蓝色有机电致发光材料OXD-7的合成及性能

重点研究了蓝色有机电致发光材料OXD-7的合成路线及提高产率的方法,并用自行设计加工的升华提纯装置进行两次OXD-7的升华提纯,可使产物纯度达到99.2%。通过真空镀膜制作出结构为ITO/CuPc/NPB/OXD-7/Alq₃/Mg-Ag/Al的器件,器件采用透明ITO导电玻璃作正极,依次真空蒸镀酞菁铜、NPB、OXD-7、Alq₃、Mg-Ag电极,最后在合金电极上覆盖一层很薄Al膜。膜厚由频率震荡计监测,测试了器件的光电性能以及寿命,研究并讨论了材料的纯度对器件寿命的影响。     

一类(噁)唑啉类化合物的合成及红外光谱分析

以3-碘苯甲酸为原料,在浓硫酸作用下,与乙醇反应制得3-碘苯甲酸乙酯(1),再与80%的水合肼反应制得3-碘苯甲酰肼(2).然后将化合物(2)分别与4-甲基苯甲醛、2-氯苯甲醛、4-氯苯甲醛、4-羟基苯甲醛、2,4-二氯苯甲醛、4-甲氧基苯甲醛、3-硝基苯甲醛、4-硝基苯甲醛、4-二甲氨基苯甲醛反应得到相应的酰腙(3a...     

1-(4-硝基苯)-3-(2-吡嗪)-三氮烯的合成及与锌(Ⅱ)的显色反应

报道了1-（4-硝基苯）-3-（2-吡嗪）-三氮烯（NPPT）的合成及与锌（Ⅱ）的显色反应。在非离子表面活性剂TritonX-100存在下,于pH8.8的KCl,H3BO3-NaOH缓冲介质中,NPPT与锌（Ⅱ）形成4∶1的黄棕色络合物,在465nm处有一最大吸收,表观摩尔吸光系数为3.15×104L·mol-1.cm-1,10mL溶液中,锌（Ⅱ）量在0—0.56μg范围内符合比尔定律。方法用于葡萄糖酸锌口服溶液中微量锌的测定,测定结果与AAS法相符。     

2-(3’,4’-二羧基苯氧基)苯甲酸配体桥联的锌(Ⅱ)配合物的合成、结构及荧光性质

以2-(3’,4’-二羧基苯氧基)苯甲酸(H3DPBA)和1,3-二(4-吡啶基)-丙烷(bpp)为配体,与Zn(Ac)2通过水热反应,获得了一维链状配合物Zn(DPBA)(bpp)。该配合物的一个不对称单元包括一个Zn(Ⅱ)离子,一个DPBA配体和一个bpp配体。Zn(Ⅱ)离子与四个氧原子及一个氮原子配位,其配位数为5。固态配合物在375nm处出现强的发射峰,来自于配体的π~*—π跃迁。与配体的荧光发射光谱比较,配合物的荧光发射峰发生了蓝移,而且配合物的荧光发射强度有大幅度增强。讨论了配合物在常见溶剂中和金属阳离子中的荧光性质。实验结果表明不同有机小分子或不同金属阳离子对配合物的荧光强度有不同程度的影响,有机小分子硝基苯和Fe~(3+)使配合物荧光猝灭,该Zn(Ⅱ)-配合物可用于硝基苯的检测以及水和乙醇体系中Fe~(3+)的检测。     

荷移反应-荧光光谱法测定氟罗沙星

提出了一种基于荷移反应简便可靠地测定氟罗沙星的荧光光谱法,研究了电子受体2,3-二氰-5,6-二氯-1,4-对苯醌(DDQ)与氟罗沙星电子给体之间的荷移反应。实验结果表明,氟罗沙星与DDQ的荷移反应可使氟罗沙星产生显著的荧光增敏效应。其最低检测限为0.1mg·L~(-1),用于片剂中氟罗沙星含量的测定,其回收率为96.6％～99.2％,相对标准偏差为1.9％～2.8％。本文还对荷移反应的机理进行了探讨。     

1-(6-硝基-2-苯并噻唑)-3-(4-硝基苯)-三氮烯与铜显色反应的研究及应用

在TritonX-100表面活性剂存在下,pH为10.0-11.0的Na2B4O7-NaOH缓冲溶液中,1-(6-硝基-2-苯并噻唑)-3-(4-硝基苯)-三氮烯(NBTNPT)与铜生成2:1配合物。配合物的最大负吸收峰是540nm,表观摩尔吸光系数为1.15×105L·mol-1·cm-1。Cu2 的质量浓度在0-360μg/L符合比耳定律。测定铝合金样品中的微量铜,结果满意。     

