CN109529779A - 一种改性zif-8/go复合膜的制备方法及其应用 - Google Patents
一种改性zif-8/go复合膜的制备方法及其应用 Download PDFInfo
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Abstract
本发明是一种ZIF‑8纳米材料与氧化石墨烯(GO)复合膜的制备方法并用3‑氨丙基三乙氧基硅烷(APTES)对其进行胺功能化改性,及对水中铜离子吸附性能的应用,属于材料制备技术和分析检测技术领域。本发明用硝酸锌(Zn(NO3)2)和2‑甲基咪唑(2‑Im)制备ZIF‑8纳米材料,先用3‑氨丙基三乙氧基硅烷(APTES)对ZIF‑8纳米材料进行改性,增强其吸附重金属离子的能力。再将氧化石墨烯溶解在蒸馏水中,用APTES对其进行改性。再将改性后的两者混合回流反应24h,冷却后,用真空抽滤法将溶液抽滤成膜。
Description
技术领域
本发明涉及一种在氧化石墨烯(GO)上负载ZIF-8金属有机骨架材料复合膜的制备方法,尤其是涉及一种胺功能改性后对溶液中铜离子具有吸附作用的 f-ZIF-8/GO复合膜的制备方法以及应用于检测水中铜离子,属于材料制备和检测技术领域。
背景技术
水体中重金属污染是严重威胁人类健康甚至生命安全的污染类型之一。其中,水中以二价离子形式存在的铜是主要的污染源。水环境中高浓度的铜离子主要来源于化学工业、印染、电镀、有色金属开采和冶炼等行业。铜离子进入水体后不能被生物降解,只能发生迁移和形态转化。在碱性环境下铜离子会以沉淀或悬浮颗粒的形式存在,不易发生迁移,而在酸性环境中,铜离子易溶于水,容易发生迁移。一旦含铜废水进入河流等水体中,易引发铜污染事故,同时高浓度的铜会引起严重的健康问题。因此,含铜废水在排放前必须进行处理达到环境要求才能排放,目前去除高浓度铜的方法有:化学沉淀法、离子交换法、生物处理法和膜吸附分离法等。其中,吸附法因操作简单、成本低廉等优点成为去除水中重金属最常用的方法。
膜吸附分离技术是膜分离技术和吸附技术相结合的集成技术,膜吸附分离是利用膜的选择性吸附分离来实现溶液中不同组分的分离、纯化和浓缩。膜吸附分离技术因其绿色、过程简单、易于控制等特征成为环境治理的首选技术之一。
氧化石墨烯(Graphene Oxide,GO)是石墨粉经过强氧化处理后又剥离的产物,具有典型的准二维空间结构,其片层上含有许多含氧基团,具有较高的比表面积、良好的亲水性和机械性能。由氧化石墨烯纳米片自组装堆叠成的氧化石墨烯薄膜以及在气体液体分离、传感、超级电容器、催化等领域展现出突破性的应用潜力。金属有机骨架材料因其优良的吸附性能,且可通过二次过滤、乙醇萃取等简单方式进行深度净化再生,是一种非常有前景的液相吸附材料。其中,ZIFs 纳米材料由二价Zn、Co等金属盐和咪唑或其衍生物配体在有机溶剂中反应生成的一种具有类沸石骨架结构的MOFs材料,具有高稳定性和化学稳定性以及结构功能的可调性。现已有研究证明MOFs材料基于氧化石墨烯复合材料适用于不同领域的应用。
发明内容
本发明是将ZIF-8纳米材料负载在GO上,将其进行胺功能化改性后对改性后溶液进行抽滤制备成膜,应用于对溶液中铜离子的吸附。
本发明的技术方案是:
一种对铜离子具有吸附性能的胺改性ZIF-8/GO复合膜的制备方法,按以下步骤进行:
(1)取硝酸锌(Zn(NO3)2)、2-甲基咪唑(2-Im)分别溶于甲醇中超声搅拌30min。所得乳状溶液离心15min,并用甲醇充分洗涤三次后过滤,所得粉末在85℃的烘箱中真空干燥。产物ZIF-8纳米材料的SEM图见图1。
(2)将真空干燥后的ZIF-8粉末在高温下真空活化12h。将ZIF-8与甲醇混合,一边搅拌一边加入3-氨丙基三乙氧基硅烷(APTES),在70℃下回流反应5 h。冷却后,产物用二氯甲烷多次洗涤后干燥。
(3)取氧化石墨烯(GO)分散在蒸馏水中,并在GO分散液中加入3-氨丙基三乙氧基硅烷(APTES)超声搅拌30min后,机械搅拌24h。
