CN106890631B - 一种pH-磁双重响应性染料吸附剂、制备方法及其应用 - Google Patents

一种pH-磁双重响应性染料吸附剂、制备方法及其应用 Download PDF

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CN106890631B
CN106890631B CN201710260091.6A CN201710260091A CN106890631B CN 106890631 B CN106890631 B CN 106890631B CN 201710260091 A CN201710260091 A CN 201710260091A CN 106890631 B CN106890631 B CN 106890631B
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胡静
张玉迪
花琴
邓维钧
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Abstract

本发明公开了一种pH‑磁双重响应性染料吸附剂的制备方法及其应用。本发明通过将甲基丙烯酸二乙基氨基乙酯，1,6‑己二醇二丙烯酸酯和光引发剂加入四氧化三铁磁液中，经超声细胞机粉碎和均质搅拌后加入光引发剂制备pH‑磁双重响应性染料吸附剂。将本发明制备的吸附剂用于染料吸附，吸附率高达96.49％，磁分离后通过pH响应性控制染料的可逆释放，释放率高达87.41％，可进行循环使用。该制备方法原料易得，工艺简单，应用前景广阔。

Description

一种pH-磁双重响应性染料吸附剂、制备方法及其应用
技术领域
本发明属于化工技术领域，具体来说是一种pH-磁双重响应性染料吸附剂、制备方法及其应用。
背景技术
染料是能够使纤维和其他被着色物质获得鲜艳牢固颜色的一类有机化合物，是典型的精细化工产品。印染、造纸和纺织等行业每年消耗大量染料，排放的废水中有机物浓度高、组分复杂、难降解物多、降解产物有毒有害、对环境危害大。
目前常用的染料废水处理方法主要有吸附法，絮凝法和化学氧化法等。其中吸附法由于成本相对较低、可避免二次污染和无毒副作用等优势而成为使用最广泛的一种方法。常用吸附剂主要有(1)活性炭吸附剂，这类吸附剂具有多孔结构，对大部分染料具有良好的吸附效果，但再生困难，重复利用性差，且对大分子染料的吸附效果差；(2)天然吸附剂，这类吸附剂由天然产品如木纤维，树皮，黏土，天然沸石等天然产物组成，具有价廉易得，无毒等优点，但再生困难，吸附量普遍较低，使用范围受到较大限制。因此，制备可再生重复利用的高效吸附剂显得尤为重要。
磁分离技术是借助磁场力的作用，对不同磁性的物质进行分离的一种技术。磁性纳米材料是纳米材料中重要的一类，纳米Fe3O4具有优越的磁性能和生物相容性，良好的热稳定性以及机械稳定性，制备工艺简单，价格低廉，无毒无污染，已被应用于染料废水处理。如申请号为201510569805.2的中国专利申请制备了一种磁性纳米吸附剂去除混合溶液中的阴离子组分。然而，磁性颗粒表面之间具有很强的范德华力，往往易于发生团聚，导致其在溶液中稳定性差而不能直接应用。将聚合物与磁性颗粒结合可改善磁性颗粒的团聚问题。pH响应性聚合物的体积和形态因外界pH值的变化而产生改变，当外界刺激消失时，pH响应性聚合物又恢复原状。由此可见将磁性和pH响应性结合制备一种双重响应可重复利用的吸附剂还鲜见报道。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种pH-磁双重响应性染料吸附剂、制备方法及其应用。本发明采用Pickering乳液法，以四氧化三铁Fe3O4纳米颗粒为稳定剂对pH响应单体甲基丙烯酸二乙基氨基乙酯进行乳化，随后通过紫外光引发一步制备了Fe3O4/聚(甲基丙烯酸二乙基氨基乙酯)纳米复合微球，作为具有磁性和pH双重响应性的染料吸附剂。本发明的吸附剂可对染料进行多次反复吸附和解吸附，循环使用。
本发明的技术方案具体介绍如下。
本发明提供一种pH-磁双重响应性染料吸附剂，其是四氧化三铁Fe3O4纳米颗粒和聚(甲基丙烯酸二乙基氨基乙酯)形成的复合物。
本发明还提供一种上述pH-磁双重响应性染料吸附剂的制备方法，具体步骤如下：
(1)取1-1.5g固含量为55～65％的Fe3O4纳米颗粒分散液超声均匀，加入35-60g去离子水，2-3g交联剂，0.1-0.15g光引发剂和1.5-4g甲基丙烯酸二乙基氨基乙酯，将混合液超声处理10-15min，均质2-5min，随后在惰性气氛保护下，搅拌20-40min，最终得到以四氧化三铁Fe3O4纳米颗粒为稳定剂的Pickering乳液；
(2)将步骤(1)得到的Pickering乳液在紫外灯下照射40-60min，得到pH-磁双重响应性染料吸附剂。
本发明中，步骤(1)中，交联剂为1，6-己二醇二丙烯酸酯。
本发明中，步骤(1)中，Fe3O4纳米颗粒分散液由六水合氯化铁、四水合氯化亚铁、氨水和油酸反应得到。
本发明进一步提供一种上述的pH-磁双重响应性染料吸附剂在吸附和解吸附染料方面的应用。
本发明中，染料为甲基橙或甲基红等。
本发明中，应用方法如下：
(1)吸附