新型含噁二唑环双元席夫碱的合成与光谱特性

4-硝基苯甲酸与硫酸联氨在H₃PO₄/P₂O₅作用下脱水环化生成2, 5-二(4-硝基苯基)-1,3, 4-噁二唑(1),(1)被Zn/CaCl₂还原为2, 5-二(4-氨基苯基)1,3, 4-噁二唑(2),(2)与芳香醛反应合成8个含噁二唑环的新型双元席夫碱,产率为65%～81%,用1H NMR,FTIR,MS对其结构进行了验证。研究了它们的UV-Vis光谱和荧光光谱,并用循环伏安法测定了其电化学性能。UV-Vis光谱表明：标题化合物没出现噁二唑环和席夫碱单元所对应的特征吸收峰,共轭效应使两个结构的能带发生了部分杂化而形成新的能带结构,在345～357 nm出现最大吸收峰。荧光光谱表明：目标化合物发射强的紫蓝色荧光,在390～407 nm出现最大发射峰。电化学性能表明：电子亲合势为2.36～3.04 eV,离子势为5.35～6.06 eV,除了3a,3h外,它们的电子传输性比常用的电子传输材料PBD(E_A=2.82 eV)优越。此研究为进一步研究其在有机电致发光器件中的应用提供了参考。     

电子传输材料1,3,4-恶二唑衍生物和1,2,4-三唑衍生物的DFT研究

采用密度泛函理论B3LYP方法,对1,3,4噁二唑衍生物和1,2,4三唑衍生物两类电子传输材料在中性、阴离子态和阳离子态下分别进行几何结构优化计算.结果表明,1,3,4噁二唑衍生物的电子传输过程主要是分子内噁二唑上的N→O电子转移,1,2,4三唑衍生物的电子传输过程主要是分子内三唑上N(双键)→N(单键)以及三唑环向与N相连的苯环电子转移.当其苯环上3位被拉电子基团取代后,其电子传输性能提高;而被给电子基团取代后,电子传输性能降低.     

含苯并咪唑环的1, 3, 4-噁二唑衍生物的核磁共振研究

在无水乙醇和KOH 存在下,将2-苯氧甲基苯并咪唑-1-乙酰肼(1)与CS₂反应,合成出了中间体5-(2-苯氧甲基苯并咪唑-1-亚甲基)-2-巯基-1,3,4-噁二唑(2),此中间体再与氯乙酰苯胺反应,得到一种新化合物-N-苯基-2-[5-(2-苯氧甲基苯并咪唑-1-亚甲基)-1,3,4-噁二唑-2-硫基]乙酰胺(3). 采用元素分析、IR及NMR技术确定了新化合物3的结构,并利用2D NMR技术对其trans和cis两种异构体的¹H和¹³C NMR谱带进行了全归属,给出了相应的偶合常数J值以及异构体所占的比例. 实验表明,新化合物3在DMSO中存在着trans和cis两种异构体的互变,并且trans异构体占主导,含量为64.5%, 而cis异构体的含量为35.5%.     

新型荧光试剂1-(8-喹啉)-3-(3,5-二溴吡啶)-三氮烯的合成及其分析应用

将具有荧光特性的8-氨基喹啉与吡啶类试剂结合,首次合成了标题化合物1-(8-喹啉)-3-(3,5-二溴吡啶)-三氮烯(QBPyT).其结构经过元素分析、红外光谱、核磁共振谱证实.研究表明,在碱性介质中,该试剂在λex/λem=248nm/496nm处产生强荧光,并且能被Sb(Ⅲ)荧光增强.基于此,建立了QBPyT测定S...     

PAN基活性炭纤维的表面及其孔隙结构解析

通过氮吸附等温线、Ｘ射线光电子能谱以及扫描电子显微镜（ＳＥＭ）对聚丙烯腈（ＰＡＮ－Ｐｏｌｙａｃｒｙｌｏｎｉｔｒｉｌｅ）－基活性炭纤维（ＡＣＦ－Ａｃｔｉｖａｔｅｄ Ｃａｒｂｏｎ Ｆｉｂｅｒ）的表面和孔隙结构进行了分析，结果表明吸附测量可以提供有关碳质吸附剂的孔结构复杂性；通过ＸＰＳ对ＰＡＮ基ＡＣＦ的表面官能团的种类及含量进行了表征，由ＳＥＭ对ＰＡＮ基ＡＣＦ的表面以及断面的孔隙结构进行直拉观察，提供了     

