CN106632505A - 一种质子导电金属有机骨架结构化合物及其制备方法 - Google Patents
一种质子导电金属有机骨架结构化合物及其制备方法 Download PDFInfo
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 20
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- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 11
- 239000001632 sodium acetate Substances 0.000 claims abstract description 11
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 11
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- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
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- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 claims description 13
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Abstract
本发明属于化学化合物制备技术领域,具体为一种新型金属有机骨架结构化合物及其制备方法。其结构式为:[Fe3(µ3‑O)(C21O6H11)2(C3N2H4)3],其中µ3为氧桥联;C21O6H11为[1,1’3’1’]三联苯‑4,5’,4’‑三羧酸;C3N2H4为咪唑;其结构单元属于三方晶系,R3空间群,其分子式为Fe3C51H31O13N6,分子量为1536.54,晶胞参数a=27.696(5) Å,b=27.696 Å,c=72.829(13) Å,α=90 º,β=90 º,γ=120 º,晶胞体积为48382(20) Å3,Z=18。本发明以乙酸钠、硝酸铁、硫酸亚铁制备Fe3簇(Fe3(μ3‑O)(COOCH3)6),并与[1,1’3’1’]三联苯‑4,5’,4’‑三羧酸和咪唑形成金属有机骨架结构化合物,具有金属有机配位形成的三维微孔孔道结构,质子传导率高。制备工艺和设备简单,材料的热稳定性高。
Description
技术领域
本发明属于化学化合物制备技术领域,具体为一种新型金属有机骨架结构化合物及其制备方法。
背景技术
在质子导电材料领域,出现了各种聚电解质和微孔聚合物。然而,大多数存在孔道粗大的不足,最终导致只是流动的质子载体而不是有效传导的质子离子。金属有机骨架(MOFs)结构特性丰富,具有较高的孔隙率,较大的比表面积,同时孔径均一而且孔径大小可调,另外MOFs材料即使在高温条件下稳定性仍然很好,基于MOFs材料的以上优点,其在质子导电材料、气体的选择性吸附等许多方面都有着广阔的应用前景。目前,如何设计并合成质子传导率高的质子导电金属有机骨架材料是质子导电材料领域的研究热点。
发明内容
本发明的目的在于提供一种具有高质子传导率的质子导电金属有机骨架结构化合物及其制备方法,该质子导电材料具有金属有机配位形成的三维微孔孔道结构,质子传导率高的优点,且制备工艺和设备简单,材料的热稳定性高。
本发明采用的技术方案为:
一种质子导电金属有机骨架结构化合物,其特征为它是下述化学式的化合物:
[Fe3(µ3-O)(C21O6H11)2(C3N2H4)3],其中µ3为氧桥联;C21O6H11为[1,1’3’1’]三联苯-4,5’,4’-三羧酸;C3N2H4为咪唑;其结构单元属于三方晶系,R3空间群,其分子式为Fe3C51H31O13N6,分子量为1536.54,晶胞参数a = 27.696(5) Å,b = 27.696 Å ,c = 72.829(13) Å, α =90 º, β = 90 º ,γ = 120 º,晶胞体积为48382(20) Å3,Z = 18。
上面所述的质子导电金属有机骨架结构化合物的制备方法,其特征为包括以下步骤:
(1)Fe3(μ3-O)(COOCH3)6的合成:在搅拌条件下,依次将乙酸钠、硝酸铁、硫酸亚铁加入到蒸馏水中,至溶液颜色棕色后,停止搅拌,静置12-24小时后,过滤、洗涤,将洗涤后的滤饼在80℃下真空干燥得Fe3(μ3-O)(COOCH3)6;
