CN112221350B - 一种基于氢氧化锌纳米线的新型纳滤膜的制备方法 - Google Patents
一种基于氢氧化锌纳米线的新型纳滤膜的制备方法 Download PDFInfo
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 26
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 22
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Abstract
本发明公开了一种基于氢氧化锌纳米线的新型纳滤膜的制备方法,利用聚偏二氟乙烯膜(PVDF)为基底,将含有氢氧化锌纳米线和海藻酸钠的溶液分别抽滤在多孔基底上得到基于氢氧化锌纳米线的新型纳滤膜。本发明制备工艺简便、安全、成本低,操作易行,且制备的纳滤膜对有机染料有较好的分离性能和稳定性、脱盐率高,因此其在有机染料的去除和染料脱盐等方面具有广阔的应用前景。
Description
技术领域
本发明属于纳滤膜技术及水分离领域,具体涉及的是一种用于有机染料去除以及染料脱盐方面的基于氢氧化锌纳米线的新型纳滤膜的制备方法。
技术背景
水在单细胞生物、复杂植物、动物和人类的生存中起着至关重要的作用。随着工业活动的不断增加,水资源遭到污染或破坏。特别是合成染料工业的废水中含有大量芳香族化合物和有机染料,对水环境造成极大威胁。一般来说,制造纺织品、塑料、纸张、化妆品等都涉及大量有机染料的使用。每年大约有10-15%的纺织工业生产的有机染料被排放到环境中。这些有机染料大多数是有毒和致癌的,由于其稳定复杂的化学结构,在自然条件下很难分解,因此它们不仅可以污染水资源,而且还通过水和食物链对人类有致命的影响。
当前,膜分离技术是传统物理化学方法的一种替代方法,与吸附分离、蒸馏和重结晶等分离手段相比,膜分离又具有高效、节能、绿色及操作简单等优点。纳滤技术在脱盐、水净化、制药、生物技术、纺织行业等现代工业中发挥着非常重要的作用。与微滤和超滤相比,纳滤具有孔径更小的特点,有助于实现小分子筛选、有机溶剂回收、药物纯化等。此外,与反渗透工艺相比,纳滤具有更大的孔隙尺寸和更高的渗透率,以及更低的跨膜压力,从而降低了纳滤工艺的能耗。因此,纳滤膜被认为是处理染料废水的一种有竞争力的无污染排放方法。但是纳滤膜也存在耐化学性差、使用寿命有限等缺点,最重要的是由于孔隙结构紊乱,其发展常常被渗透性和选择性之间的权衡所阻碍。因此,寻找和设计高渗透性和高选择性的膜材料已成为一个迫切的问题。
海藻酸钠(SA)是从海藻酸中提取的一种天然多糖,具有优良的亲水性、胶性和成膜性能。氢氧化锌纳米线具有无害性和稳定性且合成过程快速,环境友好。为了提高膜的渗透性和选择性,本研究设计制备出氢氧化锌纳米线材料,并将SA涂覆在氢氧化锌纳米线薄膜上。氢氧化锌纳米线表面带有正电荷,可以吸附带有异性电荷或者电中性的染料分子。SA本身是亲水性材料且可与Zn2+离子通过配位键结合,形成稳定的水分子孔道,从而为设计成有机染料去除的纳滤膜提供了理想的材料基础。
发明内容
本发明的目的是提供一种基于氢氧化锌纳米线的新型纳滤膜的制备方法。
为实现上述发明目的,本发明采用如下技术方案:
一种基于氢氧化锌纳米线的新型纳滤膜的制备方法,包括如下步骤:
1)将乙醇胺的醇水溶液与硝酸锌的醇水溶液混合,在磁力搅拌和室温静置后得到氢氧化锌纳米线溶液,真空抽滤到聚偏二氟乙烯膜的表面得到氢氧化锌纳米线薄膜;
2)将海藻酸钠水溶液,真空抽滤到氢氧化锌纳米线薄膜表面,得到基于氢氧化锌纳米线的新型纳滤膜。
