颗粒溶胶路线制备高通量γ-Al_2O_3纳滤膜

颗粒溶胶路线制备陶瓷膜是一种不使用有机溶剂的清洁工艺.以仲丁醇铝为前驱体,采用水作溶剂,调节pH为3~4,通过颗粒溶胶路线制备了平均粒径为16nm稳定的勃姆石溶胶.通过浸浆法,在α-Al2O3微滤底膜上制备γ-Al2O3纳滤膜,并考察了热处理过程及涂膜时间的影响.控制涂膜时间为60s,烧结温度为600℃,所制备的γ-Al2O3纳滤膜膜层厚度约为1.8μm,对PEG的截留分子量约1 000Da,计算孔径为1.6nm,其纯水通量约为20L/(m2·h)(0.1MPa).采用颗粒溶胶路线适合制备γ-Al2O3纳滤膜.     

PVA修饰的溶胶-凝胶法制备γ-Al_2O_3超滤膜的研究

以氯化铝与氨水为原料,采用溶胶-凝胶法制备陶瓷膜溶胶,在微滤α-Al2O3支撑体上制备了γ-Al2O3超滤膜.考察了聚乙烯醇(PVA)对膜性能的影响.通过扫描电镜、气体和液体渗透和截留分子量等实验方法,对所制备的不对称超滤膜进行了表征.实验结果表明:用该法制备的氧化铝超滤膜,表面无裂纹和针孔等缺陷产生,孔径分布窄,平均孔径为8 nm左右,气体和液体渗透性稳定,对分子量约为6000的PEG截留率为90%.     

PVA修饰的溶胶-凝胶法制备γ-Al2O3超滤膜的研究

以氯化铝与氨水为原料,采用溶胶-凝胶法制备陶瓷膜溶胶,在微滤α-Al2O3支撑体上制备了γ-Al2O3超滤膜.考察了聚乙烯醇(PVA)对膜性能的影响.通过扫描电镜、气体和液体渗透和截留分子量等实验方法,对所制备的不对称超滤膜进行了表征.实验结果表明:用该法制备的氧化铝超滤膜,表面无裂纹和针孔等缺陷产生,孔径分布窄,平均孔径为8 nm左右,气体和液体渗透性稳定,对分子量约为6 000的PEG截留率为90%.     

γ-Al_2O_3膜对单组分无机盐溶液的截留性能

采用孔径约为3 nm的γ-Al2O3中孔膜,在pH 4~10,压力0.4~1.0 MPa,对浓度范围为0.005~0.1 mol/L的四种单组份无机盐溶液(NaCl、CaCl2、Na2SO4和MgCl2)进行截留性能考察.研究结果表明:膜对离子截留率的大小取决于离子所带的电荷大小.按从大到小的顺序:MgCl2CaCl2NaClNa2SO4,膜的截留率逐渐降低.膜对离子的截留率随盐溶液浓度的增大而降低,随操作压力的升高而增大.在pH=5,压力为0.5 MPa,浓度为0.003 mol/L时,膜对Mg2+和Ca2+的截留率分别达到85%和87.4%.有希望用于水的软化过程.     

介孔TiO_2膜的制备及其吸附性能研究

以钛酸四异丙脂为原料,采用粒子型溶胶路线制备出稳定的TiO2溶胶,通过浸渍涂膜法,在孔径为100nm的管式Al2O3微滤膜支撑体上制备出介孔TiO2膜。研究了介孔TiO2膜的制备过程对其完整性及孔结构的影响,同时考察了非负载介孔TiO2膜对染料酸性橙7和亚甲基蓝的吸附性能。在溶胶中加入适量的PVA和HPC,控制浸涂时间,在450℃焙烧1h可获得完整的介孔TiO2膜,膜厚约0.5μm,孔径分布于3~10nm。介孔TiO2膜对酸性橙7及亚甲基蓝吸附量随pH值变化,调节pH值可减少吸附造成的膜污染。     

超声辅助的溶胶-凝胶法制备ZrO_2纳滤膜

提出采用超声辅助溶胶-凝胶法制备ZrO_2纳滤膜.以水作为溶剂,通过在溶胶的制备过程中引入超声场,避免了沉淀的产生.在前驱体水解阶段实现了对溶胶粒径的控制,获得了平均粒径为1～2nm的ZrO_2颗粒溶胶.超声场的引入不仅可以促进ZrO_2颗粒溶胶的形成,还有利于提高ZrO_2材料的热稳定性.经400℃煅烧后,获得四方相ZrO_2纳滤膜,膜层光滑完整无缺陷,膜厚较薄,约为250nm.纳滤膜表现出较高的分离性能和渗透性能,对PEG的截留相对分子质量为600左右,对应的Stokes直径约为1.2nm,纯水渗透通量为200～250L/(m~2·h·MPa).初步考察了ZrO_2纳滤膜在低聚果糖纯化中的应用,用于脱除低聚果糖中的单糖和二糖组分.     

