CN104036909B - Magnetic material [Cu3(N3)6(DMF)2]nand synthetic method - Google Patents
Magnetic material [Cu3(N3)6(DMF)2]nand synthetic method Download PDFInfo
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Abstract
The invention discloses a kind of magnetic material [Cu3(N3)6(DMF)2] n And synthetic method.(1) analytically pure for 0.125 0.25g 3 ethyoxyl 2 hydroxy benzaldehydes are dissolved in 10 20ml analytical pure N, in N ' dimethylformamide (DMF) solution.(2) it is sequentially added into the 0.128 analytically pure Copper dichloride dihydrate of 0.256g and 0.098 0.196g analytical pure Hydrazoic acid,sodium salt, stirs 10 minutes.(3) adding analytical pure triethylamine regulation pH in step (2) gained solution is 6.5, after stirring 20 minutes by the solution left standstill that obtains at room temperature, black bulk crystals is obtained after three days, filter, and with analyzing N, N ' dimethylformamide (DMF) washes clean, obtains product [Cu in air after drying3(N3)6(DMF)2] n 。[Cu3(N3)6(DMF)2] n Magnetic property: there is ferromagnetic exchange between intramolecular copper ion, its general performance is ferromagnetism.The present invention has that technique is simple, with low cost, chemical constituent is easily controllable, reproducible and yield advantages of higher.
Description
Technical field
The present invention relates to a kind of magnetic material [Cu3(N3)6(DMF)2]nAnd synthetic method.
Background technology
Modem magnetic materials has been widely used among our life, such as, permanent magnet material is used as motor, the core material being applied in transformator, the magneto-optic disk used as memorizer, computer magnetic recording floppy disk etc..It can be said that magnetic material is closely related with informationization, automatization, electromechanical integration, national defence, the every aspect of national economy.For coordination compound magnetic material, explore the mechanism of its magnetic generation and set up the foundation that rational theoretical model is its fast development.Start with from MOLECULE DESIGN, reasonable cutting molecular structure, both economy can develop magnetic partner quickly, and it can be carried out modified with functional group again and change its magnetic.Along with people are to magnetic is theoretical and Coordinative Chemistry research is goed deep into, the complex molecule magnetic material more with practical value will be synthesized, and these will have the application of coordination compound magnetic material will to cause a series of great technological innovations in fields such as space flight, aviation, military project, information, superconductions.
Summary of the invention
The purpose of the present invention is exactly the functional material for design synthesis magnetic property excellence, utilizes room temperature solwution method synthetic technology to synthesize [Cu3(N3)6(DMF)2]n。
[the Cu that the present invention relates to3(N3)6(DMF)2]nMolecular formula be: C6H14Cu3N20O2, molecular weight is: 589.02, DMF i.e. N, N '-dimethyl Methanamide；Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Table one [Cu3(N3)6(DMF)2]nCrystallographic parameter
Table two [Cu3(N3)6(DMF)2]nBond distanceWith bond angle (°)
[Cu3(N3)6(DMF)2]nSynthetic method concretely comprise the following steps:
(1) analytically pure for 0.125-0.25g 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 10-20ml analytical pure N, in N '-dimethyl Methanamide (DMF) solution.
(2) in step (1) gained solution, it is sequentially added into the analytically pure Copper dichloride dihydrate of 0.128-0.256g and 0.098-0.196g analytical pure Hydrazoic acid,sodium salt, stirs 10 minutes.
(3) adding analytical pure triethylamine regulation pH in step (2) gained solution is 6.5, after stirring 20 minutes by the solution left standstill that obtains at room temperature, black bulk crystals is obtained after three days, filter, and use analytical pure N, N '-dimethyl Methanamide (DMF) washes clean, obtains product [Cu in air after drying3(N3)6(DMF)2]n。
[Cu3(N3)6(DMF)2]nMagnetic property: there is ferromagnetic exchange between intramolecular copper ion, its general performance is ferromagnetism.
The present invention has that technique is simple, with low cost, chemical constituent is easily controllable, reproducible and yield advantages of higher.
Accompanying drawing explanation
Fig. 1 is the present invention [Cu3(N3)6(DMF)2]nStructure chart.
