离子液体[Amim]PF_6的水相法合成与表征

以N-甲基咪唑、烯丙基氯为原料,采用回流法制备中间体氯化-1-烯丙基-3-甲基咪唑离子液体([AMIM]Cl),进而采用水相法,通过离子交换制备了疏水型离子液体1-烯丙基-3-甲基咪唑六氟磷酸盐([Amim]PF6),考察了合成温度、中间体与六氟磷酸钾的摩尔配比对其产率的影响,以红外光谱、核磁共振波谱进行结构表征。结果表明,水相法能够有效地合成目标产物,大大缩短合成时间;当温度为30℃,物料比n([Amim]Cl)∶n(KPF6)为1∶1.2,反应10min可以得到产率为87%的[Amim]PF6。     

六氟磷酸盐吡啶离子液体的合成及电导率研究

采用二溴丁烷和3-甲基吡啶(物质的量之比为1.0∶2.2)为原料,以异丙醇为溶剂,温度控制在70～80℃,反应4～6h,得到吡啶溴盐离子液体。用吡啶溴盐与六氟磷酸盐发生置换反应,搅拌反应4h,得到六氟磷酸盐吡啶离子液体。测定了[C4(MPy)2][PF6]2离子液体在有机溶剂中的电导率;及离子液体在不同溶剂、不同浓度、不同温度下的电导率。结果表明:溶液的电导率随着温度升高而增大;随着浓度的增大而增大。相同温度、浓度下,乙腈的电导率最大;环丁砜的电导率最小。     

Cu纳米颗粒添加体的[BMIm]NTf_2离子液体法制备及其摩擦学性能

用离子液体法制备Cu纳米颗粒并将其用于摩擦学研究优于常用的方法,以往对此报道不多。通过微波辐射合成了1-丁基-3-甲基咪唑双三氟甲基磺酰亚胺{[BMIm]NTf2}离子液体,利用化学还原法分别在水溶液和[BMIm]NTf2中制备了Cu纳米颗粒,采用XRD,TEM,TG和DTA对其结构进行了表征;将2种纳米Cu颗粒溶于N68基础油中,采用四球摩擦磨损试验机对2种纳米Cu添加体的摩擦学性能进行了试验,并对磨痕表面进行了SEM分析。结果表明:[BMIm]NTf2离子液体中制备的Cu纳米颗粒为面心立方结构,粒径为3～25nm,能够显著改善N68基础油的抗磨减摩性能;与水溶液中制备的纳米Cu添加体相比,其摩擦系数下降了24.6%,钢球磨斑直径下降了18.8%,PB值提高了16.4%。     

离子液体[Bmim-]PF6的微波合成、表征及以[Bmim]PF6为介质的TiO2光催化剂的制备研究

采用微波两步法合成了1-丁基-3-甲基咪唑六氟磷([Bmim]PF6)离子液体,优化了离子液体的合成条件,探讨了微波辅助合成离子液体的影响因素,采用多种方法表征了离子液体的结构,并使用该离子液体制备了TiO2光催化剂.制备的TiO2具有良好的光催化活性,16h内对苯酚的降解率达到99.23%.     

以跨临界CO_2-离子液体[bmim]PF_6为工质对的吸收式制冷循环性能分析

选择跨临界CO2-[bmim]PF6作为新型的吸收式制冷工质对,考察了CO2在离子液体[bmim]PF6中的溶解度和CO2-[bmim]PF6工质体系的热物性.计算了在给定工况下循环的制冷特性并对结果进行了分析与讨论.     

