CN104021911A - Magnetic material [Co2Na2(hmb)4(N3)2(CH3CN)2] (CH3CN)2 and synthetic method thereof - Google Patents

Magnetic material [Co2Na2(hmb)4(N3)2(CH3CN)2] (CH3CN)2 and synthetic method thereof Download PDF

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CN104021911A
CN104021911A CN201410292859.4A CN201410292859A CN104021911A CN 104021911 A CN104021911 A CN 104021911A CN 201410292859 A CN201410292859 A CN 201410292859A CN 104021911 A CN104021911 A CN 104021911A
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ch3cn
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CN104021911B (en
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张淑华
赵儒霞
周玉洁
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Dongyang Ruibang Magnetic Industry Co., Ltd.
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Guilin University of Technology
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Abstract

The invention discloses a magnetic material [Co2Na2(hmb)4(N3)2(CH3CN)2](CH3CN)2 and a synthetic method thereof. The molecular formula of the magnetic material [Co2Na2(hmb)4(N3)2(CH3CN)2](CH3CN)2 is C40H40Co2N10Na2O12, and the molecular weight is 1016.66, wherein Hnmb is 3-methoxy-2-hydroxybenzaldehyde. The synthetic method comprises the following steps: dissolving 0.114-0.228g of analytical pure 3-methoxy-2-hydroxybenzaldehyde into a mixed solution of 5-10ml of absolute methanol and 5-10ml of analytical pure acetonitrile, adding 0274-0.548g of analytical pure cobalt hexahydrate perchlorate and 0.098-0.196g of analytical pure sodium azide sequentially, stirring, adding analytical pure triethylamine, adjusting the pH to be 5.5, stirring, standing, filtering, and washing. The magnetic property of the [Co2Na2(hmb)4(N3)2(CH3CN)2](CH3CN)2 is as follows: ferromagnetic exchange exists among intramolecularly cobalt ions, which shows the ferromagnetic property. The magnetic material [Co2Na2(hmb)4(N3)2(CH3CN)2](CH3CN)2 and the synthetic method thereof have the advantages of simple technology, low cost, easy chemical component control, good reproducibility, high yield and the like.

Description

Magnetic material [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2and synthetic method
Technical field
The present invention relates to a kind of magnetic material [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2(Hhmb is 3-methoxyl group-Benzaldehyde,2-hydroxy) and synthetic method.
Background technology
Modem magnetic materials has been used among our life widely, for example, permanent magnetic material is used as to motor, is applied to the core material in transformer, the magneto optical disk using as memory, computer magnetic recording floppy disk etc.Can say, magnetic material is closely related with the every aspect of informationization, automation, electromechanical integration, national defence, 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.From MOLECULE DESIGN, start with, rationally cutting molecular structure, both can economy develop magnetic complex quickly, can carry out modified with functional group to it again and change its magnetic.Along with people's going deep into magnetic theory and Coordinative Chemistry research, the organic coordination compound magnetic material more with practical value will be synthesized, and the application of these coordination compound magnetic materials will cause a series of great technological innovations in fields such as space flight, aviation, military project, information, superconductions.
Summary of the invention
Object of the present invention is exactly for designing the functional material of synthetic magnetic property excellence, utilizing normal temperature solwution method synthetic technology to synthesize [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2.
[the Co the present invention relates to 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2molecular formula be: C 40h 40co 2n 10na 2o 12, molecular weight is: 1016.66, Hhmb is 3-methoxyl group-Benzaldehyde,2-hydroxy, and crystal structure data are in Table one, and bond distance's bond angle data are in Table two.
Table one Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2crystallographic parameter
Table two [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2bond distance and bond angle (°)
[Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2synthetic method concrete steps be:
0.114-0.228 gram is analyzed to pure 3-methoxyl group-Benzaldehyde,2-hydroxy is dissolved in 5-10 milliliter absolute methanol and 5-10 milliliter is analyzed in the mixed solution of pure acetonitrile, add successively again 0.274-0.548g to analyze pure six perchloric acid hydrate cobalts and 0.098-0.196g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after three days, obtain red bulk crystals, filter, and clean with analyzing pure methanol wash, after drying, obtain product [Co in air 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2.
[Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2magnetic property: between cobalt ions, have ferromagnetic exchange in molecule, it shows as ferromagnetism.
The present invention has that technique is simple, with low cost, chemical constituent is easy to control, reproducible and output advantages of higher.
Accompanying drawing explanation
Fig. 1 is the present invention [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2structure chart, hydrogen atom and solvent molecule remove.
Fig. 2 is the present invention [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2χ m-T, χ mt-T curve chart.
Fig. 3 is the present invention [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2χ m – 1-T curve chart.
Embodiment
Embodiment 1:
[the Co the present invention relates to 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2molecular formula be:
C 40h 40co 2n 10na 2o 12molecular weight is: 1016.66.
[Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2synthetic method concrete steps be:
(1) 0.114 gram of pure 3-methoxyl group-Benzaldehyde,2-hydroxy of analysis is dissolved in the mixed solution of 5 milliliters of absolute methanols and 5 milliliters of pure acetonitriles of analysis, add successively again 0.274g to analyze pure six perchloric acid hydrate cobalts and 0.098g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after three days, obtain red bulk crystals, filter, and clean with analyzing pure methanol wash, after drying, obtain product [Co in air 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2.Output: 98mg, productive rate: 51.41%, and it measures [Co by single crystal diffraction 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2structure, crystal structure data are in Table one, bond distance's bond angle data are in Table two.
(2) after the product 0.0326 gram of step (1) being obtained pulverizes, on magnetic tester device, carry out magnetic test, obtain magnetic test curve as accompanying drawing 2,3, [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2χ at room temperature mt is 6.84cm 3kmol -1, along with temperature reduces, χ mt raises gradually, reaches maximum 11.35cm to 11K 3kmol -1, be sharply down to subsequently 8.57cm 3kmol -1.To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.58, and the magnetic exchange constant in molecule between cobalt ions is 9.48cm -1, the magnetic exchange constant of intermolecular cobalt ions is :-0.622cm -1.And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 12.55K that its matching is obtained to Wei Si constant, and Curie constant is 6.63cm 3kmol – 1.Large and positive Wei Si constant, magnetic exchange constant and χ in molecule mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism.
Embodiment 2:
[the Co the present invention relates to 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2molecular formula be:
C 40h 40co 2n 10na 2o 12molecular weight is: 1016.66.
[Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2synthetic method concrete steps be:
(1) 0.228 gram of pure 3-methoxyl group-Benzaldehyde,2-hydroxy of analysis is dissolved in the mixed solution of 10 milliliters of pure absolute methanols of analysis and 10 milliliters of pure acetonitriles of analysis, add successively again 0.548g to analyze pure six perchloric acid hydrate cobalts and 0.196g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after three days, obtain red bulk crystals, filter, and clean with analyzing pure methanol wash, after drying, obtain product [Co in air 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2.
(2) after the product 0.0325 gram of step (1) being obtained pulverizes, on magnetic tester device, carry out magnetic test, obtain magnetic test curve as Fig. 2,3, [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2χ munder T room temperature, be 6.84cm 3kmol -1, along with temperature reduces, χ mt raises gradually, reaches maximum 11.35cm to 11K 3kmol -1, be sharply down to subsequently 8.57cm 3kmol -1.To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.58, and the magnetic exchange constant in molecule between cobalt ions is 9.48cm -1, the magnetic exchange constant of intermolecular cobalt ions is :-0.622cm -1.And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 12.55K that its matching is obtained to Wei Si constant, and Curie constant is 6.63cm 3kmol – 1.Large and positive Wei Si constant, magnetic exchange constant and χ in molecule mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism.

