一步法制二甲醚工艺及催化剂的研究

本文采用共沉淀沉积法制备了一步法合成二甲醚的双功能催化剂，并在固定床高压流动反应装置上对其催化性能进行研究，考察了MnO2助剂对Cu—ZnO—ZrO2／HZSM—5催化剂性能的影响以及工艺条件对二甲醚合成的影响。采用TPR、XRD等测试方法对催化剂进行了表征，结果证明：MnO2助剂的加入，能够增加活性中心数量，提高催化剂的活性。     

乙醇和二甲醚微射流火焰燃烧特性研究

采用实验及数值计算研究了乙醇和二甲醚微圆管射流火焰燃烧特性。通过实验观察到不同燃料流速下乙醇和二甲醚火焰都具有四种典型的火焰形态；使用平面激光诱导荧光测试系统获得了微射流火焰的OH基元分布，实验结果表明在较高流速下稳定燃烧的乙醇火焰比二甲醚火焰直径小，且略高于二甲醚火焰；采用考虑详细化学反应机理的数值计算对乙醇和二甲醚火焰进行了数值模拟，计算结果与实验现象吻合较好；利用一维非预混对冲火焰计算进一步研究了这两种燃料的化学反应路径，分析结果表明乙醇和二甲醚火焰的中间产物有显著差异，两种燃料化学反应特性的差异导致了不同的微火焰结构。     

室温离子液体1-烷基-3-甲基咪唑硫酸甲酯的合成及电导率研究

利用硫酸二甲酯分别与N-甲基及N-丁基咪唑在室温下反应,一步合成了离子液体1-甲基-3-甲基咪唑硫酸甲酯和1-丁基-3-甲基咪唑硫酸甲酯,测定了在不同温度下离子液体的电导率.结果表明:随着温度的升高,离子液体的电导率迅速增加;同时电导率与温度的变化关系符合多项式方程和Vogel-Tammann-Fulcher(VTF)方程.     

Synthesis of poly(vinyl propionate) from poly(vinyl alcohol) in nonaqueous medium using ethyl nitrate dimethyl sulfoxide as a catalyst

Poly(vinyl alcohol) (PVA) can be dissolved in a nonaqueous medium in the presence of catalytic concentration of ethyl nitrate dimethyl sulfoxide, C₂H₅ONO₂·DMSO. From the PVA solution, poly(vinyl propionate), PVPR was prepared by the homogeneous esterification of PVA with propionic acid. The ester thus formed contained some unconverted hydroxyl group. The formation of the ester was confirmed by the IR and ¹H‐NMR spectra. The molecular weight of the ester was determined by GPC and intrinsic viscosity (η) was determined by viscometric method. Glass transition temperature, T_g, was obtained from differential scanning calorimetric (DSC) analysis. Thermal stabilities of the ester were checked by thermogravimetric analysis (TGA) and differential thermogravimetric (DTG) analysis. The efficiency of the ester as a flow improver of crude oil was also examined. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5675–5679, 2006     

Comments on the use of buckminsterfullerene encapsulated in zeolite Y as a potential catalyst

Buckminsterfullerene encapsulated within zeolite Y is found not to be a reactive radical initiator for the formation of dimethoxyethane from dimethyl ether below 200° C. Above this temperature the expected acid catalysed conversion of dimethyl ether to hydrocarbons is observed. Dimethoxyethane formation is observed when bibenzoyl peroxide is used as a radical initiator. These studies indicate that any radical formed by the encapsulated buckminsterfullerene is relatively unreactive.     

