CN104558061B - 二硼酸均苯三羧酸钴铟微孔晶体及其制备方法 - Google Patents
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Abstract
本发明公开了一种二硼酸均苯三羧酸钴铟微孔晶体及其制备方法，该晶体的分子式为Co5In(BTC)4[(B2O4(OH)]2，其中BTC代表1,3,5‑均苯三羧酸根，分子量为1443.18，属于单斜晶系，P21/c空间群，晶胞参数 β＝98.208(2)°，平均孔径为
Description
技术领域
本发明属于晶体材料技术领域，具体涉及一种具有吸附性和荧光性的二硼酸均苯三羧酸钴铟微孔晶体材料及其制备方法。
背景技术
金属-有机骨架(MOFs)是一类新型的晶态多孔材料，主要是由金属离子或金属簇与有机配体自组装配位连接而成。由于其孔道结构决定的许多优良的特性，如荧光性能、催化活性、离子交换性和吸附性等，在石油化工、精细化工等领域具有重要应用。这类材料也在分子识别、主-客体功能材料组装、药物嵌入等方面表现出广阔的应用前景。至今，关于具有新颖结构和不同化学组成的多孔材料的设计合成与开发仍然是非常活跃的前沿研究领域。
近几年，将第二种金属元素引入金属有机骨架中，也引起了人们极大地兴趣。主要的合成策略是将过渡金属与过渡金属进行混合(d-d)以及将过渡金属与稀土金属进行混合(d-f)。这类异金属有机骨架的多孔材料已被大量的报道。但是过渡金属与第三主族元素形成的异金属多孔材料报道甚少。如：[In3O(BBDC)3(INT)3][Co2(OH)(H2O)2]·NO3·solvent、[NH2(CH3)2]2[In3(BTC)5][Co2(DMF)6]·solvent和[(CH3)2NH2]4[In6(BTC)12]2[(Co3OH)4(H2O)36][(In2CoO)4-(BTC)4(H2O)12]·(solvent)x。
有机羧酸是构筑金属-有机骨架过程中常用的一类多功能配体，近年来，以多羧酸类桥连配体构筑的具有新颖结构的MOFs材料取得了明显的进展和显著的成果，大量的以有机羧酸为配体的MOFs材料被设计合成出来。
元素硼是亲氧元素，是典型的无机高分子元素之一，具有独特化学行为，在自然界中主要是以无机硼氧酸和硼氧酸盐形式存在。在硼酸盐晶体结构中，含有BO3平面三角形和BO4四面体两种配位键型，其中配位数为3和4的硼原子可以有所不同，这使得硼氧酸盐的种类繁多、结构复杂多样，也成为寻找新颖微孔材料的一个来源。多年来，人们已经合成了大量的碱金属、碱土金属、过渡金属及稀土金属硼酸盐，但是金属与有机羧酸或有机胺类与硼酸合成出来的孔道材料相对较少。
发明内容
本发明所要解决的技术问题在于提供一种由硼氧配阴离子和1,3,5-均苯三羧酸以及过渡金属与第三主族金属共同构筑骨架的微孔晶体材料二硼酸均苯三羧酸钴铟，以及采用离子热反应制备该微孔晶体材料的方法。
解决上述技术问题所采用的技术方案是：该二硼酸均苯三羧酸钴铟微孔晶体的分子式为Co5In(BTC)4[(B2O4(OH)]2，其中BTC代表1,3,5-均苯三羧酸根，分子量为1443.18，属于单斜晶系，P21/c空间群，晶胞参数a为b为c为β为98.208(2)°，平均孔径为
上述的二硼酸均苯三羧酸钴铟微孔晶体的制备方法为：将四水合醋酸钴、三氧化二铟、硼酸、1,3,5-均苯三羧酸、1-乙基-3-甲基-咪唑按摩尔比为3:(0.5～2):(2～6):(0.5～3):(2～6)置于聚四氟乙烯内衬的反应釜中，在140～170℃下恒温反应5～10天，得到二硼酸均苯三羧酸钴铟微孔晶体。
上述的四水合醋酸钴、三氧化二铟、硼酸、1,3,5-均苯三羧酸、1-乙基-3-甲基-咪唑的摩尔比优选3:1:4:1:6，而且更进一步优选在150℃下恒温反应7天。
本发明采用离子热反应合成得到二硼酸均苯三羧酸钴铟微孔晶体，其结构特征是通过二硼酸根和异金属形成一维链，链与链之间通过1,3,5-均苯三羧酸根配体相连形成二维的层，层与层之间再通过1,3,5-均苯三羧酸根配体相连形成三维的开放骨架结构。该晶体具有良好的吸附性和荧光性能等，可应用于石油化工、精细化工等领域具有重要。
附图说明
图1是Co5In(BTC)4[(B2O4(OH)]2的不对称分子结构示意图。
图2是Co5In(BTC)4[(B2O4(OH)]2]沿a方向的一维链状图。
图3是Co5In(BTC)4[(B2O4(OH)]2]沿a方向的二维层状图
图4是Co5In(BTC)4[(B2O4(OH)]2]沿b方向的多面体堆积微孔结构图。
图5是Co5In(BTC)4[(B2O4(OH)]2]对氮气的吸附图。
图6是Co5In(BTC)4[(B2O4(OH)]2]的荧光图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施例。
实施例1
