1D-π-A型偶氮苯衍生物合成、表征及其光致变色性能

以4-氨基硝基苯为起始原料,通过溴代、重氮去氨基、硝基还原制备出重要中间体3,5-二溴苯胺,再以3,5-二溴苯胺和3-溴苯胺分别与苯酚衍生物进行重氮偶合反应,合成了10个D-π-A型偶氮苯衍生物,利用FT-IR、NMR、ESI-MS、元素分析和X-单晶衍射等表征方法,确定目标化合物结构,并通过UV-Vis光谱研究了系列目标化合物光致变色性能,测定其光致顺反异构速率常数。研究结果表明,目标化合物表现出显著光致变色性能,顺反异构转变速率常数数量级为10-2~10-3 s-1,异构转变速率快慢主要取决于化合物分子的取代基空间位阻大小。     

联苯型三芳胺空穴传输材料的新合成工艺研究

三芳胺是一种优良的空穴传输材料,在有机电致发光和有机光导领域有着重要应用.目前的合成方法是在氯化亚铜和邻菲哆啉的催化下,以4,4'-二-碘联苯和二芳基胺反应制备.研究了以4,4'-二溴联苯与二苯胺为原料,研究了在醋酸钯、三叔丁基膦的催化作用下合成N,N,N’,N’-四苯基-1,1'-联苯-4,4’-二胺(TPD)的反应.考察了原料配比、反应时间、催化剂用量以及反应温度对产品收率的影响,得到优化工艺条件为二苯胺与4,4 '-二溴联苯的摩尔比为2.5∶1,醋酸钯用量为0.05mmol,在145℃回流反应6h,产品收率为78.89％.在此条件下,用4,4’-二溴联苯分别与3-甲基二苯胺、4-甲基二苯胺反应合成了N,N'N'-二苯基-N,N '-二(3-甲基苯基)-1,1'-联苯-4,4’-二胺(m-TPD)、N,N’-二苯基-N,N’-二(4-甲基苯基)-1,1’-联苯-4,4’-二胺(p-TPD),产品收率分别为75.59％和69.96％.通过比较,新工艺有效地降低了工艺物料平衡图(PFD)类空穴传输材料的合成成本.     

新型三苯胺树枝分子的合成及荧光发射性质

采用Wittig-Horner反应合成了一种新型三苯胺树枝分子1,2,4,5-四{4-{N,N-双{4-{4-[5-(4-叔丁基苯基)-1,3,4-噁二唑-2]苯乙烯基}苯基}氨基}苯乙烯基}苯(TPAB-OXA),并测定了化合物TPAB-OXA在不同溶剂中的紫外吸收光谱、荧光发射光谱及量子产率、荧光寿命.在二氯甲烷中...     

[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.     

四月份部分有机氟产品市场参考价格

产品名称规格型号产地价格 (元 /吨 )2 -氟 -4 -溴苄基溴≥ 99%国产 1 0 0 0 0 0 02 -氟 -4 -溴甲苯≥ 99%国产 90 0 0 0 03 ,4 -二氯三氟甲基苯 无色透明液体 99% 国产面议3 ,5-二硝基 -4 -　氯三氟甲苯 淡黄色晶体国产面议3 ,5-二硝基三氟甲苯≥ 99%国产 4 50 0 0 03 ,5-双三氟甲基　苯胺淡黄色液体 99% 国产面议3 -氨基 -4 -　氟三氟甲苯 ≥ 99%国产 650 0 05-氯 -2 -氨基　三氟甲基苯淡黄色透明液体 98 5% 国产面议氨基三氟甲苯≥ 98%国产 63 0 0 0八氟环丁烷国产面议对氟苯胺 无色透明液体 99% 国产面议对氟苯酚白色结晶 99%国产面议对…     

新型含磷双马来酰亚胺／环氧树脂的合成与性能特征

通过双(3-氨基苯基)苯基氧膦的酰亚胺化制备了一种新型可溶性的含磷双马来酰亚胺单体：双(3-马来酰亚胺基苯基)苯基氧膦(BMIPO)。并用^1H核磁，^13C核磁及傅立叶红外光谱对其结构进行了表征。BMIPO树脂中含有五元酰亚胺环及高密度的苯基，使BMIPO树脂成为一种有着较高的玻璃化温度(Tg)、高起始分解温度及高氧指数的极好的阻燃剂。可以得到任意比例且不存在相分离的均相含磷双马来酰亚胺／环氧／4，4’-亚甲基二苯胺(DDM)固化树脂。由于BMIPO／DDM之间的反应速率比4，4’-双马来酰亚胺基二苯甲烷(BMIM)／DDM大，增大混合树脂中BMIPO／BMIM的比例，也就增加了后固化阶段重新交联的危害性，使得Tg值及热稳定性有所降低。BMI／环氧固化体系的热稳定性较环氧固化体系低，这是由于在BMIPO中引入膦基造成的，但其Tg值和阻燃性都明显比环氧固化体系高。混合物中BMIPO含量越高，阻燃性越好。     

