新型(口恶)二唑类衍生物的合成及荧光光谱分析

为了开发高强度的有机电致发光材料,在吡唑的1位上引入苯基以及苯并噻唑基,在3位上引入芳基,在4位上引入醛基.用一步法合成了1,3,4-(口恶)二唑,并通过Wittig反应将(口恶)二唑与4、甲酰基吡唑相连合成了6种未见报道的(口恶)二唑类化合物,用红外光谱、质谱、核磁共振谱和元素分析对合成化合物进行了结构表征.用荧光光...     

2,5-二[4-(4-溴苯氧基亚甲基)苯基]-1,3,4-噁二唑的合成与表征

以对甲基苯甲酸、水合肼为原料,通过关环、溴化、醚化合成了一种新型含噁二唑功能基有机聚合物电致发光材料单体2,5-二[4-(4-溴苯氧基亚甲基)苯基]-1,3,4-噁二唑,其化学结构由红外光谱仪及核磁共振氢谱仪进行了表征,产品总收率22.64%.     

新型燃烧合成方法制备α-Fe2O3纳米晶

将聚乙烯醇(PVA)作为络合剂与硝酸铁反应,不调节反应体系的pH值成功地制备出α-Fe2 O3纳米晶。络合物在150℃反应后的产物灰烬经X射线分析,含有部分α-Fe2O3和γ -Fe2O3,产物灰烬经400℃煅烧1.5h后得到的是α-Fe2O3和γ-Fe2O3的混合物,X射线衍射和红外光谱分析的结果显示,此时有机组分已分解完全。在450℃煅烧1 . 5h,γ-Fe2O3全部转变为α-Fe2O3,经透射电镜观察晶粒尺寸在25～35 nm之间,且为球形,在500℃的温度下煅烧得到的产物晶粒比450℃煅烧产物晶粒稍有长大,在25 ～40nm之间。     

Lewis酸/碱络合催化剂对(口,恶)唑烷酮合成的研究

采用不同类型的催化剂对双酚A环氧树脂与甲苯二异氰酸酯合成聚(口,恶)唑烷酮(POX)的反应进行了研究.反应产物用红外光谱跟踪检测.重点考察了路易斯酸/碱络合物催化剂的类型、制备方法、络合比及催化剂的用量等对(口,恶)唑烷酮(OX)成环反应的影响.实验结果表明,由AlCl3·HMPA3组成的路易斯酸/碱络合催化剂对OX环的合成显示出极好的催化活性.且采用溶剂法(B)制备的催化剂其反应活性优于非溶剂法(A)制备的催化剂,催化剂最佳的L-酸/L-碱的配比为1/3,催化剂的含量为1%(反应物).     

聚对苯撑苯并二(口恶)唑原纤化纳米纤维制备技术及结构性能

聚对苯撑苯并二(口恶)唑(PBO)纤维是一种具有多重原纤结构的高分子聚合物.通过机械力作用可以使PBO纤维发生原纤化,制备具有直径小于100 nm的PBO原纤化纳米纤维.文中对PBO纤维发生原纤化的历程及机理进行研究,扫描电镜观察发现PBO纤维的原纤化过程包括:脱除皮层、主干破坏、进一步原纤化等阶段,剥离和劈裂是原纤化的主要方式.经过原纤化处理的PBO纤维,呈现不同尺寸纤维组成的多分散体.打浆度70°SR的PBO原纤化纳米纤维的直径可达到50 nm,其保水值118％,纤维长度分布主要集中在0.3～0.5 mm,比表面积21.89 m2/g.以PBO原纤化纳米纤维为原料,通过湿法成形方式在抄纸系统上制备的纸基材料力学性能随着原纤化程度增加而增加.     

用MBO(口恶)唑啉合成LDPE/PS合金相容剂及其对合金的增容作用

采用１,３－双－（恶唑啉基）－苯为偶联剂通过反应性加工实现ＰＳ－ｇＭＡｎ和氯化聚乙烯之间反应方法来合成ＬＤＰＥ／ＰＳ共混体系相容剂,在ＬＤＰＥ／ＰＳ共混体系中加入１０％此相容剂,其冲击强度提高２．３倍,拉伸强度和弯曲强度也有所提高。通过ＳＥＭ、ＤＭＡ和ＤＳＣ分析表征表明加入此相容剂后,ＬＤＰＥ／ＰＳ共混物的相容性有显著改善。     

