CN114957687A - 一种三(对羧基苯基)氨基-三嗪与二价铁离子构筑的配合物及其合成方法 - Google Patents
一种三(对羧基苯基)氨基-三嗪与二价铁离子构筑的配合物及其合成方法 Download PDFInfo
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- 229910001448 ferrous ion Inorganic materials 0.000 title claims abstract description 4
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Abstract
本发明公开了一种2,4,6‑三(对羧基苯基)氨基‑1,3,5‑三嗪与二价铁离子构筑的配合物及其合成方法。本发明涉及2,4,6‑三(对羧基苯基)氨基‑1,3,5‑三嗪铁配合物及其合成方法，单体分子式为C48H39ClFe2N12O16.5，分子量为1195.06g/mol，具有互穿的三维空间结构，以FeCl2·4H2O、2,4,6‑三(对羧基苯基)氨基‑1,3,5‑三嗪、K2CO3和抗坏血酸和乙醇和水的混合液、在密封反应釜中空气气氛下160℃反应72小时晶化合成获得。本发明工艺简单、化学组分易控制、重复性好。
Description
技术领域
本发明涉及一种2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪与Fe(II)构筑的配合物及合成方法。
背景技术
配位化合物是近些年发展迅速的方向之一，是一个涉及无机化学、有机化学和配位化学等多学科的研究课题。它所具有的孔洞多样性、金属活性位点、不饱和N位点以及兼有无机材料的刚性和有机材料的柔性等特性，使其在催化、气体吸附分离、磁性等众多领域呈现出巨大的潜力及发展前景。
对于配合物中的金属种类来说，Fe对生物领域、环境领域等方面的应用来说毒性较微，因此可以作为一类非常有潜力的可用于材料合成的金属。考虑到 Fe(II)对强氧化性物种的高选择性以及作为结合位点时对一些种类气体的优异结合能力，选用Fe(II)作为配合物中的金属节点是有一定研究意义和发展前景的。Fe(II)也被用于许多有机配合物的合成，它可以与羧基配体、唑类配体，嗪类配体等多种配体进行配位，形成结构新颖的配位化合物。这些合成的配位化合物广泛用于生物、气体吸附分离、磁性等领域的研究。
虽然已经有许多种类的Fe(II)配合物被成功合成，但通常是基于羧基配体或者各类含N配体的材料研究，尚未见2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪这种既含羧基官能团又含N基官能团的复合型配体与二价Fe(II)离子构筑的具有三维结构金属有机配合物的报道。2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪属于复合型配体，结构中同时包含羧基及含N基团，因此兼具这两种配体的优点。首先，结构中含有的多个羧基配体及不饱和N位点给金属提供了丰富的配位点，保证了金属与配体的成功配位；其次，邻近的苯环与杂化环产生较大的空间位阻，能一定程度上防止N与金属位点的完全配位，从而在最终结构形成时产生不饱和的N位点。理论上，2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪若能与二价Fe(II) 离子构筑具有三维结构金属有机配合物，这些不饱和N位点以及Fe(II)不饱和金属位点均可作为吸附反应位点，对NO等气体分子的吸附过程中可以达到增强材料的吸附性能效果。
发明内容
本发明目的是旨在提供一种2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪与二价铁离子构筑的配合物及其合成方法，利用溶剂热法合成2,4,6-三(对羧基苯基)氨基 -1,3,5-三嗪铁配合物，具体步骤为：
(1)将FeCl2·4H2O、2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸分别加入乙醇和水的混合溶液中，超声振荡清器震荡35分钟，充分溶解混合均匀后将混合液转移至聚四氟乙烯内衬反应器中密封。其中，乙醇与水的体积比为1：1，2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸与FeCl2·4H2O的投料摩尔比分别为 1.26～1.34:1、0.65～1.39:1和0.41～0.73:1，乙醇和水的混合溶液与FeCl2·4H2O的投料比(质量比)为275.23～550.46:1。
(2)步骤(1)装有反应混合液的反应釜置于电热恒温鼓风干燥箱中，以2℃/min 升温速率升至150～170℃反应72小时，再以5℃·h-1的速率冷却至室温。打开反应釜，将底部黄色晶体样品取出，该晶体即2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物。
本发明具有工艺简单、化学组分易控制、重复性好等优点，可在有氧环境下合成。
附图说明
图1为2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪配体的结构示意图。
图2为实施例所得2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物的单体结构示意图。
图3为实施例所得2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物的三维结构示意图。
图4为实施例所得2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物的三维堆积结构示意图。
具体实施方式
本发明涉及的2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物，单体分子式为C48H39ClFe2N12O16.5，分子量为1195.06g/mol。2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪为分析纯。晶体结构数据见表1，键长键角数据键表2。以下通过具体实施例对本发明予以详细说明。
实施例1
(1)将0.013g FeCl2·4H2O(分析纯)、0.0486g 4,6-三(对羧基苯基)氨基-1,3,5-三嗪 (分析纯)、0.010g分析纯K2CO3和0.007g分析纯抗坏血酸加入盛有3.578g乙醇和水(1：1)混合溶液的20mL聚四氟乙烯内衬反应器中，于超声振荡清器震荡35min，然后密封在20mL聚四氟隆衬里的反应器中。
