CN104485193B - A kind of magnetic material constructed for part with acylhydrazone class schiff bases and preparation method thereof - Google Patents
A kind of magnetic material constructed for part with acylhydrazone class schiff bases and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of magnetic material constructed with acylhydrazone class schiff bases and preparation method thereof for part.The chemical formula of described magnetic material is: [Dy2L2(CH3COO)2(DMF)2], wherein, L is 2 aldehyde radical 8 hydroxyquinoline contracting salicyloyl hydrazones, and DMF is N, N dimethylformamide.The preparation method of described magnetic material is: take Dy (CH3COO)3·6H2O and 2 aldehyde radical 8 hydroxyquinoline contracting salicyloyl hydrazones, with by absolute methanol and N, the mixed solvent of N dimethylformamide composition dissolves, the pH=7.5~9.5 of regulation gained solution, gained mixed liquor is placed in container, is evacuated to vacuum, sealing by fusing after liquid nitrogen freezing, then react under the conditions of 60~100 DEG C, to obtain final product.Magnetic material general performance of the present invention is paramagnetism;Preparation method of the present invention is simple, with low cost, productivity is higher and reproducible.
Description
Technical field
The present invention relates to a kind of magnetic material constructed for part with acylhydrazone class schiff bases and preparation method thereof, belong to magnetic
Field of material technology.
Background technology
Schiff bases is a very important part of class, it various informative, analyzes, R from structure1R2C=NR3(R1,R2,
R3Alkyl, hydrogen, cyclohexyl, aromatic radical or heterocycle can be respectively) in R1, R2, R3All can be replaced by various groups.Schiff bases core
The heart is C=N group, the lone pair electrons that its nitrogen-atoms hybrid orbital has, and gives its important chemistry with biologically
Meaning.Acylhydrazone, as the special schiff bases of a class, has the strongest coordination ability, it can and transition metal, rare earth ion etc.
Forming coordination compound, its coordination compound, at analysis, catalysis, optical material, magnetic material, particularly has reality at biochemical field
Application prospect.Therefore, the research of the coordination compound that acylhydrazone and derivant thereof are constructed become current Coordinative Chemistry research focus it
One.
Magnetic material due to by information technology middle-high density magnetic storage apparatus and quantum computer fast development affected,
Cause the broad interest of researcher.Along with the researcher further investigation to single molecular magnets relaxation mechanism, with
Time be synthesized along with the fast development of characterization technique, the rare earth single molecular magnets more and more with practical value, but
The rareearth magnetic material with acylhydrazone class schiff bases as part being in the news at present is fewer, and there is not yet chemical formula is [Dy2L2
(CH3COO)2(DMF)2] the relevant report of rareearth magnetic material.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of magnetic material constructed for part with acylhydrazone class schiff bases and
Its preparation method.
The magnetic material constructed for part with acylhydrazone class schiff bases of the present invention, its chemical formula is:
[Dy2L2(CH3COO)2(DMF)2]
Wherein, L is 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, and DMF is DMF.
Molecular formula C of above-mentioned rareearth magnetic material44H42N8Dy2O12, molecular weight is: 1199.86.
The crystal structural data of rareearth magnetic material of the present invention sees below table 1, and part bond distance's bond angle data see below
Table 2.
Table 1 [Dy2L2(CH3COO)2(DMF)2] crystallographic parameter
a R1=Σ | | Fo|–|Fc||/Σ|Fo|.b wR2=[Σ w (| Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
Table 2 [Dy2L2(CH3COO)2(DMF)2] bond distance () and bond angle (°)
Applicant studies discovery, and of the present invention have as follows with acylhydrazone class schiff bases for the magnetic material that part is constructed
Magnetic property: there is ferromagnetic exchange between two dysprosium ions of intramolecular, its general performance is paramagnetism.
The preparation method of the above-mentioned magnetic material constructed for part with acylhydrazone class schiff bases is: take Dy (CH3COO)3·6H2O
With 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, the mixed solvent formed with absolute methanol and DMF dissolves,
The pH=7.5~9.5 of regulation gained solution, gained mixed liquor is placed in container, is evacuated to vacuum after liquid nitrogen freezing, sealing by fusing, so
After under the conditions of 60~100 DEG C react, i.e. obtain the magnetic material [Dy constructed with acylhydrazone class schiff bases for part2L2
(CH3COO)2(DMF)2]。
In above-mentioned preparation method, described Dy (CH3COO)3·6H2Rubbing of O and 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone
That ratio is stoichiometric proportion, usually 2:1.2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone as raw material can be by existing literary composition
The method offering report is prepared (such as list of references Yong-chun Liu, Crystal structures, antioxidation
and DNA binding properties of Eu(III)complexes with Schiff-base ligands
derived from 8-hydroxyquinoline-2-carboxyaldehyde and three aroylhydrazines,
Journal of Inorganic Biochemistry 103 (2009) 1014~1022 is prepared), it is possible to designed, designed closes
Route is become to be prepared.