Fig. 2 is the embodiment of the present invention [Cu3(N3)6(DMF)2]n2D stratiform figure, in order to clear, eliminate DMF molecule.
Fig. 3 is the embodiment of the present invention [Cu3(N3)6(DMF)2]nχM-T,χMT-T curve chart.
Fig. 4 is the embodiment of the present invention [Cu3(N3)6(DMF)2]nχM – 1-T curve figure.
Detailed description of the invention
Embodiment 1:
[the Cu that the present invention relates to3(N3)6(DMF)2]nMolecular formula be: C6H14Cu3N20O2
Molecular weight is: 589.02.
[Cu3(N3)6(DMF)2]nSynthetic method concretely comprise the following steps:
(1) 0.125 gram of analytical pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 10 milliliters of analytically pure N, in N '-dimethyl Methanamide (DMF) solution.
(2) in step (1) gained solution, it is sequentially added into the analytically pure Copper dichloride dihydrate of 0.128g and the analytically pure Hydrazoic acid,sodium salt of 0.098g, stirs ten minutes.
(3) in step (2) gained solution, add analytically pure triethylamine regulate to pH=6.5, after stirring 20 minutes, obtained mixed liquor is stood at room temperature, black bulk crystals is obtained after three days, filter, and use analytical pure N, N '-dimethyl Methanamide (DMF) washes clean, obtain product [Cu after drying in air3(N3)6(DMF)2]n.Yield: 86 milligrams, productivity: 58.4%, and measure polymer [Cu by single crystal diffractometer3(N3)6(DMF)2]nMolecular structure, crystallographic parameter is shown in Table one, and bond distance's bond angle is shown in Table two.
(4) product [Cu that 0.0223 gram of step (3) is obtained3(N3)6(DMF)2]nOn Magnetic Test instrument, carry out Magnetic Test after pulverizing, obtain Magnetic Test curve such as accompanying drawing 2,3, [Cu3(N3)6(DMF)2]nAt room temperature χMT is 1.403cm3Kmol– 1, along with temperature reduces, χMT gradually rises, and reaches maximum 2.490cm to 14.5K3Kmol– 1, the most drastically it is down to 0.442cm3Kmol– 1.To χM-T,χMT T curve obtains the Lang De factor after being analyzed matching be 2.27, and the magnetic exchange constant between intramolecular copper ion is 14.49cm– 1, the magnetic exchange constant of intermolecular copper ion is :-10.84cm– 1.And χM – 1-T curve defers to Curie-Weiss law, and it is 24.59K that its matching obtains Wei Si constant, and Curie constant is 1.317cm3Kmol– 1.Big and positive Wei Si constant, intramolecular magnetic exchange constant and χMT-T curvilinear trend all implies and there is ferromagnetic exchange between intramolecular copper ion, and its general performance is ferromagnetism.
Embodiment 2:
[the Cu that the present invention relates to3(N3)6(DMF)2]nMolecular formula be: C6H14Cu3N20O2Molecular weight is: 589.02.
[Cu3(N3)6(DMF)2]nSynthetic method concretely comprise the following steps:
(1) 0.25 gram of analytically pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 20 milliliters of analytical pure N, in N '-dimethyl Methanamide (DMF) solution.
(2) in step (1) gained solution, it is sequentially added into the analytically pure Copper dichloride dihydrate of 0.256g and the analytically pure Hydrazoic acid,sodium salt of 0.196g, stirs 10 minutes.
(3) in step (2) gained solution, add analytically pure triethylamine regulate to pH=6.5, after stirring 20 minutes, stand at room temperature, black bulk crystals is obtained after three days, filter, and use analytical pure N, N '-dimethyl Methanamide (DMF) solution washes clean, obtain product [Cu after drying in air3(N3)6(DMF)2]n。
(4) product [Cu that 0.0223 gram of step (3) is obtained3(N3)6(DMF)2]nOn Magnetic Test instrument, carry out Magnetic Test after pulverizing, obtain Magnetic Test curve such as accompanying drawing 2,3, [Cu3(N3)6(DMF)2]nAt room temperature χMT is 1.403cm3Kmol– 1, along with temperature reduces, χMT gradually rises, and reaches maximum 2.490cm to 14.5K3Kmol– 1, the most drastically it is down to 0.442cm3Kmol– 1.To χM-T,χMT T curve obtains the Lang De factor after being analyzed matching be 2.27, and the magnetic exchange constant between intramolecular copper ion is 14.49cm-1, the magnetic exchange constant of intermolecular copper ion is :-10.84cm– 1.And χM – 1-T curve defers to Curie-Weiss law, and it is 24.59K that its matching obtains Wei Si constant, and Curie constant is 1.317cm3Kmol– 1.Big and positive Wei Si constant, intramolecular magnetic exchange constant and χMT-T curvilinear trend all implies and there is ferromagnetic exchange between intramolecular copper ion, and its general performance is ferromagnetism.
