CN112844300A - 用于去除水体草甘膦的磁性纳米颗粒及其制备方法 - Google Patents
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Abstract
本发明公开了一种用于去除水体草甘膦的磁性纳米颗粒及其制备方法。所述方法先将Fe3O4/SiO2核壳结构纳米粒子与镧系化合物混合在等体积的乙醇和水的混合溶剂中,超声分散后缓慢加入氢氧化钠溶液,搅拌反应得到磁性纳米颗粒Fe3O4/SiO2‑La。本发明方法简单方便,合成成本低,制得的磁性纳米颗粒吸附剂比表面积大,对草甘膦的吸附容量大,最大吸附量可达114.9mg/g,吸附速率较快,在2小时内即可达到吸附平衡,同时吸附剂有磁性,易于分离和回收,可重复利用,避免二次污染。
Description
技术领域
本发明属于草甘膦吸附剂的制备技术领域,涉及一种用于去除水体草甘膦的磁性纳米颗粒及其制备方法,具体涉及在四氧化三铁/二氧化硅层表面负载氢氧化镧纳米颗粒的制备方法。
背景技术
草甘膦作为一种光谱灭生性除草剂,已成为用量最多的除草剂用品。虽然草甘膦最初被认定为“无害的除草剂”,但最近报道显示,草甘膦与人类癌症、内分泌系统疾病有密切的联系,而草甘膦除草剂的大量使用已经对地表水和地下水造成严重的环境威胁,因此,美国环境保护署(EPA)、世界卫生组织(WHO)等都对草甘膦在饮用水中的含量作出了严格的限定标准。
目前对草甘膦的处理方法主要有:高级氧化、臭氧处理、紫外辐射、电化学氧化、反渗透、微生物降解、吸附等。但这些方法普遍能耗较高,操作复杂且成本高,而且降解和氧化等方法使草甘膦降解为无机磷,会进一步导致水体的富营养化,从而带来二次污染。吸附法由于其经济、无二次污染、易分离等优点,一直是研究热点。吸附法去除草甘膦污染物主要是利用材料表面疏松多孔的结构或者材料本身的固有性质对水体中的草甘膦产生较强粘附力和其他作用力,以实现去除目的。常见的去除草甘膦的吸附材料有:活性炭、树脂、富含多金属的污泥、铁的氧化物等,但也存在着一些缺点,如吸附容量不高,吸附慢,回复差等。文献1(Yamaguchi et al,Chem Eng J,295(2016)391–402.)采用一步热溶剂法将复合氧化物铁酸锰固定在石墨烯纳米片上合成MnFe2O4-G,这种单层氧化石墨烯和铁锰氧化物的复合材料实现对草甘膦的最大吸附量为39mg/g,但在8小时内才完成吸附平衡。文献2(Herathet al,MicroporMesopor Mat,225(2016)280-288.)通过在700℃对稻壳进行缓慢热解产生蒸汽活性生物炭(RHBC),其对草甘膦的Langmuir最大吸附量为123.03mg/g,但是受溶液pH的影响很大,只有在pH=4时获得最佳吸附效果。
发明内容
本发明的目的在于提供一种用于去除水体草甘膦的磁性纳米颗粒及其制备方法。该方法将氢氧化镧纳米颗粒负载在具有磁性的铁硅球表面,制备高吸附速率和大吸附容量于一体的易分离的草甘膦吸附剂。
实现本发明目的的技术解决方案如下:
用于去除水体草甘膦的磁性纳米颗粒的制备方法,包括如下步骤:
将Fe3O4/SiO2核壳结构纳米粒子与镧系化合物混合在等体积的乙醇和水的混合溶剂中,进行超声分散,之后缓慢加入氢氧化钠溶液,搅拌反应,得到磁性纳米颗粒Fe3O4/SiO2-La。
优选地,所述的镧系化合物为La(NO3)3·6H2O,LaCl3·7H2O或La(OH)3。
优选地,所述的镧系化合物与Fe3O4/SiO2的质量比为50%~300%,更优选为300%。
优选地,所述的氢氧化钠溶液的浓度为0.1~1mol/L,更优选为1mol/L。
优选地,所述的搅拌速度为300~500rpm。
本发明提供上述制备方法制得的磁性纳米颗粒。
进一步地,本发明提供上述磁性纳米颗粒在吸附去除水体草甘膦中的应用。
本发明首次将镧系材料应用在草甘膦吸附中,利用镧元素与草甘膦之间的强配位络合作用,吸附水体中的草甘膦污染物到吸附剂表面。
本发明与现有技术相比,其优点在于:
(1)本发明方法简单方便,合成成本低;
(2)本发明的磁性纳米颗粒吸附剂比表面积大,吸附容量大,例如Fe3O4/SiO2-300%La的最大吸附量为114.9mg/g,对草甘膦的吸附速率较快,在2小时内即可达到吸附平衡,同时吸附剂有磁性,易于分离和回收,可重复利用。
附图说明
图1是负载有氢氧化镧的磁性纳米颗粒Fe3O4/SiO2-300%La的扫描电镜图。