新型电解质材料[BMIM]ClO3离子液体的合成及其物化性能

以N-甲基咪唑为原料合成了室温离子液体1-丁基-3-甲基咪唑氯酸盐([BMIM]ClO3),用IR、NMR、DSC-TGA等手段对产物进行了表征,测定了相关物化性能,如密度、表面张力、黏度、电导率和电化学窗口等,并考察了该离子液体的溶剂性能。结果表明,该离子液体作为新型的电解质材料,具有低黏度、高电导率,密度、表面张力、黏度均随温度升高而减小,电导率随温度升高而增大,与温度符合Arrhenius方程。该离子液体与多数常规溶剂互溶,并对某些金属氧化物具有较高的溶解度,为离子液体在选矿、电解金属氧化物等方面的应用奠定了基础。     

离子液体[Omim]PF_6的合成及其深度处理焦化含酚废水的研究

采用微波两步法合成了1-辛基-3-甲基咪唑六氟磷酸([Omim]PF6)离子液体,采用多种方法表征了离子液体的结构。研究了[Omim]PF6对模拟焦化含酚废水(苯酚、甲酚、二甲酚)的萃取,考察了反应体系相比、反应时间、温度、体系pH值、微波辅助反应时长对萃取效果的影响。结果表明:在体系相比为V离子液体∶V含酚溶液=1∶1.5,反应时间为10min,反应温度为20℃,体系pH值为6,微波辅助反应时间40s的条件下,对含酚溶液的萃取率可达99.86%,并且[Omim]PF6具有良好的再生性能。     

离子液体[bmim]PF6中制备纳米金属Ni及其催化苯乙烯加氢的研究

以化学还原手段分别在水溶液和离子液体1-丁基-3-甲基咪唑六氟磷酸盐([bmim]PF6)中制备了纳米金属Ni粉末,采用X射线衍射(XRD)、透射电镜(TEM)、傅立叶红外光谱(FT-IR)、紫外可见光谱(UV-vis)及热重(TG-DTA)对所制备样品的形貌和结构进行了表征.XRD表征结果显示:与水溶液制备纳米Ni相比,在[bmim]PF6中制备的纳米Ni具有立方相结构,无氧化峰出现;TEM结果显示:在[bmim]PF6中制备的纳米Ni具有更小的粒径和更好的颗粒分布,团聚现象不明显;FT-IR显示:离子液体不仅仅作为反应的介质,而且和纳米颗粒表面间存在着一定的化学结合,吸附在纳米颗粒的表面,有效的阻止了Ni纳米颗粒的团聚和氧化;TG-DTA及UV-vis结果进一步验证了Ni表明离子液体层的存在.苯乙烯加氢产物的分析结果表明,在[bmim]PF6中制备的纳米Ni催化苯乙烯加氢的活性显著高于常规制备的Ni催化剂.     

微波法合成离子液体1-羟乙基-3-甲基咪唑四氟硼酸盐的研究

由1-甲基咪唑和2-氯乙醇通过微波法合成中间体氯化1-羟乙基-3-甲基咪唑,考察了原料配比、微波功率、加热方式和加热时间对中间体产率的影响。中间体经阴离子交换得到1-羟乙基-3-甲基咪唑四氟硼酸盐离子液体。通过测定中间体的相对分子量分析其纯度,目标产物的结构通过IR1、H-NMR表征。     

Synthesis of Calix[4, 5, 6] Resorcinarenes Using Fullerene C60 as Template

We present a new use of fullerene C₆₀ as a template for the synthesis of cyclic resorcinarenes, The cyclocondensation of 2-methyl-resorcinol with benzaldehyde and hexanal in THF, catalyzed by AlCl₃, in the presence of 1%, 5%, and 10% fullerene C₆₀, produces calix[4], [5], and [6] resorcinarenes, with the pentamer and hexamer as the major products. The resorcinarenes were characterized by ¹H, ¹³C NMR, FTIR, FAB⁺ mass spectrometry, and elemental analysis.     

