乙酰化淀粉/DL-丙交酯接枝共聚物的合成及降解性能研究

用醋酸乙烯酯和玉米淀粉反应制备出了不同取代度乙酰化淀粉，再用乙酰化淀粉同DL－丙交酯接枝共聚合成乙酰化淀粉／DL－丙交酯接枝共聚物。研究了原料配比，淀粉取代度对接枝反应单体转化率（C％），接枝率（G％）接枝效率（GE％）和接枝支链数均分子量（Mn)的影响，结果表明在给定的试验条件下接枝共聚反应的C％，G％，GE％和Mn可分别达到40％，225％，80％和1．4万。接枝共聚物在磷酸缓冲溶液和户外土壤掩埋降解实验表明，在160天内样品失重率分别为71％和60％，表明合成的乙酰化淀粉／DL－丙交酯接枝共聚物具有很好的降解性能。     

鹿角短指软珊瑚Sinularia Cervicornis Tix-Dur 中的一个新糖甙-Cervicoside

珊瑚属腔肠动物门 ( Clelenterata) ,海鸡冠目 ( Alcyonacea) ,是一种热带与亚热带海洋中广泛分布Scheme 1　 Structure of cervicoside(1 )的低等海洋生物 .软珊瑚的次生代谢物中含有萜类和甾体类等各类生理活性物质[1～ 5] .我们在对鹿角短指软珊瑚的次生代谢产物研究中 ,分离到一个新三糖甙 ,命名为 Cervicoside( 1 ) ,结构见 Scheme 1 .该化合物具有较强的体外抗癌活性 .1　实验部分1 .1　样品　鹿角短指软珊瑚采自海南岛三亚海域 .样品储藏于中山大学化学与化学工程学院天然有机化学研究室 ,编号为 98- SY- 3.种属由中国科学院南海…     

V-Ag-Ni系氧化物的表面氧性质与甲苯选择性氧化的催化性能

制备了一系列Ｖ，Ａｇ，Ｎｉ原子比不同的三元氧化物，应用ＴＰＤ－ＭＳ技术研究了样品表面氧的性质，并测定了甲苯选择性氧化生成苯甲醛的催化活性。实验结果表明，样品表面存在有多种吸附的氧物种。在脱附温度＜９００℃：当Ｎｉ含量对Ａｇ（或Ｖ）的原子比为０．２５或０．５０时，仅在低温处出现有表面的Ｏ＾－和Ｏ＾２＾－两种氧物种的脱附峰；当Ｎｉ含量对Ａｇ（或Ｖ）的原子比增高到＞０．７５时，除有表面的Ｏ＾－和Ｏ＾２＾     

希夫碱配合物的研究——Ⅵ.K[Fe(acaccn)(CN)2]·2H2O的合成及晶体结构

制备了K[Fe(acaccn)(CN)₂]·2H₂O.并测定了晶体结构.     

Effect of solvent composition on dispersing ability of reaction sialon suspensions

This work focuses on the optimization of the rheological behavior of suspensions considering different solvent compositions. The effects of methyl ethyl ketone (MEK)/ethanol (E) solvent mixtures on reaction sialon suspensions were investigated by measuring sedimentation behavior, adsorption of dispersant, and flow behavior. It was shown that both the flow behavior and the sedimentation behavior strongly depended on selection of solvent composition. Using 3 wt% KD1 as dispersant, well-dispersed colloidal suspensions could be obtained in MEK-rich solvents. The suspensions with 60 vol% MEK/40 vol% E as solvent could be fitted to the Bingham model with very low yield stress, while suspensions with pure MEK or ethanol-rich mixtures as solvent showed pseudo plastic behavior with relatively high yield stress values. A model was proposed to explain the different flow behaviors of suspensions considering the different configurations of dispersant at particles' surfaces.     

