金属蒸气合成制备有机硅化合物包裹的金属微粒催化剂

用金属蒸气合成法制备了三种有机硅包裹的金属催化剂Ni/D_4,Ni-Mn/D_4,Ni-Mn-La/D_4。用XRD,TEM,XPS,FMR,静磁对它们进行了性质表征。催化剂中金属粒子小于3.5 nm。XPS结果表明催化剂中金属以零价和氧化态多种形式存在,金属被有机硅包裹着,阻止了内层金属被氧化,FMR和静磁结果表明金属微粒呈球形,具有超顺磁性。在催化糠醛合成糠醇加氢反应中,Ni-Mn-La/D_4活性最高。     

不同方法掺杂Au对纳米α-Fe2O3气敏性能的影响

分别采用共沉淀法、浸渍法、紫外辐照法制备了掺杂不同Au含量的α-Fe2O3纳米粉体,并制作了旁热式厚膜型气敏元件.用XRD、TG-DTA和TEM技术对纳米晶的晶型、晶粒大小及形貌进行了表征.考察了掺杂方法、Au含量及焙烧温度对α-Fe2O3气敏性能的影响.结果表明,采用三种方法掺杂适量Au后,都使α-Fe2O3的气敏性有了显著提高,其中采用共沉淀法,在400℃焙烧的Au质量分数为1.5%的α-Fe2O3的气敏性最佳.     

溶剂化金属原子浸渍法制备的Ni-Ag/γ-Al2O3催化剂的结构表征

应用溶剂化金属原子浸渍法和普通浸渍法制备了三种不同摩尔比的γ－Ａｌ２Ｏ３负载Ｎｉ－Ａｇ双金属催化剂。ＸＲＤ和磁测定结果表明ＳＭＡＩ催化剂中Ｎｉ和Ａｇ的粒度均小于金属相同的ＣＩ催化剂。ＳＭＡＩ催化剂中Ｎｉ和Ａｇ未形成合金，而ＣＩ催化剂中Ｎｉ和Ａｇ形成了合金。     

PROPERTIES OF POLYMER SUPPORTED Ni-Cu BIMETALLIC CATALYSTS PREPARED BY SOLVATED METAL ATOM IMPREGNATION

D-72 resin supported nickel-copper catalysts prepared by solvated metal atom impreg-nation (SMAI) were studied by magnetic measurements and X-ray photoelectron spectro-scopy (XPS). The Ni particles on the catalysts are very highly dispersed and displaysuperparamagnetic behaviour. Ni-Cu alloy clusters were found to be formed. The sur-face compositions are different from the bulk concentrations. In contrast with the surfaceenrichment in copper generally observed on conventional Ni-Cu catalysts, the surfaces ofthese catalysts are enriched in nickel. The nickel is in both zero and valent states, whilecopper is mainly in metallic state. Catalytic data show that the formation of Ni-Cu alloyclusters has a profound effect on the catalytic activities of the catalysts in the hydrogena-tion of furfural. The activity of the Ni:Cu ratio of one bimetallic catalysts is much higherthan that of the Ni or Cu monometallic catalyst.     

金属蒸气合成在金属有机合成中的应用

本文简要地介绍了金属蒸气合成法的基本原理、仪器和实验技术, 并按金属原子分别与炔、单烯、多烯、环烯、芳烃体系、卤代烃、有机混和物的反应及有机金属硼化合物的合成, 对金属蒸气合成法在金属有机合成中的应用进行了讨论。     

SMAI法制备的Cu催化剂的CO加氢催化

用溶剂化金属原子浸渍（SMAI）法制备了SiO2、Cr2O3负载Cu催化剂.XPS测定表明三种载体上的Cu几乎全部以零价态存在．X射线增宽法测定表明随着Cu含量增加Cu颗粒增大．Cu催化剂在CO加氢中的催化活性与载体、Cu颗粒大小和Cu价态有关．Cr2O3对Cu催化活性有促进效应．Cr2O3负载Cu催化剂活性随Cu颗粒减小而增大，而SiO2作载体时，颗粒大小对活性无影响，零价Cu0为催化活性中心     

Cu－Zn／γ－Al2O3催化剂的制备及其在选择加氢反应中的催化性能

 通过浸渍法制备了不同Cu／Zn比的γ－Al2O3和改性γ－Al2O3负载的Cu－Zn催化剂，并用XRD，XPS和SEM等手段对催化剂进行了表征．XRD表征结果表明，还原活化前催化剂中的Cu和Zn分别以CuO和ZnO的形式存在；还原活化后Cu以单质的形式存在；催化剂失活后，单质Cu又转变成CuO．XPS和SEM分析结果表明，催化剂中金属的价态及颗粒的形貌在反应前后发生了变化．所制备的催化剂在糠醛加氢制糠醇反应中表现出较高的选择性．用Co改性的γ－Al2O3负载的Cu－Zn催化剂不仅具有较高的催化活性和选择性，而且还呈现出较长的寿命．催化剂中的Cu晶相是催化活性中心；催化剂中的Cu晶相转变成CuO和烧结是催化剂失活 的主要原因．     

应用新型立式逆流色谱制备分离南蛇藤中的南蛇藤素

A versatile countercurrent chromatography with upright multilayer coil planet centrifuge, named upright countercurrent chromatography (UCCC), was applied to the isolation and purification of celastrol from the roots of Celastrus orbiculatus Thunb. The crude celastrol was obtained by elution with petroleum ether from ethanol extracts using a 15 cm length and 5 cm I.D. of silica gel flash chromatography. Preparative UCCC (Fig. 1) with a two-phase system composed of petroleum ether (b. p. 60 ～ 90 ℃ )-ethyl acetate-tetrachloromethanemethanol-water ( 1:1:8:6: 1, v/v) was successfully performed, yielding 705 mg celastrol at 99.5 % purity from 1020 rng of the crude extract in one step separation.