Synthesis of 3-D ordered macroporous silicate using the template formed from monodispersed polystyrene latex

Based on the template formed from monodispersed polystyrene (PS) latex, a modified fast sol-gel process was employed to synthesize a three-dimensional (3-D) ordered macroporous silica material after removing the template by calcination at high temperature. It was indicated that there existed highly ordered packed pores within the whole silica material by SEM morphology observation. It was also found that the pores were interconnected. The pore size could be controlled mainly by varying the particle size of the latex ranging from 10¹ to 10² nm. The formation process of the ordered pores was also preliminarily discussed.     

复合模板剂制备有序介孔氧化铝

采用溶胶-凝胶法以异丙醇铝为铝源,乙醇为溶剂,非离子表面活性剂TritonX-100和三嵌段共聚物P123为复合模板剂,制备了有序介孔氧化铝。用PSD、XRD、TEM等测试技术对样品进行了结构表征,实验结果表明,合成的有序介孔氧化铝比表面积大于500m²/g,孔容超过1.0cm³/g,孔径分布窄（2～12nm）,形成的蠕虫状孔道具有一定的有序性,与采用单一模板剂P123制得的介孔氧化铝相比具有比表面积大,孔分布窄,有序性好的优点。最佳模板剂配比为 n(TritonX-100)∶n(P123)=3∶1。     

致密储层渗吸特征与孔径分布的关系

致密油气藏资源量巨大,作为重要的替代能源可以极大地缓解中国的原油对外依存度。致密储层微纳米孔隙发育,毛细管力渗吸作用强,充分发挥渗吸排驱作用对提高致密油气产出至关重要。然而,由于致密储层孔隙结构复杂,目前对于渗吸特征与孔径分布之间的关系尚不清楚。选取致密火山岩和页岩开展实验,并与致密砂岩进行对比。通过高压压汞测试和自发渗吸实验分别获得致密储层孔径分布和渗吸特征参数,并建立两者之间的相关关系。结果显示致密储层渗吸体积与时间的双对数坐标系下,自发渗吸曲线呈现三段式特征:初期直线段、曲线段和后期直线段。其中初期直线渗吸段为主要阶段,吸水速度大大超过扩散段,且吸水量占总吸水量的比例超过90%,可采用渗吸指数和扩散指数对渗吸特征进行表征。渗吸指数和扩散指数与孔径分布特征关系密切;渗吸指数约为0. 5,主要反映了宏孔孔径分布特征,渗吸指数越大,宏孔越发育;扩散指数低于0. 3,主要反映了中孔分布特征,扩散指数越大,中孔越发育。本文研究有助于理解致密储层渗吸特征与孔径分布的关系,对发挥渗吸驱替作用和提高致密油气高效产出具有重要意义。     

准噶尔盆地乌尔禾组凝灰岩孔隙特征及其主控因素

为明确东道海子凹陷乌尔禾组凝灰岩孔隙结构与主控因素,基于低压CO₂吸附、低温N₂吸附以及高压压汞实验,对凝灰岩全尺寸孔隙孔径进行表征;基于分形理论,对凝灰岩微孔和介孔的孔隙复杂程度和非均质性进行定量表征,阐明影响与控制凝灰岩孔隙结构的主要因素。结果表明,凝灰岩主要发育锥形管孔、开口的锥形平板孔和狭窄的平行板孔等形态孔隙,孔径呈多峰分布;凝灰岩总孔体积介于0.005 4～0.047 8 cm³/g,各类孔隙发育程度差异较大,凝灰岩总孔体积主要由介孔所提供,介孔体积介于0.004 2～0.041 3 cm³/g,平均0.026 0 cm³/g,平均占比75.10%;其次是微孔和宏孔,微孔体积介于0.000 6～0.005 5 cm³/g,平均0.003 1 cm³/g,宏孔体积介于0.000 6～0.005 3 cm³/g,平均0.002 8 cm³/g,二者的占比分别为11.5%和13.4%;...     

高铝粉煤灰制备氢氧化铝的比表面积及孔隙特性

以高铝粉煤灰烧结熟料为原料,经溶出、深度脱硅和分解(碳酸化分解或晶种分解)得到高白氢氧化铝,采用低温氮气吸附法分析两种分解方法制得的氢氧化铝的比表面积和孔隙分布.结果表明:氢氧化铝的等温吸附线属III类,氢氧化铝晶粒之间的孔隙以微孔为主,存在一定数量的介孔和大孔.碳分氢氧化铝BET比表面积和平均孔径远大于种分氢氧化铝,碳酸化分解时在CO2的强推动下,氢氧化铝猛烈析出并凝聚,使得晶体结构疏松,晶间空隙大.晶种分解靠晶体的长大而使晶体变粗,晶体结构致密,晶间空隙小.     

