CN105664732A - 一种有机正渗透膜的制备方法 - Google Patents
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Abstract
本发明公开了一种有机正渗透膜的制备方法,其制备方法中均加有纳米粒子,具体制备分为配比、搅拌、静置、涂覆等几个步骤。本发明制成的有机正渗透膜不仅显著提高了膜的亲水性,减少了内浓差极化,提高渗透通量,保留了高的截留率,显著增加抗菌性能且由于纳米粒径,也增强了膜的强度,更加实用。
Description
技术领域
本发明涉及一种渗透膜的制备方法,尤其涉及一种有机正渗透膜的制备方法,属于膜分离技术领域。
背景技术
FO(ForwardOsmosis)技术是一种渗透驱动膜过程,具有低能耗、低污染、高回收等特点,在海水淡化,废水处理,能源发电,食品加工,药物浓度等领域有着现实或潜在的应用前景。然而,由于缺乏高效的FO膜材料,极大地制约FO技术的发展。目前用于FO过程的膜材料都具有非对称结构,由薄的选择分离层和多孔支撑层组成,在FO过程中都存在外浓差极化和内浓差极化,尤其是内浓差极化,导致FO膜实际水通量远远小于理论水通量。通常情况下,外浓差极化发生在膜与溶液的界面处,可以通过增加流速等流体力学得以缓解;内浓差极化发生是FO过程所特有的现象,在FO过程中根据膜的取向,溶质在膜多孔支撑层内积累或稀释,形成浓缩和稀释的内浓差极化,极大的降低了膜两侧的有效渗透压差。内浓差极化发生在多孔支撑层内,难以通过改变外界条件而缓解。研究表明内浓差极化与膜多孔支撑层结构(孔隙率、孔弯曲度、膜厚度)以及膜材料本身的物理化学性质(亲疏水性、选择性)有很大的关系。支撑层厚度越小,孔隙率越高,孔弯曲度越小,亲水性越好,则膜结构参数则越小,内浓差极化越小。
现有的方法制作的有机正渗透膜其亲水性差,内浓差极化大,渗透通量小,截留率低且抗菌性差、膜的强度不高、实用性能不好。
发明内容
为了解决上述问题中的不足之处,本发明提供了一种有机正渗透膜的制备方法。
为解决以上技术问题,本发明采用的技术方案是:一种有机正渗透膜的制备方法,其制备方法为:
按体积百分比计,采用三醋酸纤维素作为聚合物,将13.1%三醋酸纤维素和0.9%的甲壳素纳米晶加入到由57.8%的1,4-二氧六环、19.6%的丙酮和8.6%的甲醇组成的混合溶剂中,在60℃的温度下搅拌9个小时溶解形成含量为0.9%的甲壳素纳米晶的铸膜液;静置24h以上使其完全脱泡;将铸膜液搅拌均匀经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将基材上的底模层在空气中静置30秒,然后将底膜层放入凝胶浴中经相转化凝胶成具有致密皮层的膜,并将膜在50℃水浴中热处理5分钟,清洗之后,得到有机正渗透膜并放在1%亚硫酸氢钠溶液中保存备用;
或按体积百分比计,采用二醋酸纤维素作为聚合物,将12.2%二醋酸纤维素和0.8%的1-芘丁酸纳米粒子加入到由55.1%的1,4-二氧六环、20.6%的丙酮、7.2%的甲醇和4.2%的乳酸混合成的混合溶剂中,在70℃的温度下搅拌24个小时溶解形成0.9%的甲壳素纳米晶的铸膜液;静置24h以上使其完全脱泡;超声分散30min;将铸膜液搅拌均匀经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将基材上的底膜层在空气中静置15秒,然后将底膜层放入凝胶浴中经相转化凝胶成具有致密皮层的膜,将所制备的膜用去离子水清洗,除去残余的有机溶剂,制得有机正渗透膜,并将膜在60℃水浴中热处理10min,充分清洗之后,得到有机正渗透膜并放在1%亚硫酸氢钠溶液中保存备用;
