异佛尔酮二胺的合成及工艺优化

以异佛尔酮为原料,经氰化、亚胺化和氢化三步反应合成了异佛尔酮二胺,并对反应工艺条件进行了优化。中间产物异佛尔酮腈合成的优化实验条件:NH4Cl为酸化试剂、DMF为反应介质、0.0669 mol异佛尔酮和0.048 mol Na CN与5 m L浓度为6 mol·L-1的NH4Cl水溶液在70℃下反应4 h,得异佛尔酮腈,收率为94.9%。中间产物异佛尔酮亚胺合成的优化实验条件为:以Ca O为催化剂、氨压0.2 MPa、70℃反应4 h,异佛尔酮腈转化率为97.4%,异佛尔酮亚胺收率为87.6%。异佛尔酮二胺合成的优化实验条件为:温度120℃、氢压6 MPa、氨压0.2 MPa、催化剂为2.0 g Raney Co,反应8 h后,异佛尔酮亚胺的转化率为100%,异佛尔酮二胺的收率为95.6%。另外,对中间产物和终产物分别进行了IR、MS、1H-NMR等分析,确认其结构无误。     

金刚烷胺/氧化石墨烯复合材料的制备及其吸附性能

以氧化石墨烯和金刚烷为原料，通过水相合成法制备了金刚烷胺功能化氧化石墨烯复合材料A/GO，以FT-IR、XRD和XPS对A/GO进行了结构表征，并考察了A/GO对有机染料的吸附性能。结果表明，与氧化石墨烯相比，A/GO对甲基蓝（AB93）表现出高效吸附性，其吸附动力学和吸附等温模型分别符合拟二级动力学和Langmuir模型，理论最大吸附容量（qm）为1250.0 mg/g。热力学分析表明，A/GO吸附AB93是自发的放热过程。A/GO吸附AB93对盐（NaCl和KCl）表现出良好的耐盐性，而CaCl2能有效地促进A/GO吸附AB93。对于刚果红和AB93等的混合染料体系，A/GO能选择性吸附AB93。     

抗水耐磨道路标线漆的研制

以有机硅改性丙烯酸树脂为基料 ,选用耐磨颜填料 ,设计出适宜的颜基比和溶剂体系 ,研制出抗水、耐磨的道路标线漆 ,改善了常温溶剂型道路标线漆存在的弊病     

Synthesis of 2-Methyl-4-methoxyaniline from o-Nitrotoluene Using Pt/C and Acidic Ionic Liquid as Catalyst System

2-Methyl-4-methoxyaniline (MMA) was synthesized by one-pot method through the hydrogenation and Bamberger rearrangement of o-nitrotoluene in methanol using acidic ionic liquid and 3% Pt/C as catalyst system. The effects of ionic liquid type, dosage of ionic liquid and 3% Pt/C, reaction temperature and reaction pressure on o-nitrotoluene conversion and MMA selectivity were investigated. The results indicated that the imidazolium-based acidic ionic liquid which contains SO₃H-functionalized cation showed higher selectivity to MMA than other acidic ionic liquids used in this work. Using 1-(propyl-3-sulfonate)-3-methylimidazolium hydrosulfate ([HSO₃-pmim][HSO₄]) as the acid catalyst, the selectivity to MMA was as high as 67.6% at 97.8% of o-nitrotoluene conversion. As 3% Pt/C increased from 0.01 g to 0.025 g, the selectivity to MMA decreased from 73.4% to 62.5%, because of the hydrogenation of intermediate o-methyl-phenylhydroxylamine to o-toluidine becoming more dominant. An increase in hydrogen pressure also had obviously dramatic effect in lowering the MMA selectivity. After easy separation from the products, the catalyst system could be reused at least 3 times.     

