CN109206443A - A kind of anionic framework magnetic refrigerating material and synthetic method - Google Patents
A kind of anionic framework magnetic refrigerating material and synthetic method Download PDFInfo
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- CN109206443A CN109206443A CN201811026675.8A CN201811026675A CN109206443A CN 109206443 A CN109206443 A CN 109206443A CN 201811026675 A CN201811026675 A CN 201811026675A CN 109206443 A CN109206443 A CN 109206443A
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- oxalic acid
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- 239000000463 material Substances 0.000 title claims abstract description 15
- 125000000129 anionic group Chemical group 0.000 title claims abstract description 14
- 238000010189 synthetic method Methods 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 claims abstract description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000005057 refrigeration Methods 0.000 claims abstract description 6
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 39
- 239000013078 crystal Substances 0.000 claims description 13
- 235000006408 oxalic acid Nutrition 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- -1 dimethyl amine cation Chemical class 0.000 claims description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 5
- 230000005588 protonation Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 230000005303 antiferromagnetism Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims 1
- 150000001455 metallic ions Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 3
- RJOJUSXNYCILHH-UHFFFAOYSA-N gadolinium(3+) Chemical compound [Gd+3] RJOJUSXNYCILHH-UHFFFAOYSA-N 0.000 description 3
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000000921 Gadolinium Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of anionic framework magnetic refrigerating material and its synthetic methods.Anionic framework magnetic refrigerating material chemical formula is { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n, molecular formula are as follows: C6NH16GdO12, molecular weight are as follows: 451.44；Gadolinium carbonate and two oxalic acid hydrates are separately added into distilled water, then mix the two, and adds n,N-Dimethylformamide, stirring controls its pH 3, is placed in 140 DEG C of baking oven constant temperature four days, cools down.When temperature is 2K and magnetic field is 7T, the magnetic entropy variate of the compound is up to 37.8J kg– 1K–1, illustrate { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nThere is potential application prospect in terms of magnetic refrigeration.The present invention has the advantages that simple process, chemical constituent are easily controllable, reproducible and performance is excellent etc..
Description
Technical field
The invention belongs to coordination polymer material preparation technical field, in particular to a kind of anionic framework magnetic refrigerating material
{(CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n((CH3)2NH2 +For protonation dimethyl amine cation, ox2-For oxalate) and
Synthetic method.
Background technique
Magnetic refrigeration, which only depends on, provides the magnetic field of energy, and without adding other refrigerants, technique should be than traditional steaming
Vapour compress technique is more environmentally friendly.Gadolinium and its alloy always are focus concerned by people, be primarily due to gadolinium 4f layer have 7 not at
To electronics, there is high spin magnetic moment and cause magnetothermal effect significant.Therefore, gadolinium class cluster compound molecular magnet is in low temperature and ultralow
The application of the cooling aspect of temperature has obtained rapid extension.The coordination polymer that the present invention is made up of gadolinium, and find its have compared with
The hot entropy of high magnetic has very big application potential in terms of magnetic refrigeration.
Summary of the invention
It is an object of the invention to provide a kind of Gd coordination compound magnetic refrigerating material and synthetic methods.
Thinking of the invention: Gd coordination compound is obtained by hydro-thermal method using gadolinium carbonate and oxalic acid.
Anionic framework materials chemistry formula of the present invention is { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n
((CH3)2NH2 +=protonation dimethylamine cation；ox2-=oxalate), belong to monoclinic system, P21/ n space group.In the cooperation
In the dissymmetrical structure unit of object, contain 20 non-hydrogen atoms, the metal gadolinium ion at respectively one center, two oxalic acid point
Son, a water of coordination molecule, the dimethyl amine cation of a protonation, three crystalline water molecules.The metal gadolinium ion at center
The mode of nine coordinations is taken, respectively with four oxalic acid molecules, hydrone is connected.Oxalic acid molecule connects in the form that two teeth chelate
Adjacent gadolinium ion is connect, 3D frame structure is constituted.Compound forms the cellular structure of hexagon shape along a axis direction, protonation
Dimethylamine ion and object hydrone are distributed on the inner wall in hexagon duct.Crystal structural data is shown in Table one, part bond distance's key
Angle is shown in Table two.
Table one: { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nCrystal parameter
a R1=Σ | | Fo|–|Fc||/Σ|Fo|.b wR2=[Σ w (| Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
Table two: { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nBond distanceWith bond angle (°)
Symmetry codes:(i)-x+1/2,y-1/2,-z+3/2；(ii)-x+1/2,y+1/2,-z+3/2；(iii)-
x,-y+1,-z+2；
(iv)-x+1,-y+1,-z+2。
{ (the CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nSynthesis specific steps:
(1) the analytically pure gadolinium carbonate of 0.3956g is weighed to be dissolved in the distilled water of 15mL, it is half of magnetic agitation small at room temperature
When, so that gadolinium carbonate powder is uniformly dispersed, obtains gadolinium carbonate suspension.