优选地,所述的聚偏二氟乙烯膜,其平均孔径为200nm;使用前需要用乙醇和水的混合液进行预处理。
优选地,所述的乙醇胺的醇水溶液的浓度为1~4mM,所述的硝酸锌溶液的浓度为2~6mM,所述的海藻酸钠水溶液的浓度为0.1~0.3g/mL。
优选地,所述的氢氧化锌纳米线溶液的具体制备方法为:将硝酸锌加入乙醇和水的混合液中,得到硝酸锌的醇水溶液;将乙醇胺加入乙醇和水的混合液中,得到乙醇胺的纯水溶液;将乙醇胺的醇水溶液快速加入硝酸锌水溶液中,室温下磁力快速搅拌5-10min后,静置30-60min得到氢氧化锌纳米线溶液。
优选地,所述的乙醇和水混合液中乙醇和水的体积比为1:1~3。
优选地,所述的氢氧化锌纳米线溶液为5-10mL。
优选地,所述的氢氧化锌纳米线中海藻酸钠的质量比为0.01%~0.2%,质量比过大或过小会造成所制备的膜通量低或选择性低,不利于纳滤膜的分离性能。
优选地,所述的真空抽滤的压力为1-5bar。
与现有技术相比,本发明的有益效果在于:本发明制备工艺简便,操作易行,无毒环保;制备的基于氢氧化锌纳米线的新型纳滤膜具有良好的有机染料去除的性能以及高效染料脱盐的性能。
附图说明
以下结合附图和本发明的实施方式来作进一步详细说明
图1为PVDF膜的表面SEM图;
图2为所制备的氢氧化锌纳米线薄膜的表面SEM图;
图3为所制备的基于氢氧化锌纳米线的新型纳滤膜的表面SEM图;
图4为所制备的不同体积的氢氧化锌纳米线薄膜对刚果红染料截留图;
图5为用不同质量比海藻酸钠所制备的纳滤膜对刚果红染料截留图;
图6为0.1%的海藻酸钠所制备的纳滤膜对不同染料截留图;MB为亚甲基蓝,CV为结晶紫,NC为新胭脂红,RB为刚果红,BB为考马斯亮蓝;
图7为0.1%的海藻酸钠所制备的纳滤膜对不同盐截留图。
具体实施方式
以下结合若干个具体实施例,示例性说明及帮助进一步理解本发明,但实施例具体细节仅是为了说明本发明,并不代表本发明构思下全部技术方案,因此不应理解为对本发明总的技术方案限定,一些在技术人员看来,不偏离发明构思的非实质性改动,例如以具有相同或相似技术效果的技术特征简单改变或替换,均属本发明保护范围。
实施例1-6:
采用德国Millipore公司生产的平均孔径约为200nm的聚偏二氟乙烯膜(PVDF)膜为基底,膜的有效直径为5cm,所用的溶剂均为超纯水;
1)首先对PVDF膜进行预处理,将PVDF膜浸泡在乙醇和水的体积比为1:3~1:1的混合溶液中30-60min后用纯水冲洗2-3遍待用;
2)取无水乙醇与超纯水的体积比为2:3进行混合,精确制备1L的混合液。将乙醇胺和硝酸锌分别溶解在该混合液中,制得浓度为1.6mmol/L的乙醇胺混合液和4mmol/L的硝酸锌混合液;
3)取10mL的乙醇胺混合液快速加入10mL的硝酸锌混合液中,室温下磁力搅拌5min后静置30min得到氢氧化锌纳米线溶液;
4)取5-10mL的纳米线溶液真空抽滤到PVDF膜上制备成氢氧化锌纳米线薄膜,压力为1bar;
5)将4)中所得的薄膜在纳滤装置中进行染料脱除性能测试,进料溶液为100mg/L的刚果红(Mw=696.66)水溶液,测试压力为1bar,测试温度为25℃。测得的氢氧化锌薄膜对刚果红的脱除性能如下:
实施例7-11:
采用德国Millipore公司生产的平均孔径约为200nm的聚偏二氟乙烯膜(PVDF)膜为基底,膜的有效直径为5cm,所用的溶剂均为超纯水。
