离子液体/H_2O_2体系脱硫实验研究

选取四种不同种类离子液体(ILs),1-丁基-3-甲基咪唑溴化物([Bmim]Br)、1-丁基-3-甲基咪唑四氟硼酸盐([Bmim]BF_4)、1-丁基-3-甲基咪唑硫酸氢盐([Bmim]HSO_4)、1-丁基-3-甲基咪唑磷酸二氢盐([Bmim]H_2PO_4)与30%H_2O_2溶液在温和条件下对两种高硫脱灰煤样(LS、QX)进行脱硫实验研究。用化学法测定脱硫前后煤样形态硫含量,并利用傅里叶变换红外光谱(FT-IR)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)及热重(TG)对脱硫前后的煤样进行表征。结果表明,离子液体的加入使H_2O_2氧化脱硫能力增强,煤中硫铁矿硫和有机硫化物硫被显著脱除;经ILs/H_2O_2体系作用后的煤样中小粒径的颗粒减少,颗粒间的缝隙增大,煤表面的凹坑明显,热重实验结果表明,ILs/H_2O_2体系作用后的煤样相对于原煤热失重增大,部分挥发性物质释放峰温提前。     

不同代硝基芳基苄醚树枝配体轴向取代硅(Ⅳ)酞菁光物理性质的比较

在二氯硅酞菁轴向位置引入硝基芳基苄醚树枝配体是一种减少酞菁配合物聚集体形成,提高其光动力活性的有效方法。本文采用UV/Vis、稳态和瞬态荧光光谱法比较了1-3代硝基芳基苄醚树枝配体轴向取代硅(Ⅳ)酞菁的光物理性质。研究结果表明,随着轴向树枝配体代数的增加,Q带最大吸收峰强度增大,酞菁核荧光强度增强,荧光量子产率降低,荧光寿命增长。研究结果将为开发轴向取代硅(Ⅳ)酞菁配合物作为新型光敏剂提供重要的理论依据。     

SPECTRAL CHARACTERISTICS OF FREE AND LINKED PYRENE-TYPE CHROMOPHORES IN SOLUTION,POLYMER MATRICES,AND INTERPENETRATING NETWORKS

Monomers, 1-pyrenylmethyl methacrylate (PyMMA), 1-pyrenylbutyl methacrylate (PyBMA), 4-(1-pyrenyl)methoxymethyl styrene (PyMMS) and allyl-(1-pyrenylmehtyl) ether (PyMAE), with pyrene as chromophore, were prepared. Their spectral properties (absorption, emission and emission decay) in solution, and doped or bonded in polymer matrices and complex polymer systems as interpenetrating polymer networks (IPN), were investigated. Spectral properties of pyrene-containing monomers doped in polystyrene (PS), polymethylmethacrylate (PMMA), polyvinylchloride (PVC), polyethylene (PE) and grafted on PE as well as copolymerized in buthylmethacrylate-co-styrene copolymer (BMA-co-S) have been compared. Absorption and emission spectra of pyrene type probes in solution and in IPN matrices exhibit typical absorption of the pyrene moiety. For IPN with grafted probes on PE, the absorption is slightly shifted to red wavelength. For monomers, PyMMA, PyBMA and PyMAE grafted to PE, the shape of the emission spectrum depends on the wavelength of excitation. The ratio of intensity of the vibrational band, I₁/I₃, (I₁ peak at 377 nm and I₃ peak at 388 nm) has been a quite useful indicator of polarity of IPN. The relative quantum yields of fluorescence in IPN matrices are lower in comparison to polymer matrices of PE, PS, PMMA for all probes under study. The fluorescence life-times for bound and free probes have been in the range 100–200 ns, which is substiantialy shorter than for the parent pyrene chromophore under the same or similar condition. Grafted probes on PE alone, or as a part of IPN, exhibit substantially shorter life-time around 10 ns and decay is rather complex.     