(2)将步骤(1)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑混合均匀后,将混合物溶于N,N′-二乙基甲酰胺中,并加入乙酸,将溶液转移至密闭反应釜中在150℃自生压力下反应30h,反应结束后在室温下自然冷却,过滤,洗涤,干燥得到具有质子导电性能的金属有机骨架结构化合物
步骤(1)所述的乙酸钠与硝酸铁和硫酸亚铁的加入量为物质的量的比乙酸钠:硝酸铁:硫酸亚铁=3:0.2:1。
步骤(2)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑的加入量为质量比Fe3(μ3-O)(COOCH3)6:[1,1’3’1’]三联苯-4,5’,4’-三羧酸:咪唑=1:1:1。
本发明的有益效果为:
(1)以乙酸钠、硝酸铁、硫酸亚铁制备Fe3簇(Fe3(μ3-O)(COOCH3)6),并与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑形成金属有机骨架结构化合物,具有金属有机配位形成的三维微孔孔道结构,质子传导率高。
(2)制备工艺和设备简单,材料的热稳定性高。
具体实施方式
下面结合实施例对本发明作进一步详细描阐述:
一种质子导电金属有机骨架结构化合物,其特征为它是下述化学式的化合物:
[Fe3(µ3-O)(C21O6H11)2(C3N2H4)3],其中µ3为氧桥联;C21O6H11为[1,1’3’1’]三联苯-4,5’,4’-三羧酸;C3N2H4为咪唑;其结构单元属于三方晶系,R3空间群,其分子式为Fe3C51H31O13N6,分子量为1536.54,晶胞参数a = 27.696(5) Å,b = 27.696 Å ,c = 72.829(13) Å, α =90 º, β = 90 º ,γ = 120 º,晶胞体积为48382(20) Å3,Z = 18。
上面所述的质子导电金属有机骨架结构化合物的制备方法,其特征为包括以下步骤:
(1)Fe3(μ3-O)(COOCH3)6的合成:在搅拌条件下,依次将乙酸钠、硝酸铁、硫酸亚铁加入到蒸馏水中,至溶液颜色棕色后,停止搅拌,静置12-24小时后,过滤、洗涤,将洗涤后的滤饼在80℃下真空干燥得Fe3(μ3-O)(COOCH3)6;
(2)将步骤(1)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑混合均匀后,将混合物溶于N,N′-二乙基甲酰胺中,并加入乙酸,将溶液转移至密闭反应釜中在150℃自生压力下反应30h,反应结束后在室温下自然冷却,过滤,洗涤,干燥得到具有质子导电性能的金属有机骨架结构化合物。
步骤(1)所述的乙酸钠与硝酸铁和硫酸亚铁的加入量为物质的量的比乙酸钠:硝酸铁:硫酸亚铁=3:0.2:1。
步骤(2)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑的加入量为质量比Fe3(μ3-O)(COOCH3)6:[1,1’3’1’]三联苯-4,5’,4’-三羧酸:咪唑=1:1:1。
本发明在如下实施例中更详细地叙述,但实施例不构成对本发明的限制。
实施例1
在搅拌的状态下,将24.6克乙酸钠(0.3 mol)溶解到100 ml蒸馏水中使其溶解,之后将溶液常压过滤以便除去不溶物杂质,向滤液中缓慢加入8.1克硝酸铁(0.02 mol),待其全部溶解后,再分批次加入27.8克硫酸亚铁( 0.1 mol),搅拌约1小时,此时溶液颜色为棕色,之后将溶液静置沉降12小时、减压抽滤、蒸馏水洗涤三次、无水乙醇洗涤三次。最后,将洗涤后的滤饼在80 ℃下,进行真空干燥得14克Fe3(μ3-O)(COOCH3)6。
将0.015克Fe3(μ3-O)(COOCH3)6与0.015克[1,1’3’1’]三联苯-4,5’,4’-三羧酸和0.015克咪唑混合均匀后,将混合物溶于4毫升N,N′-二乙基甲酰胺中,并加入0.35毫升乙酸,将溶液转移至容积为25毫升的密闭反应釜中在150℃自生压力下反应30h,反应结束后在室温下自然冷却,过滤,蒸馏水洗涤三次、无水乙醇洗涤三次,将洗涤后的滤饼在80 ℃下,进行真空干燥得到0.02克具有质子导电性能的金属有机骨架结构化合物。
通过单晶衍射(Bruker SamrtAPEXII X 射线单晶衍射仪) 对产物结构分析:
其分子式为[Fe3(µ3-O)(C21O6H11)2(C3N2H4)3],其中µ3为氧桥联;C21O6H11为[1,1’3’1’]三联苯-4,5’,4’-三羧酸;C3N2H4为咪唑;其结构单元属于三方晶系,R3空间群,其分子式为Fe3C51H31O13N6,分子量为1536.54,晶胞参数a = 27.696(5) Å,b = 27.696 Å ,c = 72.829(13) Å, α = 90 º, β = 90 º ,γ = 120 º,晶胞体积为48382(20) Å3,Z = 18。
采用交流阻抗法测试了所制备的金属有机骨架结构化合物的交流阻抗值,实验结果见表1,实验结果表明,该的金属有机骨架结构化合物具有较高的质子传导率。
表1不同湿度下的电阻及其质子导电率
Claims (4)
1.一种质子导电金属有机骨架结构化合物,其特征为它是下述化学式的化合物:
[Fe3(µ3-O)(C21O6H11)2(C3N2H4)3],其中µ3为氧桥联;C21O6H11为[1,1’3’1’]三联苯-4,5’,4’-三羧酸;C3N2H4为咪唑;其结构单元属于三方晶系,R3空间群,其分子式为Fe3C51H31O13N6,分子量为1536.54,晶胞参数a = 27.696(5) Å,b = 27.696 Å ,c = 72.829(13) Å, α =90 º, β = 90 º ,γ = 120 º,晶胞体积为48382(20) Å3,Z = 18。
2.权利要求1 中的质子导电金属有机骨架结构化合物的制备方法,其特征为包括以下步骤:
(1)Fe3(μ3-O)(COOCH3)6的合成:在搅拌条件下,依次将乙酸钠、硝酸铁、硫酸亚铁加入到蒸馏水中,至溶液颜色棕色后,停止搅拌,静置12-24小时后,过滤、洗涤,将洗涤后的滤饼在80℃下真空干燥得Fe3(μ3-O)(COOCH3)6;
(2)将步骤(1)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑混合均匀后,将混合物溶于N,N′-二乙基甲酰胺中,并加入乙酸,将溶液转移至密闭反应釜中在150℃自生压力下反应30h,反应结束后在室温下自然冷却,过滤,洗涤,干燥得到具有质子导电性能的金属有机骨架结构化合物。
3.权利要求2中的质子导电金属有机骨架结构化合物的制备方法,其特征为步骤(1)所述的乙酸钠与硝酸铁和硫酸亚铁的加入量为物质的量的比乙酸钠:硝酸铁:硫酸亚铁=3:0.2:1。
4.权利要求2中的质子导电金属有机骨架结构化合物的制备方法,其特征为步骤(2)所述的Fe3(μ3-O)(COOCH3)6与[1,1’3’1’]三联苯-4,5’,4’-三羧酸和咪唑的加入量为质量比Fe3(μ3-O)(COOCH3)6:[1,1’3’1’]三联苯-4,5’,4’-三羧酸:咪唑=1:1:1。
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CN108892774A (zh) * | 2018-05-10 | 2018-11-27 | 哈尔滨理工大学 | 一种晶态聚咪唑、制备方法及其用途 |
CN110305172A (zh) * | 2019-06-26 | 2019-10-08 | 武汉大学 | 一种钴膦酸盐及其制备方法和作为宽温域质子传导材料的应用 |
CN113354828A (zh) * | 2021-05-08 | 2021-09-07 | 沈阳大学 | 新型稳定型金属有机骨架材料的制备及应用 |
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CN108892774A (zh) * | 2018-05-10 | 2018-11-27 | 哈尔滨理工大学 | 一种晶态聚咪唑、制备方法及其用途 |
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CN110305172A (zh) * | 2019-06-26 | 2019-10-08 | 武汉大学 | 一种钴膦酸盐及其制备方法和作为宽温域质子传导材料的应用 |
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CN113354828A (zh) * | 2021-05-08 | 2021-09-07 | 沈阳大学 | 新型稳定型金属有机骨架材料的制备及应用 |
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