氮化铁催化剂的制备及其苯胺催化加氢性能

用α－Ｆｅ２Ｏ３与氨气程序升温还原方法制备出不同温度氮气的氮化铁系列催化剂。通过ＸＲＤ测试对氮化过程中的晶相转变进行了分析。在中压反应装置上考察了氮化铁系列催化剂上苯胺加氢活性以及反应条件对苯胺加氢反应活性的影响。结果表明，在７００℃氮化制香的氮化铁催化剂显示有较高的苯胺加氢活性，在氢压为３．０ＭＰａ，温度为２５０℃，ｎ（Ｈ２）／ｎ（ｏｉｌ）＝１８，液体空速（ＷＨＳＶ）为０．３ｈ＾－１时，该催化剂     

GC-MS法测定焦化厂气溶胶中多环芳烃

利用气相色谱-质谱(GC-MS),电子轰击离子化(EI)法测定焦化厂气溶胶中多环芳烃的含量。超声波抽提气溶胶样品,用GC-MS的选择离子监测(SIM)方式测定EPA提出的优先监测的16种多环芳烃的含量。该法的检出限为0.167pg·m~(-3),PAHs的回收率为85.1％～110.5％,相对标准偏差为4.62％～19.4％。应用该法测定气溶胶中PAHs获得满意的结果。     

Studies on solid state reactions of coordination compounds. LXIII. Solid state synthesis of a series of tetranuclear Mo(W)—Ag mixed-metal clusters. Crystal structures of [(n-Bu)4N]3[MoOS3Ag3Br4] and [(n-Bu)4N]3[WS4Ag3Cl4]

A series of tetranuclear Mo(W)-Ag mixed-metal clusters have been synthesized by making use of the solid state reactions of [NH₄]₂[MYS₃](M= Mo, W; Y= O, S), AgX(X= Cl, Br, I) and (n-Bu)₄NX' (X' =Cl, Br), two of which [(n-Bu)₄N]₃[MoOS₃Ag₃Br₄] (1) and [(n-Bu)₄N]₃[WS₄Ag₃Cl₄] ( 2 ) have been structurally characterized by X-ray analysis. The crystal data: 1 , cubic, P4 3m, αequals;12.093(4) Å, Z=1, R =0.076; 2 , cubic, P4 3m, αequals;12.059(2) Å, Z =1, R =0.075. The cluster anion core [Ag₃MS₃X'] of the two compounds can be viewed as a cube in which the four metal atoms and the four non-metal atoms are statistically distributed, respectively. Substitution reaction with PPh₃ ligand is also discussed for this type of tetranuclear clusters.     

Temperature-programmed desorption and adsorption of hydrogen on Mo2N

Hydrogen adsorption-desorption over Mo₂N has been studied using a temperature-programmed technique. It is revealed that hydrogen on Mo₂N exhibits very high mobility leading to migration of the surface hydrogen into the sublayer and bulk of the sample or the reverse. The surface hydrogen species are preferentially formed when adsorption is carried out below 573 K. On increasing the adsorption temperature to above 573 K, the quantity of hydrogen species located in the sublayer or/and bulk of the Mo₂N sample increases significantly.     

Solid state synthesis and structure of two novel polyoxometalates [(n-Bu)4N]4[M6O19][Ag2I4](M?Mo,W)†

The reaction of [NH₄]₂[MO₂S₂], AgI and (n-Bu)₄NBr in solid state produced the polyoxometalates [(n-Bu)₄N]₄[M₆O₁₉][Ag₂I₄] (1, M? Mo; 2, M? W) which were structurally determined. The crystals of 1 and 2 are isomorphous, monoclinic, space group P2₁/c. 1, a = l.6624(2), b=1.6699(3), c=l.7217(2) nm, β=98.29(1)°, V=4.729(1) nm³, Z=2, R=0.040, R_w“0.037; 2, a = 1.6636(3), b = 1.6733(3), c = 1.7190(3) nm, β=98.25(1)°, V=4.736(l) nm³, Z = 2, R = 0.038, R_w = 0.047. The results of the structure determination showed that the two compounds had the same structures whose skeletons are composed of [Ag₂I₄]². and [M₆O₁₉]^2-. The difference of them and heteropolymetalate compounds synthesized in solution is that the title compounds contain cluster. ion, heteropolymetalate and organic cations, while the latter is only composed of heteropolymetalate and organic cations.