Synthesis, Structure and Adsorption of AIPO-21 Prepared by Cotemplate Method

The phase of AIPO‐21 was hydrothermally synthesized in the reactant system of diethylamine‐RB‐Al₂O₃‐O₅‐H₂O‐C₂H₅OH. The crystals of AIPO‐21 growing in this system crystallizes in monoclinic system, space group P2₁/n with a = 0.8542(4) nm, b = 1.7635(8) nm, c = 0.9082(4) nm, β = 108.234(5)°, V = 1.2993(10) nm³, Z = 4, and the formula is [C₄H₁₀ NH₂]⁺ = [Al₃P₃O₁₂ (OH)]^?. The structure is resolved by the direct method and refined to R1 = 0.0767 and wR₂ = 0.1627 based on 1719 observed reflections with I > 2.0σ (I). An asymmetric unit consists of three PO₄ tetrahedra, one AIO₄ tetrahedron and two AIO₅ trigonal bipyramids. The framework is composed of 3‐D uniform channels along [100], [001] and [101] with eight‐membered oxygen ring windows. The powder sample of the MS was investigated with powder XRD, TG/DTG/DTA and the adsorption of water, methanol, n‐hexane, ethylene, and ethane. The specific property for sieving molecules was observed on the adsorption isotherms, and proves the result of the single crystal structural analysis.     

光诱导聚合制备聚噻吩/二氧化钛复合粒子的结构及光催化性能

通过光诱导噻吩在TiO2的氯仿悬浮液中聚合反应,制备了聚噻吩/二氧化钛(PTh/TiO2)复合粒子,并采用比表面积分析仪、扫描电子显微镜、粒径分析仪、X射线光电子能谱、紫外-可见漫反射光谱和红外光谱对复合粒子进行了表征.结果表明,PTh/TiO2复合粒子上的聚噻吩骨架中S原子与TiO2粒子间存在强相互作用,该复合粒子对...     

苯并咪唑基金属有机骨架/氧化石墨烯复合材料对罗丹明B的吸附

通过对溶剂热“一锅法”合成中碱性溶剂的调整,成功制备了2种形貌不同的Cd(Ⅱ)苯并咪唑基金属有机骨架(Cd-MOF)与氧化石墨烯(GO)的复合材料,利用扫描电子显微镜(SEM)、X射线粉末衍射(XRD)、X射线光电子能谱(XPS)、紫外可见吸收光谱(UV-Vis)和傅里叶红外光谱(FT-IR)对复合材料的结构和性能进行了表征,并研究了其对水中罗丹明 B(rhodamine B,RhB)的吸附性能。结果表明：GO的加入增强了Cd-MOF在水中的稳定性,提高了吸附能力;当溶液pH为3.5,吸附时间为60 min时,吸附率可达约95%。     

苯并咪唑基金属有机骨架/氧化石墨烯复合材料对罗丹明B的吸附

通过对溶剂热"一锅法"合成中碱性溶剂的调整,成功制备了2种形貌不同的Cd(Ⅱ)苯并咪唑基金属有机骨架(Cd-MOF)与氧化石墨烯(GO)的复合材料,利用扫描电子显微镜(SEM)、X射线粉末衍射(XRD)、X射线光电子能谱(XPS)、紫外可见吸收光谱(UV-Vis)和傅里叶红外光谱(FT-IR)对复合材料的结构和性能进行了表征,并研究了其对水中罗丹明B (rhodamine B,RhB)的吸附性能。结果表明:GO的加入增强了Cd-MOF在水中的稳定性,提高了吸附能力;当溶液pH为3.5,吸附时间为60 min时,吸附率可达约95%。     

Synthesis and Structure of PEDOT Prepared through a Modified LB Film Method

Adopting LB film method, an arachidic acid (AA)/PEDOT multilayer LB film and polymerized EDOT monomers in hydrophilic group of LB were chosen to prepare the arachidic acid (AA)/PEDOT multilayer LB film. UV-Vis, FT-IR and XPS analyses implied that EDOT was effectively polymerized in film, and thus PEDOT conducting polymer was produced. Analyses of XRR and SIMS indicated that the film had a well-arranged lamella structure, and further research showed that polymerization of EDOT in AA film destroyed the orderliness of the original LB film. This phenomenon could be related to the destructive effect of polymerization on the layered structure. We used four-point probe and semiconductor instrument to study the conductivity property of the film, and observed that the conductivity of AA/PEDOT film had sudden changes with the changes of processing time in an effective conduction network, which was caused by "permeability" in conducting channel of multilayer film. The test results also indicated that the conductivity of AA/PEDOT film was obviously better than that of spin-coating PEDOT/PSS or ODA-SA/PEDOT-PSS film due to the higher π structure of PEDOT structure and ordered film structure.     