如同上述实施例,优选体积为6mL的氢氧化锌纳米线溶液所制备的纳米线薄膜。制备海藻酸钠浓度为0.01%、0.05%、0.1%、0.15%、0.2%,真空抽滤到氢氧化锌纳米薄膜上制备基于氢氧化锌纳米线的新型纳滤膜。所得的纳滤膜在纳滤装置中进行染料脱除性能测试,进料溶液为100mg/L的刚果红(Mw=696.66)水溶液,测试压力为1bar,测试温度为25℃。测得的纳滤膜对刚果红的脱除性能如下:
实施例12-16:
采用德国Millipore公司生产的平均孔径约为200nm的聚偏二氟乙烯膜(PVDF)膜为基底,膜的有效直径为5cm,所用的溶剂均为超纯水。
如同上述实施例,优选浓度为0.1%的海藻酸钠所制备的基于氢氧化锌纳米线的新型纳滤膜,并在纳滤装置中进行染料脱除性能测试。进料溶液分别为100mg/L的亚甲基蓝(Mw=319.85)、结晶紫(Mw=407.98)、新胭脂红(Mw=604.47)、刚果红(Mw=696.66)和考马斯亮蓝G250(Mw=858.05)的水溶液,测试压力为1bar,测试温度为25℃。测得的纳滤膜对不同染料的脱除性能如下:
实施例17-20:
采用德国Millipore公司生产的平均孔径约为200nm的聚偏二氟乙烯膜(PVDF)膜为基底,膜的有效直径为5cm,所用的溶剂均为超纯水。
如同上述实施例,优选浓度为0.1%的海藻酸钠所制备的基于氢氧化锌纳米线的新型纳滤膜,并在纳滤装置中进行染料脱除性能测试。进料溶液分别为1000mg/L的NaCl、Na2SO4、MgCl2、MgSO4溶液,测试压力为1bar,测试温度为25℃。测得的纳滤膜对不同盐的脱除性能如下:
Claims (6)
1.一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:包括如下步骤:
1)将乙醇胺的醇水溶液与硝酸锌的醇水溶液混合,在磁力搅拌和室温静置后得到氢氧化锌纳米线溶液,真空抽滤到聚偏二氟乙烯膜的表面得到氢氧化锌纳米线薄膜;
2)将海藻酸钠水溶液,真空抽滤到氢氧化锌纳米线薄膜表面,得到基于氢氧化锌纳米线的纳滤膜;
所述的乙醇胺的醇水溶液的浓度为1~4 mM,所述的硝酸锌醇水溶液的浓度为2~6mM,所述的海藻酸钠水溶液的浓度为0.01 wt%、0.05 wt%、0.1 wt%、0.15 wt%或0.2 wt%。
2.如权利要求1所述的一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:所述的聚偏二氟乙烯膜,其平均孔径为200 nm;使用前需要用乙醇和水的混合液进行预处理。
3.如权利要求1所述的一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:所述的氢氧化锌纳米线溶液的具体制备方法为:将硝酸锌加入乙醇和水的混合液中,得到硝酸锌的醇水溶液;将乙醇胺加入乙醇和水的混合液中,得到乙醇胺的醇水溶液;将乙醇胺的醇水溶液快速加入硝酸锌醇水溶液中,室温下磁力快速搅拌5-10 min后,静置30-60 min得到氢氧化锌纳米线溶液。
4.如权利要求3所述的一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:所述的乙醇和水混合液中乙醇和水的体积比为1:1~3。
5.如权利要求1所述的一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:所述的氢氧化锌纳米线溶液为5-10 mL。
6.如权利要求1所述的一种基于氢氧化锌纳米线的纳滤膜的制备方法,其特征在于:所述的真空抽滤的压力为1-5 bar。
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