富有机质泥页岩有机质孔隙研究进展

泥页岩有机质孔隙是页岩气储层的主要孔隙类型,是页岩气的富集关键因素之一。近年来对有机质孔隙成因、控制因素及页岩气储层的储渗性能研究取得了较大的进展,研究表明:有机质孔隙的成因包括干酪根生烃形成的孔隙与沥青裂解形成的孔隙2种类型。根据有机质孔隙大小,可分为大孔、中孔(介孔)与微孔。页岩气以吸附态赋存在微孔、介孔中,以游离态保存在大孔中。吸附态主要发生在孔径10nm的孔隙中,大孔中游离态烃以非达西渗流方式流动。有机质的成熟度处于0.9%~3.6%、腐泥组与镜质组显微组分、有机碳质量分数2.0%是有机质孔隙发育的有利条件;压实程度较高、较高的流体压力、脆性矿物含量高的泥页岩是有机质孔隙保存的有利条件。     

阳极氧化铝模板的结构和性能表征及形成机理

用两步阳极氧化法在0.3 mol.L-1草酸中制备了高度有序、具有纳米级孔洞的阳极氧化铝有序阵列模板.用场发射扫描电镜、X射线衍射及荧光光谱对其进行了结构和性能表征.实验结果表明多孔氧化铝模板的蓝发光带是由氧空位缺陷所引起的.对氧化铝模板的形成机理进行了分析,认为它的形成机理可以通过综合参考溶解模型和机械应力模型加以解释,并且电渗在阳极氧化膜的生长过程中起着重要作用.     

纯粘土矿物甲烷吸附研究及吸附模型评价

粘土矿物在页岩储层无机矿物中占有重要的比例,其是页岩气吸附的重要场所。由于不同页岩储层成藏条件差异,粘土矿物相对含量有较大差异,因此也影响页岩气的吸附能力。以XRD,低压氮气吸附实验以及甲烷等温吸附实验为主要研究手段。XRD结果表明四种样品(伊利石,蒙脱石,绿泥石,高岭石)纯度较高,均大于94%。低压氮气吸附结果表明：蒙脱石以微孔与中孔为主,孔隙形态主要为四边都开口的平行板状、狭缝状等,含有墨水瓶状的孔;伊利石主要发育有中孔与大孔,绿泥石主要发育有微孔和大孔,高岭石主要发育有中孔和大孔,它们的孔隙形态同样都平行板状、狭缝状等为主;比表面积与孔隙体积的大小顺序为：高岭石>伊利石>蒙脱石>绿泥石,两者呈正相关。在61 ℃,压力为0~25 MPa条件下进行五组甲烷等温吸附试验,包括四组纯粘土矿物及一组由四种纯矿物等质量混合的矿物。纯粘土矿物甲烷吸附量大小顺序为：高岭石>伊利石>蒙脱石>绿泥石,粘土矿物的比表面积越大,其甲烷吸附量也越大。对等温吸附实验数据进行拟合发现：Langmuir, Toth以及Langmuir-Freundlich吸附模型对于不同矿物总体拟合效果都极好,对粘土矿物吸附模型精确选择具有一定意义。     

九龙矿构造煤压力作用下孔隙结构及分形变化特征

为探究邯郸九龙矿构造煤在压力作用下对煤孔隙结构造成产生的影响,选取九龙矿瓦斯突出煤层-山西组2号碎粒煤及碎裂煤为研究对象,对煤样进行加压处理,并利用低温氮吸附仪对加压前后的煤样进行低温氮吸附实验。利用传统低温氮实验数据定性分析和分形理论定量分析的方法,对实验前后煤样孔隙发育规模和结构变化进行对比分析。实验结果显示：压力对煤中的孔隙结构会造成一定的影响,加压后的碎粒煤孔隙结构变化情况较小,碎裂煤孔隙结构变化较为明显。碎粒煤孔容贡献基本不发生变化,碎裂煤孔容贡献度会发生变化,且孔容贡献度占比会更倾向于更小的孔径,表明压力在对煤产生影响时,孔径小的孔径对压力反应比孔径大的孔径反应更明显。碎裂煤和碎粒煤比表面积贡献均为较小的孔径,基本在2~4 nm左右波动,比表面积孔径贡献范围有轻微后移,但幅度不大。碎粒煤和碎裂煤在加压前后,微孔的分形维数高,拟合度均为0.99以上,小孔和中孔的分形维数较高,拟合度均为0.94以上。加压后,碎粒煤的煤样微孔复杂情况具有更简单的趋势,中孔和小孔的复杂情况具有更复杂趋势,但趋势均不明显,而碎裂煤在微孔的孔隙情况有轻微的变简单,在中孔和小孔的孔隙情况有变复杂的趋势,且趋势较为明显。九龙矿2号碎裂煤储层改造可以考虑在本煤层或在顶底板围岩进行水力压裂,而碎粒煤则需要通过水力冲孔出煤卸压或在顶底板围岩进行水力压裂。     