甲醇热还原法制备高分散Cu2O微米立方体及其光催化性能

通过简单的甲醇热还原法制备高分散Cu2O微米立方体,制备过程中无需添加表面活性剂。利用X射线衍射(XRD)、场发射扫描电镜(FESEM)、高分辨透射电镜(HRTEM)、X射线光电子能谱(XPS)等分析测试手段对样品的物相及形貌进行表征;通过紫外可见漫反射(UV-Vis)及光致发光光谱(PL)对样品的光化学性能进行表征;样品的光催化性能通过可见光(λ>400 nm)催化降解罗丹明B染料(RhB)脱色活性进行测试表征。同时,对样品光催化性能与物理化学性能之间的内在联系进行了研究。结果表明:制备温度对样品的形态及光催化性能有着重要影响,当制备温度为140℃时,可制备得到高分散Cu2O微立方体并且其显示出最优的光催化活性;当制备温度进一步提高时,得到的样品为超细铜粉,样品的光催化性能迅速降低。     

共模板法一步合成绣球状BiOCl/Br固溶体光催化剂

以乙二醇/十二烷基三甲基溴化铵(EG/DTAB)为共模板剂,一步制得BiOCl/Br的固溶体光催化剂,利用X射线衍射仪、扫描电子显微镜、能谱仪、N2吸附-脱附仪和紫外-可见漫反射光谱仪进行了表征.结果表明,与采用溶剂热法制得的BiOCl分级微球相比,采用EG/DTAB共模板法制得的BiOCl/Br固溶体具有更明显的分层结构,呈绣球状.同时,DTAB的Br-插入到BiOCl的晶格中,形成固溶体,减小了禁带宽度.绣球状BiOCl/Br固溶体具有比商用P25、二维BiOCl纳米片和三维BiOCl分级微球更优异的可见光间接敏化降解染料性能,当nDTAB/nKCl=0.75时,制得的BiOCl/Br固溶体8 min内在可见光下对罗丹明B(Rh B)的降解率达到97.2%;1 h后在可见光下对甲基橙(MO)的降解率达到83.6%.     

反相微乳法合成稀土六铝酸盐催化剂及其表征

反相微乳法合成稀土六铝酸盐催化剂及其表征;反相微乳法;甲烷;六铝酸盐;过渡金属;稀土     

过氧化氢和磷酸对以亚磷酸作磷源合成SAPO-41和AIPO-41的影响

考察了以亚磷酸作为磷源合成SAPO-41和AlPO-41时加入过氧化氢或磷酸对生成SAPO-41和AlPO-41的影响.结果表明,向反应体系中加入过氧化氢或者使用磷酸部分替代亚磷酸,都能明显缩短SAPO-41和AlPO-41的晶化时间.此外,使用混合磷源还能够降低模板剂的用量,获得小晶粒晶化产物.     

Bridged Polysilsesquioxane Xerogels Functionalizated by Amine- and Thiol- Groups: Synthesis, Structure, Adsorption Properties