In above-mentioned preparation method, in described mixed solvent, absolute methanol and DMF volume ratio
Can be any proportioning, preferably 1~3:1~3, preferably it is chosen as 1:1,1:2,2:1,1:3,3:1 or 2:1, most preferably
1:1.The consumption of described mixed solvent can determine as required, and the raw material generally reacted can dissolve participation is advisable.Specifically, with
Calculating on the basis of the 2-aldehyde radical of 1mmol-8-hydroxyquinoline contracting salicyloyl hydrazone, used by whole raw materials, total consumption of polar solvent is general
It is 1.8~5mL.In the concrete step dissolved, can be by Dy (CH3COO)3·6H2O and 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl
Hydrazone dissolves with polar solvent respectively, remixes and reacts together, it is possible to by Dy (CH3COO)3·6H2O and 2-aldehyde radical-8-hydroxyl quinoline
After the mixing of quinoline contracting salicyloyl hydrazone, additive polarity solvent dissolves again.
In above-mentioned preparation method, existing conventional alkaline matter can be used to regulate the pH value of solution, preferably use
The pH value of triethylamine regulation solution.In technical scheme of the present invention, preferably regulate the pH=7.5~9.0 of solution.
In above-mentioned preparation method, described container is usually the heavy-walled glass pipe that one end is closed, and gained mixed liquor is placed on 75
~the time reacted at 100 DEG C is usually 20~48h, it is also possible to be more than 48h;Preferably will control in the response time 24~
48h;Reaction is preferably carried out under the conditions of 75~100 DEG C.
Compared with prior art, the invention provides a kind of new magnetic material constructed with acylhydrazone class schiff bases for part
[Dy2L2(CH3COO)2(DMF)2] and preparation method thereof, the magnetic property of this magnetic material is: deposit between two dysprosium ions of intramolecular
In ferromagnetic exchange, its general performance is paramagnetism;Preparation method of the present invention is simple, low raw-material cost, reaction system
Middle chemical constituent is easily controllable, productivity is higher and repeated very well.
Accompanying drawing explanation
Fig. 1 is the [Dy that the embodiment of the present invention 1 prepares2L2(CH3COO)2(DMF)2] structure chart;
Fig. 2 is the [Dy that the embodiment of the present invention 1 prepares2L2(CH3COO)2(DMF)2] χm-T,χmT-T curve chart;
Fig. 3 is the [Dy that the embodiment of the present invention 1 prepares2L2(CH3COO)2(DMF)2] real part that exchanges and imaginary part be to temperature
Curve chart;
Fig. 4 is the [Dy that the embodiment of the present invention 1 prepares2L2(CH3COO)2(DMF)2] X-ray powder diffraction pattern figure;
Fig. 5 is the [Dy that the embodiment of the present invention 1 prepares2L2(CH3COO)2(DMF)2] infrared curve chart;
Fig. 6 is the high resolution mass spectrum figure of the 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone related in the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, preferably to illustrate the present invention's
Content, but the present invention is not limited in following example.
The 2-aldehyde radical related in following embodiment-8-hydroxyquinoline contracting salicyloyl hydrazone uses following methods to prepare:
Take 2-aldehyde radical-8-hydroxyquinoline and the salicylyl hydrazine mol ratio according to 1:1,80 DEG C of oil baths backflows in ethanol solution
24h, after reaction terminates, rotation evaporates partial solvent, stands and separates out a large amount of yellow needle-like crystals, by washing with alcohol for several times, vacuum drying
Obtain 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone.Elementary analysis (C17H13N3O3) experiment value: C, 66.42;H,4.27;N,
13.66;Theoretical value: C, 66.44;H,4.26;N,13.67.Carried out confirming that (330.0853 are to it with high resolution mass spectrum simultaneously
L+Na+, 308.1033 is L+H+), its spectrogram is as shown in Figure 6.Hence, it can be determined that products therefrom is 2-aldehyde radical-8-hydroxyl quinoline
Quinoline contracting salicyloyl hydrazone.
Embodiment 1
Magnetic material [the Dy constructed for part with acylhydrazone class schiff bases that the present invention relates to2L2(CH3COO)2(DMF)2], its
Middle L is 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, and DMF is DMF.
