CN104036909A - Magnetic material [Cu3(N3)6(DMF)2]n and synthetic method - Google Patents

Magnetic material [Cu3(N3)6(DMF)2]n and synthetic method Download PDF

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CN104036909A
CN104036909A CN201410292754.9A CN201410292754A CN104036909A CN 104036909 A CN104036909 A CN 104036909A CN 201410292754 A CN201410292754 A CN 201410292754A CN 104036909 A CN104036909 A CN 104036909A
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dmf
analytically pure
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magnetic
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CN104036909B (en
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肖瑜
赵儒霞
张淑华
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Yongchun County Product Quality Inspection Institute Fujian fragrance product quality inspection center, national incense burning product quality supervision and Inspection Center (Fujian)
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Guilin University of Technology
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Abstract

The invention discloses a magnetic material [Cu3(N3)6(DMF)2]n and a synthetic method. The method includes: (1) dissolving 0.125-0.25g of analytically pure 3-ethoxy-2-hydroxy benzaldehyde into 10-20ml of analytically pure N,N'-dimethylformamide (DMF) solution; (2) sequentially adding 0.128-0.256g of analytically pure copper chloride dihydrate and 0.098-0.196g of analytically pure sodium azide, and stirring for 10 minutes; (3) adding analytically pure triethylamine into a solution obtained in the step (2) to regulate pH (potential of hydrogen) to 6.5, stirring for 20 minutes prior to standing the obtained solution at room temperature to obtain black bulk crystals after three days, filtering, washing the crystals clean with analytical N,N'-dimethylformamide (DMF), drying the washed crystals in air to obtain the product [Cu3(N3)6(DMF)2]n. Magnetic properties of the [Cu3(N3)6(DMF)2]n are shown in that ferromagnetic exchange exist among intramolecular copper ions, and the [Cu3(N3)6(DMF)2]n is integrally ferromagnetic. The magnetic material [Cu3(N3)6(DMF)2]n and the synthetic method have the advantages of simple technology, low cost, easiness in control of chemical compositions, good repeatability, high productivity and the like.

Description

Magnetic material [Cu 3(N 3) 6(DMF) 2] nand synthetic method
Technical field
The present invention relates to a kind of magnetic material [Cu 3(N 3) 6(DMF) 2] nand 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 complex molecule magnetic material more with practical value will be synthesized, and these there is the application of coordination compound magnetic material to 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 [Cu 3(N 3) 6(DMF) 2] n.
[the Cu the present invention relates to 3(N 3) 6(DMF) 2] nmolecular formula be: C 6h 14cu 3n 20o 2, molecular weight is: 589.02, DMF is N, N '-dimethyl formamide; Crystal structure data are in Table one, and bond distance's bond angle data are in Table two.
Table one [Cu 3(N 3) 6(DMF) 2] ncrystallographic parameter
Table two [Cu 3(N 3) 6(DMF) 2] nbond distance and bond angle (°)
[Cu 3(N 3) 6(DMF) 2] nsynthetic method concrete steps be:
(1) the analytically pure 3-ethyoxyl-Benzaldehyde,2-hydroxy of 0.125-0.25g is dissolved in to 10-20ml and analyzes pure N, in N '-dimethyl formamide (DMF) solution.
(2) in step (1) gained solution, add successively the analytically pure Copper dichloride dihydrate of 0.128-0.256g and 0.098-0.196g to analyze pure sodium azide, stir 10 minutes.
(3) in step (2) gained solution, adding the pure triethylamine of analysis to regulate pH is 6.5, stir after 20 minutes by the solution left standstill obtaining at room temperature, after three days, obtain black bulk crystals, filter, and with analyzing pure N, N '-dimethyl formamide (DMF) washes clean, obtains product [Cu after drying in air 3(N 3) 6(DMF) 2] n.
[Cu 3(N 3) 6(DMF) 2] nmagnetic property: between copper ion, have ferromagnetic exchange in molecule, its general performance is 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 [Cu 3(N 3) 6(DMF) 2] nstructure chart.
Fig. 2 is the embodiment of the present invention [Cu 3(N 3) 6(DMF) 2] n2D stratiform figure, for clear, removed DMF molecule.
Fig. 3 is the embodiment of the present invention [Cu 3(N 3) 6(DMF) 2] nχ m-T, χ mt-T curve chart.
Fig. 4 is the embodiment of the present invention [Cu 3(N 3) 6(DMF) 2] nχ m – 1-T curve chart.
Embodiment
Embodiment 1:
[the Cu the present invention relates to 3(N 3) 6(DMF) 2] nmolecular formula be: C 6h 14cu 3n 20o 2
Molecular weight is: 589.02.
[Cu 3(N 3) 6(DMF) 2] nsynthetic method concrete steps be:
(1) by 0.125 gram, analyze pure 3-ethyoxyl-Benzaldehyde,2-hydroxy and be dissolved in 10 milliliters of analytically pure N, in N '-dimethyl formamide (DMF) solution.
(2) in step (1) gained solution, add successively the analytically pure Copper dichloride dihydrate of 0.128g and the analytically pure sodium azide of 0.098g, stir ten minutes.
(3) in step (2) gained solution, add analytically pure triethylamine to be adjusted to pH=6.5, stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after three days, obtain black bulk crystals, filter, and with analyzing pure N, N '-dimethyl formamide (DMF) washes clean, obtains product [Cu after drying in air 3(N 3) 6(DMF) 2] n.Output: 86 milligrams, productive rate: 58.4%, and measure polymer [Cu by single crystal diffractometer 3(N 3) 6(DMF) 2] nmolecular structure, crystallographic parameter is in Table one, bond distance's bond angle is in Table two.
(4) product [Cu 0.0223 gram of step (3) being obtained 3(N 3) 6(DMF) 2] nafter pulverizing, on magnetic tester device, carry out magnetic test, obtain magnetic test curve as accompanying drawing 2,3, [Cu 3(N 3) 6(DMF) 2] nχ at room temperature mt is 1.403cm 3kmol – 1, along with temperature reduces, χ mt raises gradually, reaches maximum 2.490cm to 14.5K 3kmol – 1, be sharply down to subsequently 0.442cm 3kmol – 1.To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.27, and the magnetic exchange constant in molecule between copper ion is 14.49cm – 1, the magnetic exchange constant of intermolecular copper ion is :-10.84cm – 1.And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 24.59K that its matching is obtained to Wei Si constant, and Curie constant is 1.317cm 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 copper ion, and its general performance is ferromagnetism.
Embodiment 2:
[the Cu the present invention relates to 3(N 3) 6(DMF) 2] nmolecular formula be: C 6h 14cu 3n 20o 2molecular weight is: 589.02.
[Cu 3(N 3) 6(DMF) 2] nsynthetic method concrete steps be:
(1) 0.25 gram of analytically pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in to 20 milliliters and analyzes pure N, in N '-dimethyl formamide (DMF) solution.
(2) in step (1) gained solution, add successively the analytically pure Copper dichloride dihydrate of 0.256g and the analytically pure sodium azide of 0.196g, stir 10 minutes.
(3) in step (2) gained solution, add analytically pure triethylamine to be adjusted to pH=6.5, stir after 20 minutes, be statically placed under room temperature, after three days, obtain black bulk crystals, filter, and with analyzing pure N, N '-dimethyl formamide (DMF) solution washing is clean, after drying, obtains product [Cu in air 3(N 3) 6(DMF) 2] n.
(4) product [Cu 0.0223 gram of step (3) being obtained 3(N 3) 6(DMF) 2] nafter pulverizing, on magnetic tester device, carry out magnetic test, obtain magnetic test curve as accompanying drawing 2,3, [Cu 3(N 3) 6(DMF) 2] nχ at room temperature mt is 1.403cm 3kmol – 1, along with temperature reduces, χ mt raises gradually, reaches maximum 2.490cm to 14.5K 3kmol – 1, be sharply down to subsequently 0.442cm 3kmol – 1.To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.27, and the magnetic exchange constant in molecule between copper ion is 14.49cm -1, the magnetic exchange constant of intermolecular copper ion is :-10.84cm – 1.And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 24.59K that its matching is obtained to Wei Si constant, and Curie constant is 1.317cm 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 copper ion, and its general performance is ferromagnetism.

