CN108570850B - 一种用于油水分离的稳定耐性优良的超润湿织布的制备方法 - Google Patents
一种用于油水分离的稳定耐性优良的超润湿织布的制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于油水分离的稳定耐性优良的超润湿织布的制备方法,该方法包括织物的前处理,氧化锌纳米棒的生长,低表面能物质的修饰等步骤。该研究通过控制织布上氧化锌的生长和选择不同的修饰剂来实现超疏水、超亲水和超双疏性能,且在加热、酸碱、磨损实验和紫外照射下具备良好的稳定性能。此外,这种纸可以用于分离油水混合物,不仅可以实现轻油、重油和水的分离,而且可达到油水的按需分离。本发明制备工艺简单,可控易得,稳定性强,适合大面积制备和应用,既适用于日常生活中的应用,同时也适用于油水分离等工业领域。
Description
技术领域
本发明属于超疏水织布、超亲水织布和超双疏织布制备技术领域,特别涉及可制备稳定的耐性优良的可用于油水分离的超润湿织布的制备方法。
背景技术
超润湿特别是超疏水现象在自然界存在广泛,如荷叶表面、蝴蝶翅膀、水黾腿等。超疏水材料表面对水的接触角大于150°、滚动角小于10°的表面。超疏水材料具有很多独特优异的表面性能:疏水、自清洁性、防腐、抗结冰、防雾等特性,使得其在众多领域都具有巨大的应用前景。
实现油水分离则是超疏水的一大应用之一。油水分离的实现对减小水分和杂质对油的品质的影响,以及解决非水溶性油渍对江河湖海污染问题等都有着重要意义。利用超疏水这种特殊湿润性,可以使油顺利通过而水完全不通过,可以实现有效地分离油水混合物。现在已经有不少研究者将超疏水应用于油水分离。中国专利CN101708384A采用湿法化学刻蚀技术,在由微米级孔径的金属网表面制备出纳米尺度的微观突起,然后在其表面修饰具有低表面能的化合物,从而制成具有超疏水性质的金属网,可有效实现油水分离。中国专利CN101518695A采用浸涂的方法,利用一定的条件和固化剂,将环氧基封端的低聚硅氧烷与双酚A 共聚,把该聚硅氧烷-双酚A共聚物与固化剂混匀配成溶液,将聚硅氧烷-双酚 A共聚物固化于100~400目的织物网上制得具有超疏水与超亲油功能的油水分离网膜。虽然这里技术方案都具有油水分离效果,但也存在着不足,如制备方法复杂,制备出的超疏水基材稳定性差,不能反复使用,或使用金属网做基材,成本高,且不具备普适性等。
发明内容
本发明的目的是提供一种简单、方便的工业化生产超疏水、超亲水和超双疏织布的方法,解决超润湿材料制备步骤繁杂,耐候性差,实用性低,耐磨性差的问题。通过简单的方法制备了具有良好稳定性,耐磨、耐紫外、耐酸碱、耐高温的超疏水、超亲水织布,获得的超疏水、超亲水织布具备良好的油水分离能力。
本发明采用前处理-生长水热两步法使ZnO纳米阵列生长在纤维织布表面上,通过改变晶体生长溶液浓度控制ZnO纳米棒阵列的长径比,从而制备ZnO 纳米棒和纳米针。为了提高晶体层与织物基体表面的粘附性,选择两种硅烷偶联剂(疏水型TTOP-12和亲水型KH550)加入到前处理溶液中,制备特殊润湿性表面。根据改变硅烷偶联剂的种类、控制ZnO晶体形态和低表面能改性剂的不同选择,成功实现了纤维织物的超疏水性、超亲水性和超双疏性等多种润湿性。为了在实际生产中应用,在不同的测试环境下,包括机械性能、化学性能、高温性能和紫外线照射下的对这种表面的耐受性和耐久性进行了研究和测量。利用对水和油润湿性的不同,可以根据需要高效地分离油水,具有很大的灵活性,有望用于处理油水混合物。
实现本发明目的的技术方案是:一种用于油水分离的稳定耐性优良的超润湿织布的制备方法,其特征在于,所述方法包括如下步骤:
A.织布的前处理:称量乙酸锌加入异丙醇中并加热搅拌,溶解后加入三乙胺混合,形成乳白色溶液后冷却至室温;然后称取上述溶液,加入疏水型硅烷偶联剂TTOP-12搅拌混合后形成混合溶液甲,或者加入亲水型硅烷偶联剂KH550 搅拌混合后形成混合溶液乙,将溶液甲或者乙中加入超声清洗后的织布,浸泡5 min后取出在120℃晾干备用;
B.纳米氧化锌的生长:配制等浓度的硝酸锌和六次亚甲基四胺水溶液,等体积混合后搅拌30min得到氧化锌生长溶液,将前处理后的织布垂直放入上述生长液中,在95℃油浴中反应8h,常温下放置12h,从而完成纳米氧化锌的生长;
