多代超支化水性聚氨酯的合成及表征

以甲苯-2,4-二异氰酸酯(TDI)、二羟甲基丙酸(DMPA)和二乙醇胺(DEOA)为原料通过偶合单体反应法合成了一系列不同代数的超支化水性聚氨酯(HPU),通过红外光谱(FT-IR)和核磁共振波谱（NMR）对其结构进行了表征,利用三检测器的凝胶渗透色谱(GPC3)测定各代产品分子量,采用热重分析仪(TG)和示差扫描量热仪(DSC)对各代HPU及类似化学组成的线性水性聚氨酯(LPU)的热性能进行测试分析对比,结果表明,合成各代HPU产率最高可达91%;TG分析表明各代数HPU与LPU具有相近的初始分解温度,大约在200℃左右,但各代HPU与LPU的分解历程明显不同;DSC结果表明各代HPU产品的玻璃化温度(Tg)明显高于LPU,同时随着代数增高,Tg逐步由115.2℃升高到150.3℃;对比各代HPU掺杂涂膜发现,随代数的增加,光泽度和硬度明显提高。     

Ag2S或CuS掺杂的Zn0.5Cd0.5S纳米晶体：溶剂热法合成及光致发光性能

以异丙醇为溶剂,醇热法制备Zn_0.5Cd_0.5S和Ag₂S或CuS掺杂的Zn_0.5Cd_0.5S纳米晶体,考察了这些纳米晶体在可见光区域的光致发光性能。结果表明,反应温度和反应时间、掺杂剂的浓度和种类对Zn_0.5Cd_0.5S的发光性能有很大的影响,相比未掺杂Zn_0.5Cd_0.5S纳米晶体而言,Ag₂S或CuS掺杂后其光致发光强度明显增强、半高宽更宽。     

室温下制备Cu7S4和Ag2S的球形空心纳米粒子

以Cu₂O和Ag₂O纳米粒子为前驱体,利用Kirkendall效应,在室温条件下制备出Cu₇S₄和Ag₂S的球形空心纳米粒子。用X-射线衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)等测试手段对产物进行了表征。结果表明,粒子的空心化程度取决于反应物的物质的量之比;空心粒子的形貌与前驱体粒子的形貌很相似。研究了这种反应的机理,并对这两种氧化物发生这类反应的难易程度作了理论探讨。     

双键可控紫外光固化超支化聚氨酯丙烯酸酯的制备与表征

以甘油为核,二乙醇胺(DEOA)和异佛尔酮二异氰酸酯(IPDI)为原料,合成了含6个端羟基的加核型超支化聚氨酯(HBPU-OH),再通过加入IPDI和丙烯酸羟乙酯(HEA)等原料引入聚氨酯基团和丙烯酸双键,制备出加核型双键数目可调的紫外光(UV)固化超支化聚氨酯丙烯酸树脂(HBPUA).用傅里叶交换红外光谱和核磁共振波谱表征了HBPUA的结构,用示差扫描量热仪和热重分析仪研究了HBPUA的热性能.结果表明,合成了超支化结构的HBPUA;HBPUA玻璃化转变温度(T_g)为67.8℃,低于HBPU-OH的T_g(110.0℃),这是由于HEA的引入增加了分子的柔性;HBPU-OH和HBPUA的热分解均出现3个阶段.     

超支化聚酯的合成与应用——纳米银粒子的制备与表征

超支化聚酯的合成与应用——纳米银粒子的制备与表征;超支化聚酯;纳米银;稳定剂;光还原     

钨硅酸银纳米晶：形貌可控合成与表征

通过聚电解质(表面活性剂)作为导向剂的液相合成路线，合成了多种形貌的多金属氧酸盐纳米晶，包括纳米球，纳米带，纳米片，纳米立方体，六角纳米粒子，三角纳米粒子，雪花状纳米粒子。形状独特的六角形空心纳米粒子也通过相似的方法合成出来。在反应过程中，银离子通过配位作用吸附在聚电解质的组装结构上，通过与氮原子或氧原子的配位作用被定位在聚电解质上，从而导致规则形貌的多酸纳米粒子的形成。结果表明，产物的形貌极大地取决于表面活性剂的组装结构和它们与反应物间的配位作用。     

Synthesis and Characterization of Silicone Modified Polyurethane Surfactant Useable at High Temperature

A series of novel silicone modified polyurethane (Si-PU) surfactants were successfully synthesized by using hydroxypropyl-terminated polydimethylsiloxane (HPMS), polyethylene glycol (PEG), dimethylolpropionic acid (DMPA) and isophoronediisocyanate (IPDI). The chemical structure of the surfactant was confirmed by FTIR and ¹H-NMR. TEM photographs showed that the micelles of the Si-PU surfactants dispersed in aqueous solution were spherical with the particle size in the range of 100–400 nm. Surface tension measurements indicated that these surfactants had low surface tension to 29.9 mN·m^?1and a definite critical micelle concentration to, approximately 5.0×10^?4–7.5×10^?4mol·L^?1. When the content of HPMS was 20 wt%, the surfactant's, emulsifying performance was superior to the traditionally available Span80/Tween80 mixed emulsifiers. In addition to that, no phase transition temperature was detected from 20°C to 90°C by fluorescence probe and DSC measurements, confirming the high thermal stability of the micelles.     