杯[6]芳烃衍生物改性壳聚糖的合成及吸附性能研究

通过单取代溴丙氧基对叔丁基杯[6]芳烃衍生物与壳聚糖发生交联,合成一种新型的杯[6]芳烃-壳聚糖聚合物,对聚合物进行了红外、X射线衍射和扫描电镜表征。并考察了聚合物对过渡金属离子Zn2 ,M n2 ,Pb2 ,C r3 ,Cu2 的吸附性能。结果表明,该聚合物兼具杯芳烃与壳聚糖的各自优势,不仅吸附能力较强,而且对部分离子表现出较高的选择性吸附。     

[Li@C60]PF6: Infrared spectra from 90K to 523K; Determination of the molar extinction coefficients and integrated molar absorptivity

Abstract

The molar extinction coefficient ε and the integrated molar absorptivity ψ values of all the mid-infrared and far-infrared absorption bands of [Li@C₆₀]⁺PF₆^- were determined in comparison to those of C₆₀. The dependence from temperature of all the infrared absorption bands of [Li@C₆₀]⁺PF₆^- was measured in the temperature range comprised from 523?K and 90?K and extrapolated to 0?K. Once again, the results were discussed in comparison to the C₆₀ analogous experimental results.     

Q[6]/CdS-Ag2S复合光催化剂的合成及光催化性质

CdS因具有独特的光电化学性能而被广泛用于光催化研究, CdS与窄带隙半导体和有机物复合是重要的光催化研究方向。研究采用化学沉淀法制备了六元瓜环(Q[6])复合和Ag₂S掺杂的硫化镉光催化剂(Q[6]/CdS-Ag₂S), 通过不同手段对复合催化剂进行表征。实验以可见光为光源, 罗丹明B为模拟污染物, 考察了六元瓜环对CdS-Ag₂S光催化性能的影响。结果表明: 经Q[6]复合后的Q[6]/CdS-Ag₂S形貌为菜花状, 颗粒粒径变小。复合催化剂Q[6]/CdS-Ag₂S的催化性能明显优于CdS-Ag₂S, 光催化反应110 min, 15 mg复合催化剂对100 mL 6 mg/L罗丹明B溶液的催化降解效率达到92.4%。     

Synthesis of Calix[4, 5, 6] Resorcinarenes Using Fullerene C60 as Template

Abstract

We present a new use of fullerene C₆₀ as a template for the synthesis of cyclic resorcinarenes, The cyclocondensation of 2‐methyl‐resorcinol with benzaldehyde and hexanal in THF, catalyzed by AlCl₃, in the presence of 1%, 5%, and 10% fullerene C₆₀, produces calix[4], [5], and [6] resorcinarenes, with the pentamer and hexamer as the major products. The resorcinarenes were characterized by ¹H, ¹³C NMR, FTIR, FAB⁺ mass spectrometry, and elemental analysis.     

Bromination of [60]Fullerene. I. High-Yield Synthesis of C60Brx (x=6, 8, 24)

The systematic study of the bromination of C₆₀ was performed under various experimental conditions. Application of some chloroarenes as reaction media resulted in the high-yield (70-96%) selective synthesis of C₆₀Br₆ and C₆₀Br₈. Direct bromination of fullerene yielded either C₆₀Br₈, C₆₀Br₁₄, or C₆₀Br₂₄ depending on the reaction time. Possible pathways of bromination of C₆₀Br₈ were analyzed using semiempirical (AM1) calculations, two most probable molecular structures are conjectured for the first isolated C₆₀Br₁₄.     

Preparation and characterization of calix[6]arene Langmuir-Blodgett thin film

Calix[6]arene monolayer/multilayer was prepared on a glass substrate and the behavior of monolayer properties investigated at the air-water interface by taking Langmuir isotherm graph. UV-visible, wettability measurements, atomic force microscopy and quartz crystal microbalance measurements were used to monitor the deposition quality of this Langmuir-Blodgett film. Our results showed that a uniform and high quality film with a transfer ratio of approximately 0.99 occurred using the calix[6]arene material at a deposition pressure of 21 mN/m. The surface free energy was determined to be 25.86 mN/m based on contact angle measurements.     

Viscosity of [bmim][PF6] and [bmim][BF4] at High Pressure

The viscosities of 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim] [PF₆]) and 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF₄]) were measured by using a rolling-ball viscometer. The experimental temperatures were from 293.15 to 353.15 K, and the pressures were from 0.1 to 20.0 MPa.Paper presented at the Seventh Asian Thermophysical Properties Conference, August 23–28, 2004, Hefei and Huangshan, Anhui, P. R. China.