在pH为1-3的条件下，将pH-磁双重响应性染料吸附剂，加入染料溶液中，在室温条件下吸附24h；
(2)解吸附
将吸附染料后的吸附剂磁分离后，在pH为9-11条件下，室温下搅拌进行染料的解吸附。
本发明所制备的pH-磁双重响应性染料吸附剂由pH响应聚合物和纳米Fe3O4组成，将pH响应性与磁分离技术相结合，应用于染料废水处理领域。以Fe3O4纳米颗粒为稳定剂对甲基丙烯酸二乙基氨基乙酯进行乳化，通过紫外光引发制备Fe3O4/聚(甲基丙烯酸二乙基氨基乙酯)纳米复合微球。聚甲基丙烯酸二乙基氨基乙酯是一种pH敏感性聚合物，其pKa大约为7，在酸性条件下亲水，碱性条件下疏水。上述得到的pH-磁双重响应性染料吸附剂可实现在低pH下对染料进行有效吸附，在高pH下对染料进行有效释放解析，并通过磁分离技术实现该染料吸附剂的重复有效利用。
本发明和已有技术相比，其技术进步是显著的。本发明以Fe3O4纳米颗粒为稳定剂，通过紫外光固化反应制备的Fe3O4/聚(甲基丙烯酸二乙基氨基乙酯)纳米复合微球，具有良好的pH和磁响应性。与此同时，紫外光固化具有操作工艺简单，无污染，原料利用率高等特点。
附图说明
图1是实施例1的pH-磁双重响应性染料吸附剂的红外光谱图。
图2是实施例1的pH-磁双重响应性染料吸附剂的扫描电镜照片。
具体实施方式
下面通过实施例对本发明进一步详细描述，但并不限制本发明。
实施例1
1)一个制备Fe3O4纳米颗粒分散液的步骤，将12g FeCl3.6H2O，10g FeCl2.4H2O，40g去离子水混合于三口烧瓶中，机械搅拌转速为300rpm，常温通氮气搅拌30min后升温至80℃加入37mL NH3.H2O，搅拌30min，加入7mL油酸，氮气保护下搅拌2h后停止反应，冷却至室温后进行洗涤分离，得Fe3O4纳米颗粒分散液；
2)一个制备Pickering乳液的步骤，取步骤(1)中得到的1gFe3O4纳米颗粒分散液(固含量为55％)超声均匀，置于100mL烧杯中，加入35g去离子水，2g交联剂1，6-己二醇二丙烯酸酯，0.1g光引发剂和1.5g甲基丙烯酸二乙基氨基乙酯，将混合液于400W超声细胞粉碎10min，均质2min，随后倒入100mL三口烧瓶中，转速为300rpm氮气保护下，搅拌20min，最终得到以Fe3O4纳米颗粒稳定的Pickering乳液；
3)一个制备pH-磁双重响应性染料吸附剂的步骤，将步骤(2)得到的Pickering乳液倒入洁净的培养皿中，在紫外灯下照射40min，得到pH-磁双重响应性染料吸附剂。图1是pH-磁双重响应性染料吸附剂的红外光谱图。图2是pH-磁双重响应性染料吸附剂的扫描电镜照片。
4)取5mg上述所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝1)，室温条件下摇床震荡吸附24h，使pH-磁双重响应性染料吸附剂对甲基橙进行吸附。上述所得的pH-磁双重响应性染料吸附剂对甲基橙染料的吸附率为85.43％；在pH＝9的室温条件下对甲基橙染料的释放率为77.56％。
实施例2
1)一个制备Fe3O4纳米颗粒分散液的步骤，将16g FeCl3.6H2O，15g FeCl2.4H2O，60g去离子水混合于三口烧瓶中，机械搅拌转速为500rpm，常温通氮气搅拌50min后升温至80℃加入42mL NH3.H2O，搅拌50min，加入10mL油酸，氮气保护下搅拌4h后停止反应，冷却至室温后进行洗涤分离三次，得Fe3O4磁液；
2)一个制备Pickering乳液的步骤，取步骤(1)中得到的1.5g纳米颗粒分散液(固含量为65％)超声均匀，置于100ml烧杯中，加入60g去离子水，3g交联剂1，6-己二醇二丙烯酸酯，0.15g光引发剂和4g甲基丙烯酸二乙基氨基乙酯，将混合液于400W超声细胞粉碎15min，均质5min，随后倒入100mL三口烧瓶中，转速为500rpm，氮气保护下搅拌40min，最终得到以Fe3O4纳米颗粒稳定的Pickering乳液；
3)一个制备pH-磁双重响应性染料吸附剂的步骤，将步骤(2)得到的Pickering乳液倒入洁净的培养皿中，在紫外灯下照射60min，得到pH-磁双重响应性染料吸附剂。
4)取5mg上述所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝2)，室温条件下摇床震荡吸附24h，使pH-磁双重响应性染料吸附剂对甲基橙进行吸附。上述所得的pH-磁双重响应性染料吸附剂对甲基红的吸附率为87.91％；在pH＝10的室温条件下对甲基红的释放率为66.20％。
实施例3
1)一个制备Fe3O4纳米颗粒分散液的步骤，将14g FeCl3.6H2O，12g FeCl2.4H2O，50g去离子水混合于三口烧瓶中，机械搅拌转速为400rpm，常温通氮气搅拌35min后升温至80℃加入38mL NH3.H2O，搅拌35min，加入8mL油酸，氮气保护下搅拌3h后停止反应，冷却至室温后进行洗涤分离三次，得Fe3O4纳米颗粒分散液；
2)一个制备Pickering乳液的步骤，取步骤(1)中得到的1.17gFe3O4纳米颗粒分散液(固含量为60％)超声均匀，置于100mL烧杯中，加入45g去离子水，2.5g交联剂1，6-己二醇二丙烯酸酯，0.13g光引发剂和4g甲基丙烯酸二乙基氨基乙酯，将混合液于400W超声细胞粉碎12min，均质4min，随后倒入100mL三口烧瓶中，转速为400rpm氮气保护下，搅拌20min，最终得到以Fe3O4纳米颗粒稳定的Pickering乳液；