亚微米级Ag2S空心球的乳液法合成

Hollow Ag₂S spheres have been prepared via hydrolyze reaction of Ag₂S₂O₃， which formed from the reaction of AgNO₃ with Na₂S₂O₃， in cyclohexane/water/polyglycol emulsion system. It was found that the component of the reaction system has a significant influence on the formation of hollow Ag₂S spheres. The possible formation mech-anism of the hollow Ag₂S spheres in the emusion system was also discussed.     

超支化聚酰胺的合成与表征

N-(二氨基苯甲酰)氨基乙酸;自缩聚;封端反应;超支化聚酰胺的合成与表征     

超支化聚合物为模板Ag纳米簇的制备

超支化聚（胺-酯）;Ag纳米簇;模板合成     

PCDL型超支化水性聚氨酯的合成与性能

以甲苯-2,4-二异氰酸酯（TDI）、聚碳酸酯二醇（PCDL）、二羟甲基丙酸（DMPA）和二乙醇胺（DEOA）为原料,采用A₂＋bB₂共聚合路线合成了具有超支化结构的水性聚氨酯（HBAPU）乳液。采用红外光谱（FT-IR）、核磁共振（13C NMR）对产物结构进行了表征,证实了超支化聚氨酯的支化度随 n(NCO)/n(OH)比值的增大而增大。用PCS、TG、电子拉力机对产物的性能进行了测试,同时也对胶膜的耐水性进行了测试,发现在DMPA含量为0.4 mmol/g时,HBAPU的粒径仅有20.57 nm,而线性水性聚氨酯粒径有130.91 nm,并且HBAPU具有良好的耐水性、热稳定性和较高的拉伸强度。     

Synthesis and Characterization of Crosslinked Hyperbranched Polyglycidol Hydrogel Films

Hyperbranched polyglycidol (PGLD) was synthesized via anionic ring‐opening polymerization of glycidol using a special anionic initiator with multiple initiation sites. The resultant polymers were characterized by ¹H and ¹³C‐NMR spectra for confirming their structures, which consisted of linear, hyperbranched and dendritic structures. Molecular weight characteristics were determined by means of the gel permeation chromatography (GPC). With the intention of investigating the possibility of broad applications, PGLD hydrogel films were prepared using various crosslinking agents, i.e., glutaraldehyde and some dicarboxylic acids, and their physical properties such as swelling behavior and tensile (or Young's) modulus were measured and compared.     

纳米ZnO脱硫剂表面结构与室温脱除H2S性能的研究

采用均匀沉淀法制备纳米ZnO，经260 ℃，360 ℃，460 ℃和550 ℃焙烧制备的纳米ZnO均具有六方纤锌矿结构，平均粒径分别为14.3 nm，21.2 nm，24.1 nm和35.3 nm。通过TEM、TPR、XRD和XPS等技术对脱硫剂进行了表征。结果表明，纳米ZnO提高了对H₂S的室温去除率，室温脱除H₂S的活性时间是分析纯ZnO的近40倍；其脱硫性能随粒径增大，氧空位减少而下降，脱硫后高结合能的硫物种增多，硫取代晶格氧的趋势增大。说明粒径大小和氧空位是纳米ZnO室温脱硫的主要影响因素。纳米ZnO(14.3 nm)可直接将H₂S选择氧化为单质硫，尾气中未见SO₂产生。     

超支化聚氨酯阻尼涂层的制备及性能

以甲苯-2,4-二异氰酸酯(TDI)和二乙醇胺(DEOA)为原料, 采用一步法合成了超支化聚氨酯, 并对其改性制备了光固化超支化聚氨酯(UV-HPU)和超支化杂化聚氨酯(HHPU)两种树脂. 用傅里叶红外光谱(FTIR)和核磁共振氢谱(1H NMR)表征了预期产物. 以其为预聚物制备阻尼涂层, 动态力学分析(DMA)研究表明, 这两种涂层都具有高阻尼因子(tanδ≥1.0)、宽阻尼温度范围(tanδ≥0.5, 大于50 ℃)和宽阻尼频率范围(20～160 Hz); 通过基本性能测试和热重分析(TGA)发现杂化涂层聚氨酯较光固化聚氨酯具有更好的机械性能和热稳定性能; 杂化涂层聚氨酯的FTIR分析可知杂化涂层中硅氧烷水解缩合, 提高了交联密度; 杂化材料的断面扫描电镜(SEM)分析表明, 硅氧烷的水解缩合并未形成大颗粒纳米粒子而是形成均相体系.     

