CN114870646A - 基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法 - Google Patents
基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于金属网‑陶瓷复合基膜的含油污水处理动态膜的制备方法。该制备方法采用多孔金属网作为动态膜基体，通过磁控溅射技术将亲水性材料陶瓷层均匀涂敷在金属网表面，形成亲水的金属网‑陶瓷复合基膜的动态膜。本发明制备方法制备得到动态膜能在确保动态膜高水通量的前提下，提高动态膜的抗油污染能力，延长动态膜酸碱等强清洗周期，减少设备运维成本和药剂消耗。
Description
技术领域
本发明属于污水处理领域，具体涉及一种基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法。
背景技术
随着经济发展我国对原油的需求量逐年增加，“增储上产”是油气开采行业需要解决的第一大问题。低渗和稠油等边际油田、进入开采中后期的油田在增储上产中扮演着不可或缺的作用。该部分油田开采难度大，为提高采收率，通常需要使用注水或注气技术方式开采。采出的原油含水率达70％～80％，有的甚至高达90％以上。因此，会产生大量难处理的高浓度含油污水，尤其是稠油污水，油水密度差小、黏度大、胶质、蜡质含量高、污染性强，对处理设备有较高要求。
动态膜具有通量大、截留能力强、抗污染性能好、清洗方便的优点，已成为高浓度含油污水处理技术的重要发展方向。常用动态膜基膜有粉体烧结金属基膜、金属烧结网基膜、陶瓷膜以及有机多孔膜等。金属烧结网孔径均一、孔隙率高，悬浮颗粒不易堵塞孔道，水处理通量大。但金属膜材料为疏水材料，在动态膜反冲洗阶段容易发生油污在膜表面富集，造成基膜的污染，需酸碱清洗恢复性能。陶瓷膜亲水性好，但是陶瓷膜孔隙率较金属网低，且孔径不均一，容易被悬浮颗粒堵塞，水处理通量偏低。
发明内容
本发明针对上述现有技术中存在的问题，提供一种基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法，保证基膜高孔隙率、大通量的同时增加膜表面亲水性、耐油污染性，该方法制备得到含油污水处理动态膜用于含油污水处理过程，延长动态膜酸碱清洗周期，降低动态膜含油污水处理运维成本。
为解决上述技术问题，本发明具体通过如下技术方案予以实现。
本发明提供了一种基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法，该制备方法包括：
1)制备金属网-陶瓷复合基膜
将陶瓷层材质通过磁控溅射法附着在金属网的一侧或两侧制得以金属网为主体结构、陶瓷层为表面修饰结构的金属网-陶瓷复合基膜；其中金属网材质为铁、铝、铜及其合金中的一种或几种，网孔径为1～100微米，所述陶瓷层材质为氧化铝、碳化硅、氮化硅、氮化硼中的一种或几种；所述陶瓷曾厚度为0.01微米～10微米；
2)基于金属网-陶瓷复合基膜的动态膜
将金属网-陶瓷复合膜为基膜，采用25～40微米涂层材料制备悬浮液，错流过滤20～40min，压差0.015～0.025MPa，制备得到含油污水处理动态膜；所述的涂层材料为涂层材料为陶瓷、氧化铝、高岭土、分子筛中的一种或几种。
本发明上述含油污水处理动态膜的制备方法中，所述金属网材质优选为铁及其合金。
本发明上述含油污水处理动态膜的制备方法中，所述金属网的孔径优选为10～50微米。
本发明上述含油污水处理动态膜的制备方法中，所述陶瓷层厚度为0.1～1.0微米。
本发明上述含油污水处理动态膜的制备方法中，所述陶瓷层附着在金属网的一侧。所述陶瓷层材质优选为氧化铝、碳化硅。
本发明上述含油污水处理动态膜的制备方法中，所述磁控溅射法包括以下步骤：
(1)金属网的清洗：将金属网在超声波中依次用溶剂A、溶剂B和去离子水清洗，然后用氮气或空气吹干，其中溶剂A为丙酮、正己烷、甲苯中的一种或几种，溶剂B为甲醇、乙醇、丙醇中的一种或几种；
(2)陶瓷靶材安装：将陶瓷靶材安装在磁控溅射靶上，溅射方向指向中心基片台；
