H-Y/β双微孔沸石分子筛催化果糖脱水生成5-羟甲基糠醛的研究

研究了以H-Y/β双微孔沸石分子筛为催化剂,果糖脱水转化为5-羟甲基糠醛(HMF)的反应,考察不同催化剂、溶剂、助剂用量、反应温度和反应时间,以确定H-Y/Beta双微孔沸石分子筛催化剂催化果糖脱水转化为HMF的最佳反应条件。研究发现,以1 g果糖为原料,最佳反应条件为:催化剂0.05 g、溶剂二甲基亚砜(DMSO)30 mL、助剂聚乙烯吡咯烷酮(PVP)0.03 g、反应温度160℃、反应时间1.5 h,利用紫外分光光度法测定产物,并计算其产率为64.6%。     

偏高岭土水热合成SAPO-5分子筛影响因素研究

以具有一定活性的偏高岭土兼作铝源与硅源、正磷酸作磷源、三乙胺作模板剂,水热法合成了SAPO-5分子筛。考察了晶化时间、三乙胺用量、HF的添加、体系中水含量等因素对产物晶相组成及结构的影响。利用X射线衍射分析（XRD）、红外光谱分析（FTIR）、扫描电镜（SEM）、X光电能谱（XPS）等手段对产物结构与组成进行了表征分析,研究结果表明原料最佳配比为MK：P2O5：2.5TEA：0.1HF：45H2O,在200℃下,晶化24h可获得结晶度较高、晶体形貌规整的SAPO-5分子筛。     

3-硝基-1,2,4-三唑-5-酮烷基咪唑离子液体的合成与表征

以N,N-二烷基咪唑(Cx-imi,x=3,4,5,6)为阳离子,3-硝基-1,2,4-三唑-5-酮(NTO)为阴离子合成了4种离子液体,利用元素分析、红外光谱和核磁共振表征其结构,并测定了其溶解性、密度、热性能和黏度。结果表明,NTO烷基咪唑离子液体在乙腈、N,N-二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)等介电常数较大的有机溶剂中溶解性较好,密度在1.897g/cm3以上,固相到液相的热转变温度在-34.4℃以下,5%的热失重在220℃左右,热稳定性较好。     

Fatty acid composition of some pine seed oils

The fatty acid composition of seeds from seven species of the genusPinus (P. pinaster, P. griffithii, P. pinea, P. koraiensis, P. sylvestris, P. mughus, andP. nigra) was established. Pine seeds are rich in oil (31–68% by weight) and contain several unusual polymethylene-interrupted unsaturated fatty acids with acis-5 ethylenic bond. These are thecis-5,cis-9 18:2,cis-5,cis-9,cis-12 18:3,cis-5,cis-11 20:2, andcis-5,cis-11,cis-14 20:3 acids, with a trace ofcis-5,cis-9,cis-12,cis-15 18:4 acid. Their percentage relative to total fatty acids varies from a low of 3.1% (P. pinea) to a high of 30.3% (P. sylvestris), depending on the species. The majorcis-5 double bond-containing acid is generally thecis-5,cis-9,cis-12 18:3 acid (pinolenic acid). In all species, linoleic acid represents approximately one-half the total fatty acids, whereas the content of oleic acid varies in the range 14–36% inversely to the sum of fatty acids containing acis-5 ethylenic bond. The easily available seeds fromP. koraiensis appear to be a good source of pinolenic acid: their oil content isca. 65%, and pinolenic represents about 15% of total fatty acids. These values appear to be rather constant.Pinus pinaster, which is grown on several thousand acres in the southwest of France, is an interesting source ofcis-5,cis-11,cis-14 20:3 acid (7% in the oil, which isca. 35% of the dehulled seed weight), an acid sharing in common three double bonds with arachidonic acid. Apparently,P. sylvestris seed oil contains the highest level ofcis-5 double bond-containing acids among pine seed oils that have ever been analyzed.     