聚(芳基醚1,3,4-噁二唑)类聚合物的合成及表征

为改善芳香族聚噁二唑的加工性,合成了一种含噁二唑的双氟单体,将其与二酚单体进行溶液缩聚,得到一系列含有醚键与C(CH3)2,CCH3C6H5等官能团的新型聚(芳基醚1,3,4-噁二唑)(PEOD),其黏度达1.0 dL/g,噁二唑成环率达100%,并通过核磁氢谱(1H-NMR)和元素分析(EA)证实了其化学结构。通过热重分析(TGA)对PEOD的热稳定性进行了表征,结果表明,这些聚合物具有优良的热性能。通过溶解性试验表明PEOD能够溶解于三氯甲烷(CHCl3)、二氯甲烷(CH2Cl2)、四氢呋喃(THF)等有机溶剂,其溶解性比聚对苯撑噁二唑(p-POD)及对间苯噁二唑(p/m-POD)有了较大的改善。     

[1,3,4]-噁二唑衍生物的固相合成及其线性、非线性光谱性质

用固相法合成了2个噁二唑衍生物类有机化合物:5-(4-叔丁基苯基)-[1,3,4]噁二唑-2-苯乙烯基-4-苯基-二苯胺 (化合物1)与9-乙基-3,6-双{5-(4-叔丁基苯基)-[1,3,4] 噁二唑-2-苯乙烯基}-咔唑 (化合物2),并测定了它们的吸收光谱、单光子荧光光谱和双光子荧光光谱.化合物1和2在二氯甲烷溶液中单光子荧光发射峰分别位于519和476nm.在锁模Nd∶YAG激光器800nm激光照射下,化合物1和2发射出很强的双光子上转换荧光,其最大波长分别在520和485nm.     

1,4-二(叠氮乙酰氧基)-2,3-二(叠氮乙酰氧甲基)-2,3-二硝基丁烷的合成

以2,3-二羟甲基-2,3-二硝基-1,4-丁二醇为原料经酯化和叠氮化两步反应合成了1,4-二(叠氮乙酰氧基)-2,3-二(叠氮乙酰氧甲基)-2,3-二硝基丁烷(BDAA),总收率为68.8%。采用1H NMR和IR对目标产物及中间体的结构进行了表征。分别采用甲苯和二甲苯两种溶剂进行酯化反应,发现二甲苯为该反应的较优溶剂;通过对催化剂硫酸﹑磷酸和对甲苯磺酸的比较,得出对甲苯磺酸为该酯化反应的较优催化剂;通过对叠氮化反应的讨论,确定了四丁基溴化铵为该反应较优相转移催化剂。DSC分析表明,BDAA的分解峰温为206.44℃。TG分析表明,BDAA的热分解可能分两步进行,在500℃时,尚未分解完全。     

主链插入苯并二(口恶)唑环的PPV聚合物的合成及其光电性质

以对氰基氯苄和4,6-二氨基间苯二酚为主要原料,首先合成2,6-二(4-氯甲基苯基)苯并[1-2,4-5']二(口恶)唑,又通过2,6-二(4-氯甲基苯基)苯并[1-2,4-5']二(口恶)唑与对苯二甲醛的Wittig反应,设计合成了一种新的主链插入苯并[1-2,4-5']二(口恶)唑环的PPV聚合物(BO-PPV),通过红外光谱、核磁共振谱、凝胶渗透色谱等分析方法对其结构进行了表征.并研究了该聚合物的光电热物理特性,结果表明:该聚合物的Tg为235℃,Td为410℃,电致发光谱峰值λmax为494 nm,由ITO/BO-PPV/A1组成的单层器件在电压15伏特,发光亮度可达650 cd/cm2,发光效率0.24cd/A.     

Electrical conduction mechanisms in thermally evaporated thin films of 2-(4-biphenylyl) -5-(4-tert-butylphenyl) -1,3,4-oxadiazole

The AC electrical behaviour of sandwich devices fabricated entirely in vacuum using thermally evaporated thin films of 99+% pure 2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1,3,4 oxadiazole (Bu–PBD) and gold electrodes, is observed over the frequency range 10⁴ to 10⁷ Hz and the temperature range 297 to 398 K. The capacitance and dissipation factor decrease with increasing frequency and at high frequency (>2×10⁶ Hz) the capacitance and dissipation factor are not temperature dependent. The results obtained show the relative importance of the variable range hopping model and band theory in describing the film conductivity.     

