CN110270312B - 一种金属有机骨架材料-活性炭复合纤维膜及其制备方法 - Google Patents
一种金属有机骨架材料-活性炭复合纤维膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种金属有机骨架材料‑活性炭复合纤维膜及其制备方法,解决现有技术中金属有机骨架材料自身化学稳定性差,以及在水体中难回收,易造成二次污染的问题。本发明所述的一种金属有机骨架材料‑活性炭复合纤维膜的制备方法,采用浸渍提拉法将金属有机骨架材料负载在活性炭纤维上,而后清洗,干燥。本发明设计科学,方法简单,环保,省时,适用投产于实际工业生产。
Description
技术领域
本发明属于复合材料领域以及吸附领域,具体涉及一种金属有机骨架材料-活性炭复合纤维膜及其制备方法。
背景技术
金属有机骨架(MOFs)是由无机金属离子或团簇与有机配体组装形成的结晶性多孔材料,具有很高的孔体积和比表面积,以及可调变的结构和功能等特点,在吸附、气体存储、分离、催化、传感以及生物医学等领域得到广泛应用。然而,MOFs材料的在实际应用中存在两个严峻的问题,一是自身化学稳定性差,二是粉末材料在水体中难回收,易造成二次污染。
因此,提供一种负载金属有机骨架的材料,稳定性好,易回收,不产生二次污染,成为了本领域技术人员亟待解决的问题。
发明内容
本发明解决的技术问题是:提供一种金属有机骨架材料-活性炭复合纤维膜的制备方法,解决现有技术中金属有机骨架材料自身化学稳定性差,以及在水体中难回收,易造成二次污染的问题。
本发明还公开了采用该制备方法制得的金属有机骨架材料-活性炭复合纤维膜。
本发明采用的技术方案如下:
本发明所述的一种金属有机骨架材料-活性炭复合纤维膜的制备方法,采用浸渍提拉法将金属有机骨架材料负载在活性炭纤维上,而后清洗,干燥。
进一步地,具体包括以下步骤:
步骤1.将预处理后的活性炭纤维毡作为基底,放入装有粘结液的烧杯中,充分浸泡,取出,干燥;
步骤2.将经步骤1反应后的活性炭纤维毡放入金属有机骨架材料分散液中,负载,取出,置于真空干燥箱中进行热处理,制得金属有机骨架材料-活性炭复合纤维膜。
步骤1中所述的充分浸泡具体为将预处理后的活性炭纤维毡放入装有粘结液的烧烧杯中浸泡2-5小时。
进一步地,所述预处理为将活性炭纤维毡裁剪后,经脱脂清洗和干燥处理。
进一步地,所述脱脂清洗是指将活性炭纤维毡用0.1mol·L-1~1mol·L-1的稀硝酸溶液在恒温25~45℃下浸泡40~120min,再用蒸馏水反复清洗至中性。
进一步地,所述干燥处理是将脱脂清洗后的活性炭纤维毡置于真空干燥箱中50~80℃,干燥2~4h。
进一步地,所述粘结液为每100mL含有0.05~0.2g蔗糖的50%的乙醇水溶液。
进一步地,所述步骤2中金属有机骨架材料分散液的制备方法为:称取0.05g~0.15g的金属有机骨架材料融入100mL超纯水中,搅拌分散后形成制得。
进一步地,所述步骤2中负载的具体操作为:将经步骤1处理后的活性炭纤维毡放入金属有机骨架材料分散液中浸泡2~10min后,再竖直地提拉出来,之后放置一定时间后,进行第二次浸涂,反复几次,记作n,n≤4。
进一步地,所述步骤2中的热处理条件为50~80℃,干燥2~4h。
本发明所述的采用上述的制备方法制成的金属有机骨架材料-活性炭复合纤维膜。
本发明中的金属有机骨架材料包括但不限于MOFs(Ni)、MOFs(Fe)、MOFs(Co)、MOFs(Cu)。
与现有技术相比,本发明具有以下有益效果:
本发明设计科学,方法简单,环保,省时,适用投产于实际工业生产。
本发明采用绿色环保的粘结剂,并通过一步浸渍提拉法,制得金属有机骨架材料-活性炭复合纤维膜,提高了材料的比表面积及稳定性,增强了材料的实际应用能力。
附图说明
图1为实施例1所制备的金属有机骨架材料-活性炭复合纤维膜的扫描电子显微镜图。其中,图1b为图1a的部分放大图。
