CN109627475A - Pd-MOF金属有机框架薄膜及其制备方法 - Google Patents
Pd-MOF金属有机框架薄膜及其制备方法 Download PDFInfo
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Abstract
本发明属于薄膜材料领域,具体涉及一种Pd‑MOF金属有机框架薄膜及其制备方法,包括下述步骤:1)Pd‑MOF金属有机框架的制备;1.1)将氯化钯以及2,5‑二羟基对苯二甲酸加入混合液中;1.2)将步骤1.1)得到的分散液于100‑150℃条件下水热;1.3)用甲醇置换反应溶液;1.4)将步骤1.3)置换完后的样品真空干燥制得Pd‑MOF金属有机框架材料;2)Pd‑MOF金属有机框架薄膜的制备;本发明将Pd‑MOF金属有机框掺杂入聚对苯二甲酸乙二酯制备了具有高化学稳定性和CO吸附能力的特种聚酯薄膜并增强了薄膜的化学稳定性,且其制备方法操作可控性好、工艺简单、成本低易于产业化生产。
Description
技术领域
本发明属于薄膜材料领域,具体涉及一种Pd-MOF金属有机框架薄膜及其制备方法。
背景技术
随着我国可持续发展战略的实施以及加入持久性有机污染物公约,有色染料的水质污染问题已成为我国函待解决的问题之一。金属有机骨架材料是由金属离子和有机配体通过配位键联接而成的有机-无机杂化材料,由于其多变的结构,高的比表面积和有序的孔结构特点,近几十年来,在多孔材料研究领域倍受关注。聚合物在气体存储、分子吸附、传感器等多个领域得到了广泛应用。
膜分离技术具有分离效率高、能耗较低、尤其易与催化反应和其它膜工艺组合联用等特点,近几十年来发展十分迅速,已成为解决当代人类面临的能源、资源、环境等关键问题的重要手段,是支撑可持续发展的重要共性技术之一。
发明内容
本发明的目的在于提供一种Pd-MOF金属有机框架薄膜及其制备方法。
本发明为实现上述目的,采用以下技术方案:
一种Pd-MOF金属有机框架薄膜的制备方法,包括下述步骤:
1)Pd-MOF金属有机框架的制备:
1.1)将氯化钯以及2,5-二羟基对苯二甲酸加入到DMF、甲醇以及去离子水的混合液中;超声分散均匀得到分散液;
1.2)将步骤1.1)得到的分散液转移到聚四氟乙烯衬里的不锈钢水热釜,于100-150℃条件下水热10-30小时后冷却至室温取出;
1.3)每隔10小时用甲醇置换不锈钢水热釜中的反应溶液;
1.4)将步骤1.3)置换完后的样品在200℃条件下真空干燥10-20小时,冷却至室温后,制得Pd-MOF金属有机框架材料;
2)Pd-MOF金属有机框架薄膜的制备:
2.1)将聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂(2,6-二异丙基苯碳二亚胺)和硬脂酸钙加入搅拌器中混合均匀,搅拌时间为2小时,温度控制为160-170℃,挤出造粒即得到的含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒;
2.2)将含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒加入流延挤出设备进行熔融,挤压成型,冷却,即得到金属有机骨架掺杂的特种聚对苯二甲酸乙二酯薄膜成品。
步骤1.1)中DMF、甲醇以及去离子水的混合液中,DMF、甲醇和水的体积比为1:(0.25-4):(0-4)。
步骤2.1)中聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂和硬脂酸钙的质量比为:100-200:2-5:0-1:2-5:0-1。
步骤1.1)中氯化钯和2,5-二羟基对苯二甲酸的摩尔比为(0.25-5):1。
步骤1.1)中超声处理条件为超声频率为80kHz的条件下,超声处理30分钟。
本申请还包括一种Pd-MOF金属有机框架薄膜,采用所述的制备方法得到。
与现有技术相比,本发明的有益效果是:
本发明将Pd-MOF金属有机框掺杂入聚对苯二甲酸乙二酯制备了具有高化学稳定性和CO吸附能力的特种聚酯薄膜并增强了薄膜的化学稳定性,且其制备方法操作可控性好、工艺简单、成本低易于产业化生产。
具体实施方式
为了使本技术领域的技术人员更好地理解本发明的技术方案,下面结合最佳实施例对本发明作进一步的详细说明。
实施例1:一种Pd-MOF金属有机框架薄膜的制备方法,包括下述步骤:
1)Pd-MOF金属有机框架的制备:
1.1)将氯化钯以及2,5-二羟基对苯二甲酸加入到DMF、甲醇以及去离子水的混合液中;氯化钯和2,5-二羟基对苯二甲酸的摩尔比为3:1;DMF、甲醇和水的体积比为1:2:2;超声分散均匀得到分散液;超声处理条件为超声频率为80kHz的条件下,超声处理30分钟;
1.2)将步骤1.1)得到的分散液转移到聚四氟乙烯衬里的不锈钢水热釜,于120℃条件下水热20小时后冷却至室温取出;
1.3)每隔10小时用甲醇置换不锈钢水热釜中的反应溶液;
1.4)将步骤1.3)置换完后的样品在200℃条件下真空干燥10-20小时,冷却至室温后,制得Pd-MOF金属有机框架材料;
2)Pd-MOF金属有机框架薄膜的制备:
2.1)将聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂2,6-二异丙基苯碳二亚胺和硬脂酸钙加入搅拌器中混合均匀,搅拌时间为2小时,温度控制为160-170℃,挤出造粒即得到的含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒;聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂和硬脂酸钙的质量比为:150:3:0.5:3:0.5;
