锌镍铝水滑石微球的制备及吸附性能

以Zn（NO₃）₂·6H₂O、Ni（NO₃）₂·6H₂O、Al（NO₃）₃·9H₂O和尿素为原料,采用一步水热法制备分散性良好的三元锌镍铝水滑石（ZnNiAl-LDHs）微球。通过X射线衍射（XRD）、傅里叶转换红外光谱（FTIR）、场发射扫描电镜（FESEM）、透射电镜（TEM）和氮气吸附-脱附等测试手段对样品的结构和形貌进行表征,并比较ZnNiAl-LDHs和ZnAl-LDHs对甲基橙（MO）的吸附性能。结果表明,ZnNiAl-LDHs是由纳米片组成、具有3D结构的微球,粒径为1~2.5 μm,比表面积为156 m²·g^-1,远大于ZnAl-LDHs的比表面积38 m²·g^-1;ZnNiAl-LDHs和ZnAl-LDHs对甲基橙的饱和吸附量分别为329.60和143.47 mg·g^-1,ZnNiAl-LDHs表现出更强的吸附能力,其吸附等温线和吸附动力学分别符合Langmuir等温线模型和准二级动力学模型。     

不同表面形貌Cu2O空心球的制备及光催化性能

采用一步溶剂热法,以Cu(NO_3)_2·3H_2O为铜源,乙二醇(EG)为还原剂,聚乙烯吡咯烷酮(PVP)为表面活性剂,高温条件下制备形貌可控的Cu_2O空心球纳米材料。研究Cu(NO_3)_2·3H_2O与PVP的质量比值(w_(Cu(NO_3)_2·3H_2O)/w_(PVP))对Cu2O结构、形貌、比表面积以及光吸收特性的影响,并结合光催化机理讨论其对Cu_2O光催化性能的影响。此外,通过改变反应时间来研究Cu_2O的生长过程。结果表明,w_(Cu(NO_3)_2·3H_2O)/w_(PVP)=45时,得到的形貌为空心球表面覆盖纳米刺的Cu_2O纳米材料光催化性能最佳,在可见光辐照10 min的条件下,对甲基橙的降解率达94.3%。     

铁酸铋的水热合成及其光催化性能

以Fe(NO_3)_3·9H_2O和Bi(NO_3)_3·5H_2O为原料,NaOH为矿化剂,用水热法合成了柱状晶体Bi_2Fe_4O_9,其结构和催化性能经XRD,SEM和UV-Vis表征.结果表明,Bi_2Fe_4O_9截面边长约500 nm,长约2μm～3μm,分散均匀.Bi_2Fe_4O_9在可见光区域有较强吸收,对甲基橙降解效果较好.     

基于4-甲基-3-苯基-5-(2-吡啶基)-1,2,4-三唑的Cu(Ⅱ)、Ni(Ⅱ)和Cd(Ⅱ)配合物的合成、晶体结构及性质（英文）

4-甲基-3-苯基-5-(2-吡啶基)-1,2,4-三唑(L)分别与CuCl_2·2H_2O、Ni(NO_3)_2·6H_2O、Cu(ClO_4)_2·6H_2O和Cd(NO_3)_2·4H_2O反应合成了配合物[CuL_2Cl]Cl·H_2O(1)、[NiL_2(H_2O)_2](NO_3)_2(2)、[CuL_2(H_2O)_2](ClO_4)_2(3)和[CdL_2(NO_3)_2]·CH_3CN(4),测定了它们的X射线单晶结构,并用红外光谱、紫外光谱、荧光和热重分析进行了表征。配合物1属于正交晶系,空间群为Fddd,中心离子Cu1(Ⅱ)具有畸变的四方锥构型[CuN_4Cl]。配合物2、3和4都属于单斜晶系,空间群分别为P2_1/n,P2_1/n和P2_1/c。配合物2、3和4的中心离子Ni1(Ⅱ)、Cu1(Ⅱ)和Cd1(Ⅱ)都为畸变的八面体构型[NiN_4O_2]、[CuN_4O_2]和[CdN_4O_2]。     