图2为实施例2不同负载时间所制备的金属有机骨架材料-活性炭复合纤维膜的吸附效果图。
具体实施方式
下面结合附图说明和实施例对本发明作进一步说明,本发明的方式包括但不仅限于以下实施例。
实施例1
本实施例提供了金属有机骨架材料MOFs(Ni)的制备方法:
称取1.75g六水合硝酸镍、1g对苯二甲酸(设置的金属离子与有机配体的摩尔比为:1:1)于250mL烧杯中,并加入70mL的DMF(N,N-二甲基甲酰胺),进行磁力搅拌30min。待其溶解完全后迅速转移至100mL的聚四氟乙烯内村中,装入反应釜,密封好后,放入恒温鼓风干燥箱中,在一定反应温度130℃与反应时间12h条件下制得MOFs(Ni)样品。再将样品转移至50mL离心管中,先后经过2次乙醇洗涤和2次高纯水洗涤,并且每次洗涤后需在4000rad/s条件下离心5min。最后将洗净的样品转移至培养皿中,放入加热干燥箱,在60℃条件下干燥2h后,研磨,得干燥纯净的MOFs(Ni)样品。
实施例2
本实施例提供了本发明的具有高效吸附性能的金属有机骨架材料-活性炭复合纤维膜的制备方法,具体为:
步骤1.预处理后活性炭纤维毡:将活性炭纤维毡裁剪成大小为10mm×30mm的长条,用1mol·L-1的稀HNO3在40℃下处理90min,以除去制备活性炭纤维毡过程中的添加剂,保温20min后用蒸馏水多次洗涤至洗液pH为7,在电热恒温干燥箱中60℃干燥2h。
步骤2.粘结液的制备:取0.1g蔗糖溶于100mL的50%乙醇,之后超声30min制成均匀分散的溶液。
将预处理过的活性炭纤维毡放入粘结液中浸渍2小时,然后放入电热恒温鼓风干燥箱中60℃干燥2h。
步骤3.将0.1g MOFs(Ni)放入99.9mL的超纯水中,磁力搅拌后形成浓度为0.1%的悬浮液。将经步骤2干燥后的活性炭纤维毡竖直浸入悬浮液中3min后再竖直地提拉出来,放置10min后,再次竖直浸入悬浮液中3min后竖直地提拉出来,反复2次,最后置于60℃的真空干燥箱的热处理2h,获得MOFs(Ni)-活性炭复合纤维膜。
通过扫描电子显微镜,可以看到MOFs(Ni)在纤维表面的分布较为均匀,分布密度较大,显示了良好的负载效果,如图1a所示。图1b为图1a的部分放大图,由图1b可知,微观形态下的碳纤维粗糙程度较大,有利于MOFs(Ni)颗粒附着在纤维上,这说明对于活性炭纤维毡的处理不仅仅是去除了多余的表面试剂,也使其表面粗糙程度发生改变。
实施例3
本实施例提供了本发明的具有高效吸附性能的金属有机骨架材料-活性炭复合纤维膜的制备方法,具体为:
步骤1.预处理后活性炭纤维毡:将活性炭纤维毡裁剪成大小为10mm×30mm的长条,用1mol·L-1的稀HNO3在40℃下处理90min,以除去制备活性炭纤维毡过程中的添加剂,保温20min后用蒸馏水多次洗涤至洗液pH为7,在电热恒温干燥箱中60℃干燥2h。
步骤2.粘结液的制备:取0.15g蔗糖溶于100mL的50%乙醇,之后超声30min制成均匀分散的溶液。
将预处理过的活性炭纤维毡放入粘结液中浸渍3小时,然后放入电热恒温鼓风干燥箱中60℃干燥2h。
步骤3.将0.12g MOFs(Ni)放入100mL的超纯水中,磁力搅拌后形成浓度为0.15%的悬浮液,将经步骤2干燥后的活性炭纤维毡竖直浸入悬浮液2min后再竖直地提拉出来,放置10min后,置于60℃中热处理2h,获得MOFs(Ni)-活性炭复合纤维膜。
实施例4
本实施例与实施例3相比,步骤3中活性炭纤维毡竖直浸入悬浮液的时间为3min,其余条件均相同。
实施例5
本实施例与实施例3相比,步骤3中活性炭纤维毡竖直浸入悬浮液的时间为4min,其余条件均相同。
实施例6
本实施例与实施例3相比,步骤3中活性炭纤维毡竖直浸入悬浮液的时间为5min,其余条件均相同。
实施例7