载体对镍催化剂催化间二硝基苯加氢制间苯二胺反应性能的影响

The hydrogenation of m-dinitrobenzene to m-phenylenediamine in liquid phase was studied with the nickel catalysts supported on SiO2, TiO2, γ-Al2O3, MgO and diatomite carders. Based on the experiments of X-ray diffraction （XRD）, X-ray photoelectron spectroscopy （XPS）, temperature-programmed reduction （TPR）, temperature-programmed desorption of hydrogen （H2-TPD） and activity evaluation, the physico-chemical and catalytic properties of the catalysts were investigated. Among the catalysts tested, the SiO2 supported nickel catalyst showed the highest activity and selectivity towards m-phenylenediamine, over which 97.3% m-dinitrobenzene conversion and 95.1% m-phenylenediamine yield were obtained at 373K under hydrogen pressure of 2.6MPa after reaction for 6 h when using ethanol as solvent. Although TiO2 and diatomite supported nickel catalysts also presented high activity, they had lower selectivity towards m-phenylenediamine. As for γ-Al2O3 and MgO supported catalysts were almost inactive for the object reaction. It was shown that both the activity and selectivity of the catalysts were strongly depended on the interaction between nickel and the support. The higher activities of Ni/SiO2, Ni/TiO2 and Ni/diatomite could be attributed to the weaker metal-support interaction, on which Ni species presented as crystallized Ni metal particles. On the other hand, there existed strong metal-support interaction in Ni/MgO and Ni γ-Al2O3, which causes these catalysts more difficult to be reduced and the availability of Ni active sites decreased, resulting in their low catalytic activity.     

Au-Ru/TiO2催化硝基苯和苯甲醛一锅法合成N-苄基苯胺

采用沉积-沉淀法制备出一系列Au-Ru/TiO2双金属催化剂,用于硝基苯与苯甲醛一锅法加氢反应合成N-苄基苯胺。考察了Ru负载量对Au-Ru/TiO2加氢性能的影响,并采用X射线衍射和扫描电镜等方法对催化剂进行表征。结果表明,Au和Ru产生协同作用共同促进加氢作用。负载Ru质量分数为1.5%的催化剂具有最好的加氢活性和N-苄基苯胺选择性。优化的N-苄基苯胺合成工艺条件为：催化剂用量占硝基苯质量的15%,溶剂为甲苯,氢压1.1 MPa,反应温度80 ℃。此条件下,硝基苯转化率100%,N-苄基苯胺选择性88.2%     

Ni-Fe/C催化剂制备及其催化苯酐选择性加氢制苯酞

以NaBH4对疏水活性炭进行处理,采用等体积浸渍法制备疏水活性炭负载掺杂助剂Fe的Ni基催化剂,用于苯酐液相选择性加氢制苯酞,考察Ni含量和活性炭处理对催化剂性能的影响。结果表明,疏水活性炭经NaBH4处理后制备的15%Ni-Fe/C催化剂对苯酐加氢表现出很好的催化性能,在180 ℃、4.0 MPa、苯酐5.0 g、催化剂用量以Ni占原料质量的1%计和甲苯50 mL条件下,苯酐转化率为100%,苯酞选择性为95.2%,催化剂重复使用5次,仍保持很好的活性和选择性。     

BSB-1型失步保护装置剖析

在发电机及系统出现失步的情况下 ,利用失步保护装置 ,能够根据振荡中心的位置 ,有选择地解列电网中失去同步的部份 ,使机组和电网安全运行。文中介绍了失步保护判据的构成及发电机失步与构成判据的各阻抗轨迹之间的关系。最后着重介绍了失步保护的整定计算 ,为其在大机组上安全有效的运行提供了重要的理论依据。     

苯甲腈非均相加氢制备苄胺的研究进展

苄胺作为一类重要的精细化工中间体，广泛应用于医药、农药、染料、树脂、橡胶等领域。苯甲腈加氢还原是制备苄胺最简便、最符合原子经济性的方法。本文综述了近年来非均相催化剂用于苯甲腈加氢制苄胺的研究进展，重点阐述了金属组分、催化剂载体、氢源、添加剂等因素对催化性能的影响，并对其未来发展进行展望。     

湖北十堰“雨点纹”绿松石的谱学特征研究

“雨点纹”是绿松石中具有类似雨滴状饱和颜色的特征图案。本文以产自湖北省十堰市的“雨点纹”绿松石为样品，利用常规宝石学测试、X射线粉晶衍射、拉曼光谱和红外光谱、电子探针等方法对样品的宝石学性质、物相组成和化学成分等方面进行分析探讨。实验结果显示，“雨点纹”绿松石样品整体为蓝绿色调，雨滴状图案无规律分布其中。本文研究的“雨点纹”绿松石与标准绿松石谱学特征相近，EMPA结果表明Cu和Fe元素为绿松石的主要致色元素。基底和“雨点纹”部分的主要矿物均为绿松石。