(4)步骤(3)的产物用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜获得胺改性后的氧化石墨烯(GO)。
(5)将步骤(2)所得产物溶于甲醇中,步骤(4)所得产物分散在超纯水 (DI H2O)中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
(6)将步骤(5)中溶液冷却后,用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。f-ZIF-8/GO复合膜材料的SEM图见图2。
其中,步骤(1)中Zn(NO3)2、2-Im的质量比为1:5~1:8,甲醇的体积为 20~50mL。
步骤(2)中ZIF-8的质量为0.1~0.3g,甲醇溶剂的量为20~40mL,APTES 的量为0.1~0.25mL。
步骤(3)中GO的量为100~300mg溶于100~300mL的蒸馏水中,再加入 1~3mL的APTES。
步骤(5)中取100~300mg胺改性后ZIF-8溶于10~30mL甲醇中,取5~15 mg胺改性后的氧化石墨烯分散在5~20mL超纯水中。
将上述复合膜应用于吸附水中铜离子,具体方法按照下述步骤进行。
(1)配置1~5mg/L的Cu2+标准溶液,绘制标准曲线。
(2)调节Cu2+溶液的pH为2~7,在不同pH条件下的溶液中加入相等量的膜吸附剂,在恒温振荡器中恒温振荡一定的时间,通过原子吸收分光光度法测量 Cu2+的吸光度。pH对吸附效果的影响见图3。
(4)将一定质量的膜吸附剂置于一定体积的Cu2+溶液中,在恒温振荡器中恒温振荡一定的时间,通过原子吸收分光光度法测量Cu2+的吸光度。温度对吸附效果的影响见图4。
(5)通过Cu2+浓度的变化来计算膜吸附剂的吸附容量。
本发明的技术优点:
(1)用共混法将ZIF-8与氧化石墨烯混合后用真空抽滤装置抽滤成膜,能将原本不易收集的ZIF-8纳米材料更好的收集起来,回收利用,起到节能环保的作用。
(2)将氧化石墨烯与ZIF-8结合,能提高所制备的材料对水中金属离子的吸附能力。
(3)对复合膜材料进行胺功能化改性,可以提高其吸附重金属离子的能力。
具体实施方式
下面结合具体实施实例对本发明做进一步说明。
实施例1
(1)取0.539g Zn(NO3)2和3.234g 2-Im分别溶于40mL的甲醇中,超声搅拌30min。离心15min,并用甲醇充分洗涤三次后过滤,所得粉末在85℃的烘箱中真空干燥。
(2)取0.2g(1)中获得的产物溶于30mL甲醇中,加入0.125mL APTES。在70℃下回流反应5h。冷却后,产物用二氯甲烷多次洗涤后干燥。
(3)取200mg氧化石墨烯分散在200mL蒸馏水中,在加入1mL的APTES,先超声搅拌30min,再机械搅拌24h。
(4)步骤(3)的产物用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜.
(5)取(2)中产物200mg溶于30mL甲醇中,取(4)中产物10mg分散在10mL超纯水(DIH2O)中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
(6)将步骤(5)中溶液冷却后,用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。
实施例2
(1)取0.539g Zn(NO3)2和3.234g 2-Im分别溶于40mL的甲醇中,超声搅拌30min。离心15min,并用甲醇充分洗涤三次后过滤,所得粉末在85℃的烘箱中真空干燥。
(2)取0.1g(1)中获得的产物溶于20mL甲醇中,加入0.1mL APTES。在70℃下回流反应5h。冷却后,产物用二氯甲烷多次洗涤后干燥。
(3)取150mg氧化石墨烯分散在150mL蒸馏水中,在加入1.5mL的APTES,先超声搅拌30min,再机械搅拌24h。
(4)步骤(3)的产物用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜.
