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MEMBRANE CHARACTERIZATION BY MICROSCOPIC AND OPTICAL METHODS: POWERFUL TOOL TO CONTROL FOULING

机译:通过显微镜和光学方法表征膜:功能强大的控制渗漏的工具

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One of the critical issues in the successful development of the ultrafiltration (UF) processes is the fouling,which arises from specific interactions between the membrane and various components present in thewater. Many parameters impacting the fouling have been already studied. They can be classified into twocategories: membrane chemical and structural parameters and water characteristics. The structuralproperties of membranes (roughness, porosity...) are specially studied to develop a fouling controlmethod. In this work, several microscopic and optical methods are used to characterise, first virginorganic membranes and secondly fouled organic membranes after operation.In this work, information obtained for organic UF PES clean and fouled flat sheet membranes accordingto the cut-off (10, 30, 100 and 300 kDa) and for PVDF hollow fibers (100 kDa) are compared. For that,different techniques were used.- A scanning electron microscopy (SEM) is used to probe the general structure of the membranes andto determine the porosity of the skin layer using image analysis software. It allows magnificationsranged from × 25 to × 650,000 with resolution of 1.2 to 2.5 nm. Energy Dispersive X-rayspectrometry (EDX) can be combined to SEM observation.- An optical profilometer through white light interferometry (WLI) and an atomic force microscopy(AFM) are used in order to assess the surface state of membranes (roughness spectrum). WLI allowsobtaining image sizes from 360x360 μm~2 to 900×900 μm~2. Moreover, the AFM technique is used onsurfaces whose scan tip allows the study of zones ranging from 10x10 μm~2 to 40×40 μm~2. These twotechniques are complementary of each other for size scale observation.The structural properties of virgin flat sheet PES membrane were determined as a function ofcharacteristics of molecular weight cut-off (MWCO). The characteristics of surface determined by SEMshowed an increasing trend with MWCO. The use of WLI and AFM with different observation scalesshowed that the determination of the roughness of a membrane significantly depends on the observationscale. The AFM was able to differentiate membrane according to their MWCO as well as to the method ofmanufacturing. Structural characterizations by SEM/EDX and AFM techniques are particularly adapted tothe study of hollow fibers (in/out or out/in configuration): comparison of observations for virgin, fouledand cleaned membranes after operation on industrial site can give information about efficacy of cleaningprocedure, irreversible fouling (decrease in pore size, increase in surface roughness), ageing of membrane(increase of pore size linked to active skin deterioration or chemical degradation of polymer).These optical and microscopic techniques combined with others such as chemical observation of surface(FTIR), or hydraulic-dynamic tests (filtration tests, molecules or micro-organisms retention) can help toimprove the understanding of fouling and/or ageing phenomena occurring during drinking waterproduction in order to manage and minimize them. These methods of microscopic analysis requirecomplex equipments associated to expenses of maintenance. They require expert staff trained specificallyin the use of these tools, in the data processing and in the interpretation of the results.These methods can be used, as complementary tool to the services proposed by the dedicated laboratoryon the membrane testing platform of CIRSEE, called “Memlab" through collaboration with expert academic laboratories in Marseille and Paris Universities. This platform is oriented on the assessment ofall the MF/UF products of the market. It aims at evaluating membrane quality and durability for varioustreatment applications.
机译:成功开发超滤(UF)工艺的关键问题之一是结垢, 这是由于膜与膜中存在的各种成分之间的特定相互作用而产生的 水。已经研究了许多影响结垢的参数。它们可以分为两种 类别:膜的化学和结构参数以及水的特性。结构 膜的特性(粗糙度,孔隙率...)经过专门研究以开发结垢控制 方法。在这项工作中,首先使用了几种微观和光学方法来表征 手术后有机膜和第二次污损有机膜。 在这项工作中,获得了有关有机超滤PES清洁和结垢的平板膜的信息,具体方法如下: 截止值(10、30、100和300 kDa)与PVDF中空纤维(100 kDa)进行了比较。为了那个原因, 使用了不同的技术。 -扫描电子显微镜(SEM)用于探测膜的一般结构和 使用图像分析软件确定表皮层的孔隙率。它可以放大 范围从×25至×650,000,分辨率为1.2至2.5 nm。能量色散X射线 光谱法(EDX)可以与SEM观察结合使用。 -通过白光干涉仪(WLI)和原子力显微镜的光学轮廓仪 (AFM)用于评估膜的表面状态(粗糙度光谱)。 WLI允许 获得的图像尺寸从360x360μm〜2到900×900μm〜2。此外,AFM技术用于 扫描尖端允许研究10x10μm〜2到40×40μm〜2范围内的区域的表面。这两个 技术在大小尺度观察中是相互补充的。 确定原始纯平型PES膜的结构性能与 截留分子量(MWCO)的特性。 SEM测定的表面特性 MWCO呈上升趋势。 WLI和AFM在不同观察尺度下的使用 表明膜粗糙度的确定很大程度上取决于观察结果 规模。原子力显微镜(AFM)能够根据其MWCO以及分离膜的方法来区分膜 制造业。通过SEM / EDX和AFM技术进行的结构表征特别适合于 中空纤维的研究(内/外或外/内构型):原始,脏污观察结果的比较 和在工业现场操作后清洗过的膜可以提供有关清洗功效的信息 程序,不可逆的结垢(孔径减小,表面粗糙度增加),膜老化 (孔径的增加与皮肤的活性降解或聚合物的化学降解有关)。 这些光学和显微镜技术与其他技术相结合,例如表面化学观察 (FTIR)或水力动力学测试(过滤测试,分子或微生物保留)可以帮助 增进对饮用水中发生的结垢和/或老化现象的了解 生产以管理和最小化它们。这些微观分析方法要求 与维修费用有关的复杂设备。他们需要经过专门培训的专家人员 在使用这些工具,数据处理和结果解释中。 这些方法可以用作专用实验室建议的服务的补充工具 与马赛和巴黎大学的专家学术实验室合作,在CIRSEE的膜测试平台上称为“ Memlab”,该平台旨在评估 市场上所有的MF / UF产品。它旨在评估各种膜的质量和耐久性 治疗应用。

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