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 共查询到18条相似文献,搜索用时 140 毫秒
1.
朱瓌之  郭红林  姜迁  漆虹 《化工学报》2015,66(4):1600-1606
通过聚合溶胶路线制备出稳定的Ti/Zr(摩尔比=1:1)复合溶胶。采用浸浆法,在平均孔径为5~6 nm的片状--Al2O3/--Al2O3载体上制备出完整无缺陷的Ti/Zr复合纳滤膜。详细考察了焙烧温度对Ti/Zr粉体的影响,并考察了Ti/Zr复合纳滤膜的性能。结果表明:在较高烧成温度下(500℃),Ti/Zr粉体依然呈无定形态且保持微孔结构。在400℃烧成温度下制备出孔径为1.49 nm的Ti/Zr复合纳滤膜,该膜的截留分子量(MWCO)为880,纯水通量为4.3 L·m-2·h-1·MPa-1。在p H=6,压力0.8 MPa的条件下,该膜对0.005 mol·L-1的Mg Cl2、Ca Cl2的截留率分别为85%和78%。  相似文献   

2.
陈加伟  陈慧如  漆虹  徐南平 《化工学报》2013,64(11):4060-4067
以五正丁氧基铌为前驱体,通过溶胶-凝胶法制备出稳定的Nb2O5聚合溶胶,详细考察了溶胶制备过程参数(体系酸度、水解比、反应温度、反应时间和螯合剂用量)对溶胶尺寸、稳定性以及制备重复性的影响。采用平均粒径为4.8 nm的Nb2O5溶胶,通过浸浆法在平均孔径为3 nm的γ-Al2O3中孔膜上制备出Nb2O5微孔膜。利用TG、XRD、NH3吸附-脱附、CO2吸附、吡啶吸附傅里叶变换红外光谱(Py-IR)和单组分气体渗透实验等手段对Nb2O5粉体及微孔膜的性能进行了表征,结果表明:在200℃、0.3 MPa条件下,350℃烧成的微孔Nb2O5膜对H2的渗透率和H2/CO2的理想分离因子分别为3.1×10-9 mol·m-2·s-1·Pa-1和21。此外,微孔Nb2O5膜经150 kPa的水蒸气处理8 h后,膜的渗透性能以及H2/CO2理想选择性基本保持不变。  相似文献   

3.
以钛酸四异丙酯为前驱体,通过颗粒溶胶路线制备出平均粒径为41nm的TiO2溶胶,并以此溶胶制备出稳定的制膜液。采用浸浆法,经过一次涂膜和在400~600℃烧成,在平均孔径约为70nm的片状α-Al2O3支撑体上制备出完整无缺陷的截留分子量小于10000的TiO2中孔膜。考察了烧成温度对非担载TiO2粉末和TiO2中孔膜性能的影响。结果表明:在400℃烧成3h可制备出孔径为4.7nm的TiO2中孔膜,其对PEG的截留分子量为8150,在0.8MPa,20℃下,纯水渗透通量为30L/(m2·h),对pH=3的Ni(NO3)2溶液的截留率达到95.14%。  相似文献   

4.
以正硅酸乙酯(TEOS)为前驱体,六水合硝酸镍(Ni(NO3)2·6H2O)为镍源,采用溶胶--凝胶法制备镍掺杂SiO2膜。研究了水用量及镍含量对镍掺杂SiO2膜的结构及形貌的影响,并对其进行CH4、CO2气体渗透性能测试。结果表明:水酯比为5.5时,制备的10%Ni掺杂SiO2膜具有良好的微孔结构,且孔径约为1.16nm,孔隙率为64.9%。一部分Ni元素以Ni和NiO晶体形式填充于SiO2孔道内,另一部分以Si—O—Ni形式进入SiO2骨架。Ni掺杂SiO2膜在84h内能够保持良好的气体渗透性能,表现出比纯SiO2膜更好的水热稳定性。CH4和CO2的气体渗透通量分别为1.56×10--7和0.64×10--7 mol/(m2·s·Pa),CH4/CO2气体分离因子达到2.43。  相似文献   

5.
γ-Al2O3中孔陶瓷膜的制备及表征   总被引:1,自引:0,他引:1  
《化工学报》2009,60(10)
以粒径为0.3~0.4 μm的α-Al2O3为原料,通过悬浮液真空抽吸法,制备出平均孔径约为70 nm的完整无缺陷的片状α-Al2O3支撑体;以仲丁醇铝为前驱体,采用颗粒溶胶路线制备出稳定的Boehmite溶胶,以此溶胶采用浸浆法,在制备的α-Al2O3支撑体上制备出完整无缺陷的γ-Al2O3中孔膜,并考察了烧成温度对γ-Al2O3中孔膜性能的影响.结果表明,本文制备出的γ-Al2O3膜的孔径约为3 nm,对PEG的截留分子量为2800~5300,纯水渗透通量为11.5~25.9 L·m-2·h-1[7.6×105 Pa,(14±1)℃].说明在孔径为70 nm左右的载体上直接制备孔径为3 nm的完整的中孔膜是可行的.  相似文献   

