CN109046037A - 一种疏水纤维素基油水分离膜的制备方法 - Google Patents
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Abstract
本发明公开了一种疏水纤维素基油水分离膜的制备方法。采用方法的要点是将纤维素基材置于含硅烷的经乙醇溶解的正硅酸四乙酯溶液中,滴加氨水,对其表面进行疏水改性,制备疏水纤维素基油水分离膜。该方法快速、高效、成本低,适用于疏水纤维素基油水分离膜制备。本发明制备纤维素基油水分离膜材料的纤维素基材为纤维滤纸,成分主要为植物纤维,具有可再生、易降解等特点,材料成本低且纤维滤纸具有合适的孔隙,适用于油水分离过程;同时,膜分离技术在油水分离过程中无相变及二次污染、能耗较低,具有重要的环境效益。
Description
技术领域
本发明涉及一种疏水性膜的制备方法,特别涉及一种疏水纤维素基油水分离膜的制备方法,属于有机高分子材料技术领域。
背景技术
随着工业含油废水排放量的不断增加和溢油事件频发,含油废水的处理已成为世界性难题,寻求合适的方法来解决该问题已迫在眉睫。含油废水传统的净化技术包括气浮、吸附、絮凝、萃取等。然而,这些技术存在效率低、运行费用高、二次污染、回收能力差等问题。膜分离技术具有分离设备简单、能耗低等优点。具有疏水性的油水分离膜可实现从水中选择性吸收或过滤油且不产生二次污染,是一种有效的油水分离材料。
目前,已有多种材料制备的分离膜用于分离油水混合物,如金属网基材料、陶瓷材料、泡沫基材料和碳基材料等。纤维素作为自然界含量最为丰富的天然有机高分子化合物,具有可再生、易降解等特性,是一种环境友好的优质基材。因此,可以考虑选用纤维素滤纸作为基材用于油水分离膜的制备过程。
疏水表面的形成过程可分为两个阶段:(1)制造微纳米结构以增强表面粗糙度;(2)表面修饰降低表面能。基于该原理,已开发了各种技术,通过利用表面粗糙度和低能量的协同效应实现疏水膜的制备,包括化学气相沉积、电化学法、水热法和喷雾法等。然而,这些方法大多由于制备工艺复杂、成本高、实验条件苛刻等原因使其大规模应用受到限制。因此,研发一种简单有效的方法,制备具有可控形态和稳定疏水性能的纤维素基分离膜膜十分必要。
在疏水分离膜制备领域,中国专利(CN 107058985 A)“一种二氧化钛疏水膜的制备方法”将有机钛源溶解至乙酸乙醋,加入稳定剂、粘合剂、调节剂搅拌形成粘稠液,然后浸泡基材进行共煮、烧结,最后进行钝化超声和密封发泡处理,得到二氧化钛疏水膜;中国专利(CN 106833253 A)“一种疏水材料及其制备方法”所述疏水性材料由基材和疏水表面涂层构成,其中表面涂层由硬脂酸改性的氢氧化镁粉末和酚醛树脂构成,基材选自不锈钢网、玻璃、棉布、高强度织布、尼龙过滤网、聚合物薄膜、铝网、镍网和铜网;中国专利(CN107970789 A)“具有微纳米结构表面功能层的疏水膜及其制备方法”将结晶或半结晶聚合物粉末或颗粒干燥,将添加剂、有机溶剂及经过干燥的聚合物按重量百分比进行混合,恒温搅拌一段时间至混合均匀,在恒温脱泡后形成均一的铸膜液,将所得铸膜液经过刮膜装置刮制成膜,再停留于一定湿度的空气中一段时间以促进部分固液相转化,将初生膜浸没于凝固浴中,浸泡一段时间后晾干,制得的疏水膜表面具有特定尺寸微纳米凸起结构,提高了疏水膜的疏水性能;中国专利(CN 107174986 A)“一种静电纺丝疏水膜的制备方法”将三元共聚物聚四氟乙烯-共聚偏氟乙烯-共聚六氟丙烯溶解于有机溶剂中,搅拌、脱泡得到铸膜液,使用静电纺丝技术,制得疏水纳米纤维多孔膜。截至目前,还未见到利用纤维滤纸作为基材,通过在其表面进行疏水改性,进而制备疏水纤维素基油水分离膜的相关工艺技术出现。
发明内容
为了克服目前制备疏水性油水分离膜存在的分离效率低、二次污染、回收能力差、制备工艺复杂、实验条件苛刻等问题,本发明的目的是提供一种简单有效的疏水纤维素基油水分离膜的制备方法。
为实现上述目的,本发明的技术方案是采用以下步骤:
1)将10mL正硅酸四乙酯溶解于乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,将步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加氨水至烧杯中,超声分散1h,置于30-60℃水浴中反应60-150min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6h后取出,得到疏水纤维素基油水分离膜。
所述的乙醇为无水乙醇,其与正硅酸四乙酯的体积比为2-5:1。
所述的硅烷为正辛基三甲氧基硅烷、氨基丙基乙氧基硅烷、苯基丙基三甲氧基硅烷中的一种,乙醇与硅烷的体积比为2-5:1。
所述的氨水浓度为25wt%,其用量为2-10mL。
