2-甲基-1,3-氧硫杂环戊烷和2-丙基-1,3-氧硫杂环戊烷的合成

以对甲苯磺酸为催化剂 ,巯基乙醇与乙醛、丁醛 (量比为 1.0∶1.1)在苯中共沸脱水 ,合成两种目标产物 :2 甲基 1,3 氧硫杂环戊烷、2 丙基 1,3 氧硫杂环戊烷。其产率分别为 81%和 88% ,质量分数分别为 99%和 98%。经红外光谱、色谱、质谱、核磁共振谱检测 ,确证了产物结构。此方法简便易行 ,产率较高     

2-乙基-1,3-氧硫杂环戊烷的合成

以对甲苯磺酸为催化剂 ,巯基乙醇与丙醛 (摩尔比 1∶ 1 .1 )在苯中共沸脱水 ,合成目标产物2 -乙基 - 1 ,3-氧硫杂环戊烷。产物产率为 91 % ,质量分数为 96%。经红外光谱、色 -质联用和核磁共振谱检测 ,确证了产物结构。此方法简便易行 ,产率较高     

4-乙酰氧基-2-氮杂环丁酮的合成

设计了以醋酸乙烯酯和氯磺酰异氰酸酯为起始原料,经加成和消除反应,中间产物不需分离,直接制备了4-乙酰氧基-2-氮杂环丁酮,产物收率为66.6%。经质谱、核磁和红外等波谱鉴定了目标分子的结构。该法与文献相比,方法简单易行,成本低。     

4-溴甲基-5-甲基-1,3-二氧杂环戊烯-2-酮的合成研究

以4,5-二甲基-1,3-二氧杂环戊烯-2-酮（DMDO）为原料,经溴化反应得4-溴甲基-5-甲基-1,3-二氧杂环戊烯-2-酮（DMDO-Br）,对反应的条件做了研究。对目标产物的结构进行核磁及质谱的表征。     

2-甲基-1，3-环戊二酮的合成

以丁二酸和丙酰氯为原料,无水A lC l3为催化剂,合成2-甲基-1,3-环戊二酮,并对工艺条件进行了优化。最佳条件为:在氮气作用下,n(丁二酸):n(丙酰氯):n(氯化铝)=1:3:3,反应温度100℃,回流时间2h,产品收率为58.9%。用红外光谱确定了产品结构。     

4-氯甲基-5-甲基-1,3-间二氧杂环戊烯-2-酮工业合成研究

介绍了 4 氯甲基 5 甲基 1,3 间二氧杂环戊烯 2 酮在医药中间体中的应用 ,研究了其工业合成路线 ,试验选择了氯化反应和重排反应的优惠工艺条件 ,并进行了产品纯化研究。在此条件下 ,收率≥ 65% ,纯度≥ 75%。     

3种2-甲基-2-烷基-1,3-二硫杂环戊烷类化合物的合成

以对甲苯磺酸为催化剂, 3种酮类化合物和二硫代乙二醇在苯中共沸脱水,合成了 2 -甲基- 2 -乙基- 1, 3 -二硫杂环戊烷、2- 甲基- 2- 异丁基- 1, 3- 二硫杂环戊烷和 -2 -甲基- 2 -异戊基 1, 3 二硫杂环戊烷,产率分别为 71. 5%、74. 3%和 75. 6%,质量分数分别为 98 .8%、99. 1%和 98. 9%。经红外光谱分析、元素分析、核磁共振分析和色 -质联机分析确定了 3种产物的结构。     

