CN102993222A - Dysprosium coordination polymer material with solvent molecule magnetic response and preparation method thereof - Google Patents
Dysprosium coordination polymer material with solvent molecule magnetic response and preparation method thereof Download PDFInfo
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- CN102993222A CN102993222A CN201210559155XA CN201210559155A CN102993222A CN 102993222 A CN102993222 A CN 102993222A CN 201210559155X A CN201210559155X A CN 201210559155XA CN 201210559155 A CN201210559155 A CN 201210559155A CN 102993222 A CN102993222 A CN 102993222A
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- dysprosium
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- 239000002904 solvent Substances 0.000 title claims abstract description 66
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052692 Dysprosium Inorganic materials 0.000 title claims abstract description 39
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 37
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 36
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003446 ligand Substances 0.000 claims abstract description 43
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000011232 storage material Substances 0.000 claims abstract description 5
- -1 dysprosium ions Chemical class 0.000 claims abstract description 4
- IOIFRTZBJMZZFO-UHFFFAOYSA-N dysprosium(3+) Chemical compound [Dy+3] IOIFRTZBJMZZFO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- PWRIYLNKKJQFGA-UHFFFAOYSA-N [N]=O.C(C1=CC=NC=C1)(=O)O Chemical compound [N]=O.C(C1=CC=NC=C1)(=O)O PWRIYLNKKJQFGA-UHFFFAOYSA-N 0.000 claims abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 claims description 4
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 36
- 238000012360 testing method Methods 0.000 description 9
- 150000000914 Dysprosium Chemical class 0.000 description 7
- TWBYWOBDOCUKOW-UHFFFAOYSA-N isonicotinic acid Chemical compound OC(=O)C1=CC=NC=C1 TWBYWOBDOCUKOW-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229910000952 Be alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
一种具有溶剂分子磁响应的镝配位聚合物材料，为具有单分子磁体行为的镝(III)配位聚合物，其化学式为{[Dy(INO)2(NO3)]}，不对称单元含有一种配位环境的镝离子和存有三种连接模式的HINO配体，双核镝单元之间通过两个配体进一步连接形成三维孔状结构；其制备方法是：将Dy(NO3)3·6H2O与HINO混合并在溶剂中溶解，加热反应后经过滤、洗涤所得固体，再与乙腈混合，加热反应后除去乙腈即可。本发明的优点是：该镝配位聚合物材料结构新颖，为基于异烟酸氮氧化物配体且含有纳米孔洞的三维配位聚合物，展现出慢磁弛豫行为，可用作信息存储材料；其制备方法工艺简单、易于实施，产率高，有利于大规模推广应用。
A Dysprosium coordination polymer material with solvent molecular magnetic response, Dysprosium(III) coordination polymer with single-molecule magnet behavior, its chemical formula is {[Dy(INO) 2 (NO 3 )]}, asymmetric The unit contains dysprosium ions in a coordination environment and HINO ligands with three connection modes, and the dinuclear dysprosium units are further connected by two ligands to form a three-dimensional porous structure; the preparation method is: Dy(NO 3 ) 3 ·6H 2 O is mixed with HINO and dissolved in a solvent. After heating and reacting, the obtained solid is filtered and washed, and then mixed with acetonitrile. After heating and reacting, the acetonitrile can be removed. The advantage of the invention is: the dysprosium coordination polymer material has a novel structure, is a three-dimensional coordination polymer based on isonicotinic acid nitrogen oxide ligand and contains nanoholes, exhibits slow magnetic relaxation behavior, and can be used as information storage material; the preparation method thereof has simple process, is easy to implement, and has high yield, which is conducive to large-scale popularization and application.
Description
[technical field]
The present invention relates to have the polymer materials of single molecular magnets behavior, particularly a kind of have solvent molecule magnetic response dysprosium coordination polymer material and a preparation method.