或按重量计,称取20g聚砜聚合物,溶解在80g由N,N-二甲基乙酰胺和聚乙二醇400组成的混合溶剂中,N,N-二甲基乙酰胺和聚乙二醇400的比例为72:8,配成聚合物浓度为20%的聚砜溶液;向配好的聚砜溶液中加入1g有机碳纳米管,在超声中分散30分钟配成含有1wt%的有机碳纳米管的铸膜液,将铸膜液搅拌均匀、经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将底模层放入凝胶浴中凝胶成膜,采用间苯二胺和均苯三甲酰氯在形成的膜上进行界面聚合反应,在110℃下反应3分钟;界面聚合反应后将所制备的膜用去离子水清洗,除去残余的有机溶剂,从而制得有机正渗透膜;
基材选自聚酯筛网、无纺布、棉、玻璃板、流延板之一或其组合。
方法的制备中均加有纳米粒子;纳米粒子选自甲壳素纳米晶、纳米有机硅、有机碳纳米管、芘衍生物纳米粒子或其组合。
膜液中聚合物的含量按铸膜液的总重量计为10-18wt%或10-20wt%或10-22wt%;所述铸膜液中纳米粒子的含量按铸膜液总重量计为0.04-20wt%或0.05-10wt%或0.1-5wt%。
底膜层的厚度为60-200μm。
本发明制成的有机正渗透膜不仅显著提高了膜的亲水性,减少了内浓差极化,提高渗透通量,保留了高的截留率,显著增加抗菌性能且由于纳米粒径,也增强了膜的强度,更加实用。
具体实施方式
以下结合实施例对本发明作进一步详细描述,有机正渗透膜的制备步骤如下:
制备方法:
实施例1:
采用三醋酸纤维素作为聚合物,将13.1%(V%)三醋酸纤维素和0.9%(V%)的甲壳素纳米晶加入到由57.8%(V%)的1,4-二氧六环、19.6%(V%)的丙酮和8.6%(V%)的甲醇组成的混合溶剂中,在60℃的温度下搅拌9个小时溶解形成含量为0.9%(V%)的甲壳素纳米晶的铸膜液;静置24h以上使其完全脱泡;将铸膜液搅拌均匀经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将基材上的底模层在空气中静置30秒,然后将底膜层放入凝胶浴(凝胶浴的成分为去离子水)中经相转化凝胶成具有致密皮层的膜,并将膜在50℃水浴中热处理5分钟,清洗之后,放在1%亚硫酸氢钠溶液中保存备用。
本实施例制备的有机正渗透膜的通量为19L·m-2·h-1,截留率在90%以上。
所制备的有机正渗透膜与不加纳米有机粒子的膜在相同的条件下进行微生物污染与强度实验。在膜表面加上大肠杆菌微生物,经过24h后采用显微镜观察膜表面的微生物附着情况,发现加入纳米有机粒子的膜无微生物附着而未加的膜表面附着了大量的微生物,表明了加入纳米有机粒子的膜具有明显的抗菌性,抗菌率大于90%。将膜在万能试验机上测试拉伸强度,将有机正渗透膜与不加纳米有机粒子的膜在相同的条件下对比,发现有机正渗透膜拉伸强度提高30%。
实施例2:
采用二醋酸纤维素作为聚合物,将12.2%(V%)二醋酸纤维素和0.8%(V%)的1-芘丁酸纳米粒子加入到由55.1%(V%)的1,4-二氧六环、20.6%(V%)的丙酮、7.2%(V%)的甲醇和4.2%(V%)的乳酸混合成的混合溶剂中,在70℃的温度下搅拌24个小时溶解形成0.9%(V%)的甲壳素纳米晶的铸膜液;静置24h以上使其完全脱泡;超声分散30min;将铸膜液搅拌均匀经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将基材上的底膜层在空气中静置15秒,然后将底膜层放入凝胶浴中经相转化凝胶成具有致密皮层的膜,将所制备的膜用去离子水清洗,除去残余的有机溶剂,制得有机正渗透膜,并将膜在60℃水浴中热处理10min,充分清洗之后,放在1%亚硫酸氢钠溶液中保存备用。