Ni(Ⅱ)-5-Cl-PADAB-SDS体系条件实验

研究发现：在阴离子表面活性剂十二烷基硫酸钠（ＳＤＳ）存在下,以混酸－氢氧化钠缓冲液控制酸度,利用镍与４－（５－氯－２－吡啶偶氮）－１,３－二胺基苯（５－Ｃｌ－ＰＡＤＡＢ）生成紫红色络合物的吸收光谱,可直接光度法测镍。该体系稳定性好,摩尔吸光系数为１．２２×１０５Ｌ·ｍｏｌ－１·ｃｍ－１,镍量在０～１５μｇ·２５ｍＬ－１范围内符合比耳定律     

2-氨基-5-(对-甲氧基苯基)-1,3,4-噻二唑稀土金属有机配合物的合成及表征

２－氨基－５－（对－甲氧基苯基）－１,３,４－噻二唑（以ＬＨ表示）与等摩尔三茂基稀土化合物反应,合成了六种文献中未见报道的稀土金属有机配合物Ｃｐ２ＬｎＬ（Ｃｐ＝η５－Ｃ５Ｈ５;Ｌｎ＝Ｙｂ,Ｔｍ,Ｅｒ,Ｈｏ,Ｄｙ,Ｎｄ）。这些配合物均经元素分析、红外光谱及质谱表征。从有关的数据推测出这类化合物可能的分子结构。     

毒死蜱的合成研究

在特定的催化剂条件下,以３,５,６－三氯吡啶－２－醇钠为原料,合成毒死啤,确定了适宜的工艺条件,收率在９３％以上。     

Adsorption of hydrocarbons by ZSM-5 zeolites with different SiO2/Al2O3 ratios: a combined FTIR and gravimetric study

In metal-free ZSM-5, the decrease in the concentration of Bronsted and Lewis acid sites parallels the increase in the SiO₂/Al₂O₃ ratio. In the presence of residual moisture, the adsorption of small alkanes does not markedly depend on the SiO₂/Al₂O₃ ratio in the range from 30 to 150. The acidity is more important for the adsorption of alkenes (propene) which oligomerize following adsorption. The addition of 5 wt.% of La does not significantly affect the strength of the surface acid sites but does decrease their concentration. It causes a transformation, in a part, of the Bronsted acid sites. These new centers could perhaps be assigned to LaO(OH) or La(OH)₂⁺ species which may be formed on the surface in La-containing ZSM-5. La could exchange only the strongest acidic sites without inducing large changes in their total concentration. La addition has a very small effect on the adsorption of small hydrocarbons. The exchange of the protons by Cu²⁺ decreases the concentration of Bronsted acid sites. At a sufficient loading of the ZSM-5 by Cu²⁺, i.e. at an atomic ratio Cu/Al > 1.0, the exchange can almost totally suppress the Bronsted acidity. Another effect of the ion exchange is the suppression of the adsorption capacity of small hydrocarbons due to lowered surface area and internal pore volume. The lowered available internal pore volume also limits the extent of the oligomerization of propene.     

An in situ infrared study of NO reduction by C3H8 over Fe‐ZSM‐5

The interactions of NO, O₂ and NO₂ with Fe‐ZSM‐5, as well as the reduction of NO by C₃H₈ in the presence of O₂, have been investigated using in situ infrared spectroscopy. The sample of Fe‐ZSM‐5 (Fe/Al =0.56) was prepared by solid‐state ion exchange. NO adsorption in the absence of O₂ produces only mono‐ and dinitrosyl species associated with Fe²⁺ cations. Adsorbed NO₂/NO₃ species are formed via the reaction of adsorbed O₂ with gas‐phase NO or by the adsorption of gas‐phase NO₂. The reduction of NO in the presence of O₂ begins with the reaction of gas‐phase C₃H₈ with adsorbed NO₂/NO₃ species to form a nitrogen‐containing polymeric species. A reaction pathway is proposed for the catalyzed reduction of NO by C₃H₈ in the presence of O₂. This revised version was published online in July 2006 with corrections to the Cover Date.     

热处理对离子束溅射Ta_2O_5薄膜特性的影响

利用离子束溅射沉积技术制备了Ta2O5薄膜,在100~600℃的大气氛围中对其进行热处理(步进温度为100℃),并对热处理后样品的光学常数(折射率、折射率非均匀性、消光系数和物理厚度)、应力、晶向和表面形貌进行了研究。研究显示,随着热处理温度增加,薄膜折射率整体呈下降趋势,折射率非均匀性和物理厚度呈增加趋势,结果有效地改善了薄膜的消光系数和应力,但薄膜的晶向和表面形貌均未出现明显的变化。结果表明:热处理可以有效改变薄膜特性,但需要根据Ta2O5薄膜具体应用综合选择最优的热处理温度。本文对离子束溅射Ta2O5薄膜的热处理参数选择具有指导意义。