CN108057422B - 一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶及其制备方法与应用 - Google Patents
一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种醇桥联增强多孔羟基氧化铁‑石墨烯纳米复合水凝胶及其制备方法与应用。它的制备方法,包括如下步骤:1)将氧化石墨烯、铁盐和溶剂混合,得到混合溶液;2)将步骤1)得到的所述混合溶液加热至凝胶成型,即得到醇桥联增强多孔羟基氧化铁‑石墨烯纳米复合水凝胶。本发明制备方法简单,且制备中避免了有毒试剂的使用,所得凝胶具有高比表面积和污染物去除性能,易于固液分离,能用于环境污染治理。
Description
技术领域
本发明涉及一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶及其制备方法与应用,属于环境功能凝胶研究技术领域。
背景技术
近年来,具有高比表面积和易分离的性能三维纳米材料因具有优异的特性吸附和催化而成为研究热点。针铁矿(α-FeOOH)具有低成本和高稳定性的优势,但是,铁纳米粒子容易团聚,并且难于从水中分离。此外,当α-FeOOH作为催化剂时会因光生载流子的快速重组而降低对污染物的去除效率。因此,为α-FeOOH寻找合适的载体十分重要,而载体性质如结晶度、形貌和表面积对产物的理化性质有很大影响。因此,具有优异的机械、电学及热性能的石墨烯凝胶成为了纳米铁的良好载体。例如申请号为201310014878.6的专利公开了一种石墨烯负载菱面体氧化铁复合材料及其水热合成方法,将石墨烯氧化物前驱体、铁盐和乙酸钠进行水热反应,所得复合材料可逆容量高、循环性能好,是一种非常具有研究价值的锂离子电池负极材料。
发明内容
本发明的目的是提供一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶及其制备方法与应用,本发明制备方法简单,且制备中避免了有毒试剂的使用,所得凝胶具有高比表面积和污染物去除性能,易于固液分离,能用于环境污染治理。
本发明提供的一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶的制备方法,包括如下步骤:1)将氧化石墨烯、铁盐和溶剂混合,得到混合溶液;
2)将步骤1)得到的所述混合溶液加热至凝胶成型,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
上述的制备方法中,所述氧化石墨烯和所述铁盐的质量比可为1:0.001~1000,具体可为1:2.781、1:5.561、1:6.951、1:11.122、1:1~100或1:0.01~500。
上述的制备方法中,所述加热的温度可为50℃~300℃,具体可为80℃、120℃、180℃、80℃~120℃、80℃~180℃、120℃~180℃或100℃~200℃,时间可为8~48h,具体可10h、24h、10~48h、24~48h、10~24h或10~40h。
上述的制备方法中,所述溶剂包括水和/或醇溶液;
所述氧化石墨烯和所述溶剂的固液比可为1:0.01~10g/L,具体可为1:0.2g/L、1:0.4g/L、1:0.1g/L、1:0.1~0.4g/L或1:0.01~5g/L。
上述的制备方法中,所述醇溶液选自甲醇、乙醇、丙醇、丁醇、戊二醇、乙二醇、丙三醇、苯甲醇和聚乙烯醇中的至少一种。
上述的制备方法中,当所述溶剂为水和醇溶液的混合溶液时,所述水和所述醇溶液的体积比可为1:0.001~1000,具体可为7:1、3:1、1:1、1:3、1:0.1~3、1:0.01~500或1:0.01~800。
上述的制备方法中,所述铁盐为二价铁盐和/或三价铁盐;
所述二价铁盐选自FeCl2、Fe(NO3)2和FeSO4中的至少一种;
所述三价铁盐选自FeCl3、Fe(NO3)3和Fe2(SO4)3中的至少一种。
本发明中所述铁盐可采用本领域常见的铁盐结晶水合物。
本发明还提供了上述的制备方法制备得到的所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
本发明所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶具有丰富的孔隙结构和优异的吸附、催化性能。
本发明进一步提供了所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶在制备具有如下1)-3)中任一项功能的产品中的应用;
1)吸附污染物;
2)降解污染物;
3)易分离回收;
4)环境污染治理。
本发明还提供了一种产品,该产品为所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶,所述产品的功能为下述至少一种:
1)吸附污染物;
2)降解污染物;
3)易分离回收;
4)环境污染治理。
本发明中,所述污染物为本领域常见的物质,具体可为四环素。
本发明在制备醇桥联增强多孔羟基氧化铁-石墨烯纳米复合凝胶的过程中,通过铁离子和石墨烯之间的氧化还原反应可以实现羟基氧化铁的生长和石墨烯片层自组装成凝胶,两者相互支撑可以缓解彼此的团聚问题。此外,因具有羟基,醇既能与铁离子形成配合物从而诱导羟基氧化铁的生长,又能与石墨烯通过氢键作用诱导石墨烯的自组装,因此能够在铁离子和石墨烯之间起到桥联的作用,此外,醇分子还能在纳米粒子之间起到阻隔物的作用来进一步降低团聚。因此,可通过醇的桥联提升多孔羟基氧化铁-石墨烯纳米复合凝胶的比表面积等性能。
本发明具有以下优点:
1)本发明工艺简单、易于推广,避免了使用有毒交联剂即可使得两种纳米材料生长为三维结构,并降低了纳米粒子之间的团聚;
2)本发明制得的醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶具有高表面积和吸附性能。
附图说明
图1为本发明醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶光学照片。
