CN114950353A - 高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂及其制备方法 - Google Patents
高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂及其制备方法 Download PDFInfo
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Abstract
本发明属于污水处理剂技术领域,提供高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂及其制备方法,该方法包括的步骤有:取醋酸杆菌纤维素用去离子水浸泡并洗涤后,置于氮气保护气氛的管式炉中升温至400‑700℃保温,得到黑色的碳纳米纤维气凝胶;称取四水合钼酸铵和硫脲,加入去离子水,超声至完全溶解,搅拌均匀,得到混合溶液A;将混合溶液A和碳纳米纤维气凝胶加入到聚四氟乙烯反应釜中;在水热条件下反应,得到的产物进行固液分离,得粗样品B;将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,得到的样品为气凝胶吸附剂。本发明得到的产物具有与金属离子更强的螯合作用和更多的吸附位点,对含汞离子的污水处理效果十分优异。
Description
技术领域
本发明涉及污水处理剂技术领域,具体涉及高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂及其制备方法。
背景技术
汞是高毒性的重金属污染物之一,其可导致人类和其他物种的出生缺陷、脑损伤和疾病,长期以来一直是对公共健康和环境的威胁。汞是不可生物降解的,因此可以在生物体中积累,通过食物链威胁人类健康。因此,设计和制备高效汞吸附剂方面的研究受到了国内外研究人员的关注。
目前,已开发出许多常规的去除废水中重金属离子的方法,如离子交换、膜分离、电化学处理、化学沉淀和吸附方法。其中,吸附法以其去除效率高、操作简单、适用性广、性价比高等优点成为人们普遍接受的选择。目前,常用的吸附剂如活性炭、沸石、黏土等被用于重金属离子的吸附,然而,由于吸附效率低,不易分离和重复使用困难等原因,降低了这些吸附剂实际应用的可行性。因此,制备一种成本低廉,过程简单,高效的汞吸附剂是十分必要的。
到目前为止,由于硫与汞之间存在强烈的软-软相互作用,各种含硫材料对Hg2+离子具有很强的结合亲和力,成为了一类独特的汞离子吸附剂。最近,研究报道了硫醇功能化的金属有机框架、有机聚合物、碳纳米管等作为Hg2+离子吸附剂(J.Colloid.Interf.Sci.2015,456:22-31;ACS Sustainable Chem.Eng.2018,6,6175-6182;Adv.Mater.2017,29,1700665)。然而,由于这些材料硫含量低或硫的利用率低等原因,仍显示出相对较低的Hg2+离子吸附能力,另外许多材料受制于复杂的合成过程和高的合成成本,限制了这些材料在大规模合成和应用方面的可能性。二硫化钼(MoS2)作为过渡金属硫化物的典型代表之一,由于拥有丰富的硫原子,独特的层状结构,层间距可控及大的比表面积等优点,具有很大的脱除重金属的潜力。但是,目前MoS2在应用过程中仍存在局限,如MoS2在水中分散性差且易聚集,使得大量的吸附位点无法被有效利用,降低其吸附能力。此外,粉末态的二硫化钼分散在水中时分离回收难度大,易造成二次污染。通过将MoS2纳米片与其他网状结构载体进行组装形成三维复合材料,可有效克服这些局限,从而提高吸附剂的分离回收能力。
由相互连接的三维(3D)网络组成的碳基气凝胶,由于其成本低廉,低密度、高电导率、孔隙率和比表面积的特点,引起了人们的极大关注。通过热解BC产生的CNF气凝胶属于生物炭的一种,可以转化为不同的三维功能纳米材料。生物炭由于其较高的碳和氢含量,较多的含氧官能团(如O-H和C=O),被作为Pb2+、Zn2+、Hg2+等重金属污染水体和土壤的改良剂。然而,生物炭对重金属离子的选择性较差,所以需要对其进行改性,通过增强特定的表面和化学性质,从而提高材料的重金属吸附能力。因此,对CNF气凝胶进行改性可以有效增强材料本身的吸附位点,对研究去除含汞离子的污水是有意义的。