(3)金属网安装及预处理：将清洗好的金属网放置于溅射仓的样品台中心，启动抽真空机组，将溅射仓抽真空，采用氩气对金属网表面进行离子清洗；
(4)喷涂陶瓷层：溅射仓在惰性气体保护下，开始镀膜，镀膜时间为1～60min。
本发明上述含油污水处理动态膜的制备方法中，磁控溅射法步骤4)的镀膜时间优选为10～30min。
所述金属网-陶瓷复合基膜的含油污水处理动态膜的涂层材料优选为氧化铝、陶瓷和高岭土。
本发明还提供了上述制备方法制得的基于金属网-陶瓷复合基膜的含油污水处理动态膜。
进一步，本发明还提供了基于金属网-陶瓷复合基膜的含油污水处理动态膜在油田含油污水处理中的应用。
本发明的有益效果如下：
本发明基于金属网-陶瓷复合基膜的含油污水处理动态膜，在多孔金属网表面涂敷一薄层亲水性陶瓷，在保持多孔金属网高水通量的同时，改善金属网的亲水性、抗油污染性，延长动态膜酸碱强清洗周期。膜制备过程简单，成本低，可广泛应用于含油污水处理过程。
具体实施方式
下面通过具体实施例对本发明进行说明，但本发明并不局限于此。
下述实施例中所使用的实验方法如无特殊说明，均为常规方法；下述实施例中所用的试剂、材料等，如无特殊说明，均可从商业途径得到。
实施例1：
采用孔径为20微米的不锈钢烧结网，不锈钢烧结网依次用丙酮、无水乙醇及去离子水超声清洗10min后，在干燥氮气中吹干。
将氧化铝陶瓷安装在磁控溅射靶上，溅射方向指向中心基片台，与竖直轴夹角30°，靶基距为100mm。将不锈钢网放置在溅射仓的样品台上关闭溅射仓舱门，溅射仓抽至真空。切换氩气至离子源，打开考夫曼离子源，对样品表面进行离子清洗300s。切换氩气至溅射室的通路，使溅射室内的工作气压保持在1Pa，设置溅射功率300W，开始镀膜，镀膜时间15min。得到厚度约0.23微米的陶瓷涂层。
以上述制备的不锈钢网-陶瓷复合膜为基膜，采用25微米氧化铝制备悬浮液，错流过滤30min，压差0.02MPa，制备得到含油污水处理动态膜。
油含量60～65mg/l的含油污水，在0.1MPa压差错流，水渗透通量620～630L/m2.h，产水油含量6～10mg/l，清洗周期48h，经50次水反清洗，产水油含量超过15mg/l。采用酸碱反清洗后，动态膜通量和产水指标恢复至初始水平。
实施例2：
采用孔径为30微米的不锈钢烧结网，不锈钢烧结网依次用丙酮、无水乙醇及去离子水超声清洗10min后，在干燥氮气中吹干。
将氧化铝陶瓷安装在磁控溅射靶上，溅射方向指向中心基片台，与竖直轴夹角30°，靶基距为100mm。将不锈钢网放置在溅射仓的样品台上关闭溅射仓舱门，溅射仓抽至真空。切换氩气至离子源，打开考夫曼离子源，对样品表面进行离子清洗300s。切换氩气至溅射室的通路，使溅射室内的工作气压保持在1Pa，设置溅射功率300W，开始镀膜，时间15min。得到厚度约0.23微米的陶瓷涂层。
以上述制备的不锈钢网-陶瓷复合膜为基膜，采用35微米氧化铝制备悬浮液，错流过滤30min，压差0.02MPa，制备得到含油污水处理动态膜。
油含量60～65mg/l的含油污水，在0.1MPa压差错流，水渗透通量710～720L/m2.h，产水油含量9～14mg/l，清洗周期48h，经35次水反清洗，产水油含量超过15mg/l。采用酸碱反清洗后，动态膜通量和产水指标恢复至初始水平。
实施例3：
采用孔径为20微米的铜网，铜网依次用丙酮、无水乙醇及去离子水超声清洗10min后，在干燥氮气中吹干。
将氧化铝陶瓷安装在磁控溅射靶上，溅射方向指向中心基片台，与竖直轴夹角30°，靶基距为100mm。将铜网放置在溅射仓的样品台上关闭溅射仓舱门，溅射仓抽至真空。切换氩气至离子源，打开考夫曼离子源，对样品表面进行离子清洗300s。切换氩气至溅射室的通路，使溅射室内的工作气压保持在1Pa，设置溅射功率300W，开始镀膜，时间10min。得到厚度约0.15微米的陶瓷涂层。
以上述制备的铜网-陶瓷复合膜为基膜，采用25微米氧化铝制备悬浮液，错流过滤30min，压差0.02MPa，制备得到含油污水处理动态膜。
