2,5-二甲基-3,4-二氢-4-氧代喹唑啉的合成研究

对2,5-二甲基-3,4-二氢-4-氧代喹唑啉的合成进行了研究。以间甲基苯胺为原料经3步反应制得2-氨基-6-甲基苯甲酸,再环化生成2,5-二甲基-3,4-二氢-4-氧代喹唑啉。中间体及标题化合物结构经1 HNMR确证。     

Synthesis and Spectroscopic Investigations of CuSO4 · 5H2O Doped Poly (m-Toluidine)

Poly (m-toluidine) has been synthesized by chemical oxidative polymerization in acidic medium. Poly (m-toluidine) so obtained has been doped with copper sulfate in different concentration and prepared samples have been characterized by UV-visible spectroscopy, FTIR spectroscopy, X-ray diffraction, and DC conductivity measurements. UV-visible study reveals that optical band gap decreases considerably with increase in dopant concentration. The FTIR spectra exhibit structural changes in the backbone of poly (m-toluidine) with doping. The XRD patterns demonstrate the amorphous nature of the samples. It is observed that DC conductivity increases with increase in temperature showing the organic semiconducting nature of doped poly (m-toluidine).     

间甲苯胺改性双氰胺固化环氧树脂的DSC研究

采用化学改性合成的间甲苯胺改性双氰胺衍生物作为环氧树脂潜伏性固化剂，通过差示扫描量热法（DSC）研究了间甲苯胺改性双氰胺／环氧树脂E-44体系的固化反应。结果表明，间甲苯胺改性双氰胺与双氰胺相比，具有较高的固化反应活性，显著降低了固化反应的温度，而且间甲苯胺改性双氰胺／环氧树脂E-44体系也具有较好的贮存稳定性。同时间甲苯胺改性双氰胺／E-44环氧树脂体系的动力学研究也表明该固化体系的活化能明显降低，固化反应活性与未改性前相比，有很大程度的提高。     

重氮化-水解法合成间甲酚的工艺研究

间甲酚是一种重要的精细化工中间体,以间甲苯胺为原料,采用重氮化-水解法制备高纯度间甲酚,通过正交实验和单因素实验对重氮化反应工艺条件进行了优化。实验结果表明该反应的最佳反应条件为：硫酸与间甲苯胺的摩尔比为2.8：1,硫酸溶液浓度为35wt%,采用顺式加料法滴加27wt%的亚硝酸钠溶液,加料时间为40min。在最佳条件下重复实验,间甲酚收率可达85.2%,纯度99.5%。采用GS-MS对其结构和含量进行了表征。     

电化学-微米电喷雾-质谱技术用于间甲苯胺电化学氧化机理研究

本实验开发了电化学-微米电喷雾-质谱技术(EC-mESI-MS),采用微米毛细管作为电化学电解池和电喷雾离子源,内置两根铂金丝分别作为工作电极和辅助电极,通过连接自制的电化学工作站,同时向样品溶液中施加电化学反应电压和电喷雾电压,实现电化学反应的实时、在线质谱分析.基于该技术研究了间甲苯胺(m-toluidine)的电...     

Self-Assembly of Methyl Substituted Polyaniline Hollow Nanospheres in a Polyelectrolyte Solution

Hollow nanospheres of poly(m-toluidine), poly(o-toluidine), and poly(N-methylaniline) were successfully prepared in a solution of poly(methyl vinyl ether-alt-maleic acid) by using ammonium persulfate as the oxidant. The polymerization processes of methyl substituted aniline were monitored by recording pH and temperature changes of the reaction medium. The experimental results showed that the substitution position of methyl group affected the characteristics of formed hollow nanospheres. The formation mechanism of such hollow nanospheres was suggested. The produced hydrophobic oligomers self-assembled at the interface of water/droplet of monomers and acted as the soft template for the formation of hollow spheres.     

Cr-Cu硅胶催化间硝基甲苯气相制备间甲苯胺

用固定床反应器作为气相加氢装置,将自制Cu硅胶催化剂用于间硝基甲苯催化加氢制备间甲苯胺的反应。通过考察Cu含量以及助剂N i、Co、Cr、Mn对催化剂性能的影响,筛选出催化性能最佳的Cr-Cu硅胶催化剂。分析了各反应因素对间甲苯胺产率的影响:当反应时间1.5 h,反应温度270℃,氢气与间硝基甲苯摩尔比为9∶1时,间甲苯胺的产率达到最大值99.4%,此时Cr-Cu硅胶催化剂的最大负荷为1.1 mL/(h.mL-cat.),满足工业化应用水平。目前该工艺的中试生产线正在805厂调试中。     

双氰乙基偶氮化合物的合成及表征

用无水AlCl3催化问甲苯胺与丙烯腈的加成反应,合成了偶合组分N,N-二氰乙基间甲苯胺,并分别与重氮组分对硝基苯胺、对硝基邻氯苯胺、2,4-二硝基-6-氯苯胺和2,4-二硝基-6-溴苯胺进行偶合反应,合成了4种双氰乙基偶氮化合物.结果表明,生成的偶氮化合物产率分别为72%、78%、91%和81%,含量均超过96%;而且...     

Comparative studies of electrochemically deposited poly(o-toluidine) and poly(m-toluidine) films

Under galvanostatic deposition conditions poly(o-toluidine) exhibits a higher rate of polymerization than poly(m-toluidine). This observation is supported by results obtained by different characterization techniques such as spectrophotometry, scanning electron microscopy and thermogravimetric analysis. The monomer concentration was found to be the predominant parameter in obtaining selectively a conducting salt phase in both cases. However, the morphology of these polymeric films does not reveal any particular relationship with monomer concentration; instead a mixed morphology, i.e. a combination of granules and fibres, is observed. Finally, the thermal stability of poly(m-toluidine) is lower than that of poly(o-toluidine) with a shift of 190°C in the final decomposition temperature.     

间甲苯胺改性双氰胺的合成及固化性能研究

通过间甲苯胺与双氰胺的反应,合成了化学改性的双氰胺衍生物,研究了反应的合成工艺,并用熔点测定、红外光谱法对反应前后双氰胺的结构进行了分析比较.间甲苯胺改性双氰胺对环氧树脂E-44的固化实验结果表明,这种固化剂具有较好的固化性能,复配制成的单组分间甲苯胺改性双氰胺/环氧树脂E-44体系具有良好的贮存稳定性.