基于细胞壁结构变化研究铈和镧影响大肠杆菌生长的机制EI北大核心CSCD

从细胞壁结构变化角度研究Ce(NO_3)_3·6H_2O和La(NO_3)_3·6H_2O对大肠杆菌生长影响的机制。以Penicillin和Lysozyme对细菌细胞壁作用靶点为参照,比浊法表征细菌的生长,红外光谱法表征细菌细胞壁肽聚糖(3427和1654 cm^(-1))和β-1,4糖苷键(890 cm^(-1))结构,扫描电镜观察菌体形态。比浊法显示Penicillin和Lysozyme抑制了细菌的繁殖,Ce(NO_3)_3·6H_2O和La(NO_3)_3·6H_2O均可以逆转这一抑制作用,促进细菌繁殖;红外光谱显示Penicillin使大肠杆菌细胞壁相应位点透过率下降,La(NO_3)_3·6H_2O使其透过率增加;Lysozyme使相应位点透过率增加,La(NO_3)_3·6H_2O使其透过率下降或基本不变,表明La(NO_3)_3·6H_2O总是可以逆转Penicillin和Lysozyme对大肠杆菌细胞壁的破坏作用;Ce(NO_3)_3·6H_2O对大肠杆菌细胞壁相应位点的红外光谱透过率影响复杂,没有表现出可逆转Penicillin和Lysozyme对细胞壁的破坏能力。La(NO_3)_3·6H_2O通过使细胞壁中相邻多糖链交联和保护β-1,4糖苷键来保护大肠杆菌细胞壁肽聚糖结构,促进细菌的生长,与前期研究La(NO_3)_3·6H_2O对枯草芽孢杆菌的作用规律一致;Ce(NO_3)_3·6H_2O促进细菌生长的机制与La(NO_3)_3·6H_2O有所不同,具体原因还有待研究。     

基于细胞壁结构变化研究铈和镧影响大肠杆菌生长的机制

从细胞壁结构变化角度研究Ce(NO_3)_3·6H_2O和La(NO_3)_3·6H_2O对大肠杆菌生长影响的机制。以Penicillin和Lysozyme对细菌细胞壁作用靶点为参照,比浊法表征细菌的生长,红外光谱法表征细菌细胞壁肽聚糖(3427和1654 cm~(-1))和β-1,4糖苷键(890 cm~(-1))结构,扫描电镜观察菌体形态。比浊法显示Penicillin和Lysozyme抑制了细菌的繁殖,Ce(NO_3)_3·6H_2O和La(NO_3)_3·6H_2O均可以逆转这一抑制作用,促进细菌繁殖;红外光谱显示Penicillin使大肠杆菌细胞壁相应位点透过率下降,La(NO_3)_3·6H_2O使其透过率增加;Lysozyme使相应位点透过率增加,La(NO_3)_3·6H_2O使其透过率下降或基本不变,表明La(NO_3)_3·6H_2O总是可以逆转Penicillin和Lysozyme对大肠杆菌细胞壁的破坏作用;Ce(NO_3)_3·6H_2O对大肠杆菌细胞壁相应位点的红外光谱透过率影响复杂,没有表现出可逆转Penicillin和Lysozyme对细胞壁的破坏能力。La(NO_3)_3·6H_2O通过使细胞壁中相邻多糖链交联和保护β-1,4糖苷键来保护大肠杆菌细胞壁肽聚糖结构,促进细菌的生长,与前期研究La(NO_3)_3·6H_2O对枯草芽孢杆菌的作用规律一致;Ce(NO_3)_3·6H_2O促进细菌生长的机制与La(NO_3)_3·6H_2O有所不同,具体原因还有待研究。     