(2) analytically pure two oxalic acid hydrate of 0.6931g is weighed to be dissolved in the distilled water of 10mL；Oxalic acid solution is made.
(3) the resulting gadolinium carbonate suspension of step (1) and the resulting oxalic acid solution of step (2) are mixed, and is added 3mL points
Pure n,N-Dimethylformamide is analysed, at room temperature one hour of magnetic agitation, be uniformly mixed it, pure oxalic acid adjusting is molten with analyzing
The pH of liquid is 3.
(4) reaction kettle that step (3) acquired solution equivalent is poured into 2 25mL polytetrafluoroethyllining linings, is placed in 140 DEG C of bakings
5 DEG C are reduced within each hour after case constant temperature 4 days, 4 days, until temperature drops to 100 DEG C, constant temperature 24 hours；Then room is naturally cooled to
Wen Shi obtains colourless bulk crystals, as anionic framework material { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n。
The anionic framework { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nIt can apply to ultralow temperature magnetic refrigerating.
The present invention has the characteristics that simple process, chemical constituent are easily controllable, reproducible and performance is excellent etc..
Under conditions of externally-applied magnetic field is 2000Oe and temperature range is 2.0-300K, { (CH is determined3)2NH2[Gd
(ox)2(H2O)]·3H2O}nVariable temperature magnetic susceptibility.It was found that the magnetic susceptibility of the compound also reduces therewith with the reduction of temperature,
Illustrate Gd3+Between there are anti-ferromagnetism effects.When temperature is 2K and magnetic field is 7T, the magnetic entropy variate of the compound reaches
It is up to 37.8J kg–1K–1, illustrate { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nHave in terms of magnetic refrigeration and potentially answers
Use prospect.
Detailed description of the invention
Fig. 1 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nMolecular structure.
Fig. 2 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nAlong the three-dimensional frame structure of [111] axis direction
Figure.
Fig. 3 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nInfrared spectrum.
Fig. 4 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nThermal multigraph.
Fig. 5 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nPowder spectrogram.
Fig. 6 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nIn externally-applied magnetic field 2000Oe variable temperature magnetic susceptibility
Curve.
Fig. 7 is the present invention { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nAlternating temperature magnetic under the conditions of different externally-applied magnetic fields
Entropy Changes curve.
Specific embodiment
Embodiment 1:
(1) the analytically pure gadolinium carbonate of 0.3956g is weighed to be dissolved in the distilled water of 15mL, it is half of magnetic agitation small at room temperature
When, so that gadolinium carbonate powder is uniformly dispersed, obtains gadolinium carbonate suspension.
(2) analytically pure two oxalic acid hydrate of 0.6931g is weighed to be dissolved in the distilled water of 10mL；Oxalic acid solution is made.
(3) the resulting gadolinium carbonate suspension of step (1) and the resulting oxalic acid solution of step (2) are mixed, and is added 3mL points
Pure n,N-Dimethylformamide is analysed, at room temperature one hour of magnetic agitation, be uniformly mixed it, pure oxalic acid adjusting is molten with analyzing
The pH of liquid is 3.
(4) reaction kettle that step (3) acquired solution equivalent is poured into the polytetrafluoroethyllining lining of 2 25mL, is placed in 140 DEG C
5 DEG C are reduced within each hour after baking oven constant temperature 4 days, 4 days, until temperature drops to 100 DEG C, constant temperature 24 hours.Then it naturally cools to
When room temperature, obtaining colourless bulk crystals is { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n, yield: 0.6228g, yield:
58.11%.{ (CH is measured by single crystal diffractometer3)2NH2[Gd(ox)2(H2O)]·3H2O}nStructure, crystal structural data is shown in
Table one, bond distance's bond angle data are shown in Table two.
Embodiment 2:
(1) the analytically pure gadolinium carbonate of 0.3956g, analytically pure two oxalic acid hydrate of 0.6931g and 3mL are analyzed into pure N, N- bis-
Methylformamide is dissolved into 25mL distilled water, is 3 with the pH for analyzing pure careless acid-conditioning solution after a hour is stirred at room temperature.