发明内容
本发明的发明目的在于:针对上述存在的问题,提供高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂及其制备方法,本发明通过改进的方法得到具有独特的分子结构的W-MoS2/CNF,不仅增加了MoS2的层间距,还避免了MoS2的聚集,减小了吸附剂二次污染的可能性;与其他螯合剂相比,具有与金属离子更强的螯合作用和更多的吸附位点,对含汞离子的污水处理效果十分优异。
为了实现上述目的,本发明采用的技术方案如下:
高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤后,置于氮气保护气氛的管式炉中升温至400-700℃保温,保温时间为100-150min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:10-1:50称取可溶性的四水合钼酸铵和可溶性硫脲,加入去离子水,固液比为1g:8-15ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:700-1750ml;在水热条件下反应,反应温度为175℃-190℃,水热时间为10-24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,得到的样品为所述高活性位点二硫化钼/碳纳米纤维W-MoS2/CNF气凝胶吸附剂。
本发明中,优选地,步骤(1)中所述的升温按照5℃/min速度进行。
本发明中,优选地,步骤(1)中所述的保温的温度为500℃,保温时间为120min。
本发明中,优选地,步骤(2)中所述的四水合钼酸铵和可溶性硫脲的摩尔比为1:30。
本发明中,优选地,步骤(3)中所述的反应温度为180℃。
本发明中,优选地,步骤(4)中所述的冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa。
本发明保护上述制备方法制备得到的高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂。
本发明还保护上述制备方法制备得到的高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂在污水处理中的应用或用作污水处理剂的应用。
综上所述,由于采用了上述技术方案,本发明的有益效果是:
1、本发明以碳纳米纤维气凝胶为载体,通过简单的一步水热反应具有其独特的分子结构的W-MoS2/CNF气凝胶纳米吸附剂。经醋酸杆菌纤维素碳化得到的碳纳米纤维气凝胶尺寸为纳米级别,相较于前人工作中所选用的微米级尺寸的天然纤维而言,具有更大的比表面积和丰富的微孔结构。醋酸杆菌纤维素(椰果)来源广泛,成本低廉。碳纳米纤维气凝胶作为生物炭的一种,它不仅能有效降低成本,也不会对环境造成污染。在此基础上,通过将二硫化钼纳米片镶嵌在多孔石墨化生物炭表面,一方面以碳纳米纤维气凝胶为载体能够实现二硫化钼纳米片较均匀地分布,最大程度地避免二硫化钼纳米片出现堆叠团聚的现象,在一定程度上可大大提高对二硫化钼的负载率。另一方面层间距扩宽和缺陷增加的二硫化钼纳米片能够使含硫位点更多地暴露,汞离子能够充分地与吸附剂结合,对含汞离子的污水处理效果十分优异,本发明的方法制备的W-MoS2/CNF气凝胶对污水中汞离子的吸附量达到1562mg/g,去除率为99%左右,对污水中汞金属离子有较高的吸附容量、较好的去除效率和优异的离子选择性,可应用于污水处理领域。
2、在最佳条件下,其他金属离子对水溶液中汞离子的选择性去除没有明显影响,吸附剂对汞离子的去除效率仍能达到99%。按照本发明提出的方法将水体净化之后,可将吸附剂用镊子夹出,即可实现污染物与水体的分离。并且可通过将吸附材料浸泡在1M盐酸溶液中从而使其回收利用。此外,2次的净化-回收-净化循环并不会打乱结构的有序性,吸附材料本身的吸附性能并没有衰减的迹象,可以重复使用,进一步分离水中的汞离子。
3、本发明的制备方法便于操作,原料廉价易得,容易工业化生产和推广使用。在水环境污染事件中有很好的应用前景,特别是对汞离子的去除具有极高的效率。
附图说明
图1为实施例2制备的高活性位点W-MoS2/CNF气凝胶的粉末衍射(XRD)图。