3)一个制备pH-磁双重响应性染料吸附剂的步骤，将步骤(2)得到的Pickering乳液倒入洁净的培养皿中，在紫外灯下照射40min，得到pH-磁双重响应性染料吸附剂。
4)取5mg上述所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝3)，室温条件下摇床震荡吸附24h，使pH-磁双重响应性染料吸附剂对甲基橙进行吸附。上述所得的pH-磁双重响应性染料吸附剂对甲基红的吸附率为73.55％；在pH＝11的室温条件下对甲基红的释放率为58.13％。
实施例4
1)一个制备Fe3O4纳米颗粒分散液的步骤，将15g FeCl3.6H2O，13g FeCl2.4H2O，45g去离子水混合于三口烧瓶中，机械搅拌转速为500rpm，常温通氮气搅拌40min后升温至80℃加入42mL NH3.H2O，搅拌40min，加入9mL油酸，氮气保护下搅拌2.5h后停止反应，冷却至室温后进行洗涤分离三次，得Fe3O4纳米颗粒分散液；
2)一个制备Pickering乳液的步骤，取步骤(1)中得到的1.33g Fe3O4纳米颗粒分散液(固含量为62.8％)超声均匀，置于100mL烧杯中，加入50g去离子水，3g交联剂1，6-己二醇二丙烯酸酯，0.14g光引发剂和3.5g甲基丙烯酸二乙基氨基乙酯，将混合液于400W超声细胞粉碎15min，均质3min，随后倒入100mL三口烧瓶中，转速为450rpm氮气保护下，搅拌30min，最终得到以Fe3O4纳米颗粒稳定的Pickering乳液；
3)一个制备pH-磁双重响应性染料吸附剂的步骤，将步骤(2)得到的Pickering乳液倒入洁净的培养皿中，在紫外灯下照射50min，得到pH-磁双重响应性染料吸附剂。
4)取5mg上述所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝1)，室温条件下摇床震荡吸附24h，使pH-磁双重响应性染料吸附剂对甲基橙进行吸附。上述所得的pH-磁双重响应性染料吸附剂对甲基橙的吸附率为92.30％；在pH＝11的室温条件下对甲基橙的释放率为72.13％。
实施例5
1)一个制备Fe3O4磁液的步骤，将14.6g FeCl3.6H2O，12g FeCl2.4H2O，50g去离子混合于三口烧瓶中，机械搅拌转速为350rpm，常温通氮气搅拌30min后升温至80℃加入40mLNH3.H2O，搅拌30min，加入8mL油酸，氮气保护下搅拌3h后停止反应，冷却至室温后进行洗涤分离三次，得Fe3O4纳米颗粒分散液；
2)一个制备Pickering乳液的步骤，取步骤(1)中得到的1.35gFe3O4纳米颗粒分散液(固含量为65％)超声均匀，置于100mL烧杯中，加入45g去离子水，2.5g交联剂1，6-己二醇二丙烯酸酯，0.125g光引发剂和2.5g甲基丙烯酸二乙基氨基乙酯，将混合液于400W超声细胞粉碎10min，均质3min，重复3次，随后倒入100mL三口烧瓶中，转速为350rpm氮气保护下，搅拌30min最终得到以Fe3O4纳米颗粒稳定的Pickering乳液；
3)一个制备pH-磁双重响应性染料吸附剂的步骤，将步骤(2)得到的Pickering乳液迅速倒入洁净的培养皿中，在紫外灯下照射60min，得到pH-磁双重响应性染料吸附剂。
4)取5mg上述所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝1)，室温条件下摇床震荡吸附24h，使pH-磁双重响应性染料吸附剂对甲基橙进行吸附。上述所得的pH-磁双重响应性染料吸附剂对甲基橙的吸附率为96.49％；在pH＝11的室温条件下对甲基橙的释放率为87.41％。
应用实施例
取5mg实施例5所得pH-磁双重响应性染料吸附剂，加入50mL浓度为0.1mg/mL的甲基橙溶液中(pH＝1)，室温条件下摇床震荡吸附24h后将样品离心分离，取上层清液测吸光度，计算吸附量，得到在pH＝1的条件下，pH-磁双重响应性染料吸附剂对甲基橙的吸附率分别为96.49％。
取吸附后样品进行磁分离，将分离产物重新分散于50mL，pH＝11的水溶液中进行解吸释放，室温条件下摇床震荡释放24h后将样品磁分离，取上层清液测吸光度，计算释放量，得染料释放率为87.41％；将上述完成解吸的样品进行磁分离，重新分散于50mL，浓度为0.1mg/mL的甲基橙溶液中(pH＝1)，室温条件下摇床震荡吸附24h后将样品磁分离，取上层清液测吸光度，计算吸附量，得到在pH＝1的条件下染料吸附剂对甲基橙的吸附率为95.56％；将第二次吸附样品再次分散于50mL的pH＝11的水溶液中进行解吸释放，室温条件下摇床震荡释放24h后将样品磁分离，取上层清液测吸光度，计算释放量，得染料释放率为75.62％；按相同步骤进行重复试验，当循环使用第5次时对甲基橙的吸附率为90.63％，pH＝11时释放率为58.75％。
以上所述内容仅为本发明构思下的基本说明，而依据本发明的技术方案所作的任何等效变换，均应属于本发明的保护范围。