[background technology]
Magnetics is an important branch in the physics, and the application of magneticsubstance has brought tremendous influence to the development and progress of human society.For a long time, the more researchs of people be the character of conventional magnet, mainly be alloy and metal oxide, metal complexes based on the long-range effect of three-dimensional extended lattice, and the macroscopic magnetization energy that under domain structure is arranged, produces.In the last few years, as emerging physics and chemistry cross discipline, the magnetic that is embodied with exploration open shell molecule and open shell molecule aggregates was characterized as the concern that the molecules of interest magnetics more and more is subject to people.In this field, single molecular magnets has numerous special performances, so become especially study hotspot because this body structure is nano magnetic unit independently.Gondola Sessoli in 1993 etc. have reported unit molecule [Mn
12O
12(O2CR)
16(H
2O)
4] have at low temperatures after the article of superparamagnetic, referring to Sessoli R etc., J.Am.Chem.Soc.1993,115,1804, the correlative study of this quasi-molecule has caused the extensive attention of countries in the world.After the people such as Sessoli and Girolami have carried out systematic study to the feature of single molecular magnets and character and have analyzed, referring to Girolami G S etc., Science 1995,268,397, single molecular magnets becomes one of international emerging research frontier of 21st century gradually.Yet the ligand polymer that has at present the single molecular magnets behavior mostly is zero dimension, have three-dimensional open-framework and change regulation and control character that can be by guest molecule monomolecular magnetic material research seldom.
[summary of the invention]
The objective of the invention is for the above-mentioned state of the art, a kind of have solvent molecule magnetic response dysprosium coordination polymer material and preparation method be provided.
Technical scheme of the present invention:
A kind of dysprosium coordination polymer material with solvent molecule magnetic response is dysprosium (III) ligand polymer with single molecular magnets behavior, and its chemical formula is { [Dy (INO)
2(NO
3)], in the formula: part HINO is the γ-picolinic acid oxynitride; Dysprosium ion and the HINO part that has three kinds of connection modes that a kind of coordination environment is arranged in this dysprosium ligand polymer; This dysprosium ligand polymer belongs to crystal and belongs to oblique system, and spacer is P2
1/ c, unit cell parameters is:
α=γ=90 °, β=108.959 (3) °; The dysprosium ion that a kind of coordination environment is arranged in the described dysprosium ligand polymer, dysprosium ion is positioned at one and is similar to the symmetric symmetry centre of C4v, with seven carboxyl oxygen atoms that come from respectively six γ-picolinic acid oxynitride with come from two oxygen atom ligands on the nitrate radical; Form a double-core dysprosium unit by two μ 2 Sauerstoffatoms and two carboxyl oxygen atom bridgings between two dysprosium ions, further be connected to form three-dimensional cavernous structure by two parts between the double-core dysprosium unit.
A kind of described preparation method with solvent molecule magnetic response dysprosium coordination polymer material, step is as follows:
1) with Dy (NO
3)
36H
2O and the polytetrafluoroethylliner liner of putting into hydrothermal reaction kettle mixing of HINO add dissolution with solvents;
2) above-mentioned hydrothermal reaction kettle is put into baking oven, 80 ° of C heating 72 hours, be cooled to 30 ° of C with 1 ° of C/h speed again, filter, with behind the solvent wash, get the ligand polymer Primary product;
3) above-mentioned ligand polymer Primary product and acetonitrile solvent are mixed in container, put into 40 degree baking ovens and heat, changed an acetonitrile solvent, and obtained ligand polymer exchange of solvent product after 72 hours in per 24 hours;
4) above-mentioned ligand polymer exchange of solvent product is heated one hour to remove acetonitrile solvent at 200 ° of C, can obtain target compound dysprosium coordination polymer material.
Described solvent is DMF (DMF) or ethanol (C
2H
5OH), Dy (NO
3)
36H
2The mol ratio of O, HINO and solvent is 4:3:68.
The mol ratio of described ligand polymer Primary product and acetonitrile solvent is 1:20.
A kind of described application with dysprosium coordination polymer material of solvent molecule magnetic response is as information storage material.