本实施例制备的有机正渗透膜的水通量为17L·m-2·h-1。
对所制备的膜进行微生物污染与强度实验,在膜表面加上大肠杆菌微生物,经过24h后采用显微镜观察膜表面的微生物附着情况,发现其表面较少微生物附着,表明该膜具有一定的抗菌性能,抗菌率大于90%。将膜在万能试验机上测试拉伸强度,将有机正渗透膜与不加纳米有机粒子的膜在相同的条件下对比,发现有机正渗透膜拉伸强度提高40%。
实施例3:
称取20g聚砜聚合物,溶解在80g由N,N-二甲基乙酰胺和聚乙二醇400组成的混合溶剂中(二者比例为72:8),配成聚合物浓度为20%的聚砜溶液;向配好的聚砜溶液中加入1g有机碳纳米管,在超声中分散30分钟配成含有1wt%的有机碳纳米管的铸膜液,将铸膜液搅拌均匀、经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将底模层放入凝胶浴中凝胶成膜,采用间苯二胺和均苯三甲酰氯在形成的膜上进行界面聚合反应,在110℃下反应3分钟;界面聚合反应后将所制备的膜用去离子水清洗,除去残余的有机溶剂,从而制得有机正渗透膜。
本实施例制备的有机正渗透膜的水通量为17L·m-2·h-1,截留率在90%以上。
对所制备的膜进行微生物污染实验,在膜表面加上大肠杆菌微生物,经过24h后采用显微镜观察膜表面的微生物附着情况,发现其表面无微生物附着,表明该膜具有明显的抗菌性能,抗菌率大于90%。将膜在万能试验机上测试拉伸强度,将有机正渗透膜与不加纳米有机粒子的膜在相同的条件下对比,发现有机正渗透膜拉伸强度提高25%。
基材选自聚酯筛网、无纺布、棉、玻璃板、流延板之一或其组合。
纳米粒子选自甲壳素纳米晶、纳米有机硅、有机碳纳米管、芘衍生物纳米粒子或其组合。
铸膜液中聚合物的含量按铸膜液的总重量计为10-18wt%或10-20wt%或10-22wt%;铸膜液中纳米粒子的含量按铸膜液总重量计为0.04-20wt%或0.05-10wt%或0.1-5wt%。
底膜层的厚度为60-180μm或60-200μm。
Claims (4)
1.一种有机正渗透膜的制备方法,其特征在于:其制备方法为:
按重量计,称取20g聚砜聚合物,溶解在80g由N,N-二甲基乙酰胺和聚乙二醇400组成的混合溶剂中,N,N-二甲基乙酰胺和聚乙二醇400的比例为72:8,配成聚合物浓度为20%的聚砜溶液;向配好的聚砜溶液中加入1g有机碳纳米管,在超声中分散30分钟配成含有1wt%的有机碳纳米管的铸膜液,将铸膜液搅拌均匀、经静置脱泡后涂覆在基材上,并采用刮刀均匀的刮在基材上形成底膜层,将底模层放入凝胶浴中凝胶成膜,采用间苯二胺和均苯三甲酰氯在形成的膜上进行界面聚合反应,在110℃下反应3分钟;界面聚合反应后将所制备的膜用去离子水清洗,除去残余的有机溶剂,从而制得有机正渗透膜。
2.根据权利要求1所述的有机正渗透膜的制备方法,其特征在于:所述基材选自聚酯筛网、无纺布、棉、玻璃板、流延板之一或其组合。
3.根据权利要求1所述的有机正渗透膜的制备方法,其特征在于:所述方法的制备中均加有纳米粒子;所述纳米粒子选自甲壳素纳米晶、纳米有机硅、有机碳纳米管、芘衍生物纳米粒子或其组合。
4.根据权利要求1所述的有机正渗透膜的制备方法,其特征在于:所述底膜层的厚度为60-200μm。
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