一种烷氧基取代聚对苯乙炔三元共聚物的合成与性能

采用强碱诱导的脱氯化氢缩合聚合法合成一种可溶性不对称烷氧基取代聚对苯乙炔三元共聚衍生物聚[2-甲氧基-5-(3′-甲基)丁氧基对苯乙炔-co-2-甲氧基-5-己氧基对苯乙炔-co-2-甲氧基-5-辛氧基对苯乙炔][P(MOMBOPV-co-MOHOPV-co-MOCOPV)]。研究表明,三元共聚物在三氯甲烷中具有良好的溶解性,利于成膜,其在400 nm~560 nm存在显著吸收,最大吸收波长位于500 nm处。热性能研究表明,其热稳定性良好,起始分解温度约为370℃,玻璃化温度为95℃。荧光光谱研究表明,P(MOM-BOPV-co-MOHOPV-co-MOCOPV)具有优良的光致发光性能,其最大发射波长为645 nm,荧光寿命为1.3 ns。     

聚对苯乙炔二元共聚物P(DHOPV-co-MOBOPV)的制备与性能

采用强碱诱导的脱氯化氢缩合聚合法合成一种可溶性烷氧基取代聚对苯乙炔二元共聚物聚(2,5-二己氧基对苯乙炔-co-2-甲氧基-5-丁氧基对苯乙炔)[P(DHOPV-co-MOBOPV)].研究表明,P(DHOPV-co-MOBOPV)在可见光区具有较强吸收,其最大吸收波长位于500 nm;当双氯苄物质的量比为l:1和6:...     

含四嗪单元的聚对苯撑乙炔类聚合物的合成及性能

通过Sonogashira偶联反应,以二(三苯基膦)二氯化钯作为催化剂,将3,6-二氯-1,2,4,5-四嗪分别与1,4-二乙炔基-2,5-二辛氧基苯和1,4-二乙炔基-2,5-二(十二烷氧基)苯交替共聚合成了主链中含四嗪单元的新型聚对苯撑乙炔类π-共轭聚合物P1、P2。经傅里叶变换红外光谱、核磁共振氢谱、紫外-可见光谱、荧光光谱、循环伏安、X射线粉末衍射、热重分析等测试手段对共聚物P1、P2进行了表征。结果表明,所得聚合物P1和P2对常用有机溶剂的溶解性不好。与P2相比,P1有一定的结晶性。P1、P2的紫外-可见最大吸收波长均在450nm处出现。P1与P2在CHCl3溶液中的最大发射峰出现在480nm处。与2-十二烷基-1,2,3-苯并三氮唑聚对苯撑乙炔类聚合物相比,P1、P2具有较高的相对荧光量子效率。循环伏安测试显示聚合物P1、P2均在0~2.0V出现明显的p-掺杂峰。     

含2-异丙基氨基-4,6-二(3,4-乙撑二氧噻基)-1,3,5-三嗪π-共轭聚合物的合成及性能

以二价钯配合物作为催化剂,将2-异丙基氨基-4,6-二(2′-溴-3,4-乙撑二氧噻基)-1,3,5-三嗪分别与1,4-二乙炔基-2,5-二辛氧基苯、1,4-二乙炔基-2,5-二(十二烷氧基)苯、2,7-二(4,4,5,5-四甲基硼烷基)-9,9-二辛基芴交替共聚合成了3种π-共轭聚合物P1,P2和P3。经傅里叶变换红外光谱、氢核磁共振谱、紫外-可见光谱、荧光光谱、循环伏安法、X射线粉末衍射和凝胶渗透色谱等测试手段对其进行了表征,并对聚合物在CHCl3溶液的酸致变色行为进行了研究。结果表明,得到的聚合物在CHCl3中的紫外-可见最大吸收波长分别在443nm和431nm处出现。在CHCl3溶液中聚合物P1,P2和P3最大发射峰分别位于507nm,511nm和543nm,其聚合物薄膜的最大发射波长分别为573nm,557nm和559nm。与P1和P2相比,P3的酸致变色敏感性高于2个数量级。聚合物P1和P2均在-2.0~0V出现n-掺杂峰。聚合物X射线衍射谱图显示聚合物均有一定的结晶性。     