对叔丁基苄胺的合成研究

摘要选择Delepine反应法的路线合成对叔丁基苄胺，并对反应投料比、反应温度及酸化后的反应时间进行了优化试验，得到了较好的反应条件：反应温度为40℃，对叔丁基苄氯与乌洛托品投料比为1：1；加入酸和醇后的保温时间为2h，从而使反应收率稳定在90％以上，含量达到95％。     

Dy_2O_3掺杂对钛酸锶钡陶瓷结构性能的影响

采用草酸盐沉淀法,以硝酸锶、硝酸钡、钛酸丁酯和草酸为原料,Dy2O3为掺杂剂,制得了Ba0.6Sr0.4TiO3粉体,并于1250℃将其烧结成Ba0.6Sr0.4TiO3系电介质陶瓷。利用扫描电镜、X射线衍射及TH2818自动元件分析仪对Dy2O3掺杂量为0.2%~2%的Ba0.6Sr0.4TiO3陶瓷的微观结构和介电性能进行研究。结果表明,Dy2O3的掺杂没有影响到BST陶瓷的主晶相钙钛矿结构,且一定量的Dy3+进入到BST晶格中。BST陶瓷的介电损耗随着掺杂量的增加而逐渐减小,介电常数随着掺杂量的增加呈现先增大后减小的趋势,当掺杂量为0.5%时,介电常数最大,为4 474.48。     

氧化胺型清洁压裂液的制备及室内评价

以油酸酰胺丙基二甲基叔胺、过氧化氢为原料制备出油酸酰胺丙基二甲基氧化叔胺(OADO)稠化剂.研究了冰乙酸、氯化铵添加量对OADO稠化性能的影响,检测了压裂液的耐温性、耐剪切性、悬砂性、耐酸碱性和破胶性.结果表明,m(氯化铵)∶m(冰乙酸)∶m(OADO)∶m(水)为0.5∶1∶1.5∶100时,压裂液pH值为6.0,粘度可达到82mPa·s,70℃时可有效悬砂,剪切60min后粘度仍大于25mPa·s,当压裂液中煤油含量大于0.8%时,120min内可完全破胶.     

MoO3/SO4^2- —TiO2 catalyst for transesterification of dimethyl cabonate with phenol

A new MoO3/SO4^2- -TiO2 catalyst was prepared by a conventional impregnation of SO42-/TiO2 as carrier with an aqueous solution of ammonium molybdate and used for the synthesis of transesterification of dimethyl carbonate （DMC） with phenol.A series of MoO3/SO42--TiO2 catalysts with different MoO3 loadings were investigated and characterized using X-ray diffraction （XRD）,Fourier transform infrared spectrometer （FTIR）,NH3-temperature programmed desorption （NH3-TPD） and X-ray photoelectron spectroscopy （XPS）.The results show that MoO3 loading is related to the activity of transesterification reaction.With the increase of MoO3 loading,the activity of transesterification reaction increases.The sulfur species in the catalyst have an influence on the molybdenum species,and lead to an increase in the electropositive of molybdenum,which promotes the catalytic activity of MoO3/SO42--TiO2.Among the series of catalysts prepared,MoO3/SO42--TiO2 with 10% MoO3 and 823 K calcinated is found to be the most active catalyst for transesterification reaction.Under the reaction conditions of 453 K and 12 h,the conversion of DMC is 30.5 %,and the yields of MPC and DPC reach 21.2 % and 8.7 %,respectively.     

凝胶法制备Cu-BTC块体及其吸附脱除二甲基二硫醚性能

金属有机骨架材料Cu-BTC具有高孔隙率、易调控的骨架结构以及含过渡金属等特点,是吸附脱除硫化物的优异材料。采用凝胶法在常温条件下制备块状样品Cu-BTC-g,并通过X射线衍射(XRD)、扫描电子显微镜(SEM)、红外光谱(FT-IR)、拉曼光谱(Raman)、X射线光电子能谱(XPS)、N₂吸附-脱附等手段对其进行分析表征,同时测定Cu-BTC-g样品对模型硫化物二甲基二硫醚(DMDS)的静态吸附容量、吸附热力学和动力学特性。结果表明：凝胶法制备的Cu-BTC-g样品晶体平均尺寸约为0.2μm、比表面积为901 m²/g、孔体积为0.40 cm³/g,晶体尺寸、比表面积和孔体积均小于溶剂热法合成的样品Cu-BTC-s;在吸附温度298 K下,Cu-BTC-g样品的DMDS吸附容量为110.8 mg/g,比Cu-BTC-s样品提高12%。