CN109705150A - A kind of halogenated P-hydroxybenzoic acid dysprosium complex and preparation method thereof - Google Patents
A kind of halogenated P-hydroxybenzoic acid dysprosium complex and preparation method thereof Download PDFInfo
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- CN109705150A CN109705150A CN201910052045.6A CN201910052045A CN109705150A CN 109705150 A CN109705150 A CN 109705150A CN 201910052045 A CN201910052045 A CN 201910052045A CN 109705150 A CN109705150 A CN 109705150A
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Abstract
The present invention relates to magnetic function material and synthetic method technical fields, more particularly to a kind of halogenated P-hydroxybenzoic acid dysprosium complex and preparation method thereof, the specific chemical formula of halogenated P-hydroxybenzoic acid dysprosium complex is Dy-L-HL-phen, L is negative the 3 of divalent, the chloro- 4-HBA anion of 5- bis-, HL is negative the 3 of monovalence, the chloro- 4-HBA anion of 5- bis-, phen is 1, 10- Phen molecule, preparation method includes the following steps S1, weigh soluble inorganic salt of rare earth, the chloro- 4-HBA of 5- bis- and 1, 10- Phen is raw material, and it is add to deionized water, the mixed solution of pH value to 7 is adjusted with sodium hydroxide solution；S2, the mixed solution for obtaining S1, which are transferred in autoclave, is warming up to 140 DEG C of 96 h of heat preservation, it is slowly dropped to room temperature and obtains colourless bulk crystals, halogenated P-hydroxybenzoic acid dysprosium complex is obtained after natural drying, the synthesis material of halogenated P-hydroxybenzoic acid dysprosium complex prepared by the present invention is from a wealth of sources, synthetic method is simple, at low cost, yield is high.
Description
Technical field
The present invention relates to magnetic function material and synthetic method technical field more particularly to a kind of halogenated P-hydroxybenzoic acid dysprosiums
Complex and preparation method thereof.
Background technique
Organolanthanide complexes have the structure and the performances such as excellent magnetics, luminous, catalysis of multiplicity, have attracted and have matched
The research interest of position chemist.In recent years, dysprosium metal organic complex is widely studied, this is because such complex is aobvious
Single molecular magnets behavior is shown, there is potential application prospect in the fields such as high density data storage and quantum treatment.To current
Until, the single molecular magnets behavior of the dysprosium metal organic complex of zero-dimension structural is ground extensively, however, about higher-dimension structure
The report of the single molecular magnets behavior of dysprosium metal organic complex is not much, and especially shows apparent null field single molecular magnets row
For higher-dimension dysprosium metal organic complex it is also seldom.Therefore, it is necessary to which synthesizing simultaneously structural characterization has single molecular magnets behavior
Higher-dimension dysprosium metal organic complex, studies its magnetic performance, to obtain magnetic function material.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, provide that synthetic method is simple, synthesis material
At low cost, a kind of halogenated P-hydroxybenzoic acid dysprosium complex for showing good magnetic property and preparation method thereof.
To achieve the goals above, present invention employs following technical solutions:
A kind of halogenated P-hydroxybenzoic acid dysprosium complex, specific chemical formula are Dy-L-HL-phen, and the L is negative the 3,5- of divalent
Two chloro- 4-HBA anion, the HL are negative the chloro- 4-HBA anion of 3,5- bis- of monovalence, the phen
For 1,10- Phen molecule.
Preferably, the halogenated P-hydroxybenzoic acid dysprosium complex is with negative divalent 3, the chloro- 4-HBA of 5- bis-
The two-dimensional network structure that anion bridging dysprosium dimer is formed.
Preferably, the halogenated P-hydroxybenzoic acid dysprosium complex is characterization object, using X-ray single crystal diffractometer and
Powder diffractometer tests the structure and Xiang Chundu of halogenated P-hydroxybenzoic acid dysprosium complex, is tested using thermal analyzer halogenated to hydroxyl
The thermal stability of yl benzoic acid dysprosium complex tests the magnetic of halogenated P-hydroxybenzoic acid dysprosium complex using Superconducting magnetic analyzer
Learn property.