1,1-二(对-二乙氨基苯基)-4-(α-萘基)-4-苯基-1,3-丁二烯的合成及其光电性能研究

以α-溴代萘和苯乙酮为主要原料合成了1-(α-萘基)-1-苯基-3-氯丙烯,该化合物与4,4'-双(二乙氨基)二苯甲酮经Grignard反应,脱水后得到目标产物1,1-二(对-二乙氨基苯基)-4-(α-萘基)-4-苯基-1,3-丁二烯(CT),产品纯度98.86%,收率36.4%.通过质谱与核磁共振对产物的结构进行了表征,并对其进行X-射线单晶衍射分析,确定了分子构型.以Y-TiOPc为电荷产生材料,CT为空穴传输材料制备的功能分离型光导体光导性能参数为:V0=-850V,VR=-20V,Rd=17.5V,E1/2=0.60lx·s,表明CT具有优良的空穴传输特性.     

双偶极半菁衍生物/普鲁士蓝自组装多层膜的制备及紫外光谱性质

合成了双偶极半菁类染料[溴化(E)-1,1'-(3烷-1,3-二基)双(4-甲基吡啶)],通过交替吸附KFeⅢ[FeⅡ(CN)6]和半菁衍生物制备了一种有机自组装多层膜,紫外可见光谱研究证实普鲁士蓝/半菁衍生物多层膜可被均匀沉积至少7层的二维有序结构。     

1-甲基-4-苯基-2(1H)喹啉酮衍生物的合成及表征

以苯丙炔酸与氮甲基苯胺合成的N-甲基-N-苯基-3-丙炔酸胺为原料,通过铁催化氧化、重氮化水解合成了一系列1-甲基-4-苯基-2(1H)喹啉酮衍生物。并对喹啉酮衍生物产物进行质谱、核磁共振氢谱和碳谱的定性及结构表征。此方法路线简单,反应条件温和,合成的各种目标产物产率和纯度较高,实验结果令人满意。     

硫杂芴-三苯胺树枝形分子的合成与电致发光特性研究

选择硫杂芴为π-中心、三苯胺为"枝",合成了新型硫杂芴-三苯胺树枝形分子-2,8-双-[4-三苯胺乙烯基-4',4"-二(三苯胺乙烯基)]硫杂芴(简称STG2),进行了核磁共振谱和质谱表征.以硫芴-三苯胺树枝形分子(简称ST-G2)为发光层,制备了结构为ITO/TCTA/ST-G2/BCP/Mg:Ag的3层发光器件,测试了器件的电致发光性能.该器件在6V开启,12V电压下亮度和效率接近1000cd/m2和0.21m/W.     

Optical humidity sensing characteristics of composite thin films of hydrolysed nafion-dye with a terminalN-phenyl group

By using composite films of hydrolysed nafion and dyes having cyanine or triphenyl structures and with a terminal N-phenyl group, an optical humidity sensor has been fabricated. In the reflection mode, the optical intensity of the absorption peaks which depend on the used dyes decreases with relative humidity. The raising and recovery times are less than 1 min. In dry air, the alkyl amine group reacted with SO₃H of hydrolysed nafion and formed a proton additive. Sorption of water molecules induces the deprotonation of the quaternized ammonium group.     

Triphenyl benzene-bridged fluorescent silsesquioxane: shape-controlled hybrid silicas by hydrolytic conditions

A new silsesquioxane molecule was synthesized, in which triphenyl benzene was connected with three Si(OC2H5)3 groups using three urea groups as the bridge. The molecule could self-assemble through the intermolecular H-bonding among urea groups and pi-pi interaction of triphenyl benzene core in the solution and it could also be transferred into hybrid silicas by hydrolysis. When the non-preorganized silsesquioxane was hydrolyzed, isolated spherical hybrid silica was gained. However, when the silsesquioxane was preorganized before the hydrolyzation uniform interconnected spherical hybrid silica and intertwined nanofibrous one could be generated under acidic and basic conditions, respectively. The photoluminescence (PL) spectra of the obtained hybrid silicas showed that they still kept the emission properties of their precursor silsesquioxane, and the shift of the emission bands was due to the pi-pi interaction of triphenyl benzene in the course of polycondensation.     