一种含羧基的PPV衍生物的制备与表征

以对甲氧基苯酚和6-溴己酸为原料,经过醚化,溴甲基化以及脱卤化氢反应,成功的合成了一种新型含羧基的聚对苯乙炔(PPV)衍生物材料-聚[2-甲氧基-5(5-羧基戊氧基)对苯乙炔]。通过傅里叶变换红外光谱(FTIR),核磁共振波谱1 HNMR和13 CNMR及紫外吸收分光光谱(UV-Vis)对中间产物及聚合物进行了结构表征,结果表明,所合成的中间产物和聚合物与目标产物的结构一致。     

可溶性聚(2-甲氧基-5-辛氧基)对苯乙炔的制备及性能

通过双醚化反应、氯甲基化反应和强碱诱导的脱氯化氢反应,制备出可溶性聚(2-甲氧基-5-辛氧基)对苯乙炔(PMOCOPV)。利用傅里叶变换红外光谱(FT-IR)、核磁共振谱(1H-NMR)、紫外-可见吸收光谱(UV-Vis)和凝胶渗透色谱(GPC)对PMOCOPV的结构进行表征。研究表明,PMOCOPV在三氯甲烷中具有良好的溶解性,利于成膜。热性能研究表明其热稳定性良好,起始分解温度约为200℃。荧光光谱研究表明,PMOCOPV具有优良的光致发光性能,其最大发射波长为641 nm,荧光寿命为7.5×10-10s。     

聚(2,5-二丁氧基)对苯乙炔的合成、表征及发光性能研究

用强碱诱导的脱氯化氢法合成了发光聚合物聚（2，5－二丁氧基）对苯乙炔（PDBOPV），并与前聚物路线合成法进行了比较。脱氯化氢法具有反应时间短和产率高等优点，而且不需要进行高温处理，有利于相关器件的制备。用紫外、红外光谱和^1H-NMR对聚（2，5－二丁氧基）对苯乙进行了表征，测定了荧光（PL）光谱，讨论了烷氧基取代对聚合物光学性质和可溶性的影响。     

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.     

2种苯并咪唑衍生交替共聚物的合成及性能

以苯并噻二唑作为初始原料,通过Sonogashira、Suzuki反应将4,7-二溴-2-己基-1,3-苯并咪唑单体分别与带有不同烷氧基链的对苯乙炔、9,9-二辛基芴进行交替共聚,得到了聚[2-己基-1,3-苯并咪唑-1,4-二乙炔基-2,5-二辛氧基苯](P1)、聚[2-己基-1,3-苯并咪唑-1,4-二乙炔基-2,5-二(十二烷氧基)苯](P2)和聚[2-己基-1,3-苯并咪唑-9,9-二辛基芴](P3)。采用红外光谱、核磁共振等手段对单体和共聚物的结构进行了表征,利用紫外-可见吸收光谱、荧光量子效率测试和循环伏安法对聚合物的光、电化学性能进行了探讨。结果表明,共聚物P1、P2均在445 nm处出现紫外-可见吸收峰,共聚物P3在376 nm处出现紫外-可见吸收峰。P2、P3共聚物的相对荧光量子效率分别为80%,66.7%,所得共聚物都有较强的荧光性能。P2共聚物在1.3 V处出现氧化掺杂峰,在-1.3 V处出现还原掺杂峰,P3共聚物在0.48 V处出现氧化掺杂峰,0.34 V处出现脱掺杂峰。     

溴甲基化法合成聚[2-甲氧基-5-(2’-乙基己氧基)对苯乙炔]

以对甲氧基苯酚和溴代异辛烷为原料,经醚化、溴甲基化、脱溴化氢反应,成功合成聚[2-甲氧基-5-(2’-乙基己氧基)对苯乙炔](MEH-PPV),其数均分子量为5.7×104。利用傅立叶变换红外光谱(FTIR)、核磁共振波谱(1H-NMR)及紫外可见分光光谱(UV-Vis)对中间产物及MEH-PPV进行结构表征,结果表明,合成的中间产物和MEH-PPV分子结构与文献报道的一致。     