碳纳米管薄膜电极电容去离子研究

采用低压化学气相沉积方法制备碳纳米管薄膜电极，研究碳纳米管薄膜的电容去离子行为.碳纳米管薄膜主要由中孔和部分大孔组成，适合电容去离子应用.详细研究了工作条件（流速、电压）和离子特性对碳纳米管薄膜电容去离子性能的影响.结果表明：电极电压越高，除盐率越高；存在一个最佳流速，此时除盐率最高；离子半径越小，电荷越小的离子，更容易吸附.     

利用原子力显微镜表征页岩孔隙结构特征

页岩储层孔隙结构复杂,非均质性强,矿物组分多样,这些储层特性加大了页岩油的开采难度。为了更好地表征页岩孔隙结构,利用原子力显微镜(atomic force microscope, AFM)技术,结合Gwyddion软件对大港、吉木萨尔和松辽盆地页岩的孔隙结构以及表面粗糙度进行了表征。结合快速傅里叶变换(fast Fourier transform, FFT)分析页岩的非均质性,采用分水岭法识别孔隙分布特征,分析不同地区页岩储层的孔隙结构差异。原子力显微镜可以对页岩的表面形貌进行表征,通过平均粗糙度、均方粗糙度、表面偏度和峰度系数等参数对表面粗糙度进行评价,可以准确表征页岩纳米级的孔隙结构,包括孔隙数量、孔隙大小、孔隙面积、孔隙体积和孔隙度等。结果表明：大港和吉木萨尔页岩的表面高度较高,松辽盆地页岩表面高度较低,大港页岩非均质性较强,孔隙主要以微孔为主,吉木萨尔页岩和松辽盆地页岩非均质性较弱,中孔和宏孔数量较多,孔隙发育较好。     

改性剂对硅胶整体柱结构性能的影响

研究了改性剂对硅胶整体柱结构性能的影响.通过采用改进的溶胶-凝胶技术,以四甲氧基硅烷和聚乙二醇为原料,表面活性剂和变形抑制剂等为改性剂,使用特殊处理手段有效抑制柱体开裂和变形弯曲现象,同时极大缩短了干燥时间;探讨了原料比例和不同制孔剂浓度对整体柱结构的影响.制备出的硅胶整体柱具有通孔和中孔双孔结构,空隙率高,通透性好.     

Synthesis of 3D ordered porous polystyrene using silica template

A rigid colloidal silica template was formed by self-assembly of the monodispersed silica spheres prepared according to Stober method. The silica template is highly ordered, which was verified by bright color effect due to Bragg diffraction and the results of SEM. The free radical polymerization of styrene was allowed within the interstices of the rigid template to result in the formation of the three-dimensional periodic silica/polystyrene nano-composites. The titled porous polystyrene was prepared by chemical decomposition of the template with concentrated aqueous hydrofluoric acid. Scanning electron microscopy characterization showed that the macroporous polystyrene has ordered arrays of the uniform pores replicated from the template. Moreover, it was found that the morphology of the as-synthesized macroporous polystyrene was greatly affected by the connectivity of the silica spheres treated under different conditions.     

Synthesis and Characterization of Ordered Meso-Macro-Porous Silica Membranes on a Porous Alumina Support

Macroporous silica materials with ordered three-dimensional pore structure can be easily prepared by the template-directed sol-gel process. However, it is still a challenge to prepare them in membrane form on a porous support, which limits their applications. In this work, we have demonstrated the feasibility of obtaining a three-dimensional ordered macroporous silica membrane on macroporous alumina support using poly-methyl methacrylate (PMMA) spheres as the template. PMMA spheres were packed on the top of an Anopore-alumina support by filtration of a PMMA aqueous suspension. Silica sol obtained by an acid-catalyzed sol-gel process was infiltrated into the voids among the spheres. Drying induced stress caused the membrane to crack or peel off from the top of the support. This can be minimized by annealing the PMMA template layer before the introduction of silica sol which increases the mechanical strength of the template. Calcination or solvent extraction to remove the template produced a highly ordered three-dimensional macroporous silica membrane with spherical pores connected by windows in the mesoporous range. The results show that the PMMA-templated infiltration method is effective in preparing three-dimensional ordered macroporous silica membranes on a porous support.     