图2是负载有氢氧化镧的磁性纳米颗粒Fe3O4/SiO2-300%La的透射电镜图。
图3是实施例1~3的磁性纳米颗粒对草甘膦的吸附等温线图。
图4是实施例1~3的磁性纳米颗粒对草甘膦的吸附动力学图。
具体实施方式
下面结合附图和实施例对本发明作进一步详细描述。
Fe3O4纳米颗粒的制备参考文献(Yang et al,Nano Res,8(2015)2503-2514.);
Fe3O4/SiO2的制备参考文献(Chen et al,Chem Eng J,360(2019)342-348.)。
实施例1
步骤1,取3.75g六水合三氯化铁与1.5g柠檬酸三钠分散在100ml的乙二醇中,随后立即加入6.5g的无水乙酸钠,通过磁子大力搅拌1小时后至淡黄色均匀澄清溶液,将液体转移到120-140ml的聚四氟乙烯的水热反应釜中,在烘箱中以200℃进行水热反应12小时,反应结束后,通过外加磁场分离,用乙醇和水交替润洗三次,得到黑色的Fe3O4纳米颗粒。
步骤2,取步骤1的Fe3O4纳米颗粒0.15g,加入到100ml异丙醇溶液中,超声处理30min,然后40℃加热,同时300~500rpm机械搅拌,使反应体系处于混匀状态,接着加入10ml氨水和20ml水,之后加入0.5ml的正硅酸四乙酯,反应时间为2小时,在外加磁铁的条件下分离得到Fe3O4/SiO2。
步骤3,取0.1g步骤2得到的Fe3O4/SiO2颗粒与50mg的La(NO3)3·6H2O超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500rpm机械搅拌,接着将20ml,1mol/L的NaOH逐滴滴加到上述溶液中,反应4小时后,通过磁铁分离得到Fe3O4/SiO2-50%La。
实施例2
取实施例1中步骤2的颗粒Fe3O4/SiO20.1g,与La(NO3)3·6H2O按照质量比为2:3混合,即La(NO3)3·6H2O取0.15g,超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500rpm机械搅拌,接着将20ml,1M NaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离得到Fe3O4/SiO2-150%La。
实施例3
取实施例1中步骤2的颗粒Fe3O4/SiO20.1g,与La(NO3)3·6H2O按照质量比为1:3混合,即La(NO3)3·6H2O取0.3g,超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500rpm机械搅拌,接着将20ml,1M NaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离得到Fe3O4/SiO2-300%La。
实施例4
取实施例1中步骤2的颗粒Fe3O4/SiO20.1g,加入50mg LaCl3·7H2O,超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500rpm机械搅拌,接着将20ml,1MNaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离后得到负载La的样品,记为Fe3O4/SiO2-50%La(2)。
实施例5
取实施例1中步骤2的颗粒Fe3O4/SiO20.1g,加入50mg La(OH)3,超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500rpm机械搅拌,接着将20ml,1M NaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离后得到负载La的样品,记为Fe3O4/SiO2-50%La(3)。
对比例1
本对比例与实施例1前两个步骤相同,不同的是步骤3中,取0.1g步骤2得到的Fe3O4/SiO2颗粒与50mg的La(NO3)3·6H2O超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以500rpm机械搅拌,接着将20ml,0.1M NaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离得到另一组负载La的样品,记为Fe3O4/SiO2-50%La(1-1)。
对比例2