6.
ZrO2中孔膜的制备及其耐酸碱腐蚀性能   总被引:2,自引:1,他引:1  
以正丙醇锆为前驱体,通过颗粒溶胶路线制备ZrO2溶胶,并以此溶胶制备出稳定的制膜液. 采用浸浆法,经过一次涂膜,在平均孔径约为70 nm的片状a-Al2O3支撑体上制备出完整无缺陷的孔径小于10 nm的中孔ZrO2陶瓷膜,详细考察了烧成温度对ZrO2粉末和ZrO2中孔膜性能的影响. 在450℃的烧成温度下制备出孔径约为7 nm的ZrO2中孔膜,该膜对PEG的截留分子量为19500,在原料液侧压力为0.76 MPa、温度(23±1)℃条件下,纯水渗透通量为30~35 L/(m2×h). 经HNO3(pH=2)和NaOH(pH=13)溶液动态腐蚀后的ZrO2中孔膜对PEG截留分子量的变化表明,所制ZrO2膜具有较高的耐酸碱腐蚀性能.  相似文献   

7.
以聚乙烯醇(PVA)和正硅酸乙酯(TEOS)为原料,经溶胶-凝胶(sol-gel)法制备了不同二氧化硅(SiO2)含量的PVA/SiO2杂化膜。傅里叶变换红外光谱(FT-IR)表明,随着SiO2含量增大,1060cm-1和970cm-1处Si—O—Si特征吸收峰的相对强度逐渐加强,说明TEOS与PVA发生了交联反应;同时膜的分解温度从248℃升高到342℃。杂化膜的SiO2含量从10%增大到40%,其玻璃态温度从115℃升高到124℃。以水为溶剂,测定了杂化膜的耐溶剂性能,与PVA膜相比,杂化膜的耐溶剂性能显著提高。以质量比为0.950/0.025/0.025的环己烷/环己醇/环己酮为原料,测定杂化膜的分离性能,结果表明SiO2含量从10%增大到40%,通量从15.94 g/(m2·h)升高到75.69 g/(m2·h),环己醇的分离因子从1.8升高到2.65。  相似文献   

8.
溶胶一凝胶法制备Al2O3一SiO2复合膜的微观结构分析   总被引:13,自引:0,他引:13  
用溶胶-凝胶法制备了Al2O3-SiO2复合膜,通过XRD,FT-IR,N2吸附等手段研究化学组成和煅烧温度对复合膜的物相组成,化学结构以及微孔结构的影响,研究表明,在600℃下煅烧的合膜,随SiO2组分的减少,其物相从单纯无定形态演化为无定形态与γ-Al2O3纳米晶共存,比表面积从484.4m^2/g减小到197.7m^2/g,孔体积炎0.337cm^3/g减小到0.165cm^3/g,主要孔径范围2-4nm,微孔占总孔体积的17%-59%,当煅烧温度从200℃升高到1100℃,复合膜经历无定形态+γ-A1OOH,无定形态+γ-Al2O3到α-Al2O3+莫来石的晶相转变过程并逐渐致密化,比表面积和孔体积减小,孔径分布从双峰分布(200-600℃)变为单峰分布(800℃),孔隙在1100℃完全消失。  相似文献   

9.
采用二次水热合成法在管状多孔莫来石支撑体上制备高耐酸性ZSM-5分子筛膜,系统地研究分子筛晶种和合成溶胶中H_2O/SiO_2摩尔比率对ZSM-5分子筛膜生长与渗透汽化性能的影响,采用X射线衍射、冷场扫描电子显微镜和电子能谱等表征技术分别对制备的ZSM-5分子筛及其ZSM-5分子筛膜的结构、形貌和Si/Al比进行表征。针对分离75℃、90%HAc/H_2O的水溶液,最优化条件下制备的ZSM-5分子筛膜表现出优良的渗透汽化性能,渗透通量和分离因子分别为0.98kg/(m2·h)和890。此外,本研究所采用制备耐酸性ZSM-5分子筛膜的方法表现出良好的重现性,重复制备的12根ZSM-5分子筛膜在75℃下分离90%HAc/H_2O的水溶液时,平均通量和分离系数分别为(0.85±0.15)kg/(m2·h)和650±290。再者,ZSM-5分子筛膜在45~75℃的温度范围内分离50%~95%HAc/H_2O水溶液时都表现出优良的渗透汽化性能。  相似文献   

