富马酸二甲酯的催化合成

在反应的第一阶段,以阳离子树脂为催化剂,用马来酸酐和无水甲醇进行酯化反应得到马来酸二甲酯,反应混合物经分离去掉催化剂并干燥除水;在反应的第二阶段,向第一阶段的反应混合物中加入溴的四氯化碳溶液,经光照异构化得到富马酸二甲酯。研究表明,反应第一阶段的较佳条件是:马来酸酐14.7 g,无水甲醇20 mL,阳离子树脂1.5 g,70℃下回流反应5 h;反应第二阶段的较佳条件是:B r2/CC l4和λ=350 nm光照射,产率可达92.5%;实验证明,阳离子树脂催化剂具有良好的重复使用性能。     

富马酸二甲酯的合成

马来酸酐与甲醇在混合催化剂的作用下,一步合成了富马酸二甲酯。确定了最佳工艺条件:三氯化铁0 5g,浓硫酸1 0ml,浓磷酸2 0ml,硫脲1 0g,溴化钠1 0g,马来酸酐4g及甲醇,回流反应2h,产率达88%,产品纯度大于99%。该法具有操作简便、反应时间短的特点。     

富马酸二甲酯的合成工艺研究

以马来酸酐和甲醇为原料,用磷钨酸作酯化催化剂制得马来酸二甲酯,再用硫脲作异构化催化剂制得富马酸二甲酯。通过正交实验确定出最佳工艺条件为:甲醇∶马来酸酐的摩尔比为8∶1,催化剂磷钨酸的用量是马来酸酐用量的10%,酯化时间为5h,催化剂硫脲用量为马来酸酐用量的2.5%,异构化时间为20～30min,产率可达87.8%。     

Microporous polyurethane/acrylate gel polymer electrolyte obtained by emulsion polymerization

A novel polyurethane/acrylate (PUA) porous gel electrolyte was prepared by a new method, emulsion polymerization. Compared with the traditional phase inversion method, the new method can eliminate the pollution from solvent and decrease the cost of production. The swelling properties and morphology of the porous polymer membranes were characterized. The porous membranes, made by emulsion polymerization, could absorb large quantities of electrolyte solution to form porous gel electrolytes. The gel electrolytes have good solvent retention ability and high ionic conductivity. Copyright © 2004 Society of Chemical Industry     

富马酸二甲酯合成研究进展

富马酸二甲酯是当前对黄曲霉菌抑制作用最佳的新型食品和饲料防霉、防腐剂。其使用安全 ,生产成本低。本文对近年来富马酸二甲酯的合成方法进行了评述。建议对近年开发的有应用前景的催化剂扩大试验与筛选。     

富马酸二甲酯的合成研究

以糠醛为原料、氯酸钾为氧化剂、ＣＴＭＡＢ为相转移催化剂,利用超声波辐射合成富马酸,再以硫酸锆为催化剂催化富马酸和甲醇酯化合成富马酸二甲酯,对影响产品产率的各种因素进行了研究。     

壳聚糖硫酸盐催化合成富马酸二甲酯

以壳聚糖硫酸盐为催化剂 ,用富马酸与甲醇反应合成了富马酸二甲酯 (DMF) ,用正交实验确定了反应条件对DMF收率的影响。最佳工艺条件为 :反应时间为 6h ,甲醇与富马酸的摩尔比为 6∶1 ,催化剂用量为1 0 g ,DMF的最高收率可达 86 0 %。催化剂重复使用实验表明 ,该催化剂对DMF的合成具有较好的催化活性及重复使用性     

氯化铁催化合成富马酸二甲酯

氯化铁可代替硫酸催化酯化反应，探讨了氯化铁催化合成富马酸二甲酯的条件，操作简便，反应温和，无腐蚀，减少了污染与产品纯化。     

富马酸二甲酯的合成新工艺研究

研究了以糠醛为原料,以KClO3为氧化剂,V2O5为催化剂制备富马酸,在固载杂多酸PW12/C催化下,富马酸和甲醇经过酯化反应合成富马酸二甲酯。考察了催化剂用量、氧化剂用量、反应时间和醇酸比对反应的影响,确定了最佳工艺条件。m(KClO3)∶m(糠醛)=1.8∶1,反应温度105℃,催化剂用量为0.2g时,反应时间4h,富马酸产率为80.7%;酯化反应中n(甲醇)∶n(富马酸)=7∶1,m(PW12/C)∶m(富马酸)=6∶100,回流反应6h,富马酸二甲酯产率达88.1%。     