4-氯-4,5-二甲基-1,3-二氧杂环戊烷-2-酮合成工艺研究

以羟基丁酮为原料 ,经酰化、环合等步骤合成医药中间体 4 氯 4 ,5 二甲基 1,3 二氧杂环戊烷 2 酮 ,合成收率达 86 %以上     

邻(1,3-二氧杂环戊-2-基)苯酚的合成

介绍了从水杨醛和乙二醇在催化剂存在下合成邻 （１,３ 二氧杂环戊 ２ 基）苯酚的新方法,并对工艺条件进行了优化试验。收率约为８６％     

1,3-二甲基-2-咪唑啉酮的制备

以乙二胺、尿素、甲醛和甲酸为原料,经过环化和甲基化反应制得目标产物1,3-二甲基-2-咪唑啉酮(1,3-DMI)。通过红外、核磁对其结构进行了确证。考察了溶剂、原料浓度、原料摩尔比、反应温度和时间、催化剂对制备(1,3-DMI)收率的影响。较佳工艺条件为:制备2-咪唑啉酮时,以水-乙二醇混合作溶剂;制备1,3-DMI时,甲醛(36%)∶甲酸(85%)摩尔比为1∶2.8,反应温度95~100℃,反应时间16 h,氯化亚铜和三乙胺作催化剂,用量分别是2-咪唑啉酮摩尔数的1.0%。总收率达到71%,纯度为98.5%。     

2-恶唑烷酮及其衍生物的应用与合成

介绍2-恶唑烷酮的应用及几种不同的合成方法，并进行简单比较。同时介绍2-恶唑烷酮五类衍生物的应用及先进的合成方法。     

基于离子凝胶电解质的TiO2(B)@C/CNT//AC准固态锂离子电容器

以微波辅助溶剂热法制备多壁碳纳米管负载的碳包覆单斜相二氧化钛纳米复合电极,通过静电纺丝技术制备聚酰亚胺纤维膜,进而制备三元离子凝胶电解质,最后与商业活性炭组装成新型准固态锂离子电容器.结果 表明,TiO2(B)@C/CNT纳米复合电极呈现出高可逆容量(291mAh/g)和高电化学反应动力学特性.PI/[EMIM] [B...     

超级电容器准固态聚合物电解质膜的研究

制备了一种介于水凝胶和全固态聚合物电解质之间的聚合物电解质膜,用于活性炭电子双电层电容器。测试表明使用该聚合物电解质膜的双电层电容器的容量为2 15mA·h,其容量、功率特性与KOH水溶液电容器相当。电容器的循环伏安曲线,稳定的充放电循环曲线及交流阻抗谱说明该种聚合物电解质膜在碳基超级电容器的使用电压范围(0～1V)内是稳定的,而且聚合物电解质膜电容器表现出良好的可逆性和循环特性。     

纳米SiO2填料对离子凝胶电解质及高压超级电容器性能的影响

以SiO2纳米颗粒为填料,通过溶液浇筑法合成了纳米复合离子凝胶电解质,研究了SiO2填料对离子输运的影响规律。基于离子凝胶电解质构筑了准固态电容器,探讨了无机填料对电容器性能的影响,以活性炭为电极、凝胶电解质为隔膜,构筑了准固态双电层电容器。结果表明,SiO2的加入没有改变隔膜电解质的微观形貌,但有效改善了浸润性,提高了离子电导率。高SiO2添加量的隔膜电解质电化学性能更优,当添加8wt% SiO2时凝胶电解质电化学性能最优。SiO2的加入可有效提高活性炭准固态电容器的性能,电容器的比容提升约15%,经4000次循环后容量保持可达100%。电解质高温稳定性良好,器件最高使用温度可达60℃。基于该复合电解质构筑的电容器具有良好的高温性能,电容器比容随温度升高而逐渐提升,60℃时能量密度可达81.36 Wh/kg。     

