苯乙烯－甲基丙烯酸共聚物和聚环氧丙烷共混体系的相容性研究

 本文用傅里叶交换红外光谱法（ＦＴＩＲ）表征了苯乙烯－甲基丙烯酸共聚物Ｐ（Ｓ－ＭＡＡ）和聚环氧丙烷（ＰＰｒＯ）共混体系的相容性．用谱带分离的技术比较准确地测定了共混体系中几种羰基的吸光系数比，并且用简明的方法定量计算了它们之间平衡的平衡常数．同时实验还表明共混组分中聚醚的分子量、分子结构、Ｐ（Ｓ－ＭＡＡ）中ＭＡＡ的含量以及共混组分的比例和体系的相容性有密切的关系．     

烯烃氢甲酰化催化剂活性物种的原位1H NMR研究

The rhodium-phosphine complex catalyst Rh(CO)(acac)(PPh3)(Ⅰ) for 1-hexene hydroformylation was studied under the following reaction conditions: CO/H2=1(mole rate), pressure 1.0 MPa, temperature 25-120℃, by using the pressurized in-situ 1H NMR technique. Experimental results indicated that the formation of a rhodium hydride complex from (Ⅰ) began at room temperature and its amount increased with increasing of reaction temperature. This intermediate complex began to decompose at 100℃ and disapeared completely at 120℃. The intensity change of the proton signal was parallel to catalytical activity in hydroformylation of olefins. Under pure CO pressure the proton signal of Ph-H bond was not observed. There was a 0.2 ppm difference in proton chemical shifts of Rh-H bond under pure H2 pressure and under H2+CO pressure. The results showed that the rhodium-hydride carbonyl complex is the active intermediate in the industrial hydroformylation process.     

羧甲基壳聚糖对胆红素的吸附性能研究

合成了不同取代度的羧甲基壳聚糖(CM-CTS)作为吸附剂，研究了不同条件对CM-CTS吸附胆红素性能的影响．结果表明：在实验条件下，随着羧甲基取代度的增加和体系温度的升高．最大吸附率和吸附速率均相应增加：在接近人体血液pH值的条件下，CM-CTS对胆红素的吸附性能较佳：人血清白蛋白和离子强度的增加对CM—CTS吸附胆红素有明显的抑制作用。     

Yb(C~6Me~6) (AlCl~4)~3·MeC~6H~5 的合成及其晶体结构

合成了一种新的芳烃络合物Yb(C~6Me~6)(AlCl~4)~3·MeC~6H~5 , 并确定了其晶体结构.     

Study of Tea Digitized Chromatographic Fingerprint Spectra Using Micellar Electrokinetic Chromatography

IntroductionTeaisthemostwidelyconsumedbeverageinpeople’slife .Theheightenedpopularityofthisbeveragethroughouttheworldinrecentyearsmaybedueinparttotheevidenceofarelationshipbetweenteaconsumptionandpreventionofcertainformsofhumandisease .Themaincomponentsofteaarepolyphenoliccompounds ,commonlyknownascatechins ,whichrepresentagroupofcom poundsbelongingtotheflavonoidfamily .Thesecom poundsarewidelydistributedinthetealeavesandconsti tuteupto 30 %ofthedryleafweight.1Muchinteresthasbeenfocusedoncat…     

SOLID STATE CHEMISTRY OF La_(1-x)Li_(x)MnO_3 AND RELATED COMPOUND

A series of perovskite type oxides La_(1-x)A_(x)MnO_3(x=0.1 for A=Li,Na,K;x=0.1～0.5 for A=Li)have been prepared by impregnation.Experimental results showed that the substitution of La~(3 ) by Li~ inLaMnO_(3 ?) greatly increased the selectivity to ethane and ethylene for theoxidative coupling of methane.Temperature-programmed desorption of oxygenproved the presence of oxygen vacancies in the oxide lattice.The higher Mn~(4 )/Mn_t ratio in oxide made the formation of oxygen vacancies easier on the oxidesurface.The general formula of the oxides is La_(1-x)Li_(x)Mn＇V＇_(y)O_(3-y),V=vacancy.     

Dense Sphene-type Solid Electrolyte Through Rapid Sintering for Solid-state Lithium Metal Battery

The sphene-type solid electrolyte with high ionic conductivity has been designed for solid-state lithium metal battery. However, the practical applications of solid electrolytes are still suffered by the low relative density and long sintering time of tens of hours with large energy consumption. Here, we introduced the spark plasma sintering technology for fabricating the sphene-type Li_1.125Ta_0.875Zr_0.125SiO₅ solid electrolyte. The dense electrolyte pellet with high relative density of ca. 97.4% and ionic conductivity of ca. 1.44×10^-5 S/cm at 30℃ can be obtained by spark plasma sintering process within the extremely short time of only ca. 0.1 h. Also the solid electrolyte provides stable electrochemical window of ca. 6.0 V(vs. Li⁺/Li) and high electrochemical interface stability toward Li metal anode. With the enhanced interfacial contacts between electrodes and electrolyte pellet by the in-situ formed polymer electrolyte, the solid-state lithium metal battery with LiFePO₄ cathode can deliver the initial discharge capacity of ca. 154 mA·h/g at 0.1 C and the reversible capacity of ca. 132 mA·h/g after 70 cycles with high Coulombic efficiency of 99.5% at 55℃. Therefore, this study demonstrates a rapid and energy efficient sintering strategy for fabricating the solid electrolyte with dense structure and high ionic conductivity that can be practically applied in solid-state lithium metal batteries with high energy densities and safeties.     

高负载率纳米Pt-Ru/C催化剂的制备和表征

以Vulcan XC-72R碳黑为载体, 通过在含十二烷基硫酸钠(SDS)的乙二醇溶液中直接还原氯铂酸和三氯化钌, 制备了负载率为60%的纳米PtRu/C催化剂. 透射电镜(TEM)和X射线衍射(XRD)分析结果表明, SDS的加入可显著改善PtRu纳米颗粒在载体表面分散性, 平均粒径达到2.7 nm. 电化学循环伏安法(CV)测试的结果显示, 利用这种方法制备的纳米PtRu/C催化剂对于甲醇氧化具有较强的抗中毒能力和较高的电催化活性.     

电化学合成镍配合物的研究

采用金属镍为“牺牲”阳极，首次在无隔膜电解槽中，电化学溶解金属镍一步 制备了纳米NiO前驱体Ni(Oet)2,Ni(Obu)2,Ni(Oet)2(acac)2，Ni(Obu)2(acac)2 [acac为乙酰丙酮基].产物通过红外光谱（FT-IR）、拉曼光谱（Raman spectrum） 进行表征。同时讨论了影响电合成镍醇盐及其配合物的关键因素。实验表明，防止 阳极钝化，温度控制在30-40℃，采用有机胺溴化物为导电盐，可以提高电合成效 率。