乙酰硅烷化，衍生物用气相色谱－质谱了用仪选择离子模式检测，用外标同时定量分析血样中10种氨基酸的浓度，结果表明苯丙酮尿症患儿尿样中的苯丙酮酸和对羟基苯乙酸，以及血样中的苯丙氨酸的浓度明显高于正常新生儿，本方法可以推广至多种有机酸定量分析，以实现同步筛查多种氨基酸代谢缺陷症及其他遗传病。     

相转移催化剂催化合成DL-扁桃酸

分子结构为C8H20BrN的季铵盐四乙基溴化铵经实验证明是合成DL-扁桃酸的一种优良的相转移催化剂。研究以苯甲醛和三氯甲烷为原料,在氢氧化钠存在下,应用相转移催化法合成扁桃酸,并探讨反应条件如反应摩尔比、反应时间、催化剂用量对产率的影响。结果表明合成DL-扁桃酸的最佳反应条件为:反应温度65℃,反应时间60min,n(苯甲醛)∶n(三氯甲烷)∶n(四乙基溴化铵)=1∶2∶0.002,产品收率可达到72.41%。     

以β-环糊精衍生物为柱层析固定相拆分氨基酸对映体

用β-环糊精和马来酸酐合成了双(6-氧-丁烯二酸单酯)-β-环糊精 (简称cpd. Ⅰ)并对其结构进行了表征,以cpd.Ⅰ作为柱层析固定相拆分DL-甲硫氨酸、酪氨酸、苯丙氨酸,结果表明,对DL-甲硫氨酸、酪氨酸、苯丙氨酸的拆分率分别可达到21%、47%和52%,研究结果显示:β-环糊精经修饰后拆分这些物质的能力比β-环糊精要好.     

N-十二烷基谷氨酸合成方法综述

N-十二烷基谷氨酸是一种新型的两性氧基酸表面活性剂，具有很好的性能。就其合成方法进行了综述，重点介绍了伯胺烷基醛缩合加氢法和保护羧基氨基选择性合成单N-烷基谷氨酸法。     

(S)-吲哚啉-2-甲酸的合成工艺

研究(S)-吲哚啉-2-甲酸的合成工艺,以草酸二乙酯和邻硝基甲苯为起始原料,在乙醇钾作用下生成邻硝基苯丙酮酸乙酯,用雷尼镍催化加氢、镁粉还原、手性分离得目标产物(S)-吲哚啉-2-甲酸,总收率为38%(以邻硝基甲苯计算).该合成工艺成本低、环境污染小.     

聚醚胺的合成

以丙烯腈和二甘醇原料合成聚醚腈,再经高压加氢制取聚醚胺。探讨了全部反应的最佳工艺条件。     

吡啶胺帕米膦酸的合成与表征

以帕米膦酸和2-氯甲基吡啶为原料,在碱性条件下以水为溶剂,成功合成了吡啶胺帕米膦酸。通过制备型高效液相分离提纯,反应收率达85%,纯度达99%。通过红外光谱、元素分析、质谱、核磁共振谱确证吡啶胺帕米膦酸的结构,并对合成条件和分离提纯条件进行探讨。     

以氨三乙酸为母体的三脚架型配体的合成

为了提高酰胺型三脚架型配体的产率,进一步研究其与稀土离子的配位形式及配合物的荧光性能,以氨三乙酸为母体,草酰氯为氯化试剂,与4种胺在较温和的条件下合成了具有三脚架型结构的配体（L1-L4）,并考察了实验条件、反应温度、反应体系溶剂、缚酸剂、反应时间及催化剂对反应产率的影响．结果表明,在无水条件下,氯化和胺化的反应温度分别不超过40℃和50℃,用少量的吡啶做缚酸剂,DMF做催化剂,溶剂为无水四氢呋喃,胺化反应10h时产率较高．该实验条件温和,分离纯化简单,氯化和胺化反应产率大大提高,从而有利于对三脚架型配合物性质的研究．     

安徽明光凹凸棒石粘土对锶、铯、钴的吸附特性研究

采用静态吸附实验方法,研究了吸附时间、溶液pH值、吸附剂投加量和溶液初始浓度等因素对凹凸棒石粘土吸附Sr₂₊、Cs₊和Co₂₊的性能,并通过等温吸附模型拟合对其吸附过程及吸附机理进行了探讨。结果表明：凹凸棒石粘土对Sr₂₊、Cs₊和Co₂₊的吸附效果依次为Co₂₊ > Cs₊> Sr₂;Freundlich和D-R等温吸附模型能较好地描述凹凸棒石粘土对Sr₂₊、Cs₊和Co₂₊的吸附过程,其中,凹凸棒石粘土对Sr₂₊和Cs₊的吸附以物理吸附为主,而凹凸棒石对Co₂₊的吸附过程以化学吸附为主,并且其吸附方式主要为离子交换的方式发生。     