具有聚集诱导发光性能的三苯甲醇侧基聚合物的制备及性能

通过Barbier反应合成了乙烯基三苯甲醇,其具有聚集诱导发光(AIE)现象;通过可逆加成-链转移(RAFT)聚合的方法将乙烯基三苯甲醇聚合得到不同相对分子质量的聚(三苯甲醇)乙烯。发现该聚合物表现出不同于小分子的AIE特性,在常温固态或溶液状态下均不产生荧光,但加热至玻璃化转变温度之后,聚合物固体的荧光发射强度明显增强,在溶液中依然不产生荧光。文中针对其特殊发光现象及发光机理进行了初步探究,通过核磁共振氢谱、红外光谱、X射线衍射与热力学表征发现其荧光的变化与激基缔合物有关。     

Demagnetization experiments on some promising new compounds for very low-temperature refrigeration

We have performed demagnetization experiments on spherical specimens of silver chloride-bonded, compacted powders of four different compounds. Pure and lanthanum-diluted cerium magnesium nitrate (CMN) was studied along with two new compounds formed from cerium iodide and antipyrine and from cerium thiocyanate and triphenyl phosphine oxide. The magnetic temperaturesT* were determined from measurements of the magnetic susceptibility perpendicular to the axis of the initial magnetizing field. Both the lanthanum-diluted CMN and the triphenyl phosphine oxide compounds yielded significantly lower values ofT* than that obtained with CMN. The problem of thermal equilibrium within the demagnetized sample is considered.Contribution of the National Bureau of Standards. Not subject to copyright.Based on work performed under the auspices of the National Bureau of Standards and the U.S. Atomic Energy Commission.     

Some promising compounds for adiabatic demagnetization

Measurements of the magnetic specific heat of a complex of cerium (III) iodide and antipyrine and of a complex of cerium (III) thiocyanate and triphenyl phosphine oxide indicate that both materials should produce lower limiting temperatures than cerium magnesium nitrate.Based on work performed under the auspices of the U.S. Atomic Energy Commission.     

亚磷酸三苯酯作为锂离子电池电解液稳定剂的研究

研究了亚磷酸三苯酯(TPPi)作为锂离子电池电解液的稳定剂对电解液稳定性和电化学性能的影响。在锂离子电池电解液中加入0.1%的TTPi通过常温储存、定期进行取样分析检测电解液的物理指标,并且用储存过的电解液和新配制的不含TPPi的电解液分别制作电池进行电化学性能测试,结果表明,TPPi的加入延长了电解液的保质期且对电池的电化学性能没有负面影响。     

Amine promoted, metal enhanced degradation of Mirex under high temperature conditions

In this study, zero-valent metal dehalogenation of mirex was conducted with amine solvents at high temperatures. Mirex was treated with excess amine in sealed glass tube reactors under nitrogen. The amines used were n-butyl amine (l), ethyl amine (l), dimethyl amine (g), diethyl amine (l), triethyl amine (l), trimethyl amine (g) and ammonia (g). The metals used were copper, zinc, magnesium, aluminum and calcium. The most suitable amine solvent and metal were selected by running a series of reactions with different amines and different zero-valent metals, in order to optimize the conditions under which complete degradation of mirex takes place. These dehalogenation reactions illustrated the role of zero-valent metals as reductants, whereas the amine solvents acted as proton donors. In this study, we report that mirex was completely degraded with diethyl amine (l) in the presence of copper at 100 degrees C and the hydrogenated products accounted for more than 94 of the degraded mirex.     

亚磷酸三苯酯扩链制备PBT/PET合金

采用亚磷酸三苯酯(TPPi)作为扩链剂熔融共混制备了聚对苯二甲酸丁二醇酯(PBT)/聚对苯二甲酸乙二醇酯(PET)合金.通过力学性能测试、毛细管流变仪、差示扫描量热法(DSC)研究了TPPi的用量对PBT/PET体系力学性能、流变行为及结晶性能的影响.结果表明,加入TPPi后PBT/PET体系的拉伸强度提高至60MPa...     

含有受阻胺构造的光稳定性复合微粒子的合成

为了制备大分子型受阻胺光稳定剂,利用1,2,2,6,6-五甲基-4-哌啶醇与酸酐在甲苯中进行反应,生成了含有酯基的三级胺盐,用FT-IR及1H-NMR对该胺盐的化学结构进行了鉴定,并利用TG-DTA技术考察其热性质.用该胺盐在甲苯-乙醇混合溶媒中与经胺基类硅烷偶联剂处理过的二氧化硅粉反应,通过共沸蒸馏及在130℃真空干燥得到了含有受阻胺构造的光稳定性复合微粒子,探讨了受阻胺光稳定复合微粒子的合成路径,推测了其反应机理.     

四氯苯醌/三苯磷可控掺杂四取代酞菁铜薄膜材料的导电性能研究

本文通过电化学沉积方法制备了一种四氯苯醌/三苯磷可控掺杂四取代酞菁铜薄膜材料体系,研究了该可控掺杂有机薄膜材料的导电性能.研究结果表明,四取代酞菁铜可控掺杂薄膜材料的电导率,随着温度的升高或掺杂剂浓度的增加而显著增加,其原因是酞菁铜给体与四氯苯醌和三苯基磷等小分子电子受体之间发生了较强的氧化还原作用.