图2为实施例4制备的MoS2/CNF气凝胶的粉末衍射(XRD)图。
图3为实施例5制备的MoS2/CNF气凝胶的粉末衍射(XRD)图。
图4为实施例2制备的高活性位点W-MoS2/CNF气凝胶的扫描电镜(SEM)图。
图5为实施例2制备的高活性位点W-MoS2/CNF气凝胶的透射电镜(TEM)图。
图6为实施例4制备的MoS2/CNF气凝胶的透射电镜(TEM)图。
图7为实施例5制备的MoS2/CNF气凝胶的透射电镜(TEM)图。
图8为实施例1-3制备的高活性位点W-MoS2/CNF气凝胶对Hg2+的吸附动力学曲线。
图9为实施例1-3制备的高活性位点W-MoS2/CNF气凝胶对Hg2+的吸附等温线。
图10为实施例1-3制备的高活性位点W-MoS2/CNF气凝胶在干扰离子环境下对Hg2+的离子选择性。
图11为实施例1-3制备的高活性位点W-MoS2/CNF气凝胶两次循环使用后的去除率。
具体实施方式
为了更清楚地表达本发明,以下通过具体实施例和对比例对本发明作进一步说明。
一、制备实施例:
实施例1
高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤3次后,置于氮气保护气氛的管式炉中以4℃/min的速度升温至400℃保温,保温时间为150min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:10称取可溶性的四水合钼酸铵1.24g和可溶性硫脲0.76g,加入去离子水16ml,固液比为1g:8ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:700ml;在水热条件下反应,反应温度为175℃,水热时间为24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa,得到的样品为所述高活性位点二硫化钼/碳纳米纤维W-MoS2/CNF气凝胶吸附剂。
实施例2
高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤数次后,置于氮气保护气氛的管式炉中以5℃/min的速度升温至500℃保温,保温时间为120min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:30称取可溶性的四水合钼酸铵1.24g和可溶性硫脲2.28g,加入去离子水35ml,固液比为1g:10ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:875ml;在水热条件下反应,反应温度为180℃,水热时间为24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa,得到的样品为所述高活性位点二硫化钼/碳纳米纤维W-MoS2/CNF气凝胶吸附剂。
实施例3
高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤数次后,置于氮气保护气氛的管式炉中以6℃/min的速度升温至700℃保温,保温时间为100min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:50称取可溶性的四水合钼酸铵1.24g和可溶性硫脲2.8g,加入去离子水60.6ml,固液比为1g:15ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:1750ml;在水热条件下反应,反应温度为190℃,水热时间为10小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa,得到的样品为所述高活性位点二硫化钼/碳纳米纤维W-MoS2/CNF气凝胶吸附剂。
实施例4