水相溶胶路线制备钇掺杂ZrO2纳滤膜及其分离性能研究

以氧氯化锆为前驱体, 采用环境友好的水相溶胶路线制备出完整无缺陷的管式钇掺杂的ZrO₂(YSZ)纳滤膜。并考察了溶胶粒径, 材料晶型与孔结构的关系。结果表明: 前驱体浓度越低, 所制备的溶胶粒径越小, 经400℃煅烧得到的粉末中单斜相含量越高, 堆积孔径增大; 向ZrOC₂O₄溶胶中添加8mol%钇, 有效抑制了ZrO₂四方相向单斜相的转变, 延缓晶粒生长, 同时防止膜层开裂。经纳滤测试表明, 实验制备的YSZ纳滤膜对PEG的截留分子量为860 Da, 纯水渗透率为200 L/(m²·h·MPa)。实验还详细考察了YSZ纳滤膜在pH=6, 压力0.8 MPa的条件下对NaCl、Na₂SO₄、CaCl₂和MgCl₂ 4种溶液的截留性能, 结果显示YSZ纳滤膜对0.005 mol/L CaCl₂和MgCl₂溶液的离子截留率分别达到65%和78%。     

辐射接枝制备中空纤维纳滤膜的性能研究

对以聚砜(PSF)中空纤维超滤膜为基体,通过低温等离子体辐照接枝2-丙烯酰胺基-2-甲基丙磺酸(AMPS)制备的纳滤膜的结构和性能进行了研究。结果表明,这种方法可以制得断裂强力高于PSF基膜,孔径约为2.6nm和纯水渗透系数为44.3L/(m2.h.MPa)的纳滤膜。在25℃,0.4MPa下对300mg/L的K2SO4、Na2SO4、MgSO4、KCl、NaCl和MgCl2的截留率为89.3%、88.3%、52%、39.6%、37.4%和13.2%,表明该纳滤膜为荷负电膜,对无机盐的截留主要依靠Donnan效应。     

溶胶-凝胶法制备TiO_2-Al_2O_3复合光催化剂及其表征

以钛酸四正丁酯为钛源,异丙醇铝为铝源,采用溶胶-凝胶法制备了TiO2-Al2O3复合光催化剂,考察其对甲基橙的吸附性能和在紫外光照射下的光催化活性。采用X射线衍射(XRD)、X射线光电子能谱(XPS)、傅里叶变换红外光谱(FT-IR)、N2吸附-脱附等对催化剂的晶相结构、化学组成及BET比表面积和孔径分布等进行了表征。结果表明TiO2-Al2O3复合光催化剂由TiO2和Al2O3组成,其中TiO2为单一的锐钛矿晶相,Al2O3为非晶态,Al2O3的存在可抑制TiO2晶粒的生长。在n(Ti)/n(Al)=12,500℃煅烧3h制得的TiO2-Al2O3复合光催化剂比表面积达99.21m2/g,平均孔径为22.39nm,累计孔容积为0.4493cm3/g。在500℃煅烧制得的复合光催化剂具有最佳的光催化活性和吸附性能。与纯TiO2相比,相同条件下TiO2-Al2O3复合光催化剂的光催化活性和吸附性能都有较大提高。     

超声辅助溶胶-凝胶法制备中空纤维TiO2超滤膜

TiO₂膜具有亲水性强和热化学稳定性好等优点而用于超滤分离, 但是TiO₂膜以管式膜为主, 渗透通量低且制备周期长。为了提高TiO₂膜的渗透通量, 并缩短膜的制备周期, 本工作以钛酸四丁酯为前驱体, 采用超声辅助溶胶-凝胶法制备高通量的中空纤维负载型TiO₂超滤膜。系统考察了硝酸与钛酸四丁酯的摩尔比(酸钛比)、超声时间和煅烧温度对TiO₂溶胶粒径及膜截留性能的影响。结果表明：当酸钛比为0.25时, 溶胶的平均粒径为3252 nm, 采用超声处理30 s后, 平均粒径减小至1817 nm。采用超声后的溶胶循环涂膜并在350 ℃煅烧两次后可得到完整无缺陷的中空纤维TiO₂超滤膜, 膜层平均厚度为1 μm, 膜的纯水渗透通量为145 L·m^-2·h^-1·bar^-1(1 bar=0.1 MPa), 葡聚糖截留分子量为2586 Da, 对应的平均孔径为2.5 nm。     