C.低表面能物质修饰:将步骤B中的织布取出,反复用蒸馏水冲洗然后干燥处理;
若前处理加入的是亲水型硅烷偶联剂KH550,无须再处理,即可得超亲水织布;
若前处理加入的是疏水型硅烷偶联剂TTOP-12,之后将织布浸入到硬脂酸乙醇溶液中2h获得超疏水性能;或者若前处理加入的是亲水型硅烷偶联剂KH550,将织布浸入全氟辛酸乙醇溶液中24h获得超双疏性能;然后将织布取出,用无水乙醇洗涤后在真空干燥箱60℃干燥,即可得到超疏水织布或者超双疏织布。
进一步地,前处理溶液中乙酸锌和三乙胺的浓度均为0.1mol/L。
进一步地,添加的硅烷偶联剂TTOP-12和硅烷偶联剂KH550与前处理溶液的比率分别为1.5w%和2w%。
进一步地,超疏水织布的生长溶液中,硝酸锌水溶液和六次亚甲基四胺的最佳浓度为0.15mol/L。
进一步地,超亲水织布的生长溶液中,硝酸锌水溶液和六次亚甲基四胺的最佳浓度为0.05mol/L。
进一步地,超双疏织布的生长溶液中,硝酸锌水溶液和六次亚甲基四胺的最佳浓度为0.025mol/L。
进一步地,硬脂酸乙醇溶液的浓度为0.05mol/L。
进一步地,全氟辛酸乙醇溶液的浓度为0.005mol/L。
本发明的有益效果是:与现有技术相比,本发明的优点在于:
1.工艺简单,原料易得,成本低廉;
2.制备的超疏水和超亲水织布具有良好的耐磨性,化学稳定性,耐热性和耐紫外性能;
3.制备的超疏水织物具有超疏水/超亲油性,水的接触角大于150°,滚动角小于10°,油的接触角约为0°,超亲水织物具有水下超疏油/油下超疏水性,水中油的接触角大于150°,油中水的接触角大于150°;
4.该超疏水和超亲水织布可用于油水分离;
5.该超润湿织布机械强度大,可反复使用,使用寿命长。
附图说明
图1:实施例1、2、3所得从原始织布到超疏水、超亲水和超双疏织布的制备流程示意图;
图2:前处理溶液中加入硅烷偶联剂的实物图,其中图( a) 为实施例1中加入的TTOP-12型硅烷偶联剂,图( b) 为实施例2、3中加入KH550型硅烷偶联剂;
图3:超疏水、超亲水和超双疏织布对不同溶液(水、茶、咖啡、牛奶、油) 的润湿情况及接触角图片,其中图( a) 为实施例1的超疏水织布,图a1和a2分别为水的接触角和滚动角照片,图( b) 为实施例2的超亲水织布,图b1和b2分别为水下油的接触角和油下水的接触角,图( c) 为实施例3的超双疏织布,图c1和c2 分别为水的接触角和油的接触角;
图4:实施例1所得的超疏水织布的扫描电镜图片;
图5:实施例2、3所得的织布表面的扫描电镜图片,其中图( a) 、( b) 为实施例 2所得的超亲水织布表面,图( c) 、( d) 为实施例3所得的超双疏织物表面;
图6:实施例1所得的超疏水织布和实施例2所得的超亲水织布的热稳定性、化学稳定性、机械稳定性和紫外稳定性的测试表征;
图7:实施例1所得的超疏水织布和实施例2所得的超亲水织布的油水分离装置;
图8:实施中所得超润湿织布的油水分离效率、通量和循环测试,其中图( a) 为实施例1所得的超疏水织布的油水分离效率、通量和循环测试,图( b) 为实施例 2所得的超亲水织布的油水分离效率、通量和循环测试。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样在本申请所列权利要求书限定范围之内。
实施例1:
1,织布的前处理:称量0.1mol/L乙酸锌加入50mL异丙醇中并加热搅拌,溶解后加入0.1mol/L三乙胺混合,形成乳白色溶液后冷却至室温。然后称取上述溶液20g加入1.5wt%疏水型硅烷偶联剂TTOP-12,搅拌混合后加入超声清洗后的织布,浸泡5min后取出在120℃晾干备用。
2,纳米氧化锌的生长:配制0.15mol/L的硝酸锌和0.15mol/L六次亚甲基四胺水溶液,各取50mL混合后搅拌30min得到氧化锌生长溶液,将前处理后的织布垂直放入上述生长液中,在95℃油浴中反应8h,常温下放置12h,从而完成纳米氧化锌的生长。
3,低表面能物质修饰:将步骤B中的织布取出,反复用蒸馏水冲洗然后干燥处理。之后将织布浸入0.05mol/L硬脂酸乙醇溶液中2h,用无水乙醇洗涤后在真空干燥箱60℃干燥获得超疏水织布。