Claims (1)
1. [a Cu3(N3)6(DMF)2]n, it is characterised in that [Cu3(N3)6(DMF)2]nMolecular formula is:
C6H14Cu3N20O2, molecular weight is: 589.02, DMF i.e. N, N '-dimethyl Methanamide；Molecular structure is brilliant
Body parameter is shown in Table one, and bond distance's bond angle is shown in Table two；
Described [Cu3(N3)6(DMF)2]nSynthetic method concretely comprise the following steps:
(1) analytically pure for 0.125-0.25g 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 10-20ml analytical pure
N, in N '-dimethyl Methanamide i.e. DMF；
(2) in step (1) gained solution, the analytically pure Copper dichloride dihydrate of 0.128-0.256g it is sequentially added into
With 0.098-0.196g analytical pure Hydrazoic acid,sodium salt, stir 10 minutes；
(3) adding analytical pure triethylamine regulation pH in step (2) gained solution is 6.5, stirs 20 points
, after three days, obtain black bulk crystals after clock by the solution left standstill that obtains at room temperature, filter, and with analysis
Pure N, N '-dimethyl Methanamide washes clean, obtain product [Cu after drying in air3(N3)6(DMF)2]n；
Table one [Cu3(N3)6(DMF)2]nCrystallographic parameter
Table two [Cu3(N3)6(DMF)2]nBond distanceWith bond angle (°)
Described [Cu3(N3)6(DMF)2]nMagnetic property:
(1) there is ferromagnetic exchange between intramolecular copper ion, its general performance is ferromagnetism；
(2)[Cu3(N3)6(DMF)2]nAt room temperature χMT is 1.403cm3Kmol–1, along with temperature reduces, χMT
Gradually rise, reach maximum 2.490cm to 14.5K3Kmol–1, the most drastically it is down to 0.442cm3
Kmol–1；To χM-T,χMT T curve obtains the Lang De factor after being analyzed matching be 2.27, intramolecular
Magnetic exchange constant between copper ion is 14.49cm–1, the magnetic exchange constant of intermolecular copper ion is:
-10.84cm-1；And χM –1-T curve defers to Curie-Weiss law, and it is 24.59K that its matching obtains Wei Si constant,
Curie constant is 1.317cm3Kmol–1；Big and positive Wei Si constant, intramolecular magnetic exchange constant and χMT-T
Curvilinear trend all implies and there is ferromagnetic exchange between intramolecular copper ion, and its general performance is ferromagnetism.
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| CN102911194A (en) * | 2012-10-15 | 2013-02-06 | 南京邮电大学 | Preparation method of nano rare earth carboxylic acid coordination polymer and application thereof |
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| CN101692366A (en) * | 2009-09-14 | 2010-04-07 | 深圳市康源新通信技术有限公司 | Composite electromagnetic medium material containing dicyclopentadienyl iron phthalocyanine metal organic magnetic body and preparation method thereof |
| CN102911194A (en) * | 2012-10-15 | 2013-02-06 | 南京邮电大学 | Preparation method of nano rare earth carboxylic acid coordination polymer and application thereof |
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| Synthesis and biological evaluation of new N-linked 5-triazolylmethyl oxazolidinones;Houxing Fan等;《European of Journal of Medicinal Chemistry》;20070926;第43卷(第8期);第1706-1714页 * |
| Synthesis,crystal structure and magnetic properties of cubane and linear trinuclear nickel complexes formed by 3,5-dichloro-2-hydroxybenzylaminoacetic acid;Yu Xiao等;《Inorganica Chimica Acta》;20110130;第366卷(第1期);第39-43页 * |
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