CN108641093B - Mononuclear manganese coordination polymer and preparation method thereof - Google Patents
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- 239000013256 coordination polymer Substances 0.000 title claims abstract description 43
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 43
- 239000011572 manganese Substances 0.000 title claims abstract description 30
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title description 7
- 239000013078 crystal Substances 0.000 claims abstract description 22
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- INARQBVWUGPGRN-UHFFFAOYSA-N 5-[(3-carboxy-1,2,4-triazol-1-yl)methyl]benzene-1,3-dicarboxylic acid Chemical compound C(=O)(O)C1=NN(C=N1)CC=1C=C(C=C(C(=O)O)C=1)C(=O)O INARQBVWUGPGRN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000696 magnetic material Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 7
- 229910021380 Manganese Chloride Inorganic materials 0.000 abstract description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 5
- 239000003446 ligand Substances 0.000 abstract description 5
- 239000011565 manganese chloride Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 4
- 230000003993 interaction Effects 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000005291 magnetic effect Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002447 crystallographic data Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 3
- 230000001808 coupling effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001437 manganese ion Inorganic materials 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000005343 Curie-Weiss law Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 229910018663 Mn O Inorganic materials 0.000 description 1
- 229910003176 Mn-O Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
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- 150000001768 cations Chemical class 0.000 description 1
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- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005292 diamagnetic effect Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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Abstract
The invention relates to a mononuclear manganese coordination polymer, which has a structural formula of [ Mn (5-Hctmia) (H)2O)2]nWherein 5-H3ctmia is 5- ((3-carboxy-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid. The coordination polymer is prepared by a hydrothermal method: mixing MnCl2·4H2O and 5-H3Dissolving a ctmia ligand in water and acetonitrile according to the mass ratio of 1:1, placing the mixture into a hydrothermal reaction kettle for reaction for 72 hours at the temperature of 160 ℃, cooling the mixture to room temperature to obtain colorless blocky crystals, washing the crystals with distilled water, drying the crystals in vacuum, and collecting the crystals. The Mn (II) ions in the coordination polymer have ferromagnetic interaction and can be used as a molecular magnetic material.
Description
Technical Field
The invention relates to a transition metal coordination polymer, in particular to a one-dimensional chain manganese coordination polymer, and particularly relates to a manganese coordination polymer which is constructed based on transition metal divalent manganese and 5- ((3-carboxyl-1, 2, 4-triazole-1-yl) methyl) -isophthalic acid and has ferromagnetic interaction and a preparation method thereof.
Background
The molecular magnetic material is a magnetic compound formed by combining free radicals or paramagnetic ions (mainly including transition metal ions and rare earth metal ions) and diamagnetic ligands through a chemical method. Compared with the traditional magnet, the molecular magnet has the advantages of small density, good solubility, easy processing, high transparency, good controllability and the like, and has potential application value in the fields of space materials, microwave materials, information recording materials, photoelectric magnetic materials, household appliances and the like. Therefore, the search for a molecular magnet with excellent performance is the focus of research in the fields of molecular magnetics and material science.
The divalent manganese ion is caused by d5The valence electron configuration can have high and low spin configuration, and is a good magnetic ion.Often selected as the source element of molecular magnetism. In coordination polymers, the linker 5- ((3-carboxy-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid has both two planar groups that facilitate charge transfer and a blocking group between the two planar groups. Therefore, the invention adopts a coordination polymer formed by divalent manganese ions and 5- ((3-carboxyl-1, 2, 4-triazole-1-yl) methyl) -isophthalic acid as a molecular magnetic material.
Disclosure of Invention
The invention aims to provide a mononuclear manganese coordination polymer capable of being used as a molecular magnetic material and a preparation method thereof.