半胱氨酸在银基底表面吸附机理的拉曼光谱研究

以具有表面增强拉曼散射 (SERS)活性的银镜为基底 ,将半胱氨酸组装到银基底表面 ;主要通过调整氨基酸溶液的pH值控制该组装过程。利用表面增强拉曼散射光谱对半胱氨酸小分子在银基底表面的吸附方式、作用机理进行了详细的探讨和研究。结果表明 ,只有当溶液的pH值接近或高于等电点时 ,半胱氨酸分子才能以 -COO- Ag+形式被有效组装到银基底的表面 ,形成表面带有自由疏基 (-SH)的半胱氨酸单分子膜 ,从而为硒代环糊精以 -S-Se-键形式组装到上述组装体系的表面提供了可能。本文的研究将为利用分子光谱探索含硒酶活性机理和进一步提高酶活性奠定基础。     

Optimum Plasma Surface Treatment of Luffa Fibers

Luffa fiber is a renewable resource material with low cost and that contributes to a healthier ecosystem by its biodegradability. Its natural structure can be considered as a naturally occurring composite consisting mainly of cellulose fibrils imbedded in a lignin matrix. Surface pretreatment is necessary to maximize their potential use. In this work, plasma treatment at atmospheric pressure was carried out on the raw luffa fibers. The orthogonal method was used to optimize the plasma treatment condition. The optimal conditions were obtained at a discharge time of 10 s, power of 110 W, and electrode distance of 6 mm for the system used. The surface characterization of untreated and pretreated luffa fibers was investigated by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermogravimetric (TGA) analysis. The results showed that plasma treatment did not cause significant harm to the fiber integrity and the inner cellulose fibrils were exposed from the lignin matrix. Plasma-treated luffa fibers also showed a slightly better thermal stability than the untreated fibers. Compared with chemical pretreatment, plasma treatment had a significantly shorter duration, no consumption of solvent, and improved the cellulose contents.     

Surface Modification of Ultrahigh-molecular-weight Polyethylene Fibers with Coupling Agent during Extraction Process

Ultrahigh molecular weight polyethylene (UHMWPE) fibers were treated with a coupling agent following the extraction of gel fibers, resulting in modified fibers after subsequent ultra-drawing. The structure and morphology of the modified UHMWPE fibers were characterized and their surface wetting, interfacial adhesion, and mechanical properties were investigated. It was found that the coupling agent was absorbed into the UHMWPE fiber and trapped on the fiber surface. Compared with unmodified UHMWPE fibers, the modified fibers had smaller contact angle, higher crystallinity, and smaller crystal size. The interfacial adhesion and mechanical properties of UHMWPE fibers were significantly improved with increasing coupling agent concentration and gradually reached a plateau value. After treatment with 1.5 wt% solution of a silane coupling agent (γ -aminopropyl triethoxysilane, SCA-KH-550), the interfacial shear strength of the UHMWPE-fiber/epoxy composites was increased by 108% and the tensile strength and modulus of modified UHMWPE fibers were increased by 11% and 37% respectively.     

PAN基碳纤维在表面处理中的拉曼光谱研究

采用激光拉曼光谱研究了PAN基碳纤维在表面处理中的微结构变化,分析了表面处理前后碳纤维的一级拉曼光谱特性。结果表明：拉曼光谱中主要的D峰和G峰的拉曼频移、半高宽以及各个不同拉曼频移位置对应肩峰的积分面积比是表征碳纤维物相结构变化的重要参数。经过不同的表面处理,PAN基碳纤维的一级拉曼光谱参数发生了一定程度变化,D峰和G峰的拉曼峰位向高波数偏移,表征石墨微晶尺寸的R值有所提高,这说明在表面处理后碳纤维的石墨微结构受到刻蚀,微晶尺寸有所减小,石墨微晶的边界活性增大;此外,表征碳纤维结构有序程度和缺陷多少的D峰和G峰的半高宽均有减小,表征无定型碳结构或某种有机官能团的A峰和D″峰的相对积分面积减小,这说明与乱层石墨结构相比,碳纤维中存在的无定型碳结构更容易被刻蚀,经过表面处理之后无定型碳的物相比例减小,这与碳纤维XRD图谱中表观结晶度提高的规律相一致。因此,利用激光拉曼光谱可研究碳纤维物相结构的变化规律。     

