共查询到19条相似文献,搜索用时 109 毫秒
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本文对2-氨基-9,9-二甲基芴的合成工艺进行研究。由芴为起始原料,通过选择不同的合成方法,改变反应条件,确定最佳的合成工艺。反应产物通过高效液相色谱检测其纯度,通过核磁共振确定结构,所得产物均与目标化合物相符。 相似文献
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由Cadogan反应,2-硝基联苯在有机磷试剂存在下,硝基被还原成环得到咔唑类化合物得到启发,设计两步反应,第-步邻溴硝基苯与9,9-二甲基2-芴硼酸为原料经Suzuki偶联反应,甲苯中回流,得到芴与2-硝基苯的C—C偶联化合物;第二步Cadogan环化反应,三苯基膦还原2-(2-硝基苯)-9,9-二甲基芴得咔唑。这-设计重点在于合成咔唑的同时成功地引入了芴核,新合成的化合物通过共用苯环而包含了咔唑和芴。尽管用Cadogan反应还原2-(2-硝基苯)-9,9-二甲基芴时有两种关环可能,但该方法仍然简单有效,易于控制。副产品包括三苯基氧化膦和咔唑异构体12,12-二甲基-11,12-二氢茚[2,1-al咔唑非常容易通过柱层析除去。 相似文献
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本文研究了双胺芴合成方法以及不同条件对反应的影响,探讨了不同酸盐的催化效果、催化剂用量、苯胺用量、反应温度、反应时间等因素对双胺芴产率的影响。实验结果表明,当n(苯胺):n(PhNH2?HCl):n(芴酮)=10:1.5:1时,控制反应温度在130 ℃,反应6小时,双胺芴的产率最高为88.3%。 相似文献
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C2-Symmetric 9,9′-spirobifluorene-containing polyesters (PEs) were synthesized by polycondensation of 2,2′-dihydroxy-9,9′-spirobifluorene (1) with bis(acyl chloride)s (2) at 230 °C in diphenylether. The molecular weights of PEs 3a-3f were sufficiently high (Mw 13,400-41,600). PEs displayed high thermal stability. The glass transition temperatures (Tg) estimated by differential scanning calorimetry analysis appeared in a range 177-352 °C depending on the spacer structure, while the 5% decomposition temperatures (Td5) measured by thermogravimetric analysis were over 416 °C both under nitrogen atmosphere and in air. PEs showed good solubility in typical organic solvents such as CHCl3 and THF easily to afford the tough, transparent, and flexible cast films. The transmittance of the polymer films reached over 90% in the wavelength range from ca. 410-900 nm. In addition, PEs exhibited higher refractive index rather than that of commercially available 9,9-diarylfluorene-containing PE, in addition to very low degree of birefringence presumably due to the C2-symmetric structure. 相似文献
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Ordered arrays of conjugated poly(9,9‐dihexylfluorene) (PF) were prepared by the spinodal dewetting of liquid thin films on mica substrates. The size of the aggregates in the arrays was controlled by the evaporation rate of the solvent. Fast solvent evaporation resulted in smaller aggregates; slower evaporation resulted in larger aggregates. The photoluminescence of the PF arrays showed a smaller red‐shift than that of the unpatterned film when compared to PF solutions, which indicated that the aggregation of PF in the arrays is smaller than that in the unpatterned films. Copyright © 2004 Society of Chemical Industry 相似文献
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磷钨杂多酸催化合成双酚芴的研究 总被引:1,自引:0,他引:1
应用磷钨杂多酸催化合成双酚芴,考察了催化剂用量、反应时间、温度、酚酮摩尔比等条件对反应的影响;结果表明,双酚芴的单程收率达65.3%。最佳工艺条件为:酚酮摩尔比10:1,反应温度115℃,反应时间11h,催化剂用量占总物料的9%。 相似文献
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Shou‐Ri Sheng Chun‐Xin Ma Jian‐Wen Jiang Zhen‐Zhong Huang Cai‐Sheng Song 《应用聚合物科学杂志》2010,116(3):1650-1659
Two novel monomers, 9,9‐bis[4‐(4‐carboxyphenoxy)phenyl]xanthene (BCAPX) and 9,9‐bis[4‐(4‐aminophenoxy)phenyl]xanthene (BAPX) were prepared in two main steps starting from nucleophilic substitution of 9,9‐bis(4‐hydroxyphenyl)xanthene (BHPX) with p‐fluorobenzonitrile and p‐chloronitrobenzene, respectively. Using triphenyl phosphite and pyridine as condensing agents, two series of polyamides containing xanthene cardo groups with the inherent viscosities (0.82–1.32 dL/g) were prepared by polycondensation from BCAPX with various aromatic diamines or from BAPX with various aromatic dicarboxylic acids in an N‐methyl‐2‐pyrrolidone (NMP) solution containing dissolved calcium chloride, respectively. All new polyamides were amorphous and readily soluble in various polar solvents such as N,N‐dimethylformamide (DMF), NMP, N,N‐dimethylacetamide (DMAc) and pyridine. These polymers showed relatively high glass transition temperatures between 264 and 308°C, decomposition temperatures at 10% weight loss ranging from 502 to 540°C and 488 to 515°C in nitrogen and air, respectively, and char yields at 800°C in nitrogen higher than 56%. Transparent, flexible, and tough films of these polymers cast from DMAc solutions exhibited tensile strengths ranging from 86 to 109 MPa, elongations at break from 13 to 22%, and initial moduli from 2.15 to 2.63 GPa. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 相似文献