Above-mentioned magnetic material [the Dy constructed for part with acylhydrazone class schiff bases2L2(CH3COO)2(DMF)2] preparation method
For:
Analytically pure Dy (CH is weighed according to the proportioning that mol ratio is 2:13COO)3·6H2O and 2-aldehyde radical-8-hydroxyquinoline
Contracting salicyloyl hydrazone (wherein Dy (CH3COO)3·6H2O is 0.1mmol, i.e. 0.0898g), be placed in beaker, be subsequently adding by
1.6mL absolute methanol and the mixed solvent of 0.8mL DMF composition, dissolve, shake up, then by analytical pure three second
The pH=8 of amine regulation gained solution;Gained mixed liquor proceeds to be about in the Pyrex heavy-walled glass pipe of 25cm, takes out with liquid nitrogen freezing
Vacuum sealing tube, insulation reaction 48h under the conditions of then the Pyrex heavy-walled glass pipe of sealing by fusing being placed in 80 DEG C;Naturally cool to room temperature,
Red hexagonal crystal is had to generate in pipe.Yield: 35mg, productivity: 68.33%.
Embodiment 1 products therefrom is characterized:
1) crystal structure analysis:
It is measured the red hexagonal crystal that surface texture is intact by Agilent company SuperNova single crystal diffractometer
To determine its mono-crystalline structures, resulting structures data are shown in that aforementioned table 2 is shown in by aforementioned table 1, bond distance's bond angle data, and gained redness hexagon is brilliant
The chemical constitution of body is as it is shown in figure 1, determine that the red crystals of gained is of the present invention with acylhydrazone class schiff bases for part structure
Magnetic material [the Dy built2L2(CH3COO)2(DMF)2], wherein L is 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, and DMF is N, N-
Dimethylformamide, the molecular formula of this magnetic material is C44H42N8Dy2O12, molecular weight is: 1199.86.
2) magnetic property measures:
Take the magnetic material [Dy constructed with acylhydrazone class schiff bases that 0.0251g the present embodiment prepares for part2L2
(CH3COO)2(DMF)2] pulverize after on Magnetic Test instrument, carry out Magnetic Test, obtain the χ of magnetic materialM-T,χMT-T curve
Figure is such as Fig. 2, and real part that magnetic material exchanges and imaginary part are to the curve chart of temperature as shown in Figure 3.
From Fig. 2 and Fig. 3, the magnetic material [Dy constructed for part with acylhydrazone class schiff bases of the present invention2L2
(CH3COO)2(DMF)2] at room temperature χMT is 31.2cm3Kmol-1, along with temperature reduces, χMT gradually rises, and reaches maximum to 2K
Value 62.4cm3Kmol-1.And χM –1-T curve defers to Curie-Weiss law, and it is 44.9K that its matching obtains Weiss constant, Curie
Constant is 58.2cm3Kmol–1.Positive Weiss constant and χMT-T curvilinear trend all shows to exist between intramolecular dysprosium ion ferromagnetic friendship
Changing, its general performance is paramagnetism.
3) X-ray powder diffraction:
Use that the present embodiment prepares by Rigaku electric machine industry Co., Ltd. D/max-2500V/PC diffractometer with acyl
Hydrazone class schiff bases is the magnetic material [Dy that part is constructed2L2(CH3COO)2(DMF)2] test at ambient temperature, gained
XRD curve chart is as shown in Figure 4.
4) Infrared Characterization:
With U.S. Nicolet 360FT-IR type Fourier transformation infrared spectrometer (KBr tabletting), the present embodiment is prepared
The magnetic material [Dy constructed for part with acylhydrazone class schiff bases2L2(CH3COO)2(DMF)2] carry out infrared analysis, take the photograph spectral limit
400~4000cm-1, gained infrared spectrum spectrogram is as shown in Figure 5.
Embodiment 2
Repeat embodiment 1, be different from:
1) by Dy (CH3COO)3·6H2The amount of O changes to 0.05mmol, i.e. 0.0449g;
2) being changed to by mixed solvent by 1.4mL absolute methanol and 0.7mLN, dinethylformamide forms;
3) pH value of solution is adjusted to 8.5;
4) reaction temperature being controlled at 90 DEG C, the response time controls at 24h.
The product of gained is carried out mono-crystalline structures sign and X-ray powder diffraction characterizes, determine that target product is with acylhydrazone
Class schiff bases is the magnetic material [Dy that part is constructed2L2(CH3COO)2(DMF)2], the Magnetic Characterization of product is understood gained
Magnetic material at room temperature χMT is 31.2cm3Kmol-1, along with temperature reduces, χmT gradually rises, and reaches maximum to 2K
62.4cm3Kmol-1.And χM –1-T curve defers to Curie-Weiss law, and it is 44.9K, Ju Lichang that its matching obtains Weiss constant
Number is 58.2cm3Kmol–1.Positive Weiss constant and χMT-T curvilinear trend all shows to there is ferromagnetic exchange between intramolecular dysprosium ion,
Its general performance is paramagnetism.