Preferably, application of the halogenated P-hydroxybenzoic acid dysprosium complex as magnetic function material.
The invention also provides a kind of preparation methods of halogenated P-hydroxybenzoic acid dysprosium complex, comprising the following steps: S1,
Weigh soluble inorganic salt of rare earth, the chloro- 4-HBA of 5- bis- and 1,10- Phen is raw material, while soluble rare earth
Inorganic salts, the chloro- 4-HBA of 5- bis- and 1,10- Phen is add to deionized water according to molar ratio for 2:3:2, is mixed
The mixed solution of pH value to 7 is adjusted after closing uniformly with sodium hydroxide solution；
S2, the mixed solution for obtaining S1, which are transferred in autoclave, is warming up to 140 DEG C of 96 h of heat preservation, is slowly dropped to room temperature
Colourless bulk crystals are obtained, filters and washs, obtain halogenated P-hydroxybenzoic acid dysprosium complex after natural drying.
Preferably, the concentration of the sodium hydroxide solution is 0.1mol/L, and the solubility inorganic salt of rare earth is six hydrations
Dysprosium trichloride.
The beneficial effects of the present invention are:
1, of the invention, the poorly water-soluble of the halogenated P-hydroxybenzoic acid dysprosium complex of synthesis, in common organic solvent also very
Indissoluble solution, it is therefore prevented that the secondary pollution to environment, while being also convenient for the collection to halogenated P-hydroxybenzoic acid dysprosium complex.
2, of the invention, 1,10- Phen and dysprosium ion are coordinated, and are prevented the coordination of aqueous solvent, be can be avoided solvent
Molecule improves single point of halogenated P-hydroxybenzoic acid dysprosium complex to the effect of magnetic influence of halogenated P-hydroxybenzoic acid dysprosium complex
Sub- magnet behavior.
3, of the invention, the halogenated P-hydroxybenzoic acid dysprosium complex being prepared presents apparent null field single molecular magnets
Behavior can be used as magnetic function material application.
In conclusion the synthesis material of halogenated P-hydroxybenzoic acid dysprosium complex prepared by the present invention is from a wealth of sources, synthesis
Method is simple, at low cost, and yield is high.
Detailed description of the invention
Fig. 1 is a kind of Dy-L-HL- of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
The dimeric structure schematic diagram of phen；
Fig. 2 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Two-dimensional structure schematic diagram；
Fig. 3 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Simulate the experimental X-ray powder diffraction schematic diagram of X-ray powder diffraction figure and Dy (L) (HL) (phen)；
Fig. 4 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Thermogravimetric curve schematic diagram；
Fig. 5 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Dependence curve synoptic diagram of the null field frequency conversion imaginary part ac magnetic susceptibility to temperature；
Fig. 6 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Dependence curve synoptic diagram of the null field alternating temperature imaginary part ac magnetic susceptibility to frequency；
Fig. 7 is a kind of Dy-L-HL-phen of halogenated P-hydroxybenzoic acid dysprosium complex proposed by the present invention and preparation method thereof
Ke Er-Ke Er curve synoptic diagram of the null field alternating temperature imaginary part ac magnetic susceptibility to real part ac magnetic susceptibility.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
A kind of halogenated P-hydroxybenzoic acid dysprosium complex, specific chemical formula are Dy-L-HL-phen, and L is negative the 3,5- of divalent
Two chloro- 4-HBA anion, HL are negative the chloro- 4-HBA anion of 3,5- bis- of monovalence, and phen 1,10- are adjacent
Phenanthroline molecule, halogenated P-hydroxybenzoic acid dysprosium complex are with negative divalent 3, the chloro- 4-HBA anion bridge of 5- bis-
Join the two-dimensional network structure that dysprosium dimer is formed, halogenated P-hydroxybenzoic acid dysprosium complex is characterization object, utilizes X-ray list
Brilliant diffractometer and powder diffractometer test the structure and Xiang Chundu of halogenated P-hydroxybenzoic acid dysprosium complex, are surveyed using thermal analyzer
The thermal stability for trying halogenated P-hydroxybenzoic acid dysprosium complex tests halogenated P-hydroxybenzoic acid dysprosium using Superconducting magnetic analyzer
The magnetic property of complex, application of the halogenated P-hydroxybenzoic acid dysprosium complex as magnetic function material.