(5)取(2)中产物100mg溶于20mL甲醇中,取(4)中产物5mg分散在10mL超纯水(DIH2O)中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
(6)将步骤(5)中溶液冷却后,用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。
实施例3
(1)取0.539g Zn(NO3)2和3.773g 2-Im分别溶于40mL的甲醇中,超声搅拌30min。离心15min,并用甲醇充分洗涤三次后过滤,所得粉末在85℃的烘箱中真空干燥。
(2)取0.3g(1)中获得的产物溶于40mL甲醇中,加入0.2mL APTES。在70℃下回流反应5h。冷却后,产物用二氯甲烷多次洗涤后干燥。
(3)取300mg氧化石墨烯分散在200mL蒸馏水中,在加入1.5mL的APTES,先超声搅拌30min,再机械搅拌24h。
(4)步骤(3)的产物用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜.
(5)取(2)中产物200mg溶于20mL甲醇中,取(4)中产物15mg分散在20mL超纯水(DIH2O)中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
(6)将步骤(5)中溶液冷却后,用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。
附图说明:
图1ZIF-8纳米材料的SEM扫描图
图2胺功能化后的ZIF-8/GO复合膜材料的SEM扫描图
图3pH对f-ZIF-8/GO膜材料吸附水中铜离子的影响
图4温度对f-ZIF-8/GO膜材料吸附水中铜离子的影响。
Claims (7)
1.一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于按照下述步骤进行:
(1)取硝酸锌(Zn(NO3)2)、2-甲基咪唑(2-Im)分别溶于甲醇中超声搅拌30min。所得乳状溶液离心15min,并用甲醇充分洗涤三次后过滤,所得粉末在85℃的烘箱中真空干燥。
(2)将真空干燥后的ZIF-8粉末在高温下真空活化12h。将ZIF-8与甲醇混合,一边搅拌一边加入3-氨丙基三乙氧基硅烷(APTES),在70℃下回流反应5h。冷却后,产物用二氯甲烷多次洗涤后干燥。
(3)取氧化石墨烯(GO)分散在蒸馏水中,并在GO分散液中加入3-氨丙基三乙氧基硅烷(APTES)超声搅拌30min后,机械搅拌24h。
(4)步骤(3)的产物用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜获得胺改性后的氧化石墨烯(GO)。
(5)将步骤(2)所得产物溶于甲醇中,步骤(4)所得产物分散在超纯水(DI H2O)中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
(6)将步骤(5)中溶液冷却后,用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。
2.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,步骤(1)中Zn(NO3)2、2-Im的质量比为1:5~1:8,甲醇的体积为20~50mL,超声搅拌30min。
3.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,步骤(2)中ZIF-8的质量为0.1~0.3g,甲醇溶剂的量为20~40mL,APTES的量为0.1~0.25mL,在70℃下回流反应5h。冷却后,产物用二氯甲烷多次洗涤后干燥。
4.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,步骤(3)中GO的量为100~300mg溶于100~300mL的蒸馏水中,再加入1~3mL的APTES,超声搅拌30min后机械搅拌24h。
5.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,步骤(4)用去离子水多洗洗涤并离心15min得到沉积物,最后在60℃下干燥过夜获得胺改性后的氧化石墨烯(GO)。
6.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,步骤(5)中取100~300mg胺改性后ZIF-8溶于10~30mL甲醇中,取5~15mg胺改性后的氧化石墨烯分散在5~20mL超纯水中,两者混合后超声搅拌60min后移至圆底烧瓶中,在70℃下回流反应12h。
7.根据权利要求1所述的一种对铜离子具有吸附性能的改性ZIF-8/GO复合膜的制备方法,其特征在于,将步骤(6)用真空抽滤法将溶液抽滤成膜,并用蒸馏水多次洗涤,得f-ZIF-8/GO复合膜材料。
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