与背景技术相比,本发明具有的有益效果是:
本发明制备疏水纤维素基油水分离膜的纤维素基材为纤维滤纸,成分主要为植物纤维,具有可再生、易降解等特点,材料成本低,且具有合适的孔隙,适用于油水分离过程;同时,制备工艺简单、能耗低、成本低。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1:
1)将10mL正硅酸四乙酯溶解于20mL乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入10mL正辛基三甲氧基硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加4mL氨水至烧杯中,超声分散1h,置于30℃水浴中反应60min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6h后取出,得到疏水纤维素基油水分离膜(a)。
实施例2:
1)将10mL正硅酸四乙酯溶解于30mL乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入10mL苯基丙基三甲氧基硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加6mL氨水至烧杯中,超声分散1h,置于40℃水浴中反应90min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6h后取出,得到疏水纤维素基油水分离膜(b)。
实施例3:
1)将10mL正硅酸四乙酯溶解于40mL乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入10mL氨基丙基乙氧基硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加8mL氨水至烧杯中,超声分散1h,置于50℃水浴中反应120min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6h后取出,得到疏水纤维素基油水分离膜(c)。
实施例4:
1)将10mL正硅酸四乙酯溶解于50mL乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入10mL氨基丙基乙氧基硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加10mL氨水至烧杯中,超声分散1h,置于60℃水浴中反应150min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6h后取出,得到疏水纤维素基油水分离膜(d)。
测定实施例1、2、3、4制备的疏水纤维素基油水分离膜的水接触角,表1为实施例1、2、3、4制备的疏水纤维素基油水分离膜水接触角测定结果。由表1可以看出,制备的疏水纤维素基油水分离膜水接触角均达120°以上,表明该油水分离膜具有较好的疏水效果,有望为含油废水的油水分离处理提供环境友好的过滤材料,进而促进其达标排放。
表1
以上列举的仅是本发明的具体实施例。本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (4)
1.一种疏水纤维素基油水分离膜的制备方法,其特征在于,包括以下步骤:
1)将10 mL正硅酸四乙酯溶解于乙醇中,在机械搅拌作用下使其均匀分散,得到经乙醇溶解的正硅酸四乙酯溶液;
2)向步骤1)中得到的经乙醇溶解的正硅酸四乙酯溶液中加入硅烷,在机械搅拌作用下使其均匀分散,得到含硅烷的经乙醇溶解的正硅酸四乙酯溶液;
3)将纤维滤纸水平放置在烧杯底部,将步骤2)中得到的含硅烷的经乙醇溶解的正硅酸四乙酯溶液倒入烧杯,缓慢滴加氨水至烧杯中,超声分散1 h,置于30-60℃水浴中反应60-150 min,得到经疏水改性的纤维滤纸;
4)将步骤3)中得到的经疏水改性的纤维滤纸取出,乙醇清洗3次,放入105℃烘箱中6 h后取出,得到疏水纤维素基油水分离膜。
2.根据权利要求1所述的一种疏水纤维素基油水分离膜的制备方法,其特征在于:所述的乙醇为无水乙醇,其与正硅酸四乙酯的体积比为2-5:1。
3.根据权利要求1所述的一种疏水纤维素基油水分离膜的制备方法,其特征在于:所述的硅烷为正辛基三甲氧基硅烷、氨基丙基乙氧基硅烷、苯基丙基三甲氧基硅烷中的一种,乙醇与硅烷的体积比为2-5:1。
4.根据权利要求1所述的一种疏水纤维素基油水分离膜的制备方法,其特征在于:所述的氨水浓度为25 wt%,其用量为2-10 mL。
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