对氟苯甲醛的合成研究

本文对氟苯甲醛的合成路线进行了深入研究,得到优化的工艺条件.选定氟化反应温度为210℃,物质的量n（对氯甲苯）∶n（KF）∶n（环丁砜）∶n（催化剂）为1∶1.5∶0.2∶0.05来合成对氟甲苯.对氟甲苯侧链氯化后分离出二三氯化物直接用90％硫酸水解得到对氟苯甲醛.对氟苯甲醛综合收率77％,副产物为对氟苯甲酸.     

制备(R)-2,2-二甲基四氢噻唑4-羧酸-L-酒石酸盐的新方法

发展了一种制备(R)-2,2-二甲基四氢噻唑4-羧酸-L-酒石酸盐(D-DMT·L-TA)的新方法,可以以73.0%的收率以及99%的光学纯度得到产品.     

生物滤池处理微污染原水中氨氮及“氮亏损”影响因素分析

为探讨饮用水生物滤池对NH4+-N去除和"氮亏损"现象的影响因素,测定生物滤池进出水中NH4+-N,NO2--N,NO3--N等指标.结果表明,陶粒生物滤池对NH4+-N的去除率从14.97%到60.99%,活性炭生物滤池对NH4+-N的去除率从16.59%到83.02%;陶粒和活性炭滤池对NH4+-N的去除率都随着流速的增加而降低;陶粒滤池内NH4+-N的去除率随着气水比和C∶N的增加而先增加后下降;NH4+-N的去除率在活性炭滤池内随C∶N的增加而降低,气∶水的增加而增加;气∶水对两种生物滤池中NH4+-N去除的影响最大.陶粒生物滤池氮亏损的量从0.10 mg/L到0.70 mg/L,活性炭生物滤池氮亏损量从0.11 mg/L到1.01 mg/L;氮亏损量随着流速增加而降低,随着气水比增加而增加,随着C∶N的增加而先下降后增加;气水比对陶粒和活性炭生物滤池的氮亏损量影响最大.     

回流法制备MnFe_2O_4纳米晶及磁性能

以NaOH为沉淀剂,通过一种简单的低温回流法制备了MnFe2O4纳米晶.采用XRD、SEM、FESEM、FTIR和VSM等手段对MnFe2O4纳米晶尺寸、晶相结构和磁性能进行了分析表征.结果表明,所制备的MnFe2O4纳米晶为尖晶石相结构,晶粒尺寸随着反应温度的升高而增大,从50℃的10 nm增大到90℃的22 nm;样品的饱和磁化度随温度的升高而增大.     

Crystal structures,antibacterial activity and thermal decomposition kinetics of lanthanide complexes with 4-chloro-2-methoxybenzoic acid and 1,10-phenanthroline

A series of lanthanide complexes [Ln(4-Cl-2-MOBA)3phen]2(Ln=Sm(1), Nd(2), Ho(3), Eu(4), Dy(5), and Tb(6); 4-Cl-2-MOBA=4-chloro-2-methoxybenzoate, phen=1,10-phenanthroline) were synthesized and characterized. The single-crystal X-ray diffraction demonstrates that 1–3 are isomorphous, which present dimeric structures with four 4-Cl-2-MOBA anions function as bridging ligands. Complexes 1 and 4–6 display their characteristic luminescence emission bands of central Ln3?ions. The heat capacities, the thermodynamic functions and the thermogravimetry–Fourier transform infrared spectra of gaseous products of complexes 1–6 were investigated.Their non-isothermal kinetics of the second decomposition stage was studied by the integral isoconversional non-linear method and Stark method. Furthermore, 1–6 exhibited excellent antibacterial activity against Candida albicans,Escherichia coli and Staphylococcus aureu.     

1,2-C_2H_4BrCl分子光解离机制的理论研究

采用考虑了旋轨耦合的从头算方法计算研究了1,2-C2H4BrCl的光解.计算了1,2-C2H4BrCl分子的若干电子态的垂直激发能.用MS-CASPT2/CASSI-SO方法计算了1,2-C2H4BrCl分子C-Br解离的势能曲线.根据计算结果清晰地指认了1,2-C2H4BrCl分子的解离通道:C2H4Cl+Br(2P3/2)和C2H4Cl+Br*(2P1/2).     

智能聚合物包覆型纳米氧化铁的催化性能

针对非均相Fenton反应效率偏低及pH值适应范围窄的问题,设计以智能聚合物调节纳米铁氧化物表面性能.通过原位共沉淀法合成纳米四氧化三铁,并将其表面健合的羧甲基纤维素钠与单体丙烯酸接枝共聚生成具有pH值响应性能的环境敏感聚合物来包覆氧化铁,形成复合纳米颗粒(PAA-co-CMCNa/Fe3O4),研究了复合材料的催化性能.结果表明:pH值在3~7的宽范围内,该复合纳米材料均可在30,min内将210,mg/L的苯酚完全去除,催化降解苯酚的矿化率高达75%,并显示良好的稳定性和重复使用性能,这是由于聚合物层在该范围内的选择性溶胀既有助于纳米磁性材料的分散稳定,又能改善界面传质,从而促进非均相催化反应.     

高速逆流色谱(盐溶液体系)分离制备白芍中的芍药苷

建立应用高速逆流色谱分离纯化芍药中的芍药苷的方法。以正丁醇-乙酸乙酯-5%Na2SO4(4:1:5,V/V)为两相溶剂体系,在流速为2.0 mL/min、主机转速为800 r/min、检测波长为254 nm的条件下进行分离,从100 mg芍药粗提物中一次性分离制备得到56.13 mg芍药苷,高效液相色谱分析其纯度在98%以上,通过质谱、核磁共振氢谱和核磁共振碳谱鉴定化合物的结构。该方法简便、快捷且重现性好,适合芍药苷的制备型分离。     

Joining of Si3N4 ceramic using PdCo(Ni SiB)–V system brazingfi ller alloy and interfacial reactions

The wettability of V-active PdCo-based alloys on Si3N4ceramic was studied with the sessile drop method. And the alloy of Pd50.0–Co33.7–Ni4.0–Si2.0–B0.7–V9.6(wt%),was developed for Si3N4ceramic joining in the present investigation. The rapidly-solidified brazing foils were fabricated by the alloy Pd50.0–Co33.7–Ni4.0–Si2.0–B0.7–V9.6. The average room-temperature three-point bend strength of the Si3N4/Si3N4joints brazed at 1453 K for 10 min was 205.6 MPa,and the newly developed braze gives joint strengths of 210.9 MPa,206.6 MPa and 80.2 MPa at high temperatures of 973 K,1073 K and 1173 K respectively. The interfacial reaction products in the Si3N4/Si3N4joint brazed at 1453 K for10 min were identified to be VN and Pd2Si by XRD analysis. Based on the XEDS analysis result,the residual brazing alloy existing at the central part of the joint was verified as Co-rich phases,in which the concentration of element Pd was high up to 18.0–19.1 at%. The mechanism of the interfacial reactions was discussed. Pd should be a good choice as useful alloying element in newer high-temperature braze candidates for the joining of Si-based ceramics.     

纳米结构9Cr-ODS钢的微观结构及对氦泡形成的影响

以采用机械合金化和热等静压法制备的纳米结构9Cr-ODS钢为研究对象,利用高分辨率透射电镜和扫描透射电镜的高角环形暗场像等手段分析了9Cr-ODS钢的微观结构特征;利用400keV离子加速器向9Cr-ODS钢及无ODS的Eurofer97钢中注入4×1017/cm2氦离子,对比了氦泡尺寸.结果表明:纳米结构9Cr-ODS钢的平均晶粒尺寸约05μm,存在两种尺寸不同的析出相:超高密度弥散分布的纳米尺度Y2Ti2O7析出相和倾向于在晶界形成的尺寸较大的Mn(Ti)Cr2O4析出相.ODS钢中的氦泡尺寸明显小于Eurofer97钢,说明纳米析出相对粗大氦泡的形成有明显的抑制作用.