Preparation and characterization of gel polymer electrolyte based on PVA-K2CO3

ABSTRACT

In this study, electrolyte materials were synthesized by mixing a highly conducting salt (K₂CO₃) with the poly(vinyl alcohol) (PVA) in different proportions (from 10 to 50 wt.%). The synthesized electrolyte was characterized using Fourier transform infrared (FTIR) spectroscopy, field-emission scanning electron microscopy (FESEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), electrochemical impedance spectroscopy (EIS), and linear sweep voltammetry (LSV) for their functional groups, morphology, thermal stability, glass transition temperature (T_g ), ionic conductivity, and potential window, respectively. Characterization results show that the complex formation between PVA and K₂CO₃ salt has been established by FTIR spectroscopic study, which indicates the detailed interaction between PVA and the salts in PVA-K₂CO₃ composites while the amorphous nature of the electrolyte after incorporation of the salts has been confirmed by FESEM analysis. Similarly, TGA and DSC analysis revealed that both decomposition temperature and T_g of the synthesized electrolytes decrease with the addition of K₂CO₃ due to the strong plasticizing effect of the salt. The results confirm that the electrolytes have sufficient thermal stability for supercapacitor operation, as well as an amorphous phase to effectively deliver high ionic conductivity. The highest ionic conductivity of 4.53 × 10^?3 S cm^?1 at 373 K and potential window of 2.7 V was exhibited by PK30 (30 wt.% K₂CO₃), which can be considered as high value for solid-state electrolytes which are superior to those electrolytes from PVA salts earlier reported. The results similarly show that the prepared electrolyte is temperature-dependent as conductivity increase with increase in temperature. Based on these properties, it can be imply that the PVA-K₂CO₃ gel polymer electrolyte (GPE) could be a promising electrolyte candidate for EDLC applications. The results indicate that the PVA-K₂CO₃ as a new electrolyte material has great potential in practical applications of portable energy-storage devices.     

Electric double layer capacitors with polymer hydrogel electrolyte based on poly(acrylamide) and modified electrode and separator materials

Activated carbon fiber cloths (AC) and hydrophobic microporous polypropylene (PP) membrane, both modified by acetone aldol condensation products, and filled with polymer hydrogel were used as electrodes, separator and electrolyte in electric double layer capacitors (EDLCs). Polymer hydrogel used was based on poly(acrylamide) (PAAM), KOH and water. Electrochemical characteristics of EDLCs were investigated by cyclic voltammetry and galvanostatic charge–discharge cycle tests and also by impedance spectroscopy, compared with a case of the capacitor with only a KOH aqueous solution used as an electrolyte. As a result, the capacitor with polymer hydrogel was found to exhibit higher capacitance than that with the KOH aqueous solution and an excellent high-rate dischargeability. The above results provide valuable information to explore novel composition of EDLCs.     

Solid electrolyte based on silicate matrix solvated by tetraalkylammonium salt solution in organic polar solvent

Solid electrolyte composed of silicate matrix solvated by tetraalkylammonium salt solution in viscous organic polar solvent (propylene carbonate or sulpholane) was prepared by sol-gel method under controlled drying conditions. The organic solution was added directly to the tetramethoxysilane (TMOS) based sol. For comparison analogous material modified with pure solvent was prepared. Gel forms within 2-4 days depending on the solvent additive. The gelation time is longer than in the presence of lithium salt or pure solvent modified material. The obtained electrolyte is transparent and it loses about 12% its mass during first 30 days of aging. It was characterised by TGA, DSC, FTIR spectroscopy and impedance spectroscopy. The shape of TGA and DSC curve is similar to that of pure solvent. The IR spectra indicates silicate network formation with some silanol groups left. No indication of specific interactions between solute, solvent and silicate matrix has been found. The magnitude of electrical conductivity is close to 10⁻³ S cm⁻¹ being one order of magnitude smaller than that of analogous liquid electrolyte. The electrical conductivity of silicate matrix modified with pure solvent is by two orders of magnitude smaller. The value of this parameter depends on time elapsed after gelation. Most substantial decrease is observed during first 10 days after gelation and it correlates with mass loss. The conductivity of TMOS based matrix solvated with pure solvent is another two orders of magnitude smaller. The obtained results indicate that silicate matrix is neutral reservoir for organic solvent. The porosity of the dried samples is to some extent affected by the presence of salt.     