二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤数次后,置于氮气保护气氛的管式炉中以5℃/min的速度升温至500℃保温,保温时间为120min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:30称取可溶性的四水合钼酸铵1.24g和可溶性硫脲2.28g,加入去离子水35ml,固液比为1g:10ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:875ml;在水热条件下反应,反应温度为170℃,水热时间为24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa,得到的样品为所述二硫化钼/碳纳米纤维MoS2/CNF气凝胶吸附剂。
实施例5
二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤数次后,置于氮气保护气氛的管式炉中以5℃/min的速度升温至500℃保温,保温时间为120min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:30称取可溶性的四水合钼酸铵1.24g和可溶性硫脲2.28g,加入去离子水35ml,固液比为1g:10ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:875ml;在水热条件下反应,反应温度为195℃,水热时间为24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa,得到的样品为所述二硫化钼/碳纳米纤维MoS2/CNF气凝胶吸附剂。
二、产品的确认
1、将实施例1-3制备所得的W-MoS2/CNF气凝胶进行X射线粉末衍射分析,从材料的X射线粉末衍射结构表征可以看出,W-MoS2/CNF气凝胶在小于10°的低角度区具有明显的特征衍射峰,对应于二硫化钼的标准卡片(PDF#37-1492)上的(002)衍射峰,通过计算得知复合材料中MoS2的层间距为未扩宽的原二硫化钼材料的层间距为说明复合材料中二硫化钼的层间距扩宽,其中,实施例2所得W-MoS2/CNF气凝胶的粉末衍射(XRD)图见图1。
对实施例4和5所得的W-MoS2/CNF气凝胶进行X射线粉末衍射分析,从材料的X射线粉末衍射结构表征可以看出,W-MoS2/CNF气凝胶在小于10°的低角度区具有明显的特征衍射峰,对应于二硫化钼的标准卡片(PDF#37-1492)上的(002)衍射峰,通过计算得知复合材料中MoS2的层间距为和说明复合材料中二硫化钼的层间距未扩大到足够宽的距离,其中,实施例4和5所得MoS2/CNF气凝胶的粉末衍射(XRD)图见图2和图3。
2、对实施例1-3制备所得的W-MoS2/CNF气凝胶进行SEM扫描电镜分析,可以看出复合材料保持了碳纳米纤维气凝胶的网状三维结构,在纤维表面覆上了MoS2,二硫化钼呈纳米级尺寸的片状结构,并有着一定程度的卷曲,这为后续Hg2+的吸附提供更大的比表面积和更多的吸附位点。其中,实施例2所得W-MoS2/CNF气凝胶的扫描电镜(SEM)图参见图4。
3、对实施例1-3制备所得的W-MoS2/CNF气凝胶进行TEM透射电镜分析,可以看出,相邻晶格条纹间的间距约为对应于MoS2的(002)晶面的间距,与XRD数据相吻合,进一步证实了W-MoS2CNF气凝胶中MoS2层间距发生扩宽。HRTEM图像显示MoS2纳米片中存在大量的晶体缺陷,从而揭示了MoS2缺陷丰富的特征以及原子由于大量的位错和扭曲而沿着基底平面进行相对无序的排列。选区电子衍射(SAED)图进一步证实了这一特征。这些缺陷可能导致在基面上形成裂纹和空穴,这些裂纹和空穴可以作为Hg2+额外的扩散通道。其中,实施例2所得W-MoS2/CNF气凝胶的透射电镜(TEM)图参见图5。
对实施例4、5制备所得的MoS2/CNF气凝胶进行TEM透射电镜分析,可以看出,相邻晶格条纹间的间距约为和对应于MoS2的(002)晶面的间距,与XRD数据相吻合,进一步证实了MoS2CNF气凝胶中MoS2层间距相对于商业化MoS2扩宽,但与例2相比,层间距略小。其中,实施例4和5所得MoS2/CNF气凝胶的透射电镜(TEM)图见图6和图7。
实施例4和5与实施例2的区别在于水热反应的温度不同,说明本发明中温度的控制对产品的形貌有较大的影响,并最终影响材料的活性,实施例4和5未能得到形貌有较大改善的W-MoS2/CNF气凝胶。
三、性能测试:
1、分别称取50mg上述实施例1-3制备的吸附剂,加入到100mL浓度为10ppm的含汞离子溶液中,25℃恒温震荡,在0-24小时内选取不同的时间进行取样,将取得的样品使用ICP-MS测定汞离子的浓度。绘制W-MoS2/CNF气凝胶的吸附动力学曲线,如图8所示,达到吸附平衡时,制备得到的吸附剂对汞离子的去除率为99%。
2、分别称取50mg的上述实施例1-3制备的吸附剂置于100mL浓度为1~500ppm范围内的含汞离子溶液中,25℃恒温震荡24h,使用ICP-MS测定反应平衡后溶液中汞离子的浓度。绘制W-MoS2/CNF气凝胶的吸附等温线,如图9所示,反应平衡后,吸附剂的最大吸附容量达到1562mg/g。高于文献(J.Colloid.Interf.Sci.2019,551,251-260.)报道的Fe3O4@MoS2吸附汞离子的最大吸附容量526mg/g。证明了本发明W-MoS2/CNF气凝胶对汞离子的吸附效果更好。
3、对本发明中合成的吸附材料的抗干扰离子能力进行测定。将50mg上述实施例1-3制备的吸附剂在100mL由锌(Zn2+)、锰(Mn2+)、镍(Ni2+)、镉(Cd2+)、钴(Co2+)、铬(Cr3+)、铜(Cu2+)、铅(Pb2+)等诸多离子(以上离子浓度均为10ppm)干扰的情况下,测定吸附剂的去除率和Kd值。对本发明中合成的W-MoS2/CNF气凝胶的抗干扰离子能力进行测定。结果如图10所示,材料对汞离子的分配系数仍然能达到105mLg-1,去除率达到99%。
4、分别称取50mg上述实施例1-3制备的吸附剂,加入到100mL浓度为10ppm的含汞离子溶液中,25℃恒温震荡,20min后使用ICP-MS测定汞离子的浓度;将吸附材料取出后浸泡在1M盐酸溶液中从而使其回收利用。取回收利用的吸附材料,洗净后加入到100mL浓度为10ppm的含汞离子溶液中,25℃恒温震荡,20min后使用ICP-MS测定汞离子的浓度;计算每次的汞离子去除率,如图11所示,可以看出,回收利用的吸附剂对汞离子的去除率仍为99%,具有较好的可回收性。
上述说明是针对本发明较佳可行实施例的详细说明,但实施例并非用以限定本发明的专利申请范围,凡本发明所提示的技术精神下所完成的同等变化或修饰变更,均应属于本发明所涵盖专利范围。
Claims (8)
1.高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂的制备方法,其特征在于,包括以下步骤:
(1)取醋酸杆菌纤维素用去离子水浸泡并洗涤后,置于氮气保护气氛的管式炉中升温至400-700℃保温,保温时间为100-150min,得到黑色的碳纳米纤维气凝胶;
(2)按摩尔比为1:10-1:50称取可溶性的四水合钼酸铵和可溶性硫脲,加入去离子水,固液比为1g:8-15ml,超声至完全溶解,搅拌均匀,得到混合溶液A;
(3)将混合溶液A和碳纳米纤维气凝胶都加入到聚四氟乙烯反应釜中;碳纳米纤维气凝胶与步骤(2)所加的去离子水的固液比为1g:700-1750ml;在水热条件下反应,反应温度为175℃-190℃,水热时间为10-24小时,得到的产物进行固液分离,得粗样品B;
(4)将粗样品B用去离子水洗涤,放入冷冻真空干燥机干燥,得到的样品为所述高活性位点二硫化钼/碳纳米纤维W-MoS2/CNF气凝胶吸附剂。
2.根据权利要求1所述的制备方法,其特征在于:步骤(1)中所述的升温按照5℃/min速度进行。
3.根据权利要求1所述的制备方法,其特征在于:步骤(1)中所述的保温的温度为500℃,保温时间为120min。
4.根据权利要求1所述的制备方法,其特征在于:步骤(2)中所述的四水合钼酸铵和可溶性硫脲的摩尔比为1:30。
5.根据权利要求1所述的制备方法,其特征在于:步骤(3)中所述的反应温度为180℃。
6.根据权利要求1所述的制备方法,其特征在于:步骤(4)中所述的冷冻真空干燥机干燥,冷冻的温度为-45℃,时间为48小时,真空度<20Pa。
7.根据权利要求1-6中任一项所述的制备方法制备得到的高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂。
8.根据权利要求1-6中任一项所述的制备方法制备得到的高活性位点二硫化钼/碳纳米纤维气凝胶吸附剂在污水处理中的应用或用作污水处理剂的应用。
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