(2) reaction kettle that step (1) acquired solution equivalent is poured into the polytetrafluoroethyllining lining of 2 25mL, is placed in 140 DEG C
5 DEG C are reduced within each hour after baking oven constant temperature 4 days, 4 days, until temperature drops to 100 DEG C, constant temperature 24 hours；Then it naturally cools to
When room temperature, obtaining colourless bulk crystals is { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n, yield: 0.6024g, yield:
56.21%.{ (CH is measured by single crystal diffractometer3)2NH2[Gd(ox)2(H2O)]·3H2O}nStructure, crystal structural data is shown in
Table one, bond distance's bond angle data are shown in Table two.
(3) { (CH obtained by step (2) is taken3)2NH2[Gd(ox)2(H2O)]·3H2O}nCrystal prototype carry out magnetic property survey
Examination, when temperature is 2K and magnetic field is 7T, the magnetic entropy variate of the compound, which reaches, is up to 37.8J kg–1K–1, explanation
{(CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nThere is potential application prospect in terms of magnetic refrigeration.
Claims (3)
1. a kind of anionic framework magnetic refrigerating material, it is characterised in that anionic framework materials chemistry formula is { (CH3)2NH2[Gd
(ox)2(H2O)]·3H2O}n, in which: CH3)2NH2 +For protonation dimethyl amine cation, ox2-For oxalate；Molecular formula are as follows:
C6NH16GdO12, molecular weight are as follows: 451.44；Crystal structural data is shown in Table one, and part bond distance's bond angle is shown in Table two；The compound belongs to
Monoclinic system, P21/ n space group, central metallic ions Gd3+；Under conditions of temperature is 2K and externally-applied magnetic field is 7T, the change
The magnetic entropy variate for closing object, which reaches, is up to 37.8J kg–1K–1, it was demonstrated that { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nIn magnetic system
Cold aspect has potential application prospect；Under conditions of externally-applied magnetic field is 2000Oe and temperature range is 2.0-300K, measurement
{(CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nVariable temperature magnetic susceptibility；With the reduction of temperature, the magnetic susceptibility of the compound
Reduce therewith, illustrates Gd3+Between there are anti-ferromagnetism effects；
Table one: { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nCrystal parameter
aR1=Σ | | Fo|–|Fc||/Σ|Fo|.bwR2=[Σ w (| Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
Table two: { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nBond distanceWith bond angle (°)
Symmetry codes:(i)-x+1/2,y-1/2,-z+3/2；(ii)-x+1/2,y+1/2,-z+3/2；(iii)-x,-y+
1,-z+2；(iv)-x+1,-y+1,-z+2.
2. anionic framework material { (CH according to claim 13)2NH2[Gd(ox)2(H2O)]·3H2O}nSynthesis side
Method, it is characterised in that specific steps are as follows:
(1) it weighs the analytically pure gadolinium carbonate of 0.3956g to be dissolved in the distilled water of 15mL, at room temperature magnetic agitation half an hour,
So that gadolinium carbonate powder is uniformly dispersed, obtains gadolinium carbonate suspension；
(2) analytically pure two oxalic acid hydrate of 0.6931g is weighed to be dissolved in the distilled water of 10mL；Oxalic acid solution is made；
(3) the resulting gadolinium carbonate suspension of step (1) and the resulting oxalic acid solution of step (2) are mixed, and it is pure that 3mL analysis is added
N,N-Dimethylformamide at room temperature one hour of magnetic agitation, is uniformly mixed it, is 3 with the pH of careless acid-conditioning solution；
(4) reaction kettle that step (3) acquired solution equivalent is poured into the polytetrafluoroethyllining lining of 2 25mL, is placed in 140 DEG C of baking ovens
5 DEG C are reduced within each hour after constant temperature 4 days, 4 days, until temperature drops to 100 DEG C, constant temperature 24 hours；Then cooled to room temperature
When, obtain colourless bulk crystals, as anionic framework magnetic refrigerating material { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}n。
3. anionic framework material { (CH according to claim 1 or 23)2NH2[Gd(ox)2(H2O)]·3H2O}nAnswer
With, it is characterised in that anionic framework the material { (CH3)2NH2[Gd(ox)2(H2O)]·3H2O}nIt can apply to ultralow temperature magnetic
Refrigeration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111647163A (en) * | 2020-06-18 | 2020-09-11 | 湖北科技学院 | Gadolinium-based framework coordination material with high magnetocaloric effect and preparation method thereof |
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| CN106279221A (en) * | 2016-07-13 | 2017-01-04 | 南京工业大学 | A kind of synthetic method of high proton conducting metal organic framework material |
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| CN111647163A (en) * | 2020-06-18 | 2020-09-11 | 湖北科技学院 | Gadolinium-based framework coordination material with high magnetocaloric effect and preparation method thereof |
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