染发对头发中重金属含量的影响

化妆品和染发剂是重金属的污染源之一。应用ICP-MS对经常染发的人群头发中的重金属含量与不染发人群作了比较。结果显示,长期染发对头发中的重金属含量有明显影响,但是不同重金属变化不同。染发人群头发中重金属Mn,Fe,Ni,Cu,Cd和Sb含量明显增加,As,Cr,Zn,Ag,Pb和 Hg等重金属含量却明显减少。分析上述结果的原因可能是染发剂中含Mn,Fe,Ni,Cu,Cd和Sb偏多,含As,Cr,Zn,Ag,Pb和Hg等重金属少,而经常染发有可能影响人体对重金属As,Cr,Zn,Ag,Pb和Hg的代谢。     

Numerical Simulation of the Melt Spinning Process of Noncircular Fibers Incorporating Surface Tension

Incorporating surface tension, a mathematical modeling system was established to simulate the melt spinning process of a noncircular fiber. A Newtonian fluid was assumed and an isothermal spinning process was considered. Finite element method was adopted to solve the system. The predicted shape of as‐spun fiber was compared with experiments. It was found that surface tension was a key factor in the spinning process of noncircular fibers, which would greatly change the fiber cross‐sectional shape. Simulation would fail to predict the noncircular fiber shape accurately if surface tension was ignored. The fiber shape change caused by the velocity rearrangement only occurs near the spinneret, but surface tension would keep changing the curvature of the fiber surface along the spinline. Die swell of fiber extrudate during the spinning process was also investigated and it was found that die swelling of fiber extrudate near the spinneret was greatly suppressed by the stretch imposed by a take‐up device, when compared with the free extrusion process.     

侧边抛磨光纤波导传输特性的理论分析

在建立侧边抛磨光纤D型光纤边界条件的基础上,用三维有限差分光束传输法计算和分析了侧边抛磨光纤器件的光功率衰减随光纤的侧边抛磨长度、光纤侧边抛磨后剩余包层的厚度、以及填充聚合物材料折射率三个参量变化的特性.结果表明,侧边抛磨光纤器件的光功率衰减随着抛磨长度的增加而增大;当抛磨长度等于9 mm时,光功率衰减随着剩余包层厚度的增大而单调递减.而当抛磨长度大于9 mm时,剩余包层厚度小于3 μm的范围内,光衰减随着剩余包层厚度的增加出现振荡;当聚合物折射率与纤芯折射率相同时,光功率衰减最大.     

光子晶体光纤接续损耗的理论分析

基于超格子构造法,采用全矢量模型计算了光子晶体光纤的模场半径,由此出发理论分析了光子晶体光纤与普通单模光纤之间接续损耗分别受横向偏移、轴向倾斜以及模场不匹配的影响,给出了光子晶体光纤在部分常用结构参量区域{Λ,d/Λ}内与SMF-28接续损耗的理论值,讨论了光子晶体光纤各结构参量与接续损耗之间的关系。并简要分析了不同结构光子晶体光纤之间的接续损耗。结果表明,接续损耗对横向偏移和轴向倾斜都非常敏感;孔距是决定接续损耗大小最主要的因素;与普通单模光纤接续,当光子晶体光纤的孔距比该单模光纤纤芯半径大一些时,接续损耗比较小;两种不同结构光子晶体光纤之间的接续损耗大小最主要取决于它们孔距的差异。     

The Controllable Surface Morphology of Polyimide (PI) Electrospun Fibers

Electrospun materials have been proposed for application for gas filtration, drug carriers, and tissue engineering. The surface morphology of electrospun fibers is the key for consideration for the above applications, such as pore size on the fiber surface, surface area, and roughness. In this work, we investigated the influence of polymer/solvent properties on soluble polyimide (PI) fibers. The studied PIs included three fluorinated aromatic polyimides containing naphthalene pendant groups. By using various solvents we adjusted the size, shape, and structure of the fibers. As a result, PI electrospun fibers could be achieved with width around 10 μm. The rough and smooth surface morphologies were studied by scanning electron microscopy (SEM). Surface wettability of the electrospun fiber membranes were characterized by contact angle measurement. The contact angles on the electrospun PI fiber mats for water and glycerol were in the range of 137.6°–144.5° and 139.1°–143.6°, respectively. Moreover, the rough fiber surface could make the electrospun fiber membrane possess good adhesive force for liquids. The results suggest that we could widen the application of electrospun membranes through controlling the fiber morphology.