A SIMPLE METHOD FOR CHIRAL RESOLUTION OF 1,1''''-BI-2-NAPHTHOL

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A simple method for chiral resolution of 1,1′-Bl-2-naphthol

An improved method for preparing enantiomerically pure 1,1′-bi-2-naphthols is described. 1,1′-bi-2-naphthol boric anhydride was generated from the reaction of racemic 1,1′-bi-2-naphthol and boric anhydride. Its two diastereoisomers, could be efficiently separated in THF using (L)-proline as the resolving agent. Treatment in three successive steps yielded 79% and 74% enantiomerically pure (S)-and (R)-1,1′-bi-2-naphthol respectively.     

水合物法分离H2+C2H4气体混合物相平衡实验研究

采用水合物吸收法,以THF为吸收剂,进行了吸收法分离(H2 C2H4)气体混合物的相平衡实验研究。结果表明,采用THF做吸收剂可望获得很好的(H2 C2H4)气体混合物吸收分离效果。     

电导法测定醋酸在H2O和THF混合溶剂中的活度系数

用电导法测定了醋酸在不同温度时和不同浓度下在H2O和THF混合溶剂中的电导丰，应用Debye-Hucker和OsagerFalkenhangen公式计算了醋酸在混合溶剂中的活度系数。并讨论了温度和浓度对电解质活度系数的影响。结果表明。电解质溶液的活度系数随着温度的增加而增大，随着浓度的增加而减小。     

INFLUENCE OF SOLVENT AND POLYMER SORT ON ANOMALOUS RHEOLOGICAL BEHAVIOR OF POLYMER SOLUTION AT HIGH DILUTION

ＩＮＴＲＯＤＵＣＴＩＯＮＰｏｌｙｍｅｒｓｉｎｍｅｄｉｕｍａｔｈｉｇｈｄｉｌｕｔｉｏｎｈａｖｅａｂｒｏａｄｒａｎｇｅｏｆａｐｐｌｉｃａｔｉｏｎｓｎｏｗａｄａｙｓ.Ｔｈｅｙｗｅｒｅｕｓｅｄａｓｐｏｕｒｐｏｉｎｔｄｅｐｒｅｓｓａｎｔａｎｄｖｉｓｃｏｓｉｔｙｒｅ ｄｕｃｅｒｏｆｃｒｕｄｅｏｉｌａｎｄｉｔｓｐｒｏｄｕｃｔｓｓｕｃｈａｓＥＶＡａｎｄｉｔｓｄｅｒｉｖａｔｉｖｅｓ(ＳｕｎｉｌＫｕｍｅｒ,1 989;Ｑｉａｎｅｔａｌ.,1 996;Ｑｉａｎｅｔａｌ.,1 996;Ｑｉｅｔａｌ.,1 992 ) ;ｄｒａｇｒｅｄｕｃｅｒｏｆｗａｔｅｒ…     

Influence of solvent and polymer sort on anomalous rheological behavior of polymer solution at high dilution

The rheological behavior of polyvinyl acetate (PVAc) in N,N′=dimethylformamide (DMF), methyl ethyl ketone (MEK), 1,2-dichloroethane (DCE), tetrahydrofuran (THF) and toluene (TOL), polystyrene (PS) in DMF, MEK, DCE, THF and cyclohexane (CYH), and random ethylene-vinyl acetate (EVA) copolymer in DCE, TOL, CYH with and without surfactant of Span80 and in the DCE/CYH solvent mixtures with surfactant of Span80 was examined at high dilution. It was shown that the extent and type of the upsweep or downsweep (anomalous rheological behavior) of the reduced viscosity-concentration curves of these different polymers at high dilution are markedly dependent on the dielectric constant of the solvent and the polarity of the polymer used. The experimental results indicated that the anomalous rheological behavior of EVA copolymer, widely used as a flow improver, is related to its efficiency in reducing viscosity and depressing pour point of crude oil and waxy solvents. Project (No.29774020) suppored by the Natural Science Foundation of China(NSFC).     