Bridged polysilsesquioxane xerogels containing amine (–NH₂; –NH(CH₂)₂NH₂; —NH) and thiol (–SH) groups were synthesized by hydrolytic polycondensation of 1,2-bis(triethoxysilyl)ethane, 1,4-bis(triethoxysilyl)benzene and appropriate trifunctionalized silanes in the presence of a fluoride-ion catalyst in an ethanol solution. ²⁹Si CP/MAS NMR give indication of the molecular framework of these materials formed by structural T¹, T² and T³ units. 3-aminopropyl or 3-mercaptopropyl groups accessible to proton or metal ions are fixed to the xerogel surface by the siloxane bonds. IR and ¹³C CP/MAS NMR data clearly show that 3-aminopropyl groups form hydrogen bonds. The same data testify that all xerogels contain non-condensed silanol groups and some fraction of non-hydrolyzed ethoxygroups. Functionalized polysilsesquioxane xerogels obtained by means of organic spacers have a porous structure (500–1000 m²/g) and a high content of functional groups (1.0–2.7 mmol/g). AFM data indicate that xerogels are formed by aggregating primary particles—the size of such aggregates is in the range 30–65 nm. It was established that the main factors influencing the structure and adsorption properties considered hybrid materials are: the nature and geometrical size of the functional groups, spacer flexibility and, in some cases, the ratio of the reacting alkoxysilanes and the ageing time of the gel.     

氮化镓粉末的溶胶凝胶法制备及其结构

报道了一种新颖而有效的二步制备氮化镓粉末的方法. 以乙氧基镓Ga(OC2H5)3作前驱体, 利用溶胶-凝胶法和高温氨化法相结合, 在950 ℃氨化温度下, 将凝胶与流动的NH3反应20 min, 合成了GaN粉末. XRD、FTIR、TEM及SAED的测量结果表明, GaN粉末是六方纤锌矿结构的单晶晶粒, 粉末粒度较均匀, FTIR吸收谱有明显的宽化现象.     

光散射/荧光比率法测定全氟辛烷磺酸

在pH=1.81的Britton Robinson（BR）缓冲溶液中,全氟辛烷磺酸（PFOS）与罗丹明B（RhB）通过静电引力和疏水作用使RhB的光散射增强,荧光发生猝灭。 利用在普通荧光光度计上单次扫描获得的340 nm处的光散射强度（I340）与596 nm处的荧光强度（F596）之比,建立了测定PFOS的光散射/荧光比率法,检出限（3σ）为17 nmol/L。 方法用于环境水样中PFOS的测定,RSD≤4.2%。     

溶胶-凝胶法制备TiO2/玻璃膜和光催化降解玫瑰红B的研究

溶胶-凝胶法制备TiO2/玻璃膜和光催化降解玫瑰红B的研究     

动力学荧光法测定药物、水果、蔬菜中的维生素C

提出了动力学荧光法测定维生素C的新方法。该法基于脱氢抗坏血酸(DAsA)对还原型罗丹明B在钒(Ⅴ)催化下自动氧化的活化作用。在pH为3.7的HAc-NaAc缓冲溶液中,还原型罗丹明B在钒(Ⅴ)催化下的氧化反应速度与DAsA的浓度成正比,采用固定时间法,测定在λ_(ex)=554 nm,λ_(em)=580 nm时的荧光强度。DAsA的线性范围为0～4.0×10~(-7)mol/L, 检测限4.0×10~(-9)mol/L。用该法测定药物、水果、蔬菜中维生素C含量,回收率在93%～108%之间。     

联苯二甲酸构筑的镍配合物的合成、晶体结构及对罗丹明B的光催化性能

通过水热方法获得了2个镍配合物:[Ni(3,3′-dpdc)(dpp)]n(1),[Ni(2,2′-dpdc)(phen)(H2O)2]n(2)(3,3′-H2dpdc=3,3′-联苯二甲酸,2,2′-H2dpdc=2,2′-联苯二甲酸、phen=菲咯啉,dpp=1,3-二(4-吡啶基)丙烷),通过X射线单晶衍射的方法测定了其晶体结构。配合物1为二维网格型结构,中心金属离子为扭曲的[NiO4N2]八面体构型,3,3′-dpdc配体的2个羧基采取双齿螯合的配位模式与Ni髤离子配位形成Ni-(3,3′-dpdc)一维链结构,dpp配体采取单氮原子桥连的配位模式连接2个Ni髤离子形成Ni-dpp一维链,两种链相互贯穿形成二维网格型结构,二维网格结构之间通过氢键C15D-H15…O2、C21-H21A…O1形成三维超分子结构。配合物2为一维之字链结构,中心金属离子为扭曲的[NiO_4N_2]八面体构型,2,2′-dpdc的2个羧基均采取单齿桥连配位模式连接2个Ni髤离子形成一维之字型链结构,一维链之间通过O-H…O和C-H…π弱作用力连接形成三维超分子结构。探究了2种配合物对有机染料罗丹明B的光催化降解性能,结果表明配合物可以高效地降解罗丹明B。     