Organic light-emitting diodes with 2-(4-biphenylyl)-5(4-tert-butyl-phenyl)-1,3,4-oxadiazole layer inserted between hole-injecting and hole-transporting layers

Organic light-emitting diodes (OLEDs) were fabricated based on copper phthalocyanine (CuPc) (hole-injecting layer), N,N′-bis(1-naphthyl)-N,N′-diphenyl-1,1′-biphenyl-4,4′-diamine (NPB) (hole-transporting layer) and tris(8-hydroxyquinoline) aluminum (Alq₃) (emission and electron-transporting layer). A 2-(4-biphenylyl)-5(4-tert-butyl-phenyl)-1,3,4-oxadiazole (PBD) layer was inserted between CuPc and NPB. The effect of different thickness of PBD layer on the performance of the devices was investigated. The device structure was ITO/CuPc/PBD/NPB/Alq₃/LiF/Al. Optimized PBD thickness was about 1 nm and the electroluminescent (EL) efficiency of the device with 1 nm PBD layer was about 48 percent improvement compared to the device without PBD layer. The inserted PBD layer improved charge carriers balance in the active layer, which resulted in an improved EL efficiency. The performance of devices was also affected by varying the thickness of NPB due to microcavity effect and surface-plasmon loss.     

聚-1,3,4-噁二唑纤维研究进展

介绍了聚-1,3,4-噁二唑(POD)的合成、改性、纺丝成形、后处理及耐老化等方面的研究进展。详述了采用一步法三阶段合成POD,并通过引入间苯二甲酸和对苯二甲酸进行共聚改性,得到的POD纤维在亲水性、抗静电性、染色性能等方面得到了改善;探讨了凝固浴条件对POD纤维结构与性能的影响,阐述了POD纤维的老化降解及防护问题。     

Adsorption and corrosion inhibition effect of 2-((5-mercapto-1,3,4-thiadiazol-2-ylimino)methyl)phenol Schiff base on mild steel

In this study, the inhibition effect of 2-((5-mercapto-1,3,4-thiadiazol-2-ylimino)methyl)phenol Schiff base (MTMP) on mild steel corrosion in 0.5 M HCl solution was studied. For this aim, electrochemical techniques such as potentiodynamic polarization curves, weight loss (WL), electrochemical impedance spectroscopy (EIS) and linear polarization resistance (LPR) were used. It was shown that, the MTMP Schiff base has remarkable inhibition efficiency on the corrosion of mild steel in 0.5 M HCl solution. Polarization measurements indicated that, the studied inhibitor acts as mixed type corrosion inhibitor with predominantly control of cathodic reaction. The inhibition efficiency depends on the concentration of inhibitor and reaches 97% at 1.0 mM MTMP. The remarkable inhibition efficiency of MTMP was discussed in terms of blocking of electrode surface by adsorption of inhibitor molecules through active centers. The adsorption of MTMP molecules on the mild steel surface obeys Langmuir adsorption isotherm.     

聚合物光伏电池材料MEH-PPV的超声合成及其表征

研究了聚[2甲氧基-5-(2'-乙基己氧基)对苯乙炔](MEH-PPV)的合成路线.采用超声合成法制备出无凝胶、完全可溶、高分子量的MEH-PPV.其教均分子量可达7.9×105,并通过红外光谱、核磁共振氢谱(1H-NMR)、拉曼光谱对产物进行了结构袁征.     

Electro-optical properties of poly(1-(difluorophenyl)-2-(4-alkylcyclohexyl phenyl)acetylene) organic light-emitting diodes

For organic light-emitting diodes (OLEDs) applications, we have investigated novel polymers, using substituted polyacetylenes (PA), poly(1-(fluorophenyl)-2-(alkylcyclohexylphenyl)acetylene) (PDPA-nF) (n = 1 or n = 2) which exhibit air stability, better solubility in common organic solvent and higher luminescence than polyacetylene. In this study, we have used poly[(1-(3,4-difluorophenyl)-2-(4-pentylcyclohexylphenyl)acetylene)] (PDPA-2F) as an emitter in OLEDs and their performance was determined by measuring the current-voltage-luminance characteristic. The devices have a maximum brightness of 827 candela (cd)/m² at 12 V and a maximum current efficiency of 0.78 cd/A at 9 V with a maximum luminescence at 536 nm. Influence of the metal electrode on the charge injection was studied using several cathode configurations (Ca, Al and Au) for the devices. Furthermore, the charge injection and transport processes were correlated to the presence of traps inside the polymer, determined by deep level transient spectroscopy (DLTS).     

Charge injection into poly[methyl(phenyl)silylene]

Space-charge-limited currents have been measured in thin films of poly[methyl(phenyl)silylene] provided with Al and hole-injecting ITO electrodes. Electroluminescence observed at high voltages was interpreted as being due to a double injection. The thermo-modulated space-charge-limited current technique has been employed to determine the structure of traps in the low-voltage (single-injection) regime.