Advantage of the present invention and positively effect:
Dysprosium coordination polymer material novel structure with single molecular magnets behavior of the present invention, for based on γ-picolinic acid oxynitride part and contain the three-dimensional coordination polymer of nano aperture, showing slow magnetic relaxation behavior under the 0Oe foreign field with under the temperature that is lower than 10K, can be used as information storage material; Preparation method's technique of the present invention is simple, easy to implement, and productive rate is high, is conducive to large-scale promotion application.
[description of drawings]
Fig. 1 is the structural representation of the asymmetric cell of this dysprosium ligand polymer.
Fig. 2 is the three-dimensional structure synoptic diagram of this dysprosium ligand polymer.
Fig. 3 is the DC magnetic rate test pattern of this dysprosium ligand polymer.
Fig. 4 is the ac magnetic susceptibility test pattern of this dysprosium ligand polymer.
Fig. 5 is that DMF is as the ac magnetic susceptibility test pattern of the ligand polymer Primary product of solvent preparation.
Fig. 6 is that ethanol is as the ac magnetic susceptibility test pattern of the ligand polymer Primary product of solvent preparation.
Fig. 7 is the ac magnetic susceptibility test pattern of ligand polymer exchange of solvent product.
[embodiment]
Embodiment 1:
A kind of described preparation method with solvent molecule magnetic response dysprosium coordination polymer material, step is as follows:
1) with 0.104g(0.75mmol) γ-picolinic acid oxynitride (HINO), 0.456g(1.00mmol) Dy (NO
3)
36H
2O is mixed to join in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, adds 0.780g(17.00 mmol) the etoh solvent dissolving, with the inner bag reactor of packing into;
2) above-mentioned hydrothermal reaction kettle is put into baking oven, 80 ° of C heating 72 hours, be cooled to 30 ° of C with 1 ° of C/h speed again, filter, with the alcohol solvent washing, obtain Primary product, outward appearance is faint yellow bulk crystals.The Primary product productive rate that calculates based on the metal dysprosium ion is 41%;
3) with 0.512g(1mmol) above-mentioned ligand polymer Primary product and 0.820g(20mmol) acetonitrile solvent mixes in container, putting into 40 degree baking ovens heats, changed an acetonitrile solvent, and obtained ligand polymer exchange of solvent product after 72 hours in per 24 hours;
4) above-mentioned ligand polymer exchange of solvent product is heated one hour to remove acetonitrile solvent at 200 ° of C, can obtain target compound dysprosium coordination polymer material.
Embodiment 2:
Basic identical with method among the embodiment 1, difference is: solvent for use changes to 1.240g(17.00mmol in the step 1)) DMF(N, dinethylformamide); Step 2) in, used cleaning solvent changes to DMF.The Primary product productive rate that calculates based on the metal dysprosium ion is 41%.
The dysprosium coordination polymer material with solvent molecule magnetic response that more than makes can be used as information storage material.
Sign with dysprosium coordination polymer material of solvent molecule magnetic response behavior:
1) structure determination of the dysprosium coordination polymer material of solvent molecule magnetic response behavior
Supernova type X-ray single crystal diffractometer is adopted in crystal structure determination, uses the Mo-K alpha-ray through the graphite monochromatization
Be incident radiation, with
Scan mode is collected point diffraction, obtains unit cell parameters through least-squares refinement, utilizes the SHELXL-97 direct method to solve crystalline structure from the difference Fourier electron density map, and through Lorentz and polarizing effect correction.All H atoms are synthetic and definite through desirable position calculation by difference Fourier.Detailed axonometry data see Table 1; Structure as depicted in figs. 1 and 2.
2) has the magnetic properties of the dysprosium coordination polymer material of solvent molecule magnetic response
Have the solvent molecule magnetic response the dysprosium coordination polymer material the dc magnetization rate curve as shown in Figure 3.As can be seen from the figure, DMF only has as the ligand polymer Primary product of solvent preparation and just shows at low temperatures obvious ferromegnetism character, and removal and change by solvent molecule, target ligand polymer, ethanol have shown omnidistance ferromegnetism behavior as ligand polymer Primary product and the ligand polymer exchange of solvent product of solvent preparation.
