CN109232667A - 一种磁性双核钴配合物及其制备方法和应用 - Google Patents
一种磁性双核钴配合物及其制备方法和应用 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000004700 cobalt complex Chemical class 0.000 title description 10
- 230000005389 magnetism Effects 0.000 title description 4
- 239000003446 ligand Substances 0.000 claims abstract description 24
- 230000005291 magnetic effect Effects 0.000 claims abstract description 21
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 15
- 239000010941 cobalt Substances 0.000 claims abstract description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 15
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001868 water Inorganic materials 0.000 claims abstract description 9
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 3
- 239000003205 fragrance Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 150000001868 cobalt Chemical class 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 241000040710 Chela Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000005303 antiferromagnetism Effects 0.000 description 1
- -1 are filtered Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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Abstract
本发明提供了一种磁性双核钴配合物及其制备方法和应用，该配合物的化学式为[Co2(L)2(1,10‑phen)4·2(H2O)]n，分子式为C86 H54 Co2 N8 O16，分子量为:1573.230 g/mol，该配合物属于三斜晶系，P‑1空间群。分别取Co(OAc)2.4H2O、4‑(1′‑羧基‑2′‑萘氧基)邻苯二甲酸与邻菲罗啉配体，加入去离子水，搅拌得混合溶液；密封，于100℃温度下恒温72小时，冷却至室温；过滤，洗涤，得到双核钴磁性配合物。该配合物采用水热法制备而成，半刚性羧酸配体作为桥联配体形成双核钴次级构筑单元。制备过程简单、重复性好、成本低廉、产量高、对环境无污染等优点。
Description
技术领域
本发明属于金属配合物技术领域，涉及一种磁性双核钴配合物及其制备方法和应用。
背景技术
半刚性羧酸配体由于结构的灵活性与多样性，容易与金属原子发生配位，这类配合物具有多功能的特性，在气体吸附与分离，电化学性能，光学性能和磁学性能等多方面表现出优异的性能，应用前景广阔而受到广泛关注。
随着科研工作者对功能性配合物的持续研究，设计多功能化配体改变有机配体的结构来调控功能配合物材料的性能变得尤为重要，邻菲罗啉配体作为一个重要的多功能螯合配体，含有可螯合配位的N原子，形成大的共轭体系，也是构筑磁性配合物的潜在配体。
发明内容
本发明的目的是提供一种基于4-(1′-羧基-2′-萘氧基)邻苯二甲酸为配体的双核钴磁性配合物及其制备方法，晶体结构和磁性能方面的应用。
本发明所述的磁性双核钴配合物，其化学式为：[Co2(L)2(1,10-phen)4·2(H2O)]n，其中L为质子化的4-(1′-羧基-2′-萘氧基)邻苯二甲酸；
该配合物属于三斜晶系，P-1空间群，晶胞参数为a＝12.0414(14)Å，b＝12.9608(15)Å，c＝12.9938(16)Å。α＝75.678(3)°，β＝73.388(3)°，γ=62.641(3)°。单胞体积为1709.8(4)。Co1是六配位的，四个氮原子( N1, N2, N3, N4 )，来自于邻菲罗啉配体，O4来自于半刚性羧酸配体，O5A来自于配位水分子，形成扭曲八面体配位几何构型。其中Co1-O4=2.084Å, Co1-O5=2.078 Å, Co1-N1=2.137 Å, Co1-N2=2.162 Å, Co1-N3=2.142 Å, Co1-N4=2.152 Å,Co1与Co1A间距离为4.79434(4) Å。
本发明所述的基于4-(1′-羧基-2′-萘氧基)邻苯二甲酸为配体的双核钴磁性配合物的分子式为C86H54Co2N8O16，分子量为:1573.230g/mol。
该双核钴配合物的制备方法：
1）按摩尔比1:1:2，分别取Co(OAc)2.4H2O、4-(1′-羧基-2′-萘氧基)邻苯二甲酸与邻菲罗啉配体，加入去离子水（8 mL），搅拌20min，将混合溶液加入到内置聚四氟乙烯内衬的不锈钢反应釜中；
2）反应釜密封，于烘箱中100℃温度下恒温72小时，关闭烘箱后，室温下自然冷却至室温；
3）在母液中形成橙色块状晶体，过滤，去离子水洗涤，得到双核钴磁性配合物。
本发明双核钴磁性配合物可用于制备磁性材料。
本发明双核钴磁性配合物采用水热法制备而成，邻菲罗啉和半刚性羧酸配体作为桥联配体形成双核钴次级构筑单元。制备过程简单、重复性好、成本低廉、产量高、对环境无污染等优点。
附图说明
图1是实施例制得的钴配合物的配位图.