硅藻土原位负载网状纳米结构硅酸镁及其对Cr(Ⅵ)吸附性能

采用MgCl_2·6H_2O作为镁源,NH_3·H_2O作为沉淀剂,十六烷基三甲基溴化铵(CTAB)作为模板剂,以水热法在硅藻土表面原位生长纳米花状Mg(OH)_2,随反应时间增加,转变成单斜晶系网状结构Mg_3Si_4O_(10)(OH)_2纳米花。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)、氮气吸附-脱附测试、傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)等测试手段对样品进行了表征,结果显示:反应时间为0.5～2.0 h时硅藻土表面以生长Mg(OH)_2为主,样品的比表面积为180 m~2·g~(-1);反应时间至3h时,硅藻土表面Mg(OH)_2转化成网状结构Mg_3Si_4O_(10)(OH)_2,样品比表面积增大到350 m~2·g~(-1),此复合结构对Cr(Ⅵ)最大吸附量可达570 mg·g~(-1)。     

1,2-环己二胺缩邻香兰素单核与四核镱稀土配合物的近红外性质（英文）

通过配体1,2-环己二胺缩邻香兰素(H2L)和不同的镱盐反应,合成了4个镱稀土配合物[Yb(H_2L)_2](ClO_4)_3·2CH_3OH·H_2O(1),[Yb_4(L)_4(NO_3)2(H_2O)_2](PF_6)_2·4CH_3CN(2),[Yb_4(L)_4(H_2O)_2Cl_2](PF6)_2·2CH_2Cl_2·2H_2O(3)和[Yb_4(L)_4(NO_3)_2(H2O)_2][Yb(NO_3)_3(H_2O)_2(CH_3OH)](NO_3)_2·4CH_2Cl_2·6CH_3OH(4)。X射线单晶衍射分析表明配合物1为零维的单核结构,配合物2~4均为四核结构。研究了4个配合物的近红外发光性能。     

常压水热法合成玉米棒状In_2O_3及其性能研究

以In(NO_3)_3·4.5H_2O和(NH_2)_2CO为原料,采用常压水热法于95℃反应22 h制得氧化铟(In_2O_3)前驱物氢氧化铟,于600℃煅烧2 h合成了In_2O_3粉体,其结构、形貌及性能经紫外-可见(UV-Vis)光谱、X-射线衍射(XRD)、拉曼光谱和扫描电镜(SEM)表征。以甲基橙为目标降解物,研究了In_2O_3粉体的光催化活性。结果表明:In_2O_3粉体为体心立方晶系方铁锰矿结构和亚稳相刚玉六方结构的混合体,In_2O_3的UV-Vis谱图中出现了明显的蓝移。当In(NO_3)_3·4.5H_2O和(NH_2)_2CO物质的量比为1∶7时,In_2O_3粉体中出现了玉米棒状结构,棒状体长度约为500 nm,直径约150 nm;该棒状结构的In_2O_3对甲基橙有较好的光催化活性,在紫外光照射6.5 h后甲基橙的降解率为69.7%。     

Fe3O4@HTlc的制备及其对甲基橙的吸附研究

采用液相非稳态共沉淀法制备了磁性镁铝类水滑石(Fe3O4@HTlc),采用透射电子显微镜、粉末X射线衍射仪、傅里叶变换红外光谱仪、振动样品磁强计、比表面分析仪、微电泳仪等对样品的形貌和结构进行了表征,并比较了 Fe3O4@HTlc和HTlc对甲基橙的吸附性能。结果表明,Fe3O4@HTlc为顺磁性、具有核-壳结构和较大比表面积、带有正电荷的近球状颗粒。甲基橙在Fe3O4@HTlc和HTlc上的吸附动力学曲线均符合准一级动力学方程;吸附等温线均符合Langmuir吸附等温式;298 K时Fe3O4@HTlc和HTlc对甲基橙的饱和吸附量分别为138.89和147.06 mg/g,但Fe3O4@HTlc对甲基橙有较强吸附推动力和较短的吸附平衡时间。二者对甲基橙的吸附量均随温度的升高和pH (5~11)的增加而降低。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

解决能源问题的新途径--光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。