Embodiment: six bis- chloro- 4-HBA 0.3mmol and 1,10- of trichloride hydrate dysprosium 0.2mmol, 5- S1, are weighed
Phen is raw material 0.2mmol, is add to deionized water, the sodium hydroxide for being after mixing 0.1mol/L with concentration is molten
The mixed solution of liquid adjusting pH value to 7；
S2, the mixed solution for obtaining S1, which are transferred in autoclave, is warming up to 140 DEG C of 96 h of heat preservation, while with per hour
10 DEG C of rate makes reaction kettle be down to room temperature, obtains colourless bulk crystals after opening kettle, filters and make to be washed with deionized, dry in the air naturally
Halogenated P-hydroxybenzoic acid dysprosium complex is obtained after dry.
Phenetic analysis is carried out to the halogenated P-hydroxybenzoic acid dysprosium complex that embodiment obtains, method particularly includes: micro-
The halogenated P-hydroxybenzoic acid dysprosium complex of the sizeable monocrystalline of picking under mirror is penetrated using Bruker SMART APEX II type X-
Line single crystal diffractometer collects diffraction data at room temperature, and carries out absorption correction to diffraction data using SADABS program, uses
SAINT and SHELXTL program parses diffraction data, refine is carried out to crystal structure using least square method, made from embodiment
Halogenated P-hydroxybenzoic acid dysprosium complex has the chloro- 4-HBA anion bridging dysprosium dimerization bodily form of 3,5- bis- of negative divalent
At two-dimensional network structure, Fig. 1 be complex in dysprosium dimer structure chart, Fig. 2 be complex two-dimensional structure figure.
Using Rigaku Ultima IV type X-ray powder diffraction instrument collect powder diffraction data, scan pattern be 2 θ/
θ, scanning range are 5 to 50 degree, are fitted powder diffraction data using Cerius2 program, are carried out using Mercury1.4.1 software
The powder diffraction of mono-crystalline structures is simulated.Fig. 3 is the powder diagram of complex made from embodiment, tests the powder diffraction measured
Figure is almost the same with simulation, shows the phase purity of bulk article.
Thermogravimetric Data is collected using PE-Pyris Diamond S-II type thermal analyzer, the rate of heat addition is 10 degrees Celsius every
Minute, temperature range is 30 to 980 degrees Celsius.Fig. 4 is the hot weight curve of complex made from embodiment, made from embodiment
Complex keeps stablizing before 350 degrees Celsius, and then molecular skeleton starts to collapse, and shows bulk article thermostabilization with higher
Property.
Alternating magnetism data are collected using Quantum Design MPMSXL7 type Superconducting magnetic analyzer.Fig. 5 is to implement
For the null field frequency conversion imaginary part ac magnetic susceptibility of complex made from example to the dependence curve graph of temperature, Fig. 6 is to match made from embodiment
Dependence curve graph of the null field alternating temperature imaginary part ac magnetic susceptibility to frequency of object is closed, Fig. 7 is the null field of complex made from embodiment
Alternating temperature imaginary part ac magnetic susceptibility shows that complex made from embodiment has to the Ke Er-Ke Er curve graph of real part ac magnetic susceptibility
There is apparent null field single molecular magnets behavior, influencing the halogenated P-hydroxybenzoic acid dysprosium complex that embodiment is prepared can be used as
Magnetic function material is applied.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of halogenated P-hydroxybenzoic acid dysprosium complex, which is characterized in that specific chemical formula is Dy-L-HL-phen, the L
The chloro- 4-HBA anion of 3,5- bis- for the divalent that is negative, the HL are negative 3, the 5- bis- chloro- 4-HBA yin of monovalence
Ion, the phen are 1,10- Phen molecule.