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The thermodynamics of the alpha (α) phase to beta (β) phase transition was investigated in solution of poly(9,9′-dioctylfluorene) in a variety of solvents with UV-vis absorption spectroscopy, differential scanning calorimetry, fluorescence spectroscopy, atomic force microscopy, and near-field scanning optical microscopy. The results show that the solvent quality has a strong affect on the α- to β-conformational change. The trend in enthalpies and transition temperatures indicates that the transition results from an increase in intramolecular interactions upon chain collapse at lower temperatures. This transition leads to subsequent gelation and/or aggregation that stabilizes the β-phase at higher temperatures and leads to a large hysteresis in the transition temperature. The enthalpy for the transition from an aggregated β-phase to a fully solvated α-phase is found to be 21.04 kJ mol−1 of monomer for toluene solutions. Differences between the measured heat and those previously reported are discussed. 相似文献
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Mingliang SUN Li WANG Yangjun XIA Bin DU Ransheng LIU Yong CAO 《Frontiers of Chemical Engineering in China》2008,2(3):257-264
A series of narrow band-gap conjugated copolymers (PFO-DDQ) derived from 9,9-dioctylfluorene (DOF) and 2,3-dimethyl-5,8-dithien-2-yl-quinoxalines
(DDQ) is prepared by the palladium-catalyzed Suzuki coupling reaction with the molar feed ratio of DDQ at around 1%, 5%, 15%,
30% and 50%, respectively. The obtained polymers are readily soluble in common organic solvents. The solutions and the thin
solid films of the copolymers absorb light from 300–590 nm with two absorbance peaks at around 380 and 490 nm. The intensity
of 490 nm peak increases with the increasing DDQ content in the polymers. Efficient energy transfer due to exciton trapping
on narrow-band-gap DDQ sites has been observed. The PL emission consists exclusively of DDQ unit emission at around 591–643
nm depending on the DDQ content in solid film. The EL emission peaks are red-shifted from 580 nm for PFO-DDQ1 to 635 nm for
PFO-DDQ50. The highest external quantum efficiency achieved with the device configuration ITO/PEDOT/PVK/PFO-DDQ15/Ba/Al is
1.33% with a luminous efficiency 1.54 cd/A. Bulk heterojunction photovoltaic cells fabricated from composite films of PFO-DDQ30
copolymer and [6,6]-phenyl C61 butyric acid methyl ester (PCBM) as electron donor and electron acceptor, respectively in device
configuration: ITO/PEDOT:PSS/PFODDQ30: PCBM/PFPNBr/Al shows power conversion efficiencies of 1.18% with open-circuit voltage
(V
oc) of 0.90 V and short-circuit current density (J
sc) of 2.66 mA/cm2 under an AM1.5 solar simulator (100 mW/cm2). The photocurrent response wavelengths of the PVCs based on PFO-DDQ30/PCBM blends covers 300–700 nm. This indicates that
these kinds of low band-gap polymers are promising candidates for polymeric solar cells and red light-emitting diodes.
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Translated from Acta Polymerica Sinica (China), 2007, 10: 952–958 [译自: 高分子学报] 相似文献
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Stable pure‐blue emission of poly(9,9‐dioctylfluorene) via suppression of the green emission
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Stable pure‐blue electroluminescence (EL) is obtained from polymer light‐emitting devices by dispersing poly(9,9‐dioctylfluorene) (PFO) into a wide band‐gap mixed‐matrix of poly(9‐vinylcarbazole) (PVK):2‐(4‐biphenylyl)‐5‐(4‐tert‐butylphenyl)‐1,3,4‐oxadiazole (PBD). From the EL spectra of the PFO‐doped films, we find that the additional green emission observed in the EL spectra of the pure PFO devices was significantly suppressed in the PFO‐doped devices. The spectral stability was also improved through evaluating the EL spectra of the PFO‐doped films annealed at different temperatures (from 80 to 150 °C). These results demonstrate that doping of PFO into a matrix to weaken the aggregate and oxidation of the PFO molecules is a simple strategy to suppress the green emission. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44950. 相似文献