超临界流体萃取仪器的研制

本文报道了以国产原配件为基础，成功地研制了分析规模的超临界流体萃取仪器、并对仪器性能进行了全面考察，仪器性能稳定，重现性良好（ＲＳＤ＜３．１％），定量线性关系可靠，可满足定量萃取的要求。     

Influence of the position of the nitro group on the structural and spectroscopic characteristics of N"-(nitrobenzylidene)isonicotinic hydrazides in the crystalline state

N"-Substituted isonicotinic hydrazides of the general formula Py—C(=O)—N(H)-N"=C(H)—R, where R is o- (1), m- (2), or p-nitrophenyl (3), were studied by IR spectroscopy and X-ray diffraction analysis. The position of the nitro group in these compounds has no effect on the type of the crystal structure. The crystal packings are based on stacks consisting of antiparallel planar molecules. The molecules from the adjacent stacks are linked to each other via the N—H...N_Py hydrogen bonds. Depending on the position of the nitro group, the N...N_Py distance increases in the series 3 > 1 > 2 and the energy of the hydrogen bonds decreases (according to the IR spectroscopic data) from 3.9 to 3.1 kcal mol^–1. Analysis of the IR spectra demonstrated that the intensity of absorption in the (C—H) stretching region of the pyridine ring increases substantially as the the N—H...N_Py hydrogen bond is strengthened. Some regularities of the changes, which are observed for the (NO₂) bands in the spectra of the nitrophenyl-containing conjugated molecules in solutions, persist in the crystalline state.     

Synthesis of New Fluorinated Derivatives of Quinolinecarboxylic Acids

Ethyl esters of 1-(7-Z-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carbamoyl)-5-X-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acids (X = H, F; Z = pyrrolidino-, piperidino-, hexamethylenimino-, morpholino-, thiomorpholino-) have been synthesized by the interaction of quinolone-3-carboxylic acid hydrazides with ethyl esters of 3-ethoxy-2-(polyfluorobenzoyl)acrylic acid . It was shown possible to cyclize intramolecularly the esters obtained with the formation of 1,3,4-oxadiazino[6,5,4-i,j]quinoline derivatives.     

舒兰褐煤树脂组分中某些分离物的化学研究

我国褐煤资源丰富 ,分布于云南、吉林、黑龙江、山东和内蒙古等地。褐煤除作燃料和腐植肥料外 ,还应用于轻化工和机械工业 ,如从褐煤制取褐煤蜡。褐煤蜡中含有较多的树脂物质 ,影响了褐煤蜡的质量 ,因此通常褐煤蜡树脂作为废弃物脱除 ,以提高褐煤蜡的质量。褐煤蜡的化学组成为纯蜡和树脂 ,前者为高碳脂肪酸和脂肪醇的酯类、游离脂肪酸和脂肪醇 ,以及烃类物等 ;后者则以萜类为主 ,并含有甾醇、羟基酸和烃化合物[1～ 5] 。 1982年唐运千等采用红外光谱和氢核磁共振谱检定 ,褐煤树脂中含有 β 谷甾醇 ;柱层析和薄层层析检出雌二醇和雌酚酮[2 ] …     

稀土元素在中草药中的应用及其前景

本文介绍了稀土元素在中草药中的应用及其前景，探讨了稀土元素对中草药药效的影响，引用文献39篇。     

腐植酸型煤气化特性及动力学研究

以低活性福建无烟粉煤为原料,采用腐植酸型煤黏结剂,制得腐植酸型煤。比较研究型煤和无烟煤在常压条件下的气化动力学和气化特性。运用等温热重法,在900~1 150℃进行水蒸气气化实验,测定了型煤和无烟煤的反应速率、转化率与时间的关系,考察了常压下温度和煤样对气化反应的影响。采用积分缩核模型对实验数据进行拟合关联,得到煤样水蒸气气化反应的动力学参数。结果表明,型煤的气化反应活化能(102.0 kJ/mol)低于福建无烟煤(122.5 kJ/mol)。950℃下型煤的化学反应性(80.0%)优于福建无烟煤(33.0%)。型煤较福建无烟煤表现出更好的化学反应性,可代替优质块煤用于工业固定床煤气化。