苯酐改性聚乙二醇型聚氨酯固态电解质的制备与性能

以异佛尔酮二异氰酸酯（IPDI）、聚对苯二甲酸-3-甲基-1,5-戊二醇酯二醇（TPA-1000）、聚乙二醇（PEG-2000）、一缩二乙二醇（DEG）为主要原料合成了一系列热塑型聚氨酯弹性体,然后加入20%的锂盐（LiTFSI）制备不同的全固态电解质（SPE）。结果表明,随着TPA-1000含量的减少和PEG-2000含量的增加,SPE的耐热性增加,玻璃化转变温度减小,拉伸强度减小,断裂伸长率增加。SPE的离子电导率与温度的关系基本符合Arrhenius方程,在80℃,SPE（除纯PEG-2000的电解质外）的电化学窗口均达到4.0V以上,其中质量比TPA-1000：PEG-2000=1：2（SPE4）综合性能最佳,力学为1.87Mpa、电导率为2.15?10-4 S cm-1、窗口为4.3V。以SPE4组装的全固态电池在80℃、0.2C下放电比容量为150 mAh/g。     

Ionic interactions and transport mechanism in polyurethane electrolytes

Alternating current (AC) impedance, Fourier transform (FT)–Raman, and Fourier transform infrared (FTIR) have been conducted on solutions of poly(ethylene oxide)_(MW=1000)–urethane electrolytes commingled with LiCF₃SO₃ as the function of temperature and salt concentration. From the analysis of the Vs(SO₃) vibration, the ionic concentration of salt in various chemical environments can be calculated approximately. The spectroscopic evidence was found for the redissociated ion pairs, and ionic congeries increased with increasing temperature. AC impedance measurements is used to calculate the ionic diffusion coefficient (D_i). Investigated the various concentrations (from O/Li = 4 ～ 20) at the different temperature (40 ～ 120°C), We found that the calculated values (D_i) with the Nernst–Einstein equation are higher than the direct measurement. The discrepancy increases with the increase of temperature. A good correlation between the conductivity and the ionic redissociation is determined from the Vs(SO₃) vibration band. The fraction of the “free” ion significantly corresponds to the revised Nernst–Einstein equation by using the Nernst–Einstein relation and compared with those direct measurement. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 785–790, 2002     

富马酸二甲酯合成工艺中催化剂的研究进展

综述了由富马酸、马来酸酐及糠醛合成富马酸二甲酯的合成新工艺及所用催化剂的研究进展。     

Effect of hard segment and concentration of NaClO4 on poly(ethylene oxide)–urethane/NaClO4 complex

Solid poly(ethylene oxide)–urethane electrolytes were prepared from blends of polyurethane and NaClO₄. The samples were characterized by FTIR, DSC, atomic force microscopy, and complex impedance analysis. The effect of the concentration of NaClO₄ on the poly(ethylene oxide)–urethane/NaClO₄ complex were studied. The results showed that the concentration of NaClO₄ had an important effect on the ion–polymer interaction, ion–ion interaction, glass‐transition temperature, morphologic structure, and ionic conductivity of the complex. We also prepared a model compound of hard segments and found that the conductivity of the complex decreased when the model compound was blended into the complex. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 2502–2510, 2001     

固载杂多酸催化合成富马酸二甲酯

以富马酸与甲醇为原料，固载杂多酸PW12／C为催化剂合成了富马酸二甲酯，详细探讨了影响酯化反应的各种因素，得到了富马酸与甲醇反应的最佳条件，在此条件下，酯化产率为91．6％。     

Composite polymer electrolytes based on the low crosslinked copolymer of linear and hyperbranched polyurethanes

Low crosslinked copolymer of linear and hyperbranched polyurethane (CHPU) was prepared, and the ionic conductivities and thermal properties of the composite polymer electrolytes composed of CHPU and LiClO₄ were investigated. The FTIR and Raman spectra analysis indicated that the polyurethane copolymer could dissolve more lithium salt than the corresponding polymer electrolytes of the non crosslinked hyperbranched polyurethane, and showed higher conductivities. At salt concentration EO/Li = 4, the electrolyte CHPU30‐LiClO₄ reached its maximum conductivity, 1.51 × 10^?5 S cm^?1 at 25°C. DSC measurement was also used for the analysis of the thermal properties of polymer electrolytes. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 3607–3613, 2007     