苄基取代茚基二价稀土配合物的合成与表征

无水EuCl3与1—苄基茚基钾在四氢呋喃(THF)中以1／2的摩尔比反应，尔后用Na／K合金原位进行还原，得到了一种新的中性的二(1—苄基茚基)稀土Ⅱ配合物(1—PhCH2C9H6)2Eu(THF)2；而用SmI2与1—苄基茚基钾在THF中以1／2的摩尔比反应，合成了一种新的苄基取代茚基稀土二价配合物(1—PhCH2C9H6)2Sm(THE)2，并对其进行了元素分析及红外光谱的表征。     

Effects of organic solvents on two retinal pigment epithelial lipofuscin fluorophores,A2E and all-trans-retinal dimer

Gene and drug therapies are being developed to alleviate vision loss in patients with Stargardt’s disease and age-related macular degeneration (AMD). To evaluate the therapeutic effects of these treatments, organic solvents are routinely used to extract and quantify bisretinoid lipofuscin constituents, such as N-retinylidene-N-retinyl-ethanolamine (A2E) and all-trans-retinal dimer (ATR-dimer). By high-performance liquid chromatography (HPLC), we found that A2E and ATR-dimer were both altered by tetrahydrofuran (THF) and chloroform, but were stable in dimethyl sulfoxide (DMSO) or methanol (MeOH). In addition, cyclohexane and ethanol (EtOH) did not alter ATR-dimer, whereas an alteration of A2E occurred in EtOH. On the basis of these findings, we designed processes II–IV, generated by modifications of process I, a routine method to measure bisretinoid compounds in vivo. Extra amounts of either ATR-dimer or A2E in mouse eyecups were released by processes II–IV versus process I. Efforts to clarify the effects of organic solvents on lipofuscin pigments are important because such studies can guide the handling of these fluorophores in related experiments.     

新型桥联茂基轻稀土氯化物的合成及表征

研究了新型二甲撑桥联茂基轻稀土氯化物的合成,首先通过环戊二烯钠与1,2－二溴乙烷在四氢呋喃中发生反应形成二甲撑桥联环戊二烯,随后二甲撑桥联环戊二烯与金属钠作用使其转化成二甲撑桥联环戊二烯二钠盐,无水三氯化稀土LnCl3（Ln=Pr,Nd）与二甲撑桥联环戊二烯二钠盐NaC5H4CH2CH2C5H4Na以1：1摩尔比在四氢呋喃溶液中反应得到新型二甲撑桥联环戊二烯基轻稀土氯化物（C5H4CH2CH2C5H4）LnCl·THF（Ln=Pr,Nd）,产物经元素分析和红外分析的表征。     

9,10-二苯乙炔基蒽的合成及光谱性质研究

本研究以二溴蒽和苯乙酮为原料,通过Sonogashira钯催化偶联反应,四氢呋喃和二乙胺混合溶剂作为偶联反应溶剂,以较高的收率获得了标题化合物,且运用IR,UV,熔点等手段进行了结构鉴定,并通过紫外光谱和荧光光谱研究了其光谱性质。     

岩石及粉尘中游离二氧化硅的测定

采用焦磷酸分离岩石及粉尘中的游离二氧化硅,再用氢氟酸-饱和氯化钾将分离出来的游离二氧化硅溶解,使硅形成K2SiF6沉淀.然后水解,应用氟离子选择性电极间接测定游离二氧化硅的含量,方法简便、准确、快速.     

一些因素对聚异戊二烯分子量分布的影响

本工作研究了以环乙烷为溶剂,以n－BuLi为引发剂,分别在t－BuOLi和四氢呋喃（THF）存在下使异成二烯聚合时t－BuOLi和四氢呋喃对聚异戊二烯分子量分布的影响;还研究了引发剂n－BuLi和sec－BuLi在聚合体系中的浓度对聚异戊二烯分子量分布的影响。实验结果表明,以n－BuLi为引发剂以环乙烷为溶剂时,向聚合体系中加入极少量t—BuOLi就会使聚异戊二烯的分子量分布变得很窄。实验结果还表明,聚合体系中引发剂的浓度对聚异戊二烯的分子量分布有明显影响。     

纳米锰钛催化剂制备及其光催化降解甲醛的研究

选取镍镉网为基体,利用硫酸氧钛和醋酸锰合成了一种锰钛光催化剂,XRD分析其主要由锐钛矿型的TiO2晶体及α-MnO2构成,根据Scherrer方程计算晶粒尺寸约为20nm和30nm。以甲醛为污染物,研究了污染物初始浓度、催化剂用量、反应相对湿度和光能量等反应条件对甲醛降解效率的影响,通过实验得出了最佳的反应条件。     