10.
耐酸ZrO2·SiO2涂层材料的低温合成研究   总被引:1,自引:0,他引:1  
采用溶胶-凝胶法,添加适量的矿化剂V2O5,在1300℃以下,合成微米级ZrO2·SiO2涂层。研究了矿化剂添加量、烧成温度和保温时间等因素对ZrO2·SiO2合成以及涂层抗酸腐蚀的影响作用关系,为ZrO2·SiO2涂层的合成与制备提供了可靠的实验依据。  相似文献   

11.
以大孔α-Al_2O_3陶瓷管(平均孔径为3μm)为载体,采用水热合成法在其表面形成一层纯硅沸石(Silicalite-1)修饰层,利用化学镀法在经过纯硅沸石修饰后的载体表面成功制备出致密钯复合膜,钯膜厚度约为5 μm.利用SEM对复合膜的结构和形貌进行了分析,并在350~500℃范围内对基于纯硅沸石修饰层的钯复合膜进行气体渗透测试表明,该沸石层修饰法制备的钯复合膜具有良好的氢渗透性.在500℃时,氧气渗透通量可达为0.12mol/(m~2·s),理想气体分离因子α(H_2/N_2)达到420.并对该钯膜与在载体表面直接制备的钯复合膜性能的差异进行了讨论.  相似文献   

12.
A microporous zirconia membrane with hydrogen permeance about 5 × 10?8 mol·m?2·s?1·Pa?1, H2/CO2 permselectivity of ca. 14, and excellent hydrothermal stability under steam pressure of 100 kPa was fabricated via polymeric sol–gel process. The effect of calcination temperature on single gas permeance of sol–gel derived zirconia membranes was investigated. Zirconia membranes calcined at 350 °C and 400 °C showed similar single gas permeance, with permselectivities of hydrogen towards other gases, such as oxygen, nitrogen, methane, and sulfur hexafluoride, around Knudsen values. A much lower CO2 permeance (3.7 × 10?9 mol·m?2·s?1·Pa?1) was observed due to the interaction between CO2 molecules and pore wall of membrane. Higher calcination tem-perature, 500 °C, led to the formation of mesoporous structure and, hence, the membrane lost its molecular siev-ing property towards hydrogen and carbon dioxide. The stability of zirconia membrane in the presence of hot steam was also investigated. Exposed to 100 kPa steam for 400 h, the membrane performance kept unchanged in comparison with freshly prepared one, with hydrogen and carbon dioxide permeances of 4.7 × 10?8 and~3 × 10?9 mol·m?2·s?1·Pa?1, respectively. Both H2 and CO2 permeances of the zirconia membrane de-creased with exposure time to 100 kPa steam. With a total exposure time of 1250 h, the membrane presented hydrogen permeance of 2.4 × 10?8 mol·m?2·s?1·Pa?1 and H2/CO2 permselectivity of 28, indicating that the membrane retains its microporous structure.  相似文献   

13.
针对两种重金属氯化物PbCl2、CdCl2,探究高岭土表面羟基对吸附重金属的作用。对高岭土进行煅烧及水热改性,并在两段式管式炉上进行高岭土捕集重金属氯化物蒸气实验,并使用原子吸收分光光度计(AAS)测量吸附剂中的重金属氯化物含量。吸附数据表明对于PbCl2及600~700℃的CdCl2吸附,高岭土经过煅烧吸附效率大幅降低,水热重新赋予羟基后吸附效率有所提升,但仍低于原高岭土。结合热重(DTG)及红外谱图(FTIR)分析可知,高岭土经800℃煅烧脱除全部羟基,经水热重新获得部分羟基,且所获数量随水热程度的加深而增多,结合XRD谱图可知羟基促进了高岭土与重金属氯化物的吸附反应;800℃以上高温下原高岭土吸附效率逐渐低于煅烧高岭土和水热高岭土,结合核磁共振谱图(NMR)分析可知其原因在于,高岭土经煅烧改性及水热改性,Al原子配位数降低,活性增强,更易与重金属氯化物蒸气结合。  相似文献   