将实施例3-6制得的样品测试对甲基橙的去除率,具体方法为:取MOFs(Ni)-活性炭复合纤维膜于黑暗条件吸附50mL,40mgL-1的甲基橙溶液,并在室温下以一定的速度进行磁力搅拌。分别在吸附30min、60min、90min、120min后移取1mL上清液定容到10mL,用分光光度计测定其吸光度,根据甲基橙浓度-吸光度标准曲线计算其浓度。根据公式可计算出吸附率η公式如下:
η=(C0-Ce)×100%/C0(1)
式中,η为吸附率(%),C0是初始浓度,Ce是吸附后的浓度,单位为mg L-1。
所得结果如附图2所示。由附图2可知,当负载时间小于等于3min时,复合材料吸附效果随着负载时间的增加而变好。而负载时间大于3min后,吸附效果随负载时间增加而逐渐下降。故经t=3min处理过的复合材料吸附效果最好,在2h的吸附过程中吸附率达到最大,吸附速率达到最快。
实施例8
本实施例提供了本发明的具有高效吸附性能的金属有机骨架材料-活性炭复合纤维膜的制备方法,具体为:
步骤1.预处理后活性炭纤维毡:将活性炭纤维毡裁剪成大小为10mm×30mm的长条,用0.1mol·L-1的稀HNO3在40℃下处理120min,以除去制备活性炭纤维毡过程中的添加剂,保温20min后用蒸馏水多次洗涤至洗液pH为7,在电热恒温干燥箱中60℃干燥2h。
步骤2.粘结液的制备:取0.2g蔗糖溶于100mL的50%乙醇,之后超声30min制成均匀分散的溶液。
将预处理过的活性炭纤维毡放入粘结液中浸渍5小时,然后放入电热恒温鼓风干燥箱中60℃干燥2h。
步骤3.将0.15g MOFs(Ni)放入100mL的超纯水中,磁力搅拌后形成浓度为0.15%的悬浮液,将经步骤2干燥后活性炭纤维毡竖直浸入悬浮液中3min后再竖直地提拉出来,放置10min后,进行第二次浸涂,反复2次,最后置于60℃的真空干燥箱的热处理2h,获得MOFs(Ni)-活性炭复合纤维膜。
对上述公开的实施例是为能够清楚地说明所作的补充举例,为后续使用能够起到相应的指引作用。对于本领域技术人员在上述说明的理论基础上以其它不同形式所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种金属有机骨架材料-活性炭复合纤维膜的制备方法,其特征在于,采用浸渍提拉法将金属有机骨架材料负载在活性炭纤维上,而后清洗,干燥;所述金属有机骨架材料为MOFs(Ni)、MOFs(Fe)、MOFs(Co)或MOFs(Cu);
所述制备方法具体包括以下步骤:
步骤1.将预处理后的活性炭纤维毡作为基底,放入装有粘结液的烧杯中,充分浸泡,取出,干燥;所述预处理为将活性炭纤维毡裁剪后,经脱脂清洗和干燥处理;所述脱脂清洗是指将活性炭纤维毡用0.1mol·L-1~1mol·L-1的稀硝酸溶液在恒温25~45℃下浸泡40~120min,再用蒸馏水反复清洗至中性;
步骤2.将经步骤1反应后的活性炭纤维毡放入金属有机骨架材料分散液中,浸泡2~3min后,再竖直地提拉出来,之后放置一定时间后,进行第二次浸涂,反复几次,记作n,n≤4;取出,置于真空干燥箱中进行热处理,制得金属有机骨架材料-活性炭复合纤维膜;
所述金属有机骨架材料分散液的制备方法为:称取0.05g~0.15g的金属有机骨架材料放入100mL超纯水中,搅拌分散后形成制得。
2.根据权利要求1所述的制备方法,其特征在于,所述干燥处理是将脱脂清洗后的活性炭纤维毡置于真空干燥箱中50~80℃,干燥2~4h。
3.根据权利要求1所述的制备方法,其特征在于,所述粘结液为每100mL含有0.05~0.2g蔗糖的50%的乙醇水溶液。
4.根据权利要求1所述的制备方法,其特征在于,所述步骤2中的热处理条件为50~80℃,干燥2~4h。
5.采用权利要求1-4任意一项制备方法制成的金属有机骨架材料-活性炭复合纤维膜。
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