图2是实施例制得的钴配合物形成的双核结构。
图3是实施例制得的配合物在298K时的X射线粉末衍射图（实验及模拟图）。
图4是本发明双核钴配合物在N2气氛下以10℃/ min的加热速率在25～800℃热重曲线图。
图5是本发明双核钴配合物在1000 oe外磁场作用下的χMT对T的曲线图。
具体实施方式
实施例：
按摩尔比1:1:2 ，分别取Co(OAc)2.4H2O（17.7mg，0.10mmol）、4-(1′-羧基-2′-萘氧基)邻苯二甲酸（H3L）（35.2mg，0.10mmol）和1,10-邻菲罗啉（36.1mg，0.2mmol），溶于去离子水（8mL）中并在空气中搅拌20分钟。将所得溶液转移至25mL Teflon内衬里的不锈钢反应器中并在100℃加热72小时，然后自然冷却至室温。从母液中分离橙色块状晶体，用水洗涤，然后在环境温度下干燥。以71%的收率获得晶体。
元素分析：理论值：C，65.66%; H，3.46%；N，7.12%。实验值：C, 65.01%；H, 3.47%；N, 7.68%。
实施例制得的双核钴配合物属于三斜晶系，P-1空间群，该配合物的非对称单元包括一个钴离子，一个半刚性羧酸配体，两个邻菲罗琳含氮配体，一个配位水分子，Co1属于六配位的，与来自于邻菲罗啉配体的N1、N2、N3、N4，一个半刚性羧酸配体O4以及一个来自配位水分子O5A配位，形成扭曲的八面体构型，见图1。两个Co原子通过两个羧酸配体进一步桥联形成一个双核单元，如图2所示；其中Co1-O4=2.084 Å, Co1-O5=2.078 Å, Co1-N1=2.137Å, Co1-N2=2.162 Å, Co1-N3=2.142 Å, Co1-N4=2.152 Å,Co1与Co1A间距离为4.79434(4)Å。
实施例制得的配合物在298K时的X射线粉末衍射图，见图3；通过图3可知，该配合物的实验值和模拟值的主要的衍射峰位置一样，可以证明所得的配合物具有较高的纯度。
在Perkin-Elmer TG-7分析仪上对实施例制得的配合物进行热重分析（TGA）实验，在N2气氛下以10℃/min的升温速率将配合物从25℃加热至800℃，得到图4所示的热重曲线图。图4显示，该配合物在180℃以下表现稳定，但在181～452℃范围内的重量损失为36.45%，表现为失去配位水分子，之后配合物骨架发生坍塌。说明实施例制得的配合物的热稳定性良好。
基于钴的双核金属有机配合物的变温磁化率测试在2～300K的温度范围内，1000oe外加磁场条件下测量，得图5所示的χMT对T的曲线图。变温磁化率的测试结果表明：在2～300 K范围内，随着温度的下降，χMT值缓慢下降，当降低到50K以后，χMT值就迅速降低，表明配合物为反铁磁相互作用。对其进行拟合可得g=2.96224，J=-4.62772。J值为负值证明了双核钴磁性配合物呈现弱的反铁磁性。
实施例制得的配合物的晶体学参数，如表1所示。
表1[Co2(L)2(1,10-phen)4·2(H2O)]n的晶体学参数
a R1 = å||Fo| － |Fc||/å |Fo|. b wR2 = |åw(|Fo|2－ |Fc|2)|/å|w(Fo)2|1/2, wherew = 1/[σ2(Fo 2) + (αP)2 + bP]. P = (Fo 2 + 2Fc 2)/3。
Claims (4)
1.一种双核钴磁性配合物，其特征在于：该配合物化学式为[Co2 (L)2 (1,10-phen)4·2 (H2O)，分子式为C86 H54 Co2 N8 O16，分子量为:1573.230 g/mol，该配合物属于三斜晶系，P-1空间群，晶胞参数为ａ＝12.0414(14)Å，b＝12.9608(15)Å，ｃ＝12.9938(16)Å，
α＝75.678(3)°，β＝73.388(3)°，γ=62.641(3)°，单胞体积为1709.8(4)，
Co1是六配位的，四个氮原子( N1, N2, N3, N4 )，来自于邻菲罗啉配体，O4来自于半刚性羧酸配体，O5A来自于配位水分子，形成扭曲的八面体配位几何构型；其中Co1-O4=2.084 Å, Co1-O5=2.078 Å, Co1-N1=2.137 Å, Co1-N2=2.162 Å, Co1-N3=2.142 Å, Co1-N4=2.152 Å,Co1与Co1A间距离为4.79434(4) Å。
2.一种权利要求1所述的双核钴磁性配合物的制备方法，其特征在于，具体步骤为：
1）按摩尔比1:1:2，分别取Co(OAc)2.4H2O、4-(1′-羧基-2′-萘氧基)邻苯二甲酸与邻菲罗啉配体，加入去离子水，搅拌，得混合溶液；
2）密封条件下，于100℃温度下恒温72小时，自然冷却至室温；
3）过滤，洗涤，得到双核钴磁性配合物。
3.一种权利要求1所述的双核钴磁性配合物的应用。
4.如权利要求3所述的双核钴磁性配合物的应用，其特征在于，该配合物可用于制备磁性材料。
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| CN112480174A (zh) * | 2020-11-26 | 2021-03-12 | 宁波大学 | 一种具有反铁磁作用的锰配合物及其制备方法 |
| CN114031647A (zh) * | 2021-12-06 | 2022-02-11 | 广西师范大学 | 双核钴配合物及其制备方法和应用 |
| CN114854037A (zh) * | 2022-03-21 | 2022-08-05 | 宿州学院 | 一种具有半导体性质的钴(ii)配合物及制备方法 |
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| CN108084455A (zh) * | 2018-01-22 | 2018-05-29 | 西北师范大学 | 一种磁性三核锰(ii)金属配合物及其制备方法 |
| CN108440766A (zh) * | 2018-04-17 | 2018-08-24 | 山西大学 | 一种钴金属有机骨架材料及其制备方法和应用 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112480174A (zh) * | 2020-11-26 | 2021-03-12 | 宁波大学 | 一种具有反铁磁作用的锰配合物及其制备方法 |
| CN112480174B (zh) * | 2020-11-26 | 2024-01-19 | 宁波大学 | 一种具有反铁磁作用的锰配合物及其制备方法 |
| CN114031647A (zh) * | 2021-12-06 | 2022-02-11 | 广西师范大学 | 双核钴配合物及其制备方法和应用 |
| CN114854037A (zh) * | 2022-03-21 | 2022-08-05 | 宿州学院 | 一种具有半导体性质的钴(ii)配合物及制备方法 |
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