实施例2:
1,织布的前处理:称量0.1mol/L乙酸锌加入50mL异丙醇中并加热搅拌,溶解后加入0.1mol/L三乙胺混合,形成乳白色溶液后冷却至室温。然后称取上述溶液20g加入2wt%亲水型硅烷偶联剂KH550,搅拌混合后加入超声清洗后的织布,浸泡5min后取出在120℃晾干备用。
2,纳米氧化锌的生长:配制0.05mol/L的硝酸锌和0.05mol/L六次亚甲基四胺水溶液,各取50mL混合后搅拌30min得到氧化锌生长溶液,将前处理后的织布垂直放入上述生长液中,在95℃油浴中反应8h,常温下放置12h,从而完成纳米氧化锌的生长。
3,干燥处理:将步骤2中的织布取出,反复用蒸馏水冲洗然后干燥处理。无须再处理,即可得超亲水织布。
实施例3:
1,织布的前处理:称量0.1mol/L乙酸锌加入50mL异丙醇中并加热搅拌,溶解后加入0.1mol/L三乙胺混合,形成乳白色溶液后冷却至室温。然后称取上述溶液20g加入2wt%亲水型硅烷偶联剂KH550,搅拌混合后加入超声清洗后的织布,浸泡5min后取出在120℃晾干备用。
2,纳米氧化锌的生长:配制0.025mol/L的硝酸锌和0.025mol/L六次亚甲基四胺水溶液,各取50mL混合后搅拌30min得到氧化锌生长溶液,将前处理后的织布垂直放入上述生长液中,在95℃油浴中反应8h,常温下放置12h,从而完成纳米氧化锌的生长。
3,低表面能物质修饰:将步骤2中的织布取出,反复用蒸馏水冲洗然后干燥处理。之后将织布浸入0.005mol/L全氟辛酸乙醇溶液中24h,用无水乙醇洗涤后在真空干燥箱60℃干燥获得超双疏织布。
本发明包括织物的前处理,氧化锌纳米棒的生长,低表面能物质的修饰等步骤。该研究通过控制织布上氧化锌的生长和选择不同的修饰剂来实现超疏水、超亲水和超双疏性能,且在加热、酸碱、磨损实验和紫外照射下具备良好的稳定性能。此外,这种纸可以用于分离油水混合物,不仅可以实现轻油、重油和水的分离,而且可达到油水的按需分离。本发明制备工艺简单,可控易得,稳定性强,适合大面积制备和应用,既适用于日常生活中的应用,同时也适用于油水分离等工业领域。
最后应当说明的是,以上内容仅用以说明本发明的技术方案,而非对本发明保护范围的限制,本领域的普通技术人员对本发明的技术方案进行的简单修改或者等同替换,均不脱离本发明技术方案的实质和范围。
Claims (1)
1.一种用于油水分离的稳定耐性优良的超润湿织布的制备方法,其特征在于,所述方法包括如下步骤:
A.织布的前处理:称量乙酸锌加入异丙醇中并加热搅拌,溶解后加入三乙胺混合,其中乙酸锌和三乙胺的浓度均为0.1mol/L,形成乳白色溶液后冷却至室温;然后称取上述溶液,加入疏水型钛酸酯偶联剂TTOP-12搅拌混合后形成混合溶液甲,或者加入亲水型硅烷偶联剂KH550搅拌混合后形成混合溶液乙,其中添加的钛酸酯偶联剂TTOP-12和硅烷偶联剂KH550与前处理溶液的比率分别为1.5w%和2w%,将溶液甲或者乙中加入超声清洗后的织布,浸泡5min后取出在120℃晾干备用;
B.纳米氧化锌的生长:配制等浓度的硝酸锌和六次亚甲基四胺水溶液,硝酸锌和六次亚甲基四胺水溶液的浓度为0.15mol/L或0.05mol/L或0.025mol/L,等体积混合后搅拌30min得到氧化锌生长溶液,将前处理后的织布垂直放入上述生长液中,在95℃油浴中反应8h,常温下放置12h,从而完成纳米氧化锌的生长;
C.低表面能物质修饰:将步骤B中的织布取出,反复用蒸馏水冲洗然后干燥处理;
若前处理加入的是亲水型硅烷偶联剂KH550,无须再处理,即可得超亲水织布;
若前处理加入的是疏水型钛酸酯偶联剂TTOP-12,之后将织布浸入到浓度为0.05mol/L的硬脂酸乙醇溶液中2h获得超疏水性能;或者若前处理加入的是亲水型硅烷偶联剂KH550,将织布浸入浓度为0.005mol/L的全氟辛酸乙醇溶液中24h获得超双疏性能;然后将织布取出,用无水乙醇洗涤后在真空干燥箱60℃干燥,即可得到超疏水织布或者超双疏织布。
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