Characterization of PEO-PAN hybrid solid polymer electrolytes

Hybrid solid polymer electrolytes (HSPE) of high ionic conductivity were prepared using polyethylene oxide (PEO), polyacrylonitrile (PAN), propylene carbonate (PrC), ethylene carbonate (EC), and LiClO₄. These electrolyte films were dry, free standing, and dimensionally stable. The HSPE films were characterized by constructing symmetrical cells containing nonblocking lithium electrodes as well as blocking stainless steel electrodes. Studies were made on ionic conductivity, electrochemical reaction, interfacial stability, and morphology of the films using alternating current impedance spectroscopy, infrared spectroscopy, and scanning electron microscopy. The properties of HSPE were compared with the films prepared using (i) PEO, PrC, and LiClO₄; and (ii) PAN, PrC, EC, and LiClO₄. The specific conductivity of the HSPE films was marginally less. Nevertheless, the dimensional stability was much superior. The interfacial stability of lithium was similar in the three electrolyte films. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 2191–2199, 1997     

新颖离子导电型聚氨酯弹性体

以低聚二氧戊环磺酸盐(SPDXL)为离子源和增塑剂,聚己二酸乙二醇酯聚氨酯弹性体(EGPU)为基质,设计了一种新颖的正离子导电型聚氨酯弹性体,并对其结构、形态及性能进行了研究。结果表明,通过选取适当平均相对分子质量的磺化低聚醚以及通过控制磺化低聚醚的质量分数,可以优化聚氨酯固体电解质体系的离子导电性能。对于EGPU/SPDXL固体电解质体系,采用SPDXL800的样品具有较高的离子导电性能,其室温离子电导率均达到10-6S/cm以上。     

气相色谱-质谱法测定玩具涂层中富马酸二甲酯

以超声波辅助水萃取、甲苯反萃方法提取玩具涂层中的富马酸二甲酯(DMF),然后用气相色谱-质谱法进行测定,建立了玩具涂层中富马酸二甲酯的测定方法,确定了较佳超声萃取温度和时间分别为55 ℃和30min.在此条件下,以气相色谱-质谱法测定玩具涂层中的富马酸二甲酯,样品回收率为92.4%～99.6%,精密度小于4.6%,方法...     

Synthesis and properties of sulfonated multiblock copolynaphthalimides

Sulfonated multiblock copolynaphthalimides (co-SPIs) with block length of 5-20 were prepared by a two-pot polymerization method from 1,4,5,8-naphthalenetetracarboxylic dianhydride, sulfonated diamines of 2,2′-bis(4-sulfophenoxy)benzidine (BSPOB) and 4,4′-bis(4-aminophenoxy)biphenyl-3,3′-disulfonic acid (BAPBDS) and nonsulfonated diamines. The scanning transmission electron microscopy showed that the BSPOB-based multiblock co-SPI membranes had well-defined microphase-separated structure where the hydrophilic and hydrophobic layer-like domains were oriented in the plane direction of membrane. On the other hand, the BAPBDS-based multiblock co-SPIs and all the random co-SPIs showed the homogeneous morphology. The water uptake, anisotropic membrane swelling, anisotropic proton conductivity and polymer electrolyte fuel cell (PEFC) performance were investigated for the multiblock and random co-SPIs. The results demonstrated strong effects of the membrane morphology on these properties. The BSPOB-based multiblock co-SPI membranes exhibited the larger through-plane swelling and the lower through-plane conductivity than the random ones, and as a result exhibited the lower PEFC performances. This study gives good understanding of the morphology-property relationship in novel block architectures' design.     

固体酸催化光异构化合成富马酸二甲酯

马来酸酐与甲醇在五水四氯化锡催化下发生酯化反应，所得产物马来酸二甲酯在光和溴存在下异构化成富马酸二甲酯。n(马来酸酐)∶n(甲醇)∶n(四氯化锡)为1.0∶5.0∶0.114时，回流反应3 h，该富马酸二甲酯收率达90.3%。比较了几种不同固体酸催化合成富马酸二甲酯的催化活性，结果表明该法操作方便，反应条件温和，产物收率高。