Thermodynamic modeling of the Ge-La binary system

The Ge-La binary system was critically assessed by means of the calculation of phase diagram (CALPHAD) technique. The associate model was used for the liquid phase containing the constituent species Ge, La, Ge₃La₅, and Ge_1.7La. The terminal solid solution diamond-(Ge) with a small solubility of La was described using the substitutional model, in which the excess Gibbs energy was formulated with the Redlich-Kister equation. The compounds with homogeneity ranges, α(Ge_1.7La), β(Ge_1.7La), and (GeLa), were modeled using two sublattices as α(Ge,La)_1.7La, β(Ge,La)_1.7La, and (Ge,La)(Ge,La), respectively. The intermediate phases with no solubility ranges, Ge₄La₅, Ge₃La₄, Ge₃La₅, and GeLa₃, were treated as stoichiometric compounds. The three allotropic modifications of La, dhcp-La, fcc-La, and bcc-La, were kept as pure element phases since no solubility of Ge in La was reported. A set of self-consistent thermodynamic parameters of the Ge-La binary system was obtained. The calculation results agree well with the available experimental data from literatures.     

Ammonium improves iron nutrition by decreasing leaf apoplastic pH of sunflower plants (<Emphasis Type="Italic">Helianthus annuus</Emphasis> L. cv. Frankasol)

The effect of nitrogen form on pH and concentration of soluble iron (Fe) in leaf apoplast was investigated in hydrophonically grown sunflower plants (Helianthus annuus L. cv. Frankasol), and the mechanism underlying the improved Fe nutrition by ammonium (NH₄) supply was also elucidated. Ammonium supply ameliorated Fe nutrition of plants grown without Fe through decreasing apoplastic pH and increasing soluble Fe concentration in apoplastic fluid of young leaves. The soluble Fe concentration in apoplastic fluid and cell sap of young leaves, and xylem exudates of NH₄ fed-plants was higher than that of nitrate (NO₃) fed-plants, and no typical Fe-deficiency chlorosis in young leaves was observed in NH₄, fed plant without Fe supply. The apoplastic pH was 6.15 and 5.94 in young leaves of Fe-deficient plants fed respectively with NO₃ and NH₄, while in Fe-sufficient plants, the apoplastic pH was 6.43 with NO₃, and 5.50 with NH₄ supply. In primary leaves, the apoplastic pH was around 6.25 irrespective of nitrogen form and Fe supply. The pH of xylem exudate was 5.72 in Fe-deficient plants fed with NO₃ and 5.49 with NH₄. Iron nutrition increased the pH of xylem exudate by 0.27 and 0.16 unit under NO₃ and NH₄ supply respectively.     

Hydrogen storage properties of MgH<Subscript>2</Subscript> co-catalyzed by LaH<Subscript>3</Subscript> and NbH

To improve the hydrogen storage properties of Mg-based alloys, a composite material of MgH₂ + 10wt%LaH₃ + 10wt%NbH was prepared by a mechanical milling method. The composite exhibited favorable hydrogen desorption properties, releasing 0.67wt% H₂ within 20 min at 548 K, which was ascribed to the co-catalytic effect of LaH₃ and NbH upon dehydriding of MgH₂. By contrast, pure MgH₂, an MgH₂ + 20wt%LaH₃ composite, and an MgH₂ + 20wt%NbH composite only released 0.1wt%, 0.28wt%, and 0.57wt% H₂, respectively, under the same conditions. Analyses by X-ray diffraction and scanning electron microscopy showed that the composite particle size was small. Energy-dispersive X-ray spectroscopic mapping demonstrated that La and Nb were distributed homogeneously in the matrix. Differential thermal analysis revealed that the dehydriding peak temperature of the MgH₂ + 10wt%LaH₃ + 10wt%NbH composite was 595.03 K, which was 94.26 K lower than that of pure MgH₂. The introduction of LaH₃ and NbH was beneficial to the hydrogen storage performance of MgH₂.     

四氧化三铁-石墨烯复合芬顿催化剂用于染料脱色的研究

芬顿催化是污水处理中最常用的技术之一,但是传统芬顿试剂需要对水体进行酸化并造成大量亚铁离子浪费.本文用水合肼还原法制备了四氧化三铁-石墨烯复合芬顿催化剂(Fe3O4-G),测试其催化脱色甲烯蓝的活性.Fe3O4-G样品用透射电镜、X射线光电子能谱和红外光谱等表征.Fe3O4-G能催化双氧水分解氧化脱色甲烯蓝.Fe3O4-G在pH3.5~9.5范围内均能有效催化脱色甲烯蓝,最佳pH为8.5.Fe3O4-G的催化活性几乎不受溶剂的影响,加入自由基淬灭剂叔丁醇对脱色也没有明显抑制.Fe3O4-G在较高的温度下催化能力更强,增大双氧水用量也能促进脱色反应.     