改进的SnCl2-TiCl3法测定铁含量

用改进的SnCl2-TiCl3法测定铁矿石中铁含量,考察了预处理时间、加入SnCl2的量、加入硫-磷混酸的量、还原温度和放置时间对测定结果的影响,做了大量的条件试验,并与经典的SnCl2-HgCl2法进行比较,经试验证明,该方法不仅结果准确度高,精确度好,同时操作简便,且不会给环境带来污染。     

Remarkable rate acceleration of SmI3-mediated iodination of acetates of Baylis-Hillman adducts in ionic liquid： facile synthesis of （Z）-allyl iodides

Stereoselective transformation of Baylis-Hillman acetates I into corresponding （Z）-allyl iodides 2 has been achieved by treatment of I with samarium triiodide in THF. Remarkable rate acceleration of samarium triiodide-mediated iodination of 1 was found when ionic liquid 1-n-butyl-3-methyl-imidazolium tetrafluroborate （[bmim]BF4） was used as reaction media in stead of THF. This novel approach proceeds readily at 50 ℃ within a few minutes to afford （Z）-allyl iodides 2 in excellent yields. A mechanism involving stereoselective iodination of the acetates of Baylis-Hillman adducts by samarium triiodide is described, in which a six-membered ring transition state played a key role in the stereoselective formation of 2.     

(CH4+C2H4+THF+H2O)体系相平衡实验研究

开发了一种水合物法分离甲烷-乙烯混合气体的新技术,利用选择性热力学促进剂THF对C1、C2气体的选择性增溶作用来提高它们的水合分离效率,并系统地测定了(CH4 C2H4 THF H2O)体系气-水合物相平衡实验数据,考察了温度、初始压力、初始气液比对(CH4 C2H4)气体混合物分离效果的影响。     

纳米二氧化钛光催化性能研究

Nano-TiO2 powders with pure anatase sturcture were prepared by the method of precipitation-solution-gelation,using H2TiO3,hydrogen peroxide and ammonia as reactants.Active red X-3B dye solution was selected as a model pollutant for the photocatalysis degradation experiments,The effects of grain sizes,dosage and microostructure of nano-TiO2 on itsphotocatalysis properties were studied.The results show that photo-activity of the nano-TiO2 is enhanced with the grain sizes reducing or dosages increasing of nano-TiO2,Howerver,excess increase in nano-TiO2 concentration is not advantageous to the enhancement of the photo-activity.Anatase TiO2 demonstrated a higher photo-activity than rutile TiO2,The dye solution hardly degraded without nano-TiO2 powders being added into it or under sunlight irradiation.     

木材结晶结构对其溶液化的影响

采用X射线衍射及气相色谱分析 ,研究未改性木材、碱处理木材及苯甲基化改性木材的结晶结构 ,以及它们在盐酸催化条件下在甲苯和四氢呋喃中的溶解性 ,并色质联用分析了苯甲基化木粉液化产物中上层溶液的组成 .实验证明 ,较大体积苯甲基基团的引入显著地改变了木材的结晶结构 ,增大了自由体积 ,有利于溶剂分子渗透到木材基体内部 ,极大地提高了木粉的溶解性 .随着增重率增加 ,溶液化产品的残余量下降而结合溶剂量上升 ,这表明了溶液化过程变得易于进行 .此外 ,考察了影响苯甲基化木材溶液化的各种因素 .实验结果表明 ,以甲苯为溶剂时 ,随着溶液化时间的延长以及催化剂用量的加大 ,苯甲基化木材的溶解性能显著提高 ,以四氢呋喃为溶剂存在着最佳的溶液化时间和催化剂用量     

TiO2纳米材料催化PBT合成的工艺条件的探讨

用溶胶－凝胶法制备TiO2纳米材料，作为PBT合成催化剂，探索其合成的工艺条件。纳米TiO2催化PBT合成的工艺条件为：PH值在5左右，酯交换温度为180－190℃，真空度越高越好（要求在90Pa以下）。     

碘量法快速测定烟气SO2

烟气SO2的测定,无论是碘量法还是光度法,都需要先采样后分析,费时较多。本文在碘量法的基础上,提出一种烟气SO2快速测定方法,采样、分析同时完成,操作简便、快速,现场适应性强。