致密皮层非对称气体分离膜的制备

以湿相转化法制备出分离性能优良的致密皮层非对称气体分离膜；建立了醋酸纤维素 丙酮 甲醇三组分制膜体系，所制得的致密皮层醋酸纤维素非对称气体分离膜，在室温、０５ＭＰａ进气压力下，该膜对ＣＯ２／ＣＨ４的分离系数３０，ＣＯ２透气速率可达１８×１０－８ｃｍ３（ＳＴＰ）／ｃｍ２·ｓ·Ｐａ；扫描电镜图显示该膜表层致密、超薄（约２００ｎｍ）、支持层疏松，为理想结构的非对称气体分离膜．     

半导体催化膜上泵氧甲烷氧化偶联反应的研究 Ⅱ.联合体系的反应

在常压及６５０℃下，以含１％Ｏ２的甲烷－氧混合气进料，考察了在ＣａＯ，ＳｒＯ，ＺｎＯ，ＴｉＯ２，ＣｅＯ２和ＭｎＯ２膜上外加电流为－９０～９０ｍＡ范围内联合体系的甲烷氧化偶联反应，结果表明，在ｐ型和ｎ型半导体催化膜上，发生ＮＥＭＣＡ效应的增强因子有一极值，联合体系中泵氧ＯＣＭ反应的Ｃ２烃选择性低于开路体系中反应的Ｃ２烃选择性，根据总反应速率求出了总传递系数及电化学影响效率，电化学影响效率随ｎ型电导率     

CO2／CH4分离膜及沸石填料影响渗透过程的研究

报导了甲基硅橡胶和纤维素（ＣＡ、ＣＴＡ、ＥＣ）膜对ＣＯ２、ＣＨ４的选择透气性能，并讨论了沸石作为填料所引起的分子筛作用的气体渗透过程。甲基硅橡胶的气体渗透系数最高，而选择性最低，且不受填料沸石的影响。纤维素膜的气体选择性较大，渗透系数可以通过沸石的加人而明显增加。特别是沸石１３Ｘ．沸石３Ａ、４Ａ、５Ａ在ＥＣ膜中对气体分子筛作用，改变了气体原有的渗透过程，提高了选择性。使用Ａｒｒｈｅｎｉｕｓ公式计算出ＥＣ－沸石３Ａ膜的气体渗透活化能。     

半导体催化膜上泵氧甲烷氧化偶联反应的研究 Ⅰ.传递体系的反应

在常压及６５０℃下,考察了ＣａＯ,ＳｒＯ,Ｌａ２Ｏ３,ＺｎＯ,ＴｉＯ２,ＣｅＯ２和ＭｎＯ２膜上外加电流为１６～９０ｍＡ时传递物系的甲烷氧化偶联反应结果,结果发现,在ｎ型ｐ型半导体催化膜上,ＣＯ２,Ｃ２Ｈ４和Ｃ２Ｈ６的生成速率都随泵氧量的增加而增大,而Ｃ２烃选择性随泵氧量的增加而下降,但ｐ型半导体膜上的Ｃ２烃选择性比ｎ型半导体膜上的要高：ｑ型半导体膜上Ｃ２烃选择性与其电导率大小顺序相一致,增强因子的     

TiO2陶瓷顶层膜的化学气相淀积生长研究

以ＴｉＣｌ和Ｔｉ（ＯＣ４Ｈ９）４为源物质采用热化学气相淀只（ＣＶＤ）法及射频ＰＣＶＤ法在多孔α－Ａｌ２Ｏ３陶瓷衬底上淀积生长ＴｉＯ２薄膜，观测ＴｉＯ２膜的生长方式、生长速率以及结构和表面形貌等，讨论其生长机制，评价ＣＶＤ改性生长的顶怪ＴｉＯ２陶瓷膜的气体渗透性。     

温度对聚苯并咪唑吡咯酮膜透气性能的影响

研究了两种聚苯并咪唑吡咯酮均质膜在一个大气压下温度对Ｈ２、Ｏ２、Ｎ２的透过性能的影响．在分子链结构中引入空间位阻大的－Ｃ（ＣＦ３）２－基因，气体的透过系数有明显增加，提高了一个数量级，其中Ｈ２的透过系数为７４Ｂａｒｒｅｒ，对Ｈ２、Ｎ２的选择分离系数为５０．随着温度的升高，两种膜的透过系数均增加，而选择性降低．     

甲烷部分氧化制合成气的钙钛矿型致密透氧膜反应器的数值模拟(英文)

采用等温理论模型,以甲烷催化氧化制合成气为模型反应,模拟非担载钙钛矿型致密透氧膜反应器的性能。分别研究了Ｌａ_０．２Ｂａ_０．８Ｆｅ_０．８Ｃｏ_０．２Ｏ_(３－δ)、Ｌ３０．２Ｓｒ０．８Ｆｅ０．８Ｃｏ０．２Ｏ３－δ和ＳｒＦｅＣｏ０．５Ｏｘ三种透氧速率不同的膜材料、膜反应器的尺寸以及反应工艺条件对ＣＨ４转化率、ＣＯ选择性和Ｈ２／ＣＯ摩尔比的影响,对膜反应实验具有指导意义。     

甲烷直接氧化制甲醇Ⅱ．催化膜反应器（CMR）

采用溶胶－凝胶（Ｓｏｌ－Ｇｅｌ）法制备了微孔结构均匀的“ＳｉＯ＿２／陶瓷”膜和“Ｍｏ－Ｃｏ－·Ｏ／ＳｉＯ＿２／陶瓷”催化功能膜，并用ＸＲＤ、ＳＥＭ和孔径测定等技术进行了表征。在常压、５００～７００℃的条件下，在催化膜反应器（ＣＭＲ）中考察了甲烷氧化制甲醇的反应。在相似的反应条件下（转化率为１．０％），用ＣＭＲ（甲醇选择性１１．２％）可获得较固定床反应器（甲醇选择性４．５％）高得多的甲醇选择性。     

甲烷直接氧化制甲醇：Ⅱ.催化膜反应器（CMR）

采用溶胶－凝胶（Ｓｏｌ－Ｇｅｌ）法制备了微孔结构均匀的“ＳｉＯ２／陶瓷”膜和“Ｍｏ－Ｃｏ－Ｏ／ＳｉＯ２／陶瓷”催化功能膜，并用ＸＲＤ、ＳＥＭ和孔径测定等技术进行了表征。在常压，５００～７００℃的条件下，在催化膜反应器（ＣＭＲ）中考察了甲烷氧化制甲醇的反应。在相似的反应条件下（转化率为１．０％），用ＣＭＲ（甲醇选择性１?．２％）可获得较固定床反应器（甲醇选择性４．５％）高得多的甲醇选择性。     

Triton X—100／C10H21OH／H2O体系层状液晶中水溶性超微粒子材…

利用溶剂在层状液晶中的渗透性和层状液晶中溶剂层厚度的限定性，在ＴｒｉｔｏｎＸ－１００／Ｃ１０Ｈ２１ＯＨ／Ｈ２Ｏ体系状液晶中，以饱和Ｎａ２Ｃ２Ｏ４水溶液代替给分水制备水溶性超微粒子材料Ｎａ２Ｃ２Ｏ４，平均粒径约为６ｎｍ。     

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。     

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.     

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.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

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.     

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。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

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^-。