本对比例与实施例1前两个步骤相同,不同的是步骤3中,取0.1g步骤2得到的Fe3O4/SiO2颗粒与0.4g的La(NO3)3·6H2O超声分散在30ml乙醇和30ml水中,超声30min后,在常温下以300~500r机械搅拌,接着将20ml,0.1M NaOH逐滴滴加到上述溶液中,反应4小时后,磁性分离得到另一批负载La的样品,记为Fe3O4/SiO2-400%La。
实施例1~3中,将合成好的三组磁性纳米吸附剂对草甘膦的吸附效果用等温吸附实验和吸附动力学实验来评价,具体的吸附等温线实验步骤如下:取10mg吸附剂加入到20ml的不同初始浓度的草甘膦溶液中(30~300mg/L),经过10h的吸附时间后,利用国标紫外分光光度法测试溶液中剩余草甘膦的浓度,并计算吸附量,得到吸附等温线,并用Langmuir和Freundlich两种模型进行拟合,如图3所示,发现吸附等温线更加符合Langmuir模型,表明了吸附剂表面的化学均一性,以及吸附剂与草甘膦之间发生的单层吸附作用。吸附动力学实验如下:取50mg吸附剂加入到100ml,初始浓度为100mg/L的草甘膦溶液中,在不同的时间间隔取样,并记录各个时刻溶液中草甘膦的浓度,所得的动力学曲线用拟一级和拟二级动力学模型分别进行拟合,如图4所示,发现三组样品的吸附动力学更加符合拟二级动力学模型,表明发生了化学吸附。
实施例1,4,5选用了不同的镧系前驱体,在同一组吸附实验中,取5mg吸附剂加入到10ml的初始浓度为10mg/L的草甘膦溶液中,发现Fe3O4/SiO2-50%La,Fe3O4/SiO2-50%La(2),Fe3O4/SiO2-50%La(3)对草甘膦的平衡吸附量分别为17,14,10mg/g,发现同质量条件下,以六水合硝酸镧为前驱体进行负载,吸附效果最好。
对比例1中,将Fe3O4/SiO2-50%La(1-1)和Fe3O4/SiO2-50%La同时对100mg/L的草甘膦进行吸附实验,发现Fe3O4/SiO2-50%La(1-1)样品的吸附效果较差,可能在0.1mol/L的NaOH条件下,镧的氢氧化物部分未沉积完全,导致吸附效果不佳。
对比例2中,对样品Fe3O4/SiO2-400%La进行吸附等温线实验,但最终Langmuir模型拟合出的最大吸附量约为120mg/g,尽管镧的质量分数相比实施例3中Fe3O4/SiO2-300%La有增加,但结果表明更多的La并不会对吸附量有较大的提升,表明镧的有效活性位点的负载已达到饱和。
图1是负载有氢氧化镧的磁性纳米颗粒Fe3O4/SiO2-300%La的扫描电镜图。从图中可以看出,样品外观呈球形,颗粒直径在100~250nm范围,样品表面呈现一定的粗糙度,也表明了氢氧化镧的负载。
图2是负载有氢氧化镧的磁性纳米颗粒Fe3O4/SiO2-300%La的透射电镜图。从图中可以看出,负载氢氧化镧纳米颗粒后,样品不再呈现Fe3O4/SiO2的核壳形结构,单纯呈球形状态。表明了氢氧化镧对原有二氧化硅空间的争夺,因此破坏了核壳结构,侧面证实了氢氧化镧纳米颗粒的有效负载。
图3是实施例1~3的磁性纳米颗粒对草甘膦的Langmuir吸附等温线图,表明了吸附剂表面的化学均一性,以及吸附剂与草甘膦之间发生的单层吸附作用。
图4是实施例1~3的磁性纳米颗粒对草甘膦的拟二级吸附动力学图,表明吸附剂与草甘膦之间发生了化学吸附。
Claims (7)
1.用于去除水体草甘膦的磁性纳米颗粒的制备方法,其特征在于,包括如下步骤:
将Fe3O4/SiO2核壳结构纳米粒子与镧系化合物混合在等体积的乙醇和水的混合溶剂中,进行超声分散,之后缓慢加入氢氧化钠溶液,搅拌反应,得到磁性纳米颗粒Fe3O4/SiO2-La。
2.根据权利要求1所述的制备方法,其特征在于,所述的镧系化合物为La(NO3)3·6H2O,LaCl3·7H2O或La(OH)3。
3.根据权利要求1所述的制备方法,其特征在于,所述的镧系化合物与Fe3O4/SiO2的质量比为50%~300%。
4.根据权利要求1所述的制备方法,其特征在于,所述的氢氧化钠溶液的浓度为0.1~1mol/L。
5.根据权利要求1所述的制备方法,其特征在于,所述的搅拌速度为300~500rpm。
6.根据权利要求1至5任一所述的制备方法制得的磁性纳米颗粒。
7.根据权利要求6所述的磁性纳米颗粒在吸附去除水体草甘膦中的应用。
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