(2)将反应釜置于电热恒温鼓风干燥箱中，以2℃/min升温速率升至160℃反应72h，再以5℃·h-1的速率冷却至室温。打开高压反应釜，底部有黄色晶体即2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物。通过单晶衍射仪测定该配合物的结构，晶体结构数据见表1，键长键角数据键表2。
根据单晶分析结果，配合物单体由48个C原子、39个H原子、1个Cl原子、2个Fe 原子、12个N原子和16.5个O原子构成。晶体相对分子质量为1195.06g/mol，晶系属于立方型晶系，空间群为Pa-3。从配位上看，Fe与配体上的O进行配位，常见的O-Fe-O键角包括74.8(7)°、87.7(3)°、125.9(5)°、103.6(7)°等，键长包括
等。并且最终结构中包含多个不饱和N，C-N-C之间的键角主要包括114.2(4)°、130.6(4)°等，键长包括
等。拓扑结构上，金属与配体相互连接，在一定的方向呈现出层状结构，由于配体本身结构中的三苯环共面，支链相互穿插，形成最终互穿的空间结构。
表1. 2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物的晶体结构数据
表2. 2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物的部分键长
和键角(°)数据
Claims (4)
1.一种2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪与二价铁离子构筑的配合物及其合成方法，本发明的配合物为黄色晶体，单体分子式为C48H39ClFe2N12O16.5，晶体相对分子质量为1195.06g/mol；配合物单体由48个C原子、39个H原子、1个Cl原子、2个Fe原子、12个N原子和16.5个O原子构成，晶系属于立方型晶系，空间群为Pa-3；Fe与配体上的O进行配位，O-Fe-O键角包括74.8(7)°、87.7(3)°、125.9(5)°、103.6(7)°等，键长包括
等；结构中包含多个不饱和N，C-N-C之间的键角主要包括114.2(4)°、130.6(4)°等，键长包括
等；拓扑结构上，金属与配体相互连接，在一定的方向呈现出层状结构，配体本身结构中的三苯环共面，支链相互穿插，三维结构具有互穿的空间结构；合成方法主要包括如下步骤：
(1)将FeCl2·4H2O、2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸分别加入乙醇和水的混合溶液中，超声振荡清器震荡35分钟，充分溶解混合均匀后将混合液转移至聚四氟乙烯内衬反应器中密封；其中，乙醇与水的体积比为1：1，2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸与FeCl2·4H2O的投料摩尔比分别为1.26～1.34:1、0.65～1.39:1和0.41～0.73:1，乙醇和水的混合溶液与FeCl2·4H2O投料的质量比为275.23～550.46:1；
(2)步骤(1)装有反应混合液的反应釜置于电热恒温鼓风干燥箱中，以2℃/min升温速率升至150～170℃反应72小时，再以5℃·h-1的速率冷却至室温；打开反应釜，将底部黄色晶体样品取出，该晶体即2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪铁配合物。
2.根据权利要求1所述的合成方法，其特征在于：合成原料为FeCl2·4H2O、2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸、乙醇和水的混合液；其中，乙醇与水的体积比为1：1，2,4,6-三(对羧基苯基)氨基-1,3,5-三嗪、K2CO3和抗坏血酸与FeCl2·4H2O的投料摩尔比分别为1.26～1.34:1、0.65～1.39:1和0.41～0.73:1，乙醇和水的混合溶液与FeCl2·4H2O投料的质量比为275.23～550.46:1。
3.根据权利要求1所述的合成方法，其特征在于：合成条件为密封反应釜中空气气氛下以2℃/min升温速率升至150～170℃反应72小时，再以5℃·h-1的速率冷却至室温。
4.根据权利要求1所述的合成产物三嗪铁配合物，其特征在于：配合物单体由48个C原子、39个H原子、1个Cl原子、2个Fe原子、12个N原子和16.5个O原子构成；晶体相对分子质量为1195.06g/mol，晶系属于立方型晶系，空间群为Pa-3；从配位上看，Fe与配体上的O进行配位，常见的O-Fe-O键角包括74.8(7)°、87.7(3)°、125.9(5)°、103.6(7)°等，键长包括
等；并且最终结构中包含多个不饱和N，C-N-C之间的键角主要包括114.2(4)°、130.6(4)°等，键长包括
等；拓扑结构上，金属与配体相互连接，在一定的方向呈现出层状结构，配体本身结构中的三苯环共面，支链相互穿插，三维结构具有互穿的空间结构。
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| CN107383072A (zh) * | 2017-06-19 | 2017-11-24 | 许昌学院 | 一种多羧酸与铕配合物发光材料及其制备方法 |
| CN110128307A (zh) * | 2019-06-12 | 2019-08-16 | 禄丰天宝磷化工有限公司 | 一种稳定的氨基酸亚铁配合物的制备方法 |
| CN111727170A (zh) * | 2018-02-13 | 2020-09-29 | 加兹纳特股份公司 | Fe-N-C催化剂，制备方法及其用途 |
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| CN107383072A (zh) * | 2017-06-19 | 2017-11-24 | 许昌学院 | 一种多羧酸与铕配合物发光材料及其制备方法 |
| CN111727170A (zh) * | 2018-02-13 | 2020-09-29 | 加兹纳特股份公司 | Fe-N-C催化剂，制备方法及其用途 |
| CN110128307A (zh) * | 2019-06-12 | 2019-08-16 | 禄丰天宝磷化工有限公司 | 一种稳定的氨基酸亚铁配合物的制备方法 |
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