Synthesis of Crystalline Nanosized Titanium Dioxide via a Reverse Micelle Method at Room Temperature

Crystalline TiO2 nanoparticles were synthesized by hydrolysis of titanium tetrabutoxide in the presence of hydrochloric acid in Np-5(lgepal CO-520)/ cyclohexane reverse micelle solution at room temperature.Pure rutile nanoparticles were obtained at an appropriate acid concentration.The influences of various reaction conditions such as the concentration of acids,water content value (2=[H2O]/[Np-5]) on the formation,erystal phase,morphology,and size of the TiO2 particles were investigated.     

Infrared spectra of Ag2BrNO3 and Ag2ClNO3

The infrared spectra of Ag₂BrNO₃ and Ag₂ClNO₃ are reported. Vibration assignments are proposed on the basis of the group theoretical analysis and D_2h symmetry. Factor group, site and TO-LO splittings are observed. The internal and external mode frequencies are correlated with those of AgNO₃ and KNO₃(II).     

碲化银纳米晶的室温合成及表征

在室温下制备了碲化银纳米粒子,制备过程中选用了新型的还原剂多聚甲醛。所得产物用X射线光电子能谱、X射线粉末衍射和透射电镜进行了表征。     

Ag3PO4/Ag2S/g-C3N4复合光催化剂的制备与性能

通过沉积法和离子交换法成功地制备了Ag_3PO_4/Ag_2S/g-C_3N_4复合型光催化剂。利用X射线多晶粉末衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、N_2吸附-脱附等温线、紫外-可见漫反射光谱、荧光光谱等手段对样品进行了表征。通过降解罗丹明B考察其可见光催化活性及稳定性,研究了硫化钠与磷酸银物质的量的比值(n_(Na_2S)/n_(Ag_3PO_4))、g-C_3N_4添加量对所制备复合光催化材料性能的影响,同时对光催化机理进行了探讨。结果表明,随着n_(Na2S)/n_(Ag3PO4)的增加,所得复合催化材料活性先增加后降低;当n_(Na2S)/n_(Ag_3PO_4)为1.5%、g-C_3N_4与Ag_3PO_4的质量比为3∶7时制备的催化剂ASC1.5的光催化活性最好,在可见光照射下,40 min内可将罗丹明B完全降解,且5次循环使用后仍保持较高的催化活性。和Ag_3PO_4相比,Ag_3PO_4/Ag_2S/g-C_3N_4复合型光催化材料的活性与稳定性都得到明显提高,这主要归因于复合催化剂比表面积和孔结构的增加,载流子分离效率的提高。光催化机理研究表明,空穴(h~+)、超氧阴离子自由基(·O~(2-))和羟基自由基(·OH)都是光催化过程中的主要活性物种。三者作用大小依次为:h~+·O~(2-)·OH。     

Ag2S/Ag3PO4/Ni复合薄膜的制备及其光催化性能

采用电化学方法制备Ag₂S/Ag₃PO₄/Ni复合薄膜,以扫描电子显微镜（SEM）、X射线衍射（XRD）、紫外-可见漫反射光谱（UV-Vis DRS）对薄膜的表面形貌、晶相结构、光谱特性及能带结构进行了表征,以罗丹明B为模拟污染物对薄膜的光催化活性和稳定性进行了测定,采用向溶液中加入活性物种捕获剂的方法对薄膜的光催化机理进行了探索。结果表明：最佳工艺制备的Ag₂S/Ag₃PO₄/Ni是由均匀的球形纳米颗粒构成的薄膜,其光催化活性明显优于纯Ag₃PO₄/Ni薄膜和纯Ag₂S/Ni薄膜,且在保持薄膜光催化活性基本不变的前提下可循环使用6次。提出了可见光下Ag₂S/Ag₃PO₄/Ni复合薄膜光催化降解罗丹明B的反应机理。     

水热法合成多孔Ag_2S敏化二氧化钛催化剂及其可见光催化活性(英文)

Porous Ag2S sensitized TiO2 catalysts were synthesized by the hydrothermal process.The crystallization and porous structure of the Ag2S/TiO2 composite photocatalysts were investigated by X-ray diffraction,scanning electron microscopy with energy dispersive X-ray analysis,UV-Vis diffuse reflectance spectroscopy,and N2 adsorption.The Ag2S/TiO2 composites were mainly composed of anatase TiO2 and acanthite Ag2S.The absorption edge wavelengths of TiO2 and the Ag2S/TiO2 composite prepared with 3 mmol Na2S.5H2O were 400 and 800 nm,respectively,that is,the absorption edge of the composite had a pronounced red shift.The photocatalytic activity under visible light was investigated by the degradation of methylene blue with a UV-Vis spectrophotometer.The photocatalytic activities under visible light of the Ag2S/TiO2 photocatalysts were much higher than that of TiO2.