CN104844663A - Nickel coordination polymer and preparation method thereof - Google Patents
Nickel coordination polymer and preparation method thereof Download PDFInfo
- Publication number
- CN104844663A CN104844663A CN201510160203.1A CN201510160203A CN104844663A CN 104844663 A CN104844663 A CN 104844663A CN 201510160203 A CN201510160203 A CN 201510160203A CN 104844663 A CN104844663 A CN 104844663A
- Authority
- CN
- China
- Prior art keywords
- nickel
- complex
- ligand polymer
- preparation
- coordination polymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229920001795 coordination polymer Polymers 0.000 title abstract 3
- 239000013256 coordination polymer Substances 0.000 title abstract 3
- 239000003446 ligand Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQEZHWGJSWHXPJ-UHFFFAOYSA-N 5-(4-carboxyphenyl)benzene-1,3-dicarboxylic acid Chemical group C1=CC(C(=O)O)=CC=C1C1=CC(C(O)=O)=CC(C(O)=O)=C1 LQEZHWGJSWHXPJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 229920000642 polymer Polymers 0.000 claims description 17
- 239000000696 magnetic material Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 5
- 230000003993 interaction Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 230000005291 magnetic effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005343 Curie-Weiss law Effects 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000005292 diamagnetic effect Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention provides a nickel coordination polymer. The molecular formula of the nickel coordination polymer is {Ni5(HBPT)4(OH)2(H2O)12}n, and H3BPT represents 3,4',5-biphenyltricarboxylic acid. The above complex is prepared through a hydrothermal or solvothermal technology. A preparation method of the complex comprises the following steps: dissolving Ni(NO3)2.6H2O and the H3BPT ligand in an H2O/ethanol mixed solution according to a molar ratio of 2:1, and reacting in a hydrothermal reaction kettle at 160DEG C for 72h; and carrying out room temperature cooling to obtain pale green acicular crystals, washing by using a mother liquor, and carrying out vacuum drying. Weak ferromagnetic interaction exists among Ni(II) ions in the complex, so the complex can be used as a potential molecular magnet.
Description
Technical field
The present invention relates to transition-metal coordination polymkeric substance, particularly the one ligand polymer with ferromagnetic interaction of constructing based on transiting metal nickel and 3,4', 5-biphenyl tricarboxylic acid, specifically a kind of ligand polymer and preparation method thereof of nickel.
Background technology
Molecular magnetic materials is a class by chemical process by free radical or paramagnetic ion (mainly containing transition metal ion and rare earth ion) and diamagnetic ligand combination and the magnetic compound formed.Compared with conventional magnet, molecular magnet has the advantages such as density is little, solvability good, be easy to processing, transparency is high, controllability is good.There is potential application in fields such as space material, microwave material, information-recording material, optomagnetic and electromagnetic materials, therefore the research of molecular magnetism has been become to the study hotspot in the fields such as chemistry, physics and Materials science in recent years.Therefore, the molecular magnet finding excellent property is the focus of molecule magnetics and material science research.
Summary of the invention
The object of the invention is to based on the above-mentioned state of the art, provide a kind of can as the ligand polymer of the nickel of molecular magnetic materials and
Its preparation method.
The ligand polymer of a kind of nickel provided by the invention, its molecular formula is: { Ni
5(HBPT)
4(OH)
2(H
2o)
12}
n, wherein H
3bPT represents 3,4', 5-biphenyl tricarboxylic acid.Structural formula is:
The preparation method of the ligand polymer of nickel provided by the invention, comprises the steps:
(1) by mol ratio be the Ni (NO of 2:1
3)
2.6H
20 and 3,4', 5-biphenyl tricarboxylic acid, add the H containing volume ratio 2:1
20, with the polyfluortetraethylene pipe of the mixed solvent of ethanol, adjusts pH to be 6.5 with the KOH of 0.2mmol/L;
(2) this polyfluortetraethylene pipe is placed in stainless steel cauldron to seal, at 160 DEG C, reacts 72h, Temperature fall, precipitation light green needle-like crystal overnight, dry with mother liquor washing final vacuum.