Embodiment 3
Repeat embodiment 1, be different from: the pH value of solution is adjusted to 9.0.
The product of gained is carried out mono-crystalline structures sign and X-ray powder diffraction characterizes, determine that target product is with acylhydrazone
Class schiff bases is the magnetic material [Dy that part is constructed2L2(CH3COO)2(DMF)2], the Magnetic Characterization of product is understood gained
Magnetic material at room temperature χMT is 31.2cm3Kmol-1, along with temperature reduces, χmT gradually rises, and reaches maximum to 2K
62.4cm3Kmol-1.And χM –1-T curve defers to Curie-Weiss law, and it is 44.9K, Ju Lichang that its matching obtains Weiss constant
Number is 58.2cm3Kmol–1.Positive Weiss constant and χMT-T curvilinear trend all shows to there is ferromagnetic exchange between intramolecular dysprosium ion,
Its general performance is paramagnetism.
Embodiment 4
Repeat embodiment 1, be different from:
1) being changed to by mixed solvent by 1.8mL methanol and 0.6mLN, dinethylformamide forms;
2) pH value of solution is adjusted to 7.5.
The product of gained is carried out mono-crystalline structures sign and X-ray powder diffraction characterizes, determine that target product is with acylhydrazone
Class schiff bases is the magnetic material [Dy that part is constructed2L2(CH3COO)2(DMF)2], the Magnetic Characterization of product is understood gained
Magnetic material at room temperature χMT is 31.2cm3Kmol-1, along with temperature reduces, χmT gradually rises, and reaches maximum to 2K
62.4cm3Kmol–1.And χM –1-T curve defers to Curie-Weiss law, and it is 44.9K, Ju Lichang that its matching obtains Weiss constant
Number is 58.2cm3Kmol–1.Positive Weiss constant and χMT-T curvilinear trend all shows to there is ferromagnetic exchange between intramolecular dysprosium ion,
Its general performance is paramagnetism.
Claims (5)
1. the magnetic material constructed with acylhydrazone class schiff bases for part, its chemical formula is:
[Dy2L2(CH3COO)2(DMF)2]
Wherein, L is 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, and DMF is DMF;
The space group of this magnetic material constructed for part with acylhydrazone class schiff bases is as P21/ c, cell parameter is:α=90 °, β=101.4790
(10) °, γ=90 °.
2. the preparation method of the magnetic material constructed for part with acylhydrazone class schiff bases described in claim 1, it is characterised in that:
Take Dy (CH3COO)3·6H2O and 2-aldehyde radical-8-hydroxyquinoline contracting salicyloyl hydrazone, with by absolute methanol and N, N-dimethyl formyl
The mixed solvent of amine composition dissolves, and the pH=7.5~9.5 of regulation gained solution, gained mixed liquor is placed in container, cold through liquid nitrogen
It is evacuated to vacuum, sealing by fusing after freezing, then reacts under the conditions of 60~100 DEG C, i.e. obtain the magnetic constructed with acylhydrazone class Schiff base ligand
Property material [Dy2L2(CH3COO)2(DMF)2]。
Preparation method the most according to claim 2, it is characterised in that: in described mixed solvent, absolute methanol and N, N-
The volume ratio of dimethylformamide is 1~3:1~3.
Preparation method the most according to claim 2, it is characterised in that: with the pH value of triethylamine regulation solution.
Preparation method the most according to claim 2, it is characterised in that: the time of reaction is 20~48h or more than 48h.
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CN105153242A (en) * | 2015-07-23 | 2015-12-16 | 广西师范大学 | Multifunctional metal organic complex and preparation method therefor |
CN107089999B (en) * | 2017-04-21 | 2019-03-12 | 广西师范大学 | A kind of monokaryon dysprosium complex and its preparation method and application |
CN106966971B (en) * | 2017-04-21 | 2019-06-28 | 广西师范大学 | It is a kind of using 2- methyl -5,7-dichloro-8-hydroxyquinoline as monokaryon dysprosium complex of ligand and its preparation method and application |
CN106966972B (en) * | 2017-05-19 | 2019-06-28 | 广西师范大学 | A kind of dysprosium complex constructed using 8-hydroxyquinoline acyl hydrazone derivative as ligand and its synthetic method and application |
CN107098921B (en) * | 2017-05-19 | 2019-03-19 | 广西师范大学 | The dysprosium complex and its synthetic method constructed using 8-hydroxyquinoline acyl hydrazone derivative as ligand and application |
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