超声辅助法合成的石墨烯-TiO2复合材料声催化降解罗丹明B（英文）

A series of graphene-TiO2 composites was fabricated from graphene oxide and titanium n-butoxide(TNB) by an ultrasonic-assisted method.The structure and composition of the nanocomposites were characterized by Raman spectroscopy,BET surface area measurements,X-ray diffraction,transmission electron microscopy,and ultraviolet-visible absorption spectroscopy.The average size of the TiO2 nanoparticles on the graphene nanosheets was controlled at around 10-15 nm without using surfactant,which is attributed to the pyrolysis and condensation of dissolved TNB into TiO2 by ultrasonic irradiation.The catalytic activity of the composites under ultrasonic irradiation was determined using a rhodamine B(RhB) solution.The graphene-TiO2 composites possessed a high specific surface area,which increased the decolorization rate for RhB solution.This is because the graphene and TiO2 nanoparticles in the composites interact strongly,which enhances the photoelectric conversion of TiO2 by reducing the recombination of photogenerated electron-hole pairs.     

完全液相法制备中原料配比对二甲醚合成催化剂结构和性能的影响

利用完全液相法制备了Cu-Zn-Al双功能催化剂,考察了原料配比对催化剂结构和催化CO加氢合成二甲醚反应性能的影响,用XRD,N2吸附,XPS和H2-TPR等方法对催化剂进行了表征.结果表明,在Cu-Zn-Al基二甲醚合成催化剂中,Zn和Al在催化剂表面的竞争富集是主要过程,增加投料中Cu的比例并不能显著增加Cu在催化剂表面的含量,因为在反应环境中,Al也会富集,并且在Cu含量高时富集得更快.当投料组成为n(Cu)∶n(Zn)∶n(Al)=2∶1∶4时,催化剂的体相结构和表面性质最好(Cu晶粒度最小,Cu分散度最高,还原性能最佳,组分间相互作用最强,最可几孔径最大),催化剂的综合性能最好.     

基于异亮氨酸衍生物配体的配位聚合物的合成及其荧光应用

在溶剂热条件下,利用L-异亮氨酸衍生物配体(C₁₃H₁₉NO₃)与Zn(NO₃)₂·6H₂O合成了配位聚合物[Zn₂(C₁₃H₁₇NO₃)₂]_n(1)。单晶X射线衍射结果显示化合物1结晶于单斜晶系P2₁空间群,配体与金属离子桥联形成二维层状结构,层与层间通过范德瓦耳斯力形成了三维超分子网络结构。在化合物1合成过程中加入罗丹明B(Rho-B),可以得到复合材料2。荧光测试结果显示,在激发波长为370nm时,化合物1主要是基于配体的发光,而复合物2除配体的发光外,在580nm处出现了Rho-B的发射峰。利用配体与Rho-B发射峰相对强度的比值为检测信号,将复合物2应用于金属阳离子和挥发性有机物(VOCs)检测。实验结果显示该材料能在水溶液中选择性识别Cr³⁺离子,并且在短时间内对苯甲醛蒸气作出响应。     

共振瑞利散射法测定痕量银的研究

在聚乙烯醇存在的硫酸介质中,银与过量的I^-形成配阴离子,并进一步与罗丹明B反应形成离子缔合物[AgI2]^-时,共振瑞利散射（RRS）强度明显增强并与银离子含量成正比,其最大RRS波长位于331．5nm处。研究了体系的共振瑞利散射光谱特征、主要影响因素和反应的最佳条件。结果表明,银离子质量浓度在0．06-2．0μg／mL范围内与RRS增强程度呈良好的线性关系（r=0．9973）。方法检出限为0．05仙g／mL,RSD4．78％,样品加标回收率为98．0％-102．0％。该法具有较高的灵敏度,操作简便,用于环境水样中痕量银的测定,结果令人满意。