Advantage of the present invention and effect:
Nickel ligand polymer of the present invention obtains under water (solvent) thermal synthesis condition, and reparation technology is simple, and productive rate, purity are higher.
Nickel ligand polymer provided by the invention is based on 3,4', 5-biphenyl tricarboxylic acid part is constructed, under 1000Oe foreign field, draw in this ligand polymer to there is weak ferromagnetic interaction between nickel ion by variable temperature magnetic susceptibility experimental data, can as molecular magnetic materials.
Accompanying drawing explanation
The crystalline structure figure of the ligand polymer of Fig. 1 nickel of the present invention
The ligand polymer of Fig. 2 nickel of the present invention is at the X-ray powder diffraction figure of 298K
The variable temperature magnetic susceptibility graphic representation of ligand polymer under 1000Oe external magnetic field of Fig. 3 nickel of the present invention
Embodiment
Embodiment 1
Take 0.2mmol H
3bPT and 0.1mmol Ni (NO
3)
2.6H
20 adds containing 4ml H
2in the 13ml polyfluortetraethylene pipe of 0/2ml ethanol, adjust pH for 6.5 with 0.2mmol KOH.Be sealed in stainless steel cauldron by this polyfluortetraethylene pipe, heat 72h at 160 DEG C after, Temperature fall, precipitation light green needle-like crystal overnight, dry with mother liquor washing final vacuum, productive rate is 45%.Ultimate analysis: theoretical value: C 42.88, H 3.48; Experimental value: C 42.84, H 3.51.
The ligand polymer structure determination of nickel:
Crystal structure determination adopts X-ray diffraction, and with the Mo-K alpha-ray of Bruker Smart Apex II detector by graphite monochromator monochromatization, scan mode ω, the temperature of collecting data is 293K.Raw data, after SAINT reduction, uses SADABS to carry out absorption correction.Crystalline structure is solved by SHELXL-97 direct method.Detailed axonometry data are in table 1; Crystalline structure is shown in Fig. 1.
The crystallographic data of table 1 title complex 1
Powdery diffractometry:
It is consistent with simulation collection of illustrative plates that X-ray powder diffraction result obtains experimental diffraction collection of illustrative plates, shows that nickel complex crystal prototype thing of the present invention is mutually homogeneous, see Fig. 2.
The magnetic property of the complex material of nickel:
As shown in Figure 3, as can be seen from the figure, nickel complex is χ when room temperature for variable temperature magnetic susceptibility curve
mt value is 5.07cm
3kmol
-1, the room temperature magnetic moment (5.0cm of Ni (II) ion that is not coupled a little more than 5 independences
3kmol
-1).Along with the reduction of temperature, χ
mt value slowly raises, as χ after 60K
mt value raises rapidly, reaches maximum value 6.47cm when 8K
3kmol
-1, show to there is weak ferromagnetic interaction between five core nickel ions.In addition, Curie-Weiss law matching χ is utilized
m -1-T, can obtain C=2.43cm
3mol
-1, θ=2.19K, θ >0 proves to there is weak ferromagnetic interaction between this ligand polymer nickel ion again.
Claims (3)
1. a ligand polymer for nickel, is characterized in that, structural formula is:
2. the preparation method of the ligand polymer of a kind of nickel according to claim 1, is characterized in that, comprise the steps:
(1) by mol ratio be the Ni (NO of 2:1
3)
2.6H
20 and 3,4', 5-biphenyl tricarboxylic acid, add the H containing volume ratio 2:1
20, with the polyfluortetraethylene pipe of the mixed solvent of ethanol, adjusts pH to be 6.5 with the KOH of 0.2mmol/L;
(2) this polyfluortetraethylene pipe is placed in stainless steel cauldron to seal, at 160 DEG C, reacts 72h, Temperature fall, precipitation light green needle-like crystal overnight, dry with mother liquor washing final vacuum.