将0.75g(3mmol)四水合醋酸钴、0.26g(1mmol)三氧化二铟、0.25g(4mmol)硼酸、0.22g(1mmol)1,3,5-均苯三羧酸、1.0g(6mmol)1-乙基-3-甲基-咪唑加入聚四氟乙烯内衬中混合均匀，然后将聚四氟乙烯内衬放入反应釜中，在150℃下恒温反应7天，然后以10℃/min的降温速率降温至常温，得到紫色的菱形微孔晶体二硼酸均苯三羧酸钴铟，其收率为65％，分子式为Co5In(BTC)4[(B2O4(OH)]2，其中BTC代表1,3,5-均苯三羧酸根，分子量为1443.18，属于单斜晶系，P21/c空间群，晶胞参数a为b为c为β为98.208(2)°。
如图1所示，二硼酸均苯三羧酸钴铟微孔晶体的不对称分子结构中含有1个In3+、5个Co3+、2个[B2O4(OH)]2-和4个-3价的1,3,5-均苯三羧酸根配体。In1和Co3原子处在同一个位置，分别占据此位置的1/2，0.5In1/0.5Co3原子是六配位的，分别和来自于4个不同的1,3,5-均苯三羧酸根配体上的氧原子(O3、O9、O5和O8c)进行单齿配位，以及与来自于[B2O4(OH)]2-配体上的氧原子(O14、O16)螯合；Co1也是六配位的，分别和来自于4个不同的1,3,5-均苯三羧酸根配体上的氧原子(O1、O4、O9、和O11)以及来自于2个[B2O4(OH)]2-配体上的氧原子(O14、O17)进行单齿配位；Co2是五配位的，分别和来自于4个不同的1,3,5-均苯三羧酸根配体上的氧原子(O2、O6、O7、O11)以及来自于[B2O4(OH)]2-配体上的氧原子O16进行单齿配位。如图2所示，[B2O4(OH)]2-配体上的氧原子与金属In和Co原子通过氧桥键形成了一维链状结构(图2)，一维链通过与-3价的1,3,5-均苯三羧酸根配体相连形成了二维层状结构(图3)，二维层状结构再与-3价的1,3,5-均苯三羧酸根配体相连则形成了三维孔道结构，如图4所示。
由图5分析结果可知，二硼酸均苯三羧酸钴铟微孔晶体的最大孔容为0.008859cm3/g，平均孔径为如图6所示，当激发波长为205nm时，二硼酸均苯三羧酸钴铟微孔晶体在390nm波长处荧光强度最大，说明了该微孔晶体具有荧光性质。
实施例2
将0.75g(3mmol)四水合醋酸钴、0.12g(0.5mmol)三氧化二铟、0.13g(2mmol)硼酸、0.13g(0.5mmol)1,3,5-均苯三羧酸、0.35g(2mmol)1-乙基-3-甲基-咪唑加入聚四氟乙烯内衬中混合均匀，然后将聚四氟乙烯内衬放入反应釜中，在150℃下恒温反应10天，然后以10℃/min的降温速率降温至常温，得到紫色的菱形微孔晶体二硼酸均苯三羧酸钴铟，其收率为54％，分子式、晶体结构参数、孔容、孔径与实施例1相同。
实施例3
将0.75g(3mmol)四水合醋酸钴、0.50g(2mmol)三氧化二铟、0.4g(6mmol)硼酸、0.65g(3mmol)1,3,5-均苯三羧酸、1.0g(6mmol)1-乙基-3-甲基-咪唑加入聚四氟乙烯内衬中混合均匀，然后将聚四氟乙烯内衬放入反应釜中，在170℃下恒温反应5天，然后以10℃/min的降温速率降温至常温，得到紫色的菱形微孔晶体二硼酸均苯三羧酸钴铟，其收率为57％，分子式、晶体结构参数、孔容、孔径与实施例1相同。
Claims (4)
1.一种二硼酸均苯三羧酸钴铟微孔晶体，其特征在于：该晶体的分子式为Co5In(BTC)4[B2O4(OH)]2，其中BTC代表1,3,5-均苯三羧酸根，分子量为1443.18，属于单斜晶系，P21/c空间群，晶胞参数a为b为c为β为98.208(2)°，平均孔径为
2.一种权利要求1所述的二硼酸均苯三羧酸钴铟微孔晶体的制备方法，其特征在于：将四水合醋酸钴、三氧化二铟、硼酸、1,3,5-均苯三羧酸、1-乙基-3-甲基-咪唑按摩尔比为3:(0.5～2):(2～6):(0.5～3):(2～6)置于聚四氟乙烯内衬的反应釜中，在140～170℃下恒温反应5～10天，得到二硼酸均苯三羧酸钴铟微孔晶体。
3.根据权利要求2所述的二硼酸均苯三羧酸钴铟微孔晶体的制备方法，其特征在于：所述的四水合醋酸钴、三氧化二铟、硼酸、1,3,5-均苯三羧酸、1-乙基-3-甲基-咪唑的摩尔比为3:1:4:1:6。
4.根据权利要求2或3所述的二硼酸均苯三羧酸钴铟微孔晶体的制备方法，其特征在于：在150℃下恒温反应7天。
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| 基于异金属钴-铟簇构筑的3D配位聚合物：[C6H11N2]2[CoIn2(OH)2(BTC)2Br2];李飒英等;《中国化学会第29届学术年会》;20140804 * |
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