The invention provides a mononuclear manganese coordination polymer, which has a simple structure formula as follows: [ Mn (5-Hctmia) (H)2O)2]nWherein 5-H3ctmia is 5- ((3-carboxy-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid; the structural formula is as follows:
the crystals of the coordination polymer belong to a monoclinic system and have a space group of P21C, unit cell parameters:
α is 90 °, β is 102.742(4 °), and γ is 90 °. The manganese ion in the coordination polymer is a divalent cation and is in a six-coordination octahedral configuration { MnNO5Is composed of five oxygen atoms and one nitrogen atom. Wherein O1 and N1 are provided by a triazole nitrogen atom and a carboxyl oxygen atom on the same ligand to chelate and coordinate to Mn2+Ions, forming a chelate five-membered ring, O2A and O3B (symmetric operation code is (A) -x +1, y +1/2, -z +1/2, (B) x, y +1, z) from two other molecules of symmetrically related ligands Hctmia2-Anion and the four atoms are in the equatorial plane of the octahedron. O7 and O8 are derived from two coordinated water molecules, in the octahedral axial position. Wherein the bond of Mn-NA length of 2.253(6), and a bond length of Mn-O in the range of
The coordination polymer is a one-dimensional chain structure. X-ray powder diffraction confirmed that the crystalline sample was homogeneous and stable. Through the temperature-changing magnetic susceptibility experiment, the experimental value of the effective magnetic moment of the coordination polymer is 5.81 mu at 300KBWith the temperature decreasing, the effective magnetic moment value slowly increases and reaches a maximum value of 5.91 mu at 103KBThen gradually decreases to reach a minimum value of 4.30 mu at 2KBFrom this phenomenon, it can be seen that there is a weak ferromagnetic coupling between mn (ii); according to Curie-Weiss law χmThe coefficient is obtained by fitting C/(T-theta) at 2-300K, and the Curie constant C is 4.29cm3K mol–1The exos constant θ is 0.082K greater than 0, and the weak ferromagnetic coupling effect between mn (ii) in the coordination polymer is verified again. Therefore, the manganese coordination polymer of the present invention can be used as a magnetic material.
The invention provides a preparation method of a mononuclear manganese coordination polymer, which comprises the following steps:
1) MnCl with a molar ratio of 1:12·4H2Adding O and 5- ((3-carboxyl-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid into a polytetrafluoroethylene tube containing a mixed solvent of water and acetonitrile in a volume ratio of 5: 2;
2) the polytetrafluoroethylene tube is placed in a stainless steel reaction kettle to be sealed, the temperature is increased to 160 ℃, the reaction lasts for 60 to 90 hours, the temperature is naturally reduced to the room temperature, colorless blocky crystals are obtained, the crystals are washed by distilled water for a plurality of times and then are dried in vacuum, and the yield is 58 percent.
The reaction time in step 2) is preferably 72 hours.
The choice and proportion of solvent in step 1) above is important because the coordination polymer of the present invention cannot be obtained using other mixed solvents under the same conditions.
The invention has the beneficial effects that:
the manganese coordination polymer is synthesized under hydrothermal conditions, and has the advantages of simple preparation process, high yield and high purity.
The manganese coordination polymer is constructed based on 5- ((3-carboxyl-1, 2, 4-triazole-1-yl) methyl) -isophthalic acid, and the Mn (II) ions in the coordination polymer have ferromagnetic interaction through a temperature-changing magnetic susceptibility experiment under a 1000Oe external magnetic field, so that the manganese coordination polymer can be used as a molecular magnetic material.
Drawings
FIG. 1 is a diagram showing coordination environments of coordination polymers of the present invention. Wherein the symmetric operation code is a ═ x +1, y +1/2, -z +1/2, and B ═ x, y +1, z.
FIG. 2 is an X-ray powder diffraction pattern at 298K for coordination polymers of the present invention (experimental and simulated).
FIG. 3 is a thermogram of a coordination polymer of the present invention.
FIG. 4 shows that under the action of 1000Oe external magnetic field, the coordination polymer of the invention has 2-300K variable temperature magnetic susceptibility and chiMT graph.
Detailed Description
Example 1 coordination Polymer [ Mn (5-Hctmia) (H)2O)2]nPreparation method of (1)
Weighing MnCl2·4H2O (19.80mg,0.10mmol), and 5-H3cmtia (29.10mg,0.10mmol) was added 5.0mL H2O and 2.0mL acetonitrile in a 13mL Teflon tube were sealed in a stainless steel reaction vessel, and they were placed in an oven at 160 ℃ and reacted for 3d, cooled to room temperature overnight, and colorless block crystals were obtained after opening the vessel. The collected colorless bulk crystals were washed three times with distilled water and then naturally dried (yield: 58%).