Ordered mesoporous tungsten oxide and titanium oxide composites and their photocatalytic degradation behavior

Highly ordered mesoporous WO3/TiO2 (MWTs) composite materials with tunable chemical compositions were obtained by a surfactant template-assisted evaporation-induced selfassembly (EISA) processes. The structure properties of the MWT materials were characterized by small angle XRD, TEM and N2 sorption. The resultant materials showed large amount of ordered mesopores and high chemical homogeneity. With increasing crystallinity degree, the order degrees of mesostructure turned worse gradually. The MWT hybrids exhibited excellent visible light response due to the addition of WO3 with narrow band gap. Photocatalytic performances of the MWT samples were determined by measuring the photo-degradation of rhodamine B dye and phenol under simulated solar light irradiation. The effect of material parameters such as surface area, crystallinity and chemical compositions in the binary heterostructured system on photocatalytic performance were discussed in details.     

龙马溪组岩相类型及其对孔隙特征的影响因素

以川南黔北地区下志留统龙马溪组下段页岩储层为研究对象,以全岩矿物分析为手段,结合岩芯薄片观察,划分出4种页岩岩相,其中,黏土质页岩岩相和混合页岩岩相是本研究区发育的主要岩相.基于扫描电镜、有机碳含量和低温氮气吸附实验,系统地分析了两种主要岩相孔隙结构特征.结果表明,黏土质页岩岩相储层中较大孔隙以细颈瓶状、开放型孔隙和半...     

新集一矿孔隙结构特征研究

为进一步了解新集一矿煤层孔隙结构特征,通过压汞法和低温氮等温吸附法实验手段对新集一矿主采煤层孔隙发育特征进行研究。发现新集一矿主采煤层孔隙度较比两淮矿区其他地区高。其中以8煤层8XJ5号样为代表孔隙分布以小孔最发育,大孔较发育,中孔少见为特征和以13-1煤层13XJ10号样为代表孔隙分布以小孔最发育为特征的基质孔,孔隙之间的连通差,不利于瓦斯的抽排;以11-2煤层11XJ3号样和6-1煤层6XJ15号样为代表中孔发育,孔隙以裂隙性为主,孔隙之间的连通较好,有利于瓦斯的运移。     

不同溶剂萃取回收SBA-15中有机模板剂的研究

利用3种不同的溶剂对SBA-15分子筛中有机模板剂P123(EO20PO70EO20)的最佳萃取工艺条件进行了研究,考察了溶剂种类、萃取温度、萃取时间、溶剂量对回收率的影响。实验确定的最佳萃取工艺条件为甲醇作为溶剂,萃取温度75℃,萃取时间3.5h,溶剂量300mL,在此条件下P123回收率可达80.7%。制备得到的SBA-15分子筛通过X射线衍射、热重分析、Fourier红外光谱及N2吸附脱附等手段进行表征,结果表明通过溶剂萃取得到的SBA-15骨架有序性保持良好,比表面积更大。溶剂萃取过程不会造成骨架硅羟基脱除,克服了高温焙烧所引起的孔道收缩问题。回收得到的模板剂P123通过液体红外光谱和凝胶渗透色谱等手段进行表征,表明其在宏观和微观方面具有与标准样品相同的性质。     

交流电沉积条件对沉积Ni纳米线的影响

采用恒压40V二次阳极氧化方法制备了阳极氧化铝(AAO)模板,模板的孔径均匀有序。在二次阳极氧化的基础上阶梯降低电压至10V,可有效减薄阻隔层,有利于Ni纳米线的交流电沉积。利用扫描电子显微镜和透射电子显微镜对AAO模板以及Ni纳米线的形貌进行表征。探索了阶梯降低氧化电压、电源滤波以及电沉积频率对沉积Ni纳米线的影响。结果表明,阶梯降低氧化电压、适当的频率以及滤波可以明显提高电沉积效果,得到比较均匀有序的Ni纳米线。     

CNTs/mesostructured silica core-shell nanowires via interfacial surfactant templating

Carbon nanotubes (CNTs)/mesostructured silica core-shell nanowires with a carbon nanotube core and controllable highly ordered periodic mesoporous silica shell are syntheiszed via the interfacial surfactant template. The core-shell nanowires are characterized by transmission electron microscope (TEM), X-ray diffraction pattern (XRD) and nitrogen sorption/desorption. The results indicate that the core-shell nanowires have highly ordered periodic mesoporous silica shell (space group p6mm), high BET surface area and narrow pore size distribution. Moreover, the morphology of core-shell nanowires can be controlled by the pH value. The core-shell nanowires have promising applications in biosensors, nanoprobes and energy storage due to their good dispersibility in polar solvents. Supported by the Australian Research Council (ARC) through Discovery Project program (DP0452461)