油含量60～65mg/l的含油污水，在0.1MPa压差错流，水渗透通量630～640L/m2.h，产水油含量8～12mg/l，清洗周期48h，经40次水反清洗，产水油含量超过15mg/l。采用酸碱反清洗后，动态膜通量和产水指标恢复至初始水平。
实施例4：
采用孔径为20微米的不锈钢烧结网，不锈钢烧结网依次用丙酮、无水乙醇及去离子水超声清洗10min后，在干燥氮气中吹干。
将氧化锆陶瓷安装在磁控溅射靶上，溅射方向指向中心基片台，与竖直轴夹角30°，靶基距为100mm。将不锈钢网放置在溅射仓的样品台上关闭溅射仓舱门，溅射仓抽至真空。切换氩气至离子源，打开考夫曼离子源，对样品表面进行离子清洗300s。切换氩气至溅射室的通路，使溅射室内的工作气压保持在1Pa，设置溅射功率300W，开始镀膜，时间15min。得到厚度约0.0.25微米的陶瓷涂层。
以上述制备的不锈钢网-陶瓷复合膜为基膜，采用25微米高岭土制备悬浮液，错流过滤30min，压差0.02MPa，制备出动态膜。
油含量60～65mg/l的含油污水，在0.1MPa压差错流，水渗透通量580～600L/m2.h，产水油含量8～12mg/l，清洗周期48h，经45次水反清洗，产水油含量超过15mg/l。采用酸碱反清洗后，动态膜通量和产水指标恢复至初始水平。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
本发明未尽事宜为公知技术。
Claims (10)
1.一种基于金属网-陶瓷复合基膜的含油污水处理动态膜的制备方法，包括如下步骤：
1)制备金属网-陶瓷复合基膜
将陶瓷层材质通过磁控溅射法附着在金属网的一侧或两侧制得以金属网为主体结构、陶瓷层为表面修饰结构的金属网-陶瓷复合基膜；所述陶瓷层厚度为0.01微米～10微米；
其中金属网材质为铁、铝、铜及其合金中的一种或几种，金属网孔径为1～100微米，所述陶瓷层材质为氧化铝、碳化硅、氮化硅、氮化硼中的一种或几种；
2)基于金属网-陶瓷复合基膜的动态膜
将金属网-陶瓷复合膜为基膜，采用25～40微米氧化铝制备悬浮液，错流过滤20～40min，压差0.015～0.025MPa，制备得到含油污水处理动态膜。
2.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述金属网材质为铁及其合金。
3.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述金属网的孔径为10～50微米。
4.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述陶瓷层厚度为0.1～1.0微米。
5.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述陶瓷层附着在金属网的一侧。
6.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述陶瓷层材质为氧化铝或碳化硅。
7.根据权利要求1所述的含油污水处理动态膜的制备方法，其特征在于，所述的磁控溅射法包括以下步骤：
1)金属网的清洗：将金属网在超声波中依次用溶剂A、溶剂B和去离子水清洗，然后用氮气或空气吹干，其中溶剂A为丙酮、正己烷、甲苯中的一种或几种，溶剂B为甲醇、乙醇、丙醇中的一种或几种；
2)陶瓷靶材安装：将陶瓷靶材安装在磁控溅射靶上，溅射方向指向中心基片台；
3)金属网安装及预处理：将清洗好的金属网放置于溅射仓的样品台中心，启动抽真空机组，将溅射仓抽真空，采用氩气对金属网表面进行离子清洗；
4)喷涂陶瓷层：溅射仓在惰性气体保护下，开始镀膜，镀膜时间为1～60min。
8.根据权利要求7所述的含油污水处理动态膜的制备方法，其特征在于，所述步骤4)的镀膜时间为10～30min。
9.一种权利要求1～8所述的制备方法制得的基于金属网-陶瓷复合基膜的含油污水处理动态膜。
10.一种权利要求9所述的基于金属网-陶瓷复合基膜的含油污水处理动态膜在油田含油污水处理中的应用。
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