Claims (1)

1. [a Cu 3(N 3) 6(DMF) 2] n, it is characterized in that [Cu 3(N 3) 6(DMF) 2] nmolecular formula is: C 6h 14cu 3n 20o 2, molecular weight is: 589.02, DMF is N, N '-dimethyl formamide; Molecular structure crystallographic parameter is in Table one, and bond distance's bond angle is in Table two;
Described [Cu 3(N 3) 6(DMF) 2] nsynthetic method concrete steps be:
(1) the analytically pure 3-ethyoxyl-Benzaldehyde,2-hydroxy of 0.125-0.25g is dissolved in to 10-20ml and analyzes pure N, N '-dimethyl formamide is in DMF;
(2) in step (1) gained solution, add successively the analytically pure Copper dichloride dihydrate of 0.128-0.256g and 0.098-0.196g to analyze pure sodium azide, stir 10 minutes.
(3) in step (2) gained solution, adding the pure triethylamine of analysis to regulate pH is 6.5, stir after 20 minutes by the solution left standstill obtaining at room temperature, after three days, obtain black bulk crystals, filter, and with analyzing pure N, N '-dimethyl formamide washes clean, obtains product [Cu after drying in air 3(N 3) 6(DMF) 2] n;
Table one [Cu 3(N 3) 6(DMF) 2] ncrystallographic parameter
Table two [Cu 3(N 3) 6(DMF) 2] nbond distance and bond angle (°)
Described [Cu 3(N 3) 6(DMF) 2] nmagnetic property:
(1) in molecule, between copper ion, have ferromagnetic exchange, its general performance is ferromagnetism;
(2) [Cu 3(N 3) 6(DMF) 2] nχ at room temperature mt is 1.403cm 3kmol – 1, along with temperature reduces, χ mt raises gradually, reaches maximum 2.490cm to 14.5K 3kmol – 1, be sharply down to subsequently 0.442cm 3kmol – 1; To χ m-T, χ mt – T curve is analyzed and obtained the Lang De factor after matching is 2.27, and the magnetic exchange constant in molecule between copper ion is 14.49cm – 1, the magnetic exchange constant of intermolecular copper ion is :-10.84cm -1; And χ m – 1-T curve is deferred to Curie-Weiss law, and it is 24.59K that its matching is obtained to Wei Si constant, and Curie constant is 1.317cm 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 copper ion, and its general performance is ferromagnetism.
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CN114181232A (en) * 2021-12-06 2022-03-15 郑州轻工业大学 Chiral one-dimensional copper chain ferromagnetic molecular base material and preparation method thereof

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CN114181232A (en) * 2021-12-06 2022-03-15 郑州轻工业大学 Chiral one-dimensional copper chain ferromagnetic molecular base material and preparation method thereof

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