Claims (1)

1. a magnetic material [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2, it is characterized in that Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2molecular formula be: C 40h 40co 2n 10na 2o 12, molecular weight is: 1016.66, Hhmb is 3-methoxyl group-Benzaldehyde,2-hydroxy, and crystal structure data are in Table one, and bond distance's bond angle data are in Table two; [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2magnetic property: between cobalt ions, have ferromagnetic exchange in (1) molecule, it shows as ferromagnetism; (2) [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2χ at room temperature mt is 6.84cm 3kmol- 1, along with temperature reduces, χ mt raises gradually, reaches maximum 11.35cm to 11K 3kmol -1, be sharply down to subsequently 8.57cm 3kmol -1; To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.58, and the magnetic exchange constant in molecule between cobalt ions is 9.48cm -1, the magnetic exchange constant of intermolecular cobalt ions is :-0.622cm -1; And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 12.55K that its matching is obtained to Wei Si constant, and Curie constant is 6.63cm 3kmol – 1; Large and positive Wei Si constant, magnetic exchange constant and χ in molecule mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism;
Described [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2synthetic method concrete steps be:
0.114-0.228 gram is analyzed to pure 3-methoxyl group-Benzaldehyde,2-hydroxy is dissolved in 5-10 milliliter absolute methanol and 5-10 milliliter is analyzed in the mixed solution of pure acetonitrile, add successively again 0.274-0.548g to analyze pure six perchloric acid hydrate cobalts and 0.098-0.196g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after three days, obtain red bulk crystals, filter, and clean with analyzing pure methanol wash, after drying, obtain product [Co in air 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2,
Table one [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2crystallographic parameter
Table two [Co 2na 2(hmb) 4(N 3) 2(CH 3cN) 2] (CH 3cN) 2bond distance and bond angle (°)
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CN105225779A (en) * 2015-10-19 2016-01-06 广西大学 A kind of cobalt-based single-chain magnets and synthetic method thereof
CN106220687A (en) * 2016-09-13 2016-12-14 桂林理工大学 { [Co3k (emimp)4(DCA)2] ClO4}6(H2and synthetic method O)

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CN106220687A (en) * 2016-09-13 2016-12-14 桂林理工大学 { [Co3k (emimp)4(DCA)2] ClO4}6(H2and synthetic method O)

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