Graded bandgap semiconductor thin film photoelectrodes

A graded bandgap oxide semiconductor thin film electrode was designed in order to obtain a photoelec-trochemically stable photoelectrode, with wide absorption range. The graded bandgap Ti_1−x V _x O₂ film electrode was prepared by heating the stacked layers of V/Ti in varying ratios, which were coated on the substrate by the sol-gel method using the starting solution with various V/Ti ratios. XPS result showed that the composition gradient was achieved for the film. The Ti_1−x V _x O₂ film electrode was found to be photoelectrochemically stable. Its photovoltage was about 360 mV. Obvious visible light photoresponse was observed for the Ti_1−x V _x O₂ film electrode. Compared with the pure TiO₂ electrode, the photocurrent onset potential of the Ti_1−x V _x O₂ film electrode was shifted positively, probably because the accumulation of vanadium at the electrode surface causes the recombination of the electrons and holes, and the lowest level of the conduction band of Ti_1−x V _x O₂ is lower than that of TiO₂. Impedance analysis showed that the donor density of the Ti_1−x V₂O₂ film electrode was higher than that of TiO₂ film electrode.     

Syntheses and lyotropic liquid crystal properties of a series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30

A series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30, Na16[As4W30M4(H2O)2O112]·XH2O (M = Zn,Cu,Co,Ni,Mn and Cd), have been synthesized for the first time and structurally characterized by elemental analysis, IR and 183W NMR spectra. The crystal structure of Na16[As4W30Cu4(H2O)2O112]·63H2O was determined to be a triclinic system, of P1 symmetry, a = 1.2721(3) nm, b = 2.451 6(5) nm, c = 2.6450(5) nm, α= 89.90(3)°,β= 77.32(3)°, γ= 89.96(3)°, 2=2. Using tetrahepty lammonium bromide as a phase transfer reagent, [As4W30Cu4(H2O)2O112]16- was transferred from aqueous solution to organic phase (benzene), and the heteropolyanion lost the coordination water molecules to form the coordination-unsaturated ion. After lactic acid was added to the benzene solution, the coordination-saturation was recovered. By esterification reaction between lactic acid and cholesterin, the latter was attached to the heteropolyanion indirectly. Therefore, a new type of lyotropic liquid crystal was obtained, which was characterized by a polarimicroscope, DSC and variable temperature wide-angle X-ray diffraction.     

Structure and corrosion resistance of Al–Cu–Fe alloys

The microstructure and electrochemical properties of Al–Cu–Fe alloys with the atomic compositions of Al_(65)Cu_(20)Fe_(15),Al_(78)Cu_7Fe_(15)and Al_(80)Cu_5Fe_(14)Si_1have been studied.The alloys were produced by induction melting of pure elements with copper mold casting.The microstructure of the alloys was analyzed by X-ray diffraction and high-resolution transmission electron microscopy.The formation of quasicrystalline phases in the Al–Cu–Fe alloys was confirmed.The presence of intermetallic phases was observed in the alloys after crystallization in a form of ingots and plates.The electrochemical measurements were conducted in 3.5%NaCl solution.The electronic structure of the alloys was determined by X-ray photoelectron spectroscopy.The post corrosion surface of the samples was checked using a scanning electron microscope equipped with the energydispersive X-ray detector.It was observed that the Al_(65)Cu_(20)Fe_(15)alloy had the highest corrosion resistance.The improved corrosion resistance parameters were noted for the plate samples rather than those in the as-cast state.And the hardness of the Al_(65)Cu_(20)Fe_(15)alloy was significantly higher than the other alloy samples.     

玻璃粉对混凝土酸侵蚀性能的影响

采用试验方法,研究了玻璃粉替代胶凝材料在不同掺量(0、5%、8%、15%)时对混凝土抗压强度和耐酸侵蚀性的影响。对比了各个试样在5%H2SO4溶液和5%CH3COOH溶液中腐蚀28 d后的质量亏损和抗压强度损失,并采用SEM分析了试样腐蚀后的表面形貌。结果表明,玻璃粉有利于提高混凝土的耐H2SO4和CH3COOH侵蚀性,耐CH3COOH侵蚀差于耐H2SO4腐蚀,H2SO4侵蚀后的试样表面形成了大量石膏,CH3COOH侵蚀后试样表面疏松并出现了大量孔洞和裂纹。当玻璃粉掺量为8%时,试样的耐H2SO4和CH3COOH侵蚀性最佳。     

钕铁硼强磁性材料的冲击加载实验和数值模拟研究

为了研究钕铁硼(Nd2Fe14B)强磁体在冲击加载作用下的动态力学性能,建立了炸药爆炸平面波冲击加载实验装置,进行了冲击加载实验.采用锰铜压阻测压技术测量了磁体中冲击波压力,获得了不同强度冲击波加载作用下磁体中冲击波压力.建立了Nd2Fe14B磁体冲击加载实验的计算模型,对炸药爆炸冲击加载磁体过程进行了数值模拟计算,计算结果与实验结果相吻合.分析了Nd2Fe14B磁体中冲击波传播规律,给出了Nd2Fe14B磁体中冲击波压力按指数规律衰减的计算公式.