Elemental analysis (%). anal.Calcd (%). for C12H11N3O8Mn is C, 37.88; h, 2.89; n,11.04 Experimental value C, 37.87; h, 2.90; n,11.05.
Example 2 coordination Polymer [ Mn (5-Hctmia) (H)2O)2]nCrystal structure determination of (1):
the crystal diffraction data was collected by a Mo-K alpha ray source. The first step is to find the crystal with proper size, regular shape and brightness, the second step is to stick the found crystal onto the thin glass filament, and the third step is to fix the crystal onto the stone as the radiation sourceOn a Bruker APEX-II CCD diffractometer of the Mo-Ka ink monochromator, the wavelength of the light source used is
Finally, single crystal diffraction data of the sample are collected by using an omega-2 theta scanning mode. After the measurement, SAINTPlus was used to reduce and correct the diffraction data, SMART program was used to determine the crystal cell parameters, and SADAB program was used to correct the absorption. The detailed crystal determination data are shown in table 1. The structure is shown in figure 1.
TABLE 1 crystallographic data for coordination polymers of the invention
Example 3 coordination Polymer [ Mn (5-Hctmia) (H)2O)2]nAnalysis of phase of
Powder diffraction: the experimental diffraction pattern obtained by the X-ray powder diffraction result is consistent with the theoretical simulation pattern, which shows that the divalent manganese coordination polymer crystal sample phase of the invention is uniform, and is shown in figure 2.
Example 4 coordination Polymer [ Mn (5-Hctmia) (H)2O)2]nThermal stability of
The thermal stability is shown in FIG. 3, and the coordination polymer [ Mn (Hctmia) (H)2O)2]nA weight loss platform exists between room temperature and 90 ℃, corresponding to a crystal water molecule, and the mass loss is 4.80%. The second weight loss, starting from 90 ℃ to 200 ℃, corresponds to another molecule of crystalline water (theoretical 4.73%, experimental 4.80%). Then, the temperature is continuously raised, and the coordination polymer [ Mn (5-Hctmia) (H)2O)2]nThe main structure of (a) begins to collapse.
Example 5 coordination Polymer [ Mn (5-Hctmia) (H)2O)2]nThe magnetic property of (2):
the temperature-changing magnetic susceptibility and the effective magnetic moment curve are shown in FIG. 4, and the experimental value of the effective magnetic moment of the coordination polymer is 5.81 mu at 300KBSlightly below a theoretical value of 5.92 for a high spin of mn (ii) (S-5/2, g-2)μBWith the temperature decreasing, the effective magnetic moment value slowly increases and reaches a maximum value of 5.91 mu at 103KBThen gradually decreases to reach a minimum value of 4.30 mu at 2KBFrom this phenomenon, it can be seen that there is a weak ferromagnetic coupling effect between mn (ii); according to Curie-Weiss law χmThe Curie constant C is 4.29cm and is obtained by fitting C/(T-theta) at 2-300K (an insert in figure 4)3K mol–1And the Weiss constant theta is larger than 0.082K, and weak ferromagnetic coupling effect between Mn (II) in coordination polymer is verified again.
Comparative example 1 weighing of MnCl2·4H2O (39.60mg,0.20mmol), and 5-H3cmtia (29.10mg,0.10mmol) was added 5mL H2O and 2mL of acetonitrile in a 13mL polytetrafluoroethylene tube, sealing the polytetrafluoroethylene tube in a stainless steel reaction kettle, heating at 160 ℃ for 72 hours, naturally cooling, standing overnight, and observing that no crystal is separated out after filtering a colorless clear solution.
Comparative example 2 weighing of MnCl2·4H2O (19.80mg,0.10mmol), and 5-H3cmtia (29.10mg,0.10mmol) was added 6mL of H2O and 1mL of acetonitrile in a 13mL polytetrafluoroethylene tube, sealing the polytetrafluoroethylene tube in a stainless steel reaction kettle, heating at 160 ℃ for 72 hours, naturally cooling, standing overnight, and observing that no crystal is separated out from a colorless clear solution.
Comparative example 3 weighing of MnCl2·4H2O (19.80mg,0.10mmol), and 5-H3cmtia (29.10mg,0.10mmol) was added to 12mL of H2O and 4mL of ethanol in