Synthesis and characterization of Rosebengal/folicacid-functionalized multiwall carbon nanotubes

Multiwall carbon nanotubes (MWCNTs) were functionalized with a photosensitizer, rosebengal (RB), and folicacid (FA), an anti-cancer drug simultaneously and individually, which was characterized with various analytical instruments like Fourier Transform Iinfrared (FTIR) spectroscopy, UV–Vis spectroscopy, Thermogravimetric analysis (TGA), Photoluminescence (PL) spectroscopy, X-ray photoelectron spectroscopy (XPS), and Transmission electron microscopy (TEM). FTIR spectra confirmed the chemical modification of MWCNT. The chemical functionalization of MWCNT with RB was further supported by UV–Vis and PL spectra.     

Ruthenium Olefin Metathesis Catalysts Bearing Carbohydrate-Based N-Heterocyclic Carbenes

Ru-based olefin metathesis catalysts containing carbohydrate-derived NHCs from glucose and galactose were synthesized and characterized by NMR spectroscopy. 2D-NMR spectroscopy revealed the presence of Ru-C (benzylidene) rotamers at RT and the rate of rotation was measured using magnetization transfer and VT-NMR spectroscopy. The catalysts were found to be effective at ring-opening metathesis polymerization (ROMP), ring closing metathesis (RCM), cross metathesis (CM), and asymmetric ring opening cross metathesis (AROCM) and showed surprising selectivity in both CM and AROCM.     

Synthesis, characterization and magnetic properties of NiS1+x nanocrystals from [bis(salicylidene)nickel(II)] as new precursor

[Bis(salicylidene)nickel(II)] was used as a precursor to prepare nickel sulfides nanoparticles of average size 20 nm by a chemical process in oleylamine. The products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible spectroscopy (UV-vis) and photoluminescence (PL) spectroscopy. Magnetization measurement indicates that both of the α-NiS and Ni₃S₄ nanoparticles show pramagnetism due to the size effect.     

An effective and scale-up self-assembly route to prepare the rigid and smooth oligo(o-phenylenediamine) microfibers in acidic solution by NaClO2

Oligo(o-phenylenediamine) (OoPD) microfibers were successfully synthesized in acidic solution by mixing o-phenylenediamine (oPD) and NaClO₂ solutions together. As proved by the mass spectroscopy (MS), 1H nuclear magnetic resonance spectroscopy (¹H NMR) and Fourier transform infrared spectroscopy (FTIR), the OoPD is composed of 2,3-diaminophenazine and 2,2’-diaminoazobenzene. Based on the scanning electron microscopy (SEM), these microfibers were observed to be rigid and smooth. However, the smooth microfibers became the saw-like materials when pH value of oPD solution increased. The method used is facile and large-scale.     

纳米羟基磷灰石的预处理及在聚醚醚酮中的分散性

对纳米羟基磷灰石(n-HA)浆料进行了分析和纯化处理,研究了纯化处理后的n-HA在聚醚醚酮(PEEK)中的分散性,进而采用溶液共混法制备了一系列n-HA/PEEK复合材料。结果表明,n-HA原料(浆料)中含有的Ca、Na元素以及碳酸根可通过洗涤除去。XRD、FT-IR以及SEM等分析表明,添加硅烷偶联剂,以聚乙二醇作为分散剂,并采用超声振荡的方法能使n-HA均匀分散在聚醚醚酮(PEEK)中,其中的硅烷偶联剂与n-HA形成了新的键。     

Preparation and characterization of LiNiVO4 powder and non-stoichiometric LiNixVyOz films

Inverse spinel type structured oxide, LiNiVO₄, was synthesized by using solid-state method and the crystalline powder was characterized by Rietveld refinement and X-ray photoelectron spectroscopy. Non-stoichiometric lithium nickel vanadate thin films were prepared by physical vapour deposition technique. The amorphous films were characterized by Rutherford back-scattering spectroscopy (RBS), nuclear reaction analysis (NRA), Auger electron spectroscopy (AES), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) analytical methods. Films crystal growth at various temperatures was also studied by XRD and SEM. The HRTEM analysis of sputtered film shows nanocrystalline domains of NiO and LiNiVO₄ phases with characteristic lattice parameters of the host compound and the results correlate well with the XRD data. Electrochemical properties of the films were discussed.     