3. the ligand polymer of nickel as claimed in claim 1 is used as molecular magnetic materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160203.1A CN104844663B (en) | 2015-04-07 | 2015-04-07 | A kind of coordination polymer of nickel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160203.1A CN104844663B (en) | 2015-04-07 | 2015-04-07 | A kind of coordination polymer of nickel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104844663A true CN104844663A (en) | 2015-08-19 |
| CN104844663B CN104844663B (en) | 2017-08-25 |
Family
ID=53844691
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510160203.1A Expired - Fee Related CN104844663B (en) | 2015-04-07 | 2015-04-07 | A kind of coordination polymer of nickel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104844663B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131045A (en) * | 2015-09-10 | 2015-12-09 | 辽宁大学 | Salicylaldehyde schiff base ligand nickel metallic complex, and preparation method and application thereof |
| CN105153243A (en) * | 2015-08-31 | 2015-12-16 | 陕西师范大学 | Cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and preparation method of porous crystal |
| CN108484647A (en) * | 2018-04-17 | 2018-09-04 | 山西大学 | A kind of Nd complex and its preparation method and application |
| CN108912341A (en) * | 2018-07-23 | 2018-11-30 | 重庆师范大学 | Host-guest type lead coordination polymer, preparation method and its application in cation detection |
| CN109575304A (en) * | 2018-12-13 | 2019-04-05 | 山西大学 | A kind of nickel coordination polymer and its preparation method and application |
| CN113372394A (en) * | 2021-06-10 | 2021-09-10 | 重庆师范大学 | Double-core host-guest supramolecule and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130184456A1 (en) * | 2011-06-20 | 2013-07-18 | University Of South Florida | Heterocyclic macrocycle templated metal-organic materials |
| CN103833793A (en) * | 2014-03-06 | 2014-06-04 | 山西大学 | Nickel-coordination polymer and preparation method thereof |
-
2015
- 2015-04-07 CN CN201510160203.1A patent/CN104844663B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130184456A1 (en) * | 2011-06-20 | 2013-07-18 | University Of South Florida | Heterocyclic macrocycle templated metal-organic materials |
| CN103833793A (en) * | 2014-03-06 | 2014-06-04 | 山西大学 | Nickel-coordination polymer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王代银，: "基于3,4’,5-联苯三甲酸的微孔结构的调控化研究", 《广西民族大学硕士学位论文》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153243A (en) * | 2015-08-31 | 2015-12-16 | 陕西师范大学 | Cluster base heterocaryosis N-(phosphonic acid methyl) iminodiacetic acid trimesicate magnesium-nickel porous crystal and preparation method of porous crystal |
| CN105153243B (en) * | 2015-08-31 | 2018-05-08 | 陕西师范大学 | Cluster base heteronuclear N- (phosphonomethyl) iminodiacetic acid trimesic acid magnesium nickel porous crystalline and preparation method thereof |
| CN105131045A (en) * | 2015-09-10 | 2015-12-09 | 辽宁大学 | Salicylaldehyde schiff base ligand nickel metallic complex, and preparation method and application thereof |
| CN108484647A (en) * | 2018-04-17 | 2018-09-04 | 山西大学 | A kind of Nd complex and its preparation method and application |
| CN108912341A (en) * | 2018-07-23 | 2018-11-30 | 重庆师范大学 | Host-guest type lead coordination polymer, preparation method and its application in cation detection |
| CN108912341B (en) * | 2018-07-23 | 2020-11-27 | 重庆师范大学 | Host-guest lead coordination polymer, preparation method and application thereof in cation detection |
| CN109575304A (en) * | 2018-12-13 | 2019-04-05 | 山西大学 | A kind of nickel coordination polymer and its preparation method and application |
| CN113372394A (en) * | 2021-06-10 | 2021-09-10 | 重庆师范大学 | Double-core host-guest supramolecule and preparation method and application thereof |
| CN113372394B (en) * | 2021-06-10 | 2023-06-27 | 重庆师范大学 | Dual-core host-guest supermolecule and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104844663B (en) | 2017-08-25 |
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Granted publication date: 20170825 Termination date: 20200407 |