Fig. 4 is the ac magnetic susceptibility test pattern of this dysprosium ligand polymer, Fig. 5 is that DMF is as the ac magnetic susceptibility test pattern of the ligand polymer Primary product of solvent preparation, Fig. 6 is ethanol as the ac magnetic susceptibility test pattern of the ligand polymer Primary product of solvent preparation, and Fig. 7 is the ac magnetic susceptibility test pattern of ligand polymer exchange of solvent product.As can be seen from the figure, DMF the imaginary part peak value do not occur as the ligand polymer Primary product of solvent preparation, and removal and change by solvent molecule, target ligand polymer, ethanol have shown obvious peak value as the ligand polymer Primary product of solvent preparation and the ac magnetic susceptibility imaginary part of ligand polymer exchange of solvent product, show that they have the single molecular magnets behavior.And it can be confirmed that target ligand polymer, ethanol have solvent molecule magnetic response behavior as ligand polymer Primary product and the ligand polymer exchange of solvent product of solvent preparation.
Table 1 has the crystallographic data of the dysprosium ligand polymer of single molecular magnets behavior
Claims (5)
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Cited By (7)
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|---|---|---|---|---|
| CN103219148A (en) * | 2013-04-27 | 2013-07-24 | 黑龙江大学 | Preparation method of single-molecule magnetic body |
| CN104497027A (en) * | 2015-01-08 | 2015-04-08 | 黑龙江大学 | Dy monomolecular magnetic material and preparation method thereof |
| CN107556341A (en) * | 2017-09-15 | 2018-01-09 | 南开大学 | Hexa-coordinate chirality dysprosium single ion magnet and its synthetic method with electromagnetic coupling effect |
| CN109485869A (en) * | 2018-11-27 | 2019-03-19 | 广东工业大学 | Two core dysprosium coordination polymers of a kind of one-dimensional chain mixing and preparation method thereof |
| CN112316911A (en) * | 2020-10-28 | 2021-02-05 | 青岛理工大学 | Dual-functional metal organic framework membrane material and preparation method and application thereof |
| CN114524831A (en) * | 2022-02-21 | 2022-05-24 | 温州大学 | Dysprosium complex and preparation method and application thereof |
| CN114656491A (en) * | 2022-04-24 | 2022-06-24 | 郑州轻工业大学 | Multinuclear rare earth based organic-inorganic hybrid magnetic material and preparation method and application thereof |
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Cited By (13)
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| CN107556341B (en) * | 2017-09-15 | 2019-03-26 | 南开大学 | Hexa-coordinate chirality dysprosium single ion magnet and its synthetic method with electromagnetic coupling effect |
| CN107556341A (en) * | 2017-09-15 | 2018-01-09 | 南开大学 | Hexa-coordinate chirality dysprosium single ion magnet and its synthetic method with electromagnetic coupling effect |
| CN109485869A (en) * | 2018-11-27 | 2019-03-19 | 广东工业大学 | Two core dysprosium coordination polymers of a kind of one-dimensional chain mixing and preparation method thereof |
| CN109485869B (en) * | 2018-11-27 | 2021-07-13 | 广东工业大学 | A kind of one-dimensional chain mixed dinuclear dysprosium coordination polymer and preparation method thereof |
| CN112316911A (en) * | 2020-10-28 | 2021-02-05 | 青岛理工大学 | Dual-functional metal organic framework membrane material and preparation method and application thereof |
| CN114524831A (en) * | 2022-02-21 | 2022-05-24 | 温州大学 | Dysprosium complex and preparation method and application thereof |
| CN114524831B (en) * | 2022-02-21 | 2023-06-13 | 温州大学 | Dysprosium complex and preparation method and application thereof |
| CN114656491A (en) * | 2022-04-24 | 2022-06-24 | 郑州轻工业大学 | Multinuclear rare earth based organic-inorganic hybrid magnetic material and preparation method and application thereof |
| CN114656491B (en) * | 2022-04-24 | 2024-01-30 | 郑州轻工业大学 | Polynuclear rare earth-based organic-inorganic hybrid magnetic material, and preparation method and application thereof |
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