微乳液法制备掺杂铁的纳米二氧化钛及其表征

为了研究掺杂铁的纳米二氧化钛的性质,以TiCl4为原料,在CTAB/正丁醇/环己烷/水组成的微乳液体系中制备了掺杂铁的TiO2纳米粉末。采用热分析仪(TG-DTA)、X射线衍射分析(XRD)、透射电子显微镜(TEM)和比表面分析仪(BET)等对粉体的结构、粒径大小、物相、形貌和比表面积等进行了表征。经600℃焙烧2h后,0.04%Fe3+-TiO2粉末为单一的锐钛型结构,其平均晶粒度约为16nm,比表面积达120.4m2.g-1,D101为16.1nm。由于在XRD图谱上未发现有新相的生成,因此,Fe3+经过焙烧渗入到了二氧化钛的晶格中,掺杂所引起的变化主要是由于Fe3+渗入TiO2晶格所引起的。     

溶胶／凝胶法制备纳米TiO2／Al2O3

采用溶胶-凝胶法制备纳米TiO2／Al2O3，考察了陈化温度及络舍比对TiO2／Al2O3比表面积及孔结构参数的影响。结果表明，TiO2／Al2O3平均粒径〈70nm，比表面积超过210m^2／g，平均孔径0．8-1．4nm。适当降低陈化温度及加络合剂有利于TiO2／Al2O3粒子的分散。Al2O3的存在提高了TiO2／Al2O3的热稳定性。     

Preparation of nanocrystalline TiN coated cubic boron nitride powders by a sol-gel process

Cubic boron nitride (cBN) particles coated with 20 wt% nanocrystalline TiN were prepared by coating the surface of cBN particles with TiO2, followed by nitridation with NH3 gas at 900 degrees C. Coating of TiO2 on cBN powders was accomplished by a sol-gel process from a solution of titanium (IV) isopropoxide and anhydrous ethanol. An amorphous TiO(x) layer of 50 nm thickness was homogenously formed on the surface of the cBN particles by the sol-gel process. The amorphous layer was then crystallized to an anatase TiO2 phase through calcination in air at 400 degrees C. The crystallized TiO2 layer was 50 nm in thickness, and the size of TiO2 particles comprising the layer was nearly 10 nm. The TiO2 on cBN surfaces was completely converted into nanocrystalline TiN of uniform particles 20 nm in size on cBN particles by nitridation under flowing NH3 gas.     

Synthesis and structure analysis of La0.5SR0.5TiO3 nanoparticles prepared by thermal decomposition method

La0.5Sr0.5TiO3 (LSTO) nanoparticles were synthesized by thermal decomposition method using Cl3La, CI2Sr x 6H2O and C16H28O6Ti as starting materials. The obtained precursor in a powder form was calcined at 700, 900, 1100 and 1300 degrees C for 3, 6 and 9 h in air. The structures of all samples were analyzed by XRD and some of them were taken for SEM, TEM and VSM measurements. The results from SEM showed the parallelpipe like shape of the particles with sizes distributed between 80 and 180 nm and the sizes of these particles were increased with the increasing of calcination temperature and time. The XRD's results showed the perovskite structure with the lattice type of orthorhombic at the calcination temperature of 900, 1100 and 1300 degrees C for 3, 6 and 9 h. The TiO and others unknown phase were found at low calcination temperature and they were disappeared as the calcination temperature and time were increased. The results of TEM support the orthorhombic structure of LSTO nanoparticles with crystallite size less than 200 nm as revealed by SEM and XRD. The magnetic property of all samples was measured by VSM and revealed that those prepared at 700, 900, and 1100 degrees C exhibit diamagnetic behavior, whereas one at 1300 shows ferromagnetism at room temperature. In this work, it is found that the nano-LSTO of high crystalline phase and purity can be prepared by thermal decomposition method at calcination temperature of 900 to 1300 degrees C in air for 6-9 h.     

TiO2纳滤膜对重金属离子的截留性能

采用孔径为1.5 nm的TiO2纳滤膜,在压力0.4～0.8 MPa,pH值3～7的条件下,考察了膜对浓度范围为50～500 mg/L的Cu(NO3)2、Ni(NO3)2、ZnC12和CdC12四种单组份重金属溶液的截留性能.结果表明:除Cd2+外,膜对重金属离子的截留率随溶液浓度的增大先增大,当浓度达到200 mg/L后趋于稳定;升高压力膜的离子截留率会略有增加;当pH=6时,膜对Ni2+和Cd2+的截留率最低,而对Cu2+和Zn2+的截留率在pH=5～6时达到最高.TiO2膜对Cu2+、Ni2+、Zn2+和Cd2+的最高截留率分别可以达到96.9％、95.9％、92.5％和83.2％.     