有机介质体系锂离子电容器

锂离子电容器（lithium ion capacitor,LIC）是一种新型的电化学储能器件,可以填补锂离子电池和超级电容器两者之间的性能空白,是下一代高能量密度超级电容器的前进方向。本文首先介绍了锂离子电容器的储能原理分为电解液消耗机制、锂离子交换机制以及混合机制,并围绕高能量密度的有机介质体系锂离子电容器,着重阐述了各类电容及电池型正负极材料的性质特点、优化方向及其研究现状,指出不同材料的优缺点及改性方法。同时叙述了与产业应用相关的预嵌锂技术、隔膜、电解液以及体系匹配等方面的研究现状,总结归纳了这些部件的研究对于比能量、功率、安全、稳定性等性能的提升。在产业化应用方面,针对锂离子电容器不同于锂离子电池和传统超级电容器的性能指标,总结其在智能物流、起重机电源、机器人电源及轨道交通等方面独特的应用前景。最后展望了电极材料微观结构优化及功能集成、电解液专用化,预嵌锂成本进一步压缩、以及检测及原位表征方法的开发等锂离子电容器未来的发展方向。     

Solid electrolyte based on silicate matrix functionalised with tetraalkylammonium group solvated by organic solvent

Solid electrolyte composed of hybrid organic–inorganic silicate matrix functionalised with tetraalkylammonium group, solvated by viscous organic polar solvent (propylene carbonate (PC) or sulpholane (TMS)), was prepared by the sol–gel method under controlled drying conditions. Tetramethoxysilane (TMOS), N-trimethoxysilylpropyl-N,N,N-tributylammonium chloride (TMOSPTBACl) and organic solvent were principal sol components. Gel formed within 2 h and 2 days depending on substrate ratio and the solvent additive. The obtained material was transparent and it loosed about 15% of its mass during first 30 days of ageing. It was characterised by thermogravimetry (TGA), differential scanning calorimetry (DSC), NMR, FT-IR spectroscopy, small angle X-ray scattering (SAXS), and impedance spectroscopy. The transport of redox active molecules was studied by electrochemical methods. The porosity of samples dried in supercritical CO₂ was also estimated. The shape of TGA and DSC curve appeared to be similar to that of pure solvent. The IR spectra indicated the silicate network formation with some silanol groups left. The NMR spectrum of the solution used to wash crushed sample indicated that all organic substrate is embedded in silicate matrix. The magnitude of electrical conductivity was close to 10⁻⁴ to 10⁻⁵ S cm⁻¹, i.e. least more than one order of magnitude larger than that of TMOS based silicate matrix modified with a pure solvent. This conductivity is high enough for electrochemical experiments. Both conductivity and diffusion coefficient of redox probe-ferrocene (Fc) depended on time elapsed after gelation. Their most substantial decrease was observed during first 10 days after gelation and it correlated with mass loss.     

Carbon/PbO2 asymmetric electrochemical capacitor based on methanesulfonic acid electrolyte

A new hybrid electrochemical capacitor based on an activated carbon negative electrode, lead dioxide thin film and nanowire array positive electrode with an electrolyte made of a lead salt dissolved in methanesulfonic acid was investigated. It is shown that the maximum energy density and specific capacity of the C/PbO₂ nanowire system increase during the first 50 cycles before reaching their maximum values, which are 29 Wh kg⁻¹ and 34 F g⁻¹, respectively, at a current density of 10 mA cm⁻² and a depth of discharge (positive active electrode material) of 3.8%, that corresponds to a 22C rate. This is 7–8 times higher than the corresponding maximum values reached with a C/PbO₂ thin film cell operated in the same conditions. After an initial activation period, the performances of the C/PbO₂ nanowire system stay constant and do not show any sign of degradation during more than 5000 cycles. For comparison, the C/PbO₂ thin film system exhibits a 50% decrease of its performances in similar conditions.