2. a kind of halogenated P-hydroxybenzoic acid dysprosium complex according to claim 1, which is characterized in that described halogenated to hydroxyl
Yl benzoic acid dysprosium complex is the two dimension formed with the chloro- 4-HBA anion bridging dysprosium dimer of negative divalent 3,5- bis-
Reticular structure.
3. a kind of halogenated P-hydroxybenzoic acid dysprosium complex according to claim 1, which is characterized in that described halogenated to hydroxyl
Yl benzoic acid dysprosium complex is characterization object, tests halogenated para hydroxybenzene first using X-ray single crystal diffractometer and powder diffractometer
The structure and Xiang Chundu of sour dysprosium complex test the thermal stability of halogenated P-hydroxybenzoic acid dysprosium complex using thermal analyzer,
The magnetic property of halogenated P-hydroxybenzoic acid dysprosium complex is tested using Superconducting magnetic analyzer.
4. a kind of halogenated P-hydroxybenzoic acid dysprosium complex according to claim 1, which is characterized in that described halogenated to hydroxyl
Application of the yl benzoic acid dysprosium complex as magnetic function material.
5. a kind of preparation method of halogenated P-hydroxybenzoic acid dysprosium complex, which comprises the following steps:
S1, soluble inorganic salt of rare earth, the chloro- 4-HBA of 5- bis- and 1 are weighed, 10- Phen is raw material, while solvable
Property inorganic salt of rare earth, the chloro- 4-HBA of 5- bis- and 1,10- Phen according to molar ratio be 2:3:2 be added to deionization
In water, the mixed solution of pH value to 7 is adjusted with sodium hydroxide solution after mixing；
S2, the mixed solution for obtaining S1, which are transferred in autoclave, is warming up to 140 DEG C of 96 h of heat preservation, is slowly dropped to room temperature
Colourless bulk crystals are obtained, filters and washs, obtain halogenated P-hydroxybenzoic acid dysprosium complex after natural drying.
6. a kind of preparation method of halogenated P-hydroxybenzoic acid dysprosium complex according to claim 5, which is characterized in that institute
The concentration for stating sodium hydroxide solution is 0.1mol/L, and the solubility inorganic salt of rare earth is six trichloride hydrate dysprosiums.
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|---|---|---|---|---|
| CN114524831A (en) * | 2022-02-21 | 2022-05-24 | 温州大学 | Dysprosium complex and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786540A (en) * | 2012-09-12 | 2012-11-21 | 东华理工大学 | Preparation method for coordination compound with reversible phase change dynamic single molecule |
| CN104098612A (en) * | 2014-07-01 | 2014-10-15 | 天津师范大学 | 3d-4f heteronuclear metal magnetic complex and preparing method and application thereof |
-
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- 2019-01-21 CN CN201910052045.6A patent/CN109705150A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786540A (en) * | 2012-09-12 | 2012-11-21 | 东华理工大学 | Preparation method for coordination compound with reversible phase change dynamic single molecule |
| CN104098612A (en) * | 2014-07-01 | 2014-10-15 | 天津师范大学 | 3d-4f heteronuclear metal magnetic complex and preparing method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| VISHNOI,PRATAP 等: "Zinc dialkylhydroxybenzoates with unusual structures: first example of a discrete three-blade paddle-wheel and a solvent engulfed coordination polymer", 《CHEMISTRYSELECT 》 * |
| 宿素玲: "镝芳香族羧酸与邻菲罗啉配合物的合成、结构、热分解机理及动力学的研究", 《河北师范大学硕士学位论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524831A (en) * | 2022-02-21 | 2022-05-24 | 温州大学 | Dysprosium complex and preparation method and application thereof |
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