纳米氧化铝粉体的绿色合成及其物相转变控制研究

以氯化铝、碳酸钠为原料,采用直接沉淀法,并于500～1,200℃煅烧,制备纳米Al2O3粉体。然后用TiO2、BaO对纳米Al2O3粉体掺杂,控制其物相转变过程。通过X射线衍射仪、差式扫描量热仪和透射电子显微镜分析纯净和掺杂后的纳米Al2O3的物相转变过程。结果表明,直接沉淀法所得水合Al2O3,经500℃煅烧后可转变为纳米活性Al2O3,粒径约为10 nm;纯净和掺杂Al2O3样品经1,200℃煅烧2 h后均为纳米粉体,其粒径为40～50 nm;在较高温度下,掺杂氧化钡对Al2O3的物相转变具有强烈抑制作用,粉体直至1,200℃仍未转变为结晶良好的α-Al2O3物相;而氧化钛则对其物相转变有显著促进作用,在1,000℃时粉体的主要物相即为α-Al2O3,1,100℃之后粉体已完全转变为α-Al2O3。     

Sol-gel synthesis and characterization of nanostructured TiO2/gamma-Al2O3 composite membranes

Nanostructured TiO2/gamma-Al2O3 composite membranes with various compositions were prepared by sol-gel method. The structural and textural properties of the composite membranes could be modified by the mixing ratio of boehmite sol and titania sol, and calcination temperature. The existence of alumina in the composite membranes retarded anatase-to-rutile phase transformation, resulting in stabilization of textural properties. Defect-free composite membranes were confirmed by gas permeation test.     

H(2)O(2)-sensitized TiO(2)/SiO(2) composites with high photocatalytic activity under visible irradiation

TiO(2)/SiO(2) composite photocatalysts were prepared by depositing of TiO(2) onto nano-SiO(2) particles. X-ray diffraction (XRD), transmission electron micrograph (TEM), Raman spectrometer, UV-Vis diffuse reflectance spectroscopy, Fourier transform infrared spectroscopy (FT-IR) were employed to characterize the properties of the synthesized TiO(2)/SiO(2) composites. These results indicated that the products without calcination were amorphous, and calcination could enhance the crystallinity of TiO(2). Increases in the amount of TiO(2) would decrease the dispersion in the composites. H(2)O(2)-sensitized TiO(2)/SiO(2) composite photocatalysts could absorb visible light at wavelength below 550 nm. The photocatalytic activity of as-prepared catalysts was characterized by methyl-orange degradation. The results showed the uncalcined composite photocatalysts with amorphous TiO(2) exhibited higher photocatalytic activity under visible light, and the activity of catalysts with TiO(2) content over 30% decreased with increasing of TiO(2) content. Increases in the calcination temperature and TiO(2) content promote the formation of bulk TiO(2) and result in a decrease in activity.     

液氨沉淀法制备ZnO超微粉

以Zn(NO3 ) 2 为原料 ,NH3 ·H2 O为沉淀剂 ,采用直接沉淀法制备Zn(OH) 2 白色沉淀 ,经洗涤、干燥、煅烧后生成ZnO超微粉末。通过TEM观察到ZnO为球形晶体 ,平均粒径 15 0nm。探讨了溶液pH值、沉淀剂浓度、反应时间、反应温度对前躯体Zn(OH) 2 粒度的影响以及煅烧过程中煅烧温度与煅烧时间对ZnO粒度的影响 ,得出了最佳工艺条件。     

铂修饰的TiO2柱撑膨润土复合光催化剂的制备及光催化活性研究

钛酸四异丙酯在醋酸溶液中水解生成的多核钛离子经离子交换反应插入到膨润土层间，制得钛柱撑膨润土(TiO2-PILC)，再通过光沉积法合成了一系列不同铂量修饰的钛柱撑膨润土(Pt-TiO2-PILCs)；用XRD、BET和TEM对制得的复合催化剂进行了性能表征；以五氯酚钠为目标污染物，考察了它们的催化活性．结果表明：柱撑膨润土中TiO2主要以锐钛型存在，含铂的Pt-TiO2-PILCs的催化活性明显高于TiO2-PILC．此外该复合催化剂还具有回收容易、重复使用性好等特点．