Claims (5)

1.一种pH-磁双重响应性染料吸附剂的制备方法，其特征在于，其是四氧化三铁Fe3O4纳米颗粒和聚甲基丙烯酸二乙基氨基乙酯形成的复合物，具体步骤如下：
(1)取1-1.5g固含量为55～65％的Fe3O4纳米颗粒分散液超声均匀，加入35-60g去离子水，2-3g交联剂，0.1-0.15g光引发剂和1.5-4g甲基丙烯酸二乙基氨基乙酯，将混合液超声处理10-15min，均质2-5min，随后在惰性气氛保护下，搅拌20-40min，最终得到以四氧化三铁Fe3O4纳米颗粒为稳定剂的Pickering乳液；
(2)将步骤(1)得到的Pickering乳液在紫外灯下照射40-60min，得到pH-磁双重响应性染料吸附剂；
步骤(1)中，Fe3O4纳米颗粒分散液由六水合氯化铁、四水合氯化亚铁、氨水和油酸反应得到。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)中，交联剂为1，6-己二醇二丙烯酸酯。
3.一种根据权利要求1所述的制备方法制得的pH-磁双重响应性染料吸附剂在吸附和解吸附染料方面的应用。
4.根据权利要求3所述的应用，其特征在于，染料为甲基橙或甲基红。
5.根据权利要求3所述的应用，其特征在于，应用方法如下：
(1)吸附
在pH为1-3的条件下，将pH-磁双重响应性染料吸附剂，加入染料溶液中，在室温条件下吸附24h；
(2)解吸附
将吸附染料后的吸附剂磁分离后，在pH为9-11条件下，室温下搅拌进行染料的解吸附。
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