2.2)将含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒加入流延挤出设备。挤出机温度为160℃,在常温下冷却成型,即得到金属有机骨架掺杂的特种聚对苯二甲酸乙二酯薄膜成品。对得到的薄膜成品进行稳定性以及CO吸附测试,测试结果表明:Pd-MOF金属有机框架薄膜的拉伸强度在156MPa(常温常压);热收缩率为0.6%(横向)、1.2%(纵向)(150℃,30min);CO吸附量在0.57cm3/g(常温常压)。
实施例2:实施例2与实施例1的区别仅在于,步骤1.1)中DMF、甲醇以及去离子水的混合液中,DMF、甲醇的体积比为1:0.25;氯化钯和2,5-二羟基对苯二甲酸的摩尔比为0.25:1。步骤2.1)中聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂2,6-二异丙基苯碳二亚胺和硬脂酸钙的质量比为:100:2:0:2:0。得到的薄膜成品进行稳定性以及CO吸附测试,测试结果表明:Pd-MOF金属有机框架薄膜的拉伸强度在138MPa(常温常压);热收缩率为1.1%(横向)、2.4%(纵向)(150℃,30min);CO吸附量在0.42cm3/g(常温常压)。
实施例3:实施例3与实施例1的区别仅在于,步骤1.1)中DMF、甲醇以及去离子水的混合液中,DMF、甲醇和水的体积比为1:4:4;氯化钯和2,5-二羟基对苯二甲酸的摩尔比为5:1;步骤2.1)中聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS168、稳定剂2,6-二异丙基苯碳二亚胺和硬脂酸钙的质量比为:200:5:1:5:1。得到的薄膜成品进行稳定性以及CO吸附测试,测试结果表明:Pd-MOF金属有机框架薄膜的拉伸强度在168MPa(常温常压);热收缩率为0.7%(横向)、1.4%(纵向)(150℃,30min);CO吸附量在0.64cm3/g(常温常压)。
实施例4:实施例4与实施例1的区别仅在于,步骤1.2)中将步骤1.1)得到的分散液转移到聚四氟乙烯衬里的不锈钢水热釜,于100℃条件下水热30小时后冷却至室温取出。得到的薄膜成品进行稳定性以及CO吸附测试,测试结果表明:Pd-MOF金属有机框架薄膜的拉伸强度在160MPa(常温常压);热收缩率为0.7%(横向)、1.1%(纵向)(150℃,30min);CO吸附量在0.62cm3/g(常温常压)
实施例5:实施例4与实施例1的区别仅在于,步骤1.2)中将步骤1.1)得到的分散液转移到聚四氟乙烯衬里的不锈钢水热釜,于150℃条件下水热10小时后冷却至室温取出;得到的薄膜成品进行稳定性以及CO吸附测试,测试结果表明:Pd-MOF金属有机框架薄膜的拉伸强度在153MPa(常温常压);热收缩率为0.5%(横向)、1.1%(纵向)(150℃,30min);CO吸附量在0.28cm3/g(常温常压)。
以上内容仅为本发明的较佳实施例,对于本领域的普通技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处,本说明书内容不应理解为对本发明的限制。
Claims (6)
1.一种Pd-MOF金属有机框架薄膜的制备方法,其特征在于,包括下述步骤:
1)Pd-MOF金属有机框架的制备:
1.1)将氯化钯以及2,5-二羟基对苯二甲酸加入到DMF、甲醇以及去离子水的混合液中;超声分散均匀得到分散液;
1.2)将步骤1.1)得到的分散液转移到聚四氟乙烯衬里的不锈钢水热釜,于100-150℃条件下水热10-30小时后冷却至室温取出;
1.3)每隔10小时用甲醇置换不锈钢水热釜中的反应溶液;
1.4)将步骤1.3)置换完后的样品在200℃条件下真空干燥10-20小时,冷却至室温后,制得Pd-MOF金属有机框架材料;
2)Pd-MOF金属有机框架薄膜的制备:
2.1)将聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS 168、稳定剂和硬脂酸钙加入搅拌器中混合均匀,搅拌时间为2小时,温度控制为160-170℃,挤出造粒即得到的含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒;
2.2)将含有Pd-MOF金属有机框的聚对苯二甲酸乙二酯薄膜聚合颗粒加入流延挤出设备进行熔融,挤压成型,冷却,即得到金属有机骨架掺杂的特种聚对苯二甲酸乙二酯薄膜成品。
2.根据权利要求1所述的Pd-MOF金属有机框架薄膜的制备方法,其特征在于,步骤1.1)中DMF、甲醇以及去离子水的混合液中,DMF、甲醇和水的体积比为1:(0.25-4):(0-4)。
3.根据权利要求1所述的Pd-MOF金属有机框架薄膜的制备方法,其特征在于,步骤2.1)中聚对苯二甲酸乙二酯、Pd-MOF金属有机框架、IRGAFOS 168、稳定剂和硬脂酸钙的质量比为:100-200:2-5:0-1:2-5:0-1。
4.根据权利要求1所述的Pd-MOF金属有机框架薄膜的制备方法,其特征在于,步骤1.1)中氯化钯和2,5-二羟基对苯二甲酸的摩尔比为(0.25-5):1。
5.根据权利要求1所述的Pd-MOF金属有机框架薄膜的制备方法,其特征在于,步骤1.1)中超声处理条件为超声频率为80kHz的条件下,超声处理30分钟。
6.一种Pd-MOF金属有机框架薄膜,其特征在于,采用权利要求1-5任一项所述的制备方法得到。
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