14.
Ceramic membranes specially zeolite membranes are usually used for dewatering of organics by pervaporation. In the previous work, it was observed that kaolin calcined at 1050 °C has a separation factor 19.25 while kaolin calcined at 800 °C does not show any separation activity and its separation factor is equal to 1. In this research, effect of calcination temperature on flux and separation factor of kaolin modules that prepared by electrophoresis as a support of zeolite membranes was investigated. By increasing the kaolin calcination temperature, the flux of membrane increases due to many pores created in the module. This was confirmed by SEM micrographs. The highest flux was about 18 kg/m2 h for modules calcined at 1200 °C with ethanol 95%. Their separation factors were almost the same for each module. It was very low but comparable with some porous and non-porous polymeric membranes. Increasing calcination temperature causes module strength to enhance. It was found that the module calcined at 1200 °C may be suitable as a support for zeolite A membranes.  相似文献   

15.
The hydrothermal stability of microporous silica hybrid sol-gel derived membranes is often only tested for either the mesoporous intermediate membrane layer or the microporous separation layer. In this work an investigation is done on the interaction between the intermediate γ-alumina layer and the hybrid (BTESE-derived) silica separation layer during hydrothermal treatment. Although bare γ-alumina is degraded during a hydrothermal treatment, a coating of hydrophobic BTESE on γ-alumina retains its gas separation performance, albeit with a lower mechanical adhesion between the hybrid silica separation layer and the γ-alumina intermediate layer. Applying a monoaluminumphosphate (MAP) coating between the α-alumina support and the γ-alumina layer stabilizes the γ-alumina membrane. A BTESE coating on a MAP modified γ-alumina membrane did not show any signs of delamination after hydrothermal testing. Moreover, a significant increase in the H2/N2 (perm)selectivity, factor 3, was observed for these membranes.  相似文献   

16.
This paper reports on ¬¬¬a new microporous composite silica membrane prepared via acid-catalyzed polymeric route of sol-gel method with tetraethylorthosilicate (TEOS) and a bridged silsesquioxane [1, 2-bis(triethoxysilyl)ethane, BTESE] as precursors. A stable nano-sized composite silica sol with a mean volume size of ~5 nm was synthesized. A 150 nm-thick defect-free composite silica membrane was deposited on disk support consisting of macroporous α-Al2O3 and mesoporous γ-Al2O3 intermediate layer by using dip-coating ap-proach, followed by calcination under pure nitrogen atmosphere. The composite silica membranes exhibit molecular sieve properties for small gases like H2, CO2, O2, N2, CH4 and SF6 with hydrogen permeances in the range of (1-4)107 mol•m2•s1•Pa1 (measured at 200 C, 3.0×105 Pa). With respect to the membrane calcined at 500 C, it is found that the permselectivities of H2 (0.289 nm) with respect to N2 (0.365 nm), CH4 (0.384 nm) and SF6 (0.55 nm) are 22.9, 42 and >1000, respectively, which are all much higher than the corresponding Knudsen values (H2/N2 3.7, H2/CH4 2.8, and H2/SF6 8.5).  相似文献   

17.
采用并流共沉淀法制备Ni负载质量分数为15%的Ni/Al2O3催化剂,用于CO加氢甲烷化反应。结合紫外可见光漫反射、氢气程序升温还原、N2物理吸附-脱附和X射线粉末衍射等技术,考察焙烧温度对催化剂结构、活性与稳定性的影响。结果表明,低温[(350-500)℃]焙烧的样品中活性组分Ni主要以孤立的Ni O物种和高分散的无定形Ni O物种存在,相应的还原态样品中Ni粒子尺寸较小,是其新鲜态样品低温活性较高的主要原因。800℃焙烧的样品中活性组分Ni主要以高分散的无定形Ni O物种和Ni Al2O4尖晶石微晶形式存在于催化剂表面,活性组分Ni与载体Al2O3间的作用力较强,稳定性较高,且经过800℃水热老化处理10 h后仍具有较大的比表面积(125 m2·g-1),是其具有较佳低温活性同时突显良好水热稳定性的主要原因。  相似文献   

18.
李翠  刘化章  陈珍珍  李瑛 《工业催化》2014,22(10):751-755
氧化铝作为常用工业催化剂载体,其水热稳定性对催化剂寿命起至关重要作用。采用N2吸附、扫描电镜、X射线衍射、傅里叶红外光谱和NH3-TPD等对拟薄水铝石经800 ℃(升温速率10 ℃·min-1)焙烧4 h得到的氧化铝及水热处理后的氧化铝结构进行表征,研究拟薄水铝石结构对γ-Al2O3水热稳定性的影响。结果表明,拟薄水铝石前驱体结晶程度越好,焙烧所得γ-Al2O3的表面羟基越少,酸性越弱,水热稳定性越好。  相似文献   

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