煤气化过程中生成氮化物的研究

对煤中N在气化条件下的转化进行了研究，详细考察了在CO2和水蒸气气氛中转化生成HCN和NH3的过程，并对热解和气化条件下煤中N转化规律的差别进行了讨论。实验结果表明：在气化条件下煤中N转化为HCN和NH3的量随温度的升高而增大，在水蒸气气氛下HCN和NH3的生成量明显大于热解条件的实验结果。在本实验条件下半焦中N含量的15％－20％可以转化为NH3，水蒸汽气氛条件下NH3生成量的提高主要来源于半焦的气化反应过程。     

A New Technique of Synthesizing 10—Hydroxy—5—methyl—5,10—dihydrophenophosphazine 10—Oxide

10-Hydroxy-5-methyl-5,10-dihydrophenophosphazine 10-oxide(1)was prepared by a new technique of treating 10-methoxy-5,10-dihydrophenophosphazine 10-oxide(2)with an equivalent of NaH in anhydrous DMF,and then at 120℃ for 3-4h,which not only avoided poisonous and expensive methyl iodide used in literature,but made the consumption of NaH greatly decrease as well.The possible reaction mechanism was also described.The chemical structure of 1 was confiremed by IR,NMR,and mass spectroscopy.     

绝热法研究己内酰胺阴离子聚合尼龙动力学

采用己内酰胺钠盐、N-75缩二脲作为反应催化体系, 确定反应温度在145-160 ℃之间, 通过计算得到动力学参数: 反应级数为准一级、活化能在73.2-77.1 kJ·mol-1之间、指前因子在2.9×1011-3.6×1011 mol1-n·s-1范围内. 本实验条件下测定并计算的反应热为134.5-137.3 J·g-1, 与文献值(138.6 J·g-1)吻合. 并在前人基础上修正并建构了己内酰胺阴离子绝热反应动力学模型, 对反应过程的模拟结果与实验数据基本吻合, 从而证明了本模型的正确合理.     

Investigation of Aconitine-type Alkaloids from Processed Tuber of Aconitum carmiechaeli by HPLC-ESI-MS/MS~n

Introduction Aconitine-type alkaloids isolated from the roots of Aconitum carmiechaeli show a potential toxicity and a broad spectrum of bioactivity[1-4].On the basis of the C8-substituent of C19-diterpenoid skeleton,aconitine-type alkaloids can be divided into diester-diterpenoid alkaloids(DDAs),monoester-diterpenoid alkaloids(MDAs),and lipo-alkaloids(Fig.1).     

Synthesis and Characterization of Dual Acidic Ionic Liquids

Novel ionic liquids with dual acidity, of which the cation contains Brφnsted acidity and anions contain Lewis acidity were synthesized. These ionic liquids obtained were identified by NMR, FF-IR, SDT and FAB-MS. Their acidities were determined by pyridine probe on IR spectrography.     

Triterpenoid Saponins from Schefflera arboricola

Four new triterpenoid saponins, named scheffarboside A – D ( 1 – 4 ), along with five known saponins were isolated from the stems of Schefflera arboricola. The structures of the four new saponins were determined as 3‐O‐(O‐β‐glucuronopyranosyl‐(1 → 3)‐O‐α‐rhamnopyranosyl‐(1 → 2)‐α‐arabinopyranosyl)oleanolic acid ( 1 ), 3‐O‐(O‐α‐arabinopyranosyl‐(1 → 4)‐O‐α‐arabinopyranosyl‐(1 → 3)‐O‐α‐rhamnopyranosyl‐(1 → 2)‐α‐arabinopyranosyl)oleanolic acid ( 2 ), 3‐O‐(O‐α‐arabinopyranosyl‐(1 → 4)‐O‐α‐arabinopyranosyl‐(1 → 3)‐O‐α‐rhamnopyranosyl‐(1 → 2)‐α‐arabinopyranosyl)hederagenin ( 3 ), 3‐O‐(O‐α‐arabinopyranosyl‐(1 → 4)‐O‐α‐arabinopyranosyl‐(1 → 3)‐O‐α‐rhamnopyranosyl‐(1 → 2)‐α‐arabinopyranosyl)oleanolic acid O‐α‐rhamnopyranosyl‐(1 → 4)‐O‐β‐glucopyranosyl‐(1 → 6)‐β‐glucopyranosylester ( 4 ), respectively, on the basis of spectroscopic and chemical degradation methods.     

铱(III)离子催化铈(IV)离子氧化四氢糠醇的动力学及机理

在酸性介质中用氧化还原滴定法研究了铈(IV)离子在痕量铱(III)离子催化作用下，于298~313 K区间氧化四氢糠醇(THFA)的反应动力学. 结果表明，反应对铈(IV)离子为一级，对铱(III)离子也为一级，对四氢糠醇的表观反应级数为正分数. 准一级速率常数kobs随[H+]增加而增大，而随[HSO₄－]增加而减小. 在氮气保护下，反应能引发丙烯腈聚合，说明在反应中有自由基产生. 通过kobs与[HSO₄－]的依赖关系，找到本反应体系的动力学活性物种是Ce(SO₄)₂，并计算出平衡常数，速控步骤的速率常数及相应的活化参数.     

1,2-萘醌-4-磺酸钠为显色剂吸光度差值法测定盐酸普鲁卡因

1,2-萘醌-4-磺酸钠与盐酸普鲁卡因在pH 4.70的条件下反应,产物在300和483 nm处有两个吸收峰,可用两波长下吸光度差值测定盐酸普鲁卡因,本文对吸光度差值与分析物浓度之间的关系作了理论推导。吸光度差值(ΔA)与盐酸普鲁卡因质量浓度在2.0~36.0 mg/L范围内具有良好线性关系,线性回归方程为:ρ=37.092 0ΔA-0.332 3,线性相关系数为0.999 1,相对标准偏差为1.49%,回收率为97%~105%。试验了pH值、放置时间及干扰离子对测定的影响。此法简便、快速、准确,可用于注射液中盐酸普鲁卡因含量的测定,与药典方法对照,结果满意。     

A novel fluorescent method for determination of peroxynitrite using folic acid as a probe

A novel method for the determination of peroxynitrite using folic acid as a fluorescent probe is described. The method is based on the oxidation of the reduced, low-fluorescent folic acid by peroxynitrite to produce a high-fluorescent emission product. The fluorescence increase is linearly related to the concentration of peroxynitrite in the range of 3 × 10⁻⁸ to 5.0 × 10⁻⁶ mol L⁻¹ with a correlation coefficient of 0.998, and the detection limit is 1 × 10⁻⁸ mol L⁻¹. Interferences from some metal ions normally seen in biological samples, and also some anions structurally similar to peroxynitrite were studied. The optimal conditions for the detection of peroxynitrite were evaluated.     

A strategy for synthesis of polymer-protective bimetallic colloids

A strategy for the synthesis of polymer-protective bimetallic sols is proposed which has the advantage of the strong protective effect of the polymer agent on one of the composites to stabilize the bimetallic colloidal particles. This strategy is certified to be useful to the predication of the formation of stable bimetallic colloids protected by polymer and to the control of the particle size to a certain extent. A series of new PVP-protective bimetallic colloidal dispersions containing noble metal element (Pt, Rh, Pd), light transition metal element (Co, Fe), and boron are obtained from the corresponding salts by the methods of reduction by stage and coreduction, using the NaBH4 as reductant. The TEM, XRD and EPMA measurements indicate the formation of bimetallic colloids. An interesting kind of coil aggregation is observed in the systems of PVP-Pt-Co and PVP-Rh-Co prepared by the method of reduction by stage.