Preparation of silica hollow fibers by surface-initiated atom transfer radical polymerization from electrospun fiber templates

Silica hollow fibers were produced by surface-initiated atom transfer radical polymerization (ATRP) from poly(methyl methacrylate-co-vinylbenzyl chloride) (P(MMA-co-VBC)) electrospun fibers combined with sol-gel process and subsequent calcination. Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) were used to characterize the intermediate products and the silica hollow fibers. The resulting silica hollow fibers are of high purity with amorphous morphology. The thickness of the hollow fibers is approximately 0.25 µm.     

Synthesis of tetra-aminophthalocyanine/graphite composites by chemical grafting method for styrene oxidation

1,8,15,22-Tetra-aminophthalocyanine/graphite (ZnTAPc/Gr) composites were prepared by chemical grafting method. The property of styrene oxidation in the presence of tert-butyl hydroperoxide (TBHP) as an oxidant was studied. The prepared catalysts were characterized by UV-Vis spectroscopy (UV-Vis), X-ray diffraction (XRD), infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), Raman spectroscopy, UV-vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The obtained ZnTAPc/Gr composites were employed as catalyst for styrene oxidation in presence of tert-butyl hydroperoxide (TBHP) as oxidant. The results showed that styrene was oxidized efficiently in the ZnTAPc/Gr-TBHP system. The enhancement of the catalytic activity of ZnTAPc/Gr composites was investigated in terms of different oxidation conditions. It was found that the optimum oxidation condition was 0.04 g catalyst, 10 h reaction time and reaction temperature of 100°C. Under this condition, the conversion and the selectivity of styrene oxide was up to 73% and 84%.     

Effect of D-fructose on the in-vitro corrosion behavior of AZ31 magnesium alloy in simulated body fluid

The effect of addingd-fructose to simulated body fluid(SBF) on the corrosion behavior of AZ31 magnesium(Mg) alloy at 37.C and at a pH of 7.4 was studied by potentiodynamic polarization(PDP), electrochemical impedance spectroscopy(EIS), potentiostatic polarization and hydrogen(H2) collecting techniques,Raman spectroscopy technique, scanning electron microscopy(SEM), energy dispersive spectroscopy(EDS), X-ray diffraction(XRD), X-ray photoelectron spectroscopy analysis(XPS) and Fourier transformed infrared(FTIR). The results demonstrated that the addition of fructose enhanced the deposition of phosphates forming thick and compact corrosion products, which inhibited the transmission of aggressive ions into the Mg substrate. As a result, both the anodic dissolution of Mg and negative difference effect(NDE) were suppressed. Thus, the corrosion resistance of AZ31 Mgalloy in SBF was significantly improved.     

Synthesis of Fe3O4@PbS hybrid nanoparticles through the combination of surface-initiated atom transfer radical polymerization and acidolysis by H2S

A versatile approach to fabricate nanoparticles with multiple functionalities through the combined use of both surface-initiated ATRP and acidolysis by H2S techniques was demonstrated. The hybrid nanoparticles exhibited the core-shell structure having the magnetite nanoparticles as the core and the polymethacrylate as the shell with PbS nanoparticles distributing in the shell. The structure and morphology of the synthesized nanoparticles were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The optical and magnetic properties of the nanoparticles were investigated by UV-Vis spectroscopy, photoluminescence spectroscopy and vibrating sample magnetometer (VSM), respectively. It is observed that the absorption and emission behaviors of the Fe3O4@PbS hybrid nanoparticles were seriously influenced by the ATRP time and the reaction time with H2S. The saturated magnetization (Ms) decreased with the increase of ATRP time due to the formation of thicker shells coating on the surfaces of magnetite nanoparticles.