图2为本发明醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶投射电镜照片,其中图2(a)为FG-0的投射电镜照片,图2(b)为FG-1的投射电镜照片,图2(c)为FG-2的投射电镜照片,图2(d)为FG-3的投射电镜照片,图2(e)为FG-4的投射电镜照片。
图3为本发明醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶比表面积。
图4为本发明醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶对四环素的吸附和催化降解性能。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1、
本实施例中醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶采用以下具体步骤制备而成:
取5个烧杯,配置40mL水/乙二醇混合溶液,其成分分别为40mL水、35mL水+5mL乙二醇、30mL水+10mL乙二醇、20mL水+20mL乙二醇、10mL水+30mL乙二醇。向每组溶液中均溶解20mg GO(氧化石墨烯)和0.4mmol FeSO4·7H2O,超声1h形成均匀溶液。将溶液放入50mL聚四氟乙烯内衬不锈钢反应釜中在120℃下加热24h,反应结束后蒸馏水清洗凝胶,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶,产物分别标记为FG-0,FG-1,FG-2,FG-3和FG-4。
上述制备得到的凝胶的光学照片如图1所示,由图1中可以看出,随着乙二醇含量增大,本发明凝胶尺寸明显增大,表明本发明凝胶具有更加丰富的孔隙结构。
上述制备得到的凝胶的投射电镜图如图2所示,由图2中可以看出,随着乙二醇含量增大,分散在石墨烯上的铁粒子的聚集程度先减小后增大,表明当水与乙二醇体积比为1:1时最有利于降低纳米粒子之间的团聚。
上述制备得到的凝胶的比表面积如图3所示,可见本发明凝胶的比表面积随乙二醇含量的增加先增大后减小,进一步证实了适量的乙二醇可以增加凝胶的孔隙率和抑制羟基氧化铁和石墨烯的团聚。其中,当溶剂为纯水时,本发明凝胶FG-0的比表面积为150.47m2/g,当水与乙二醇体积比为1:1时,本发明凝胶FG-3的比表面积高达240.32m2/g。
上述制备得到的凝胶对四环素(初始浓度100mg/L)的吸附和催化降解性能如图4所示,由图4可见本发明凝胶的对污染物的去除率随乙二醇使用含量的增加先增大后减小,表明适量的乙二醇可以提高本发明凝胶的吸附和催化性能。当水与乙二醇体积比为1:1时,本发明凝胶对四环素通过吸附和可见光催化的去除率分别高达88.46%和97.55%。
实施例2、
配置40mL水/丙三醇混合溶液,其中含20mL水和20mL丙三醇,向其中溶解40mg GO和0.4mmol FeSO4·7H2O,超声1h形成均匀溶液。将溶液放入50mL聚四氟乙烯内衬不锈钢反应釜中在120℃下加热24h,反应结束后蒸馏水清洗凝胶,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
实施例3、
配置40mL水/丙三醇混合溶液,其中含20mL水和20mL丙三醇,向其中溶解40mg GO和1.0mmol FeSO4·7H2O,超声1h形成均匀溶液。将溶液放入50mL聚四氟乙烯内衬不锈钢反应釜中在180℃下加热24h,反应结束后蒸馏水清洗凝胶,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
实施例4、
配置40mL水/甲醇混合溶液,其中含10mL水和30mL甲醇,向其中溶解40mg GO和0.4mmol FeSO4·7H2O,超声1h形成均匀溶液。将溶液放入50mL聚四氟乙烯内衬不锈钢反应釜中在80℃下加热24h,反应结束后蒸馏水清洗凝胶,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
实施例5、
配置40mL水/聚乙烯醇混合溶液,其中含30mL水和10mL聚乙烯醇,向其中溶解10mgGO和0.2mmol FeSO4·7H2O,超声1h形成均匀溶液。将溶液放入50mL聚四氟乙烯内衬不锈钢反应釜中在180℃下加热10h,反应结束后蒸馏水清洗凝胶,即得到得醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
Claims (7)
1.一种醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶的制备方法,包括如下步骤:1)将氧化石墨烯、铁盐和溶剂混合,得到混合溶液;
所述溶剂为水和醇的混合溶液,其中所述水和醇的体积比为1:1;
所述醇选自甲醇、乙醇、丙醇、丁醇、戊二醇、乙二醇、丙三醇、苯甲醇和聚乙烯醇中的至少一种;
2)将步骤1)得到的所述混合溶液加热至凝胶成型,即得到醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶;
所述加热的温度为120℃~180℃,时间为8~48h。
2.根据权利要求1所述的制备方法,其特征在于:所述氧化石墨烯和所述铁盐的质量比为1:0.001~1000。
3.根据权利要求1或2所述的制备方法,其特征在于:所述氧化石墨烯和所述溶剂的固液比为1:0.01~10 g/L。
4.根据权利要求1或2所述的制备方法,其特征在于:所述铁盐为二价铁盐和/或三价铁盐;
所述二价铁盐选自FeCl2、Fe(NO3)2和FeSO4中的至少一种;
所述三价铁盐选自FeCl3、Fe(NO3)3和Fe2(SO4)3中的至少一种。
5.权利要求1-4中任一项所述的制备方法制备得到的所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶。
6.权利要求5中所述醇桥联增强多孔羟基氧化铁-石墨烯纳米复合水凝胶在制备具有环境污染治理功能的产品中的应用。
7.根据权利要求6所述的应用,其特征在于:所述环境污染治理指的是吸附污染物或降解污染物。
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