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.     

Ca0.85Bi0.10Cu3Ti4O12陶瓷的介电性能研究

利用固相反应法制备了Ca0.85Bi0.10Cu3Ti4O12 （BCCTO）高介电陶瓷材料.通过X射线衍射、介电频谱、阻抗谱和I-V特性曲线等测试,研究了不同烧结时间对BCCTO陶瓷结构和介电性能的影响.研究发现不同烧结温度的BCCTO陶瓷均为立方相钙钛矿结构,随烧结时间的延长其介电常数和非线性特性均有明显提高,样品表现出明显的Maxwell-Wagner （M-W）弛豫特征,表明样品中包含半导型的晶粒和绝缘层,这种IBLC结构对其介电和I-V特性都有重要贡献,延长烧结时间可以显著增强M-W弛豫特性.     

二氨基二苯醚型聚酰亚胺材料阻尼性能及研究进展

有机高分子材料聚酰亚胺是耐高温的航空航天材料,且其隔热性可保护不耐高温的材料在高温环境下不被破坏,其应用已成为航空航天新复合材料领域的研究热点。综述了近年来不同结构聚酰亚胺（PI）的动态力学性能的研究进展,重点介绍了含二氨基二苯醚（ODA）结构的聚酰亚胺,指出并说明了聚酰亚胺作为阻尼材料应用的可能性。     

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.     

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.     

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.     

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。     

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.     

含氟杯[4]芳烃离子盐LB膜及二元羧酸阴离子识别研究

合成了含氟杯[4]芳烃离子盐化合物1,利用表面压一面积(π-A)等温线、压缩/扩张循环等温线与膜稳曲线、紫外与红外光谱等手段研究了该化合物在空气/水相界面、空气/二元羧酸水溶液界面的成膜性能及阴离子识别。结果表明:化合物1在水或者二元羧酸水溶液的亚相表面均能很好地形成稳定的Langmuir膜,在界面能识别二元羧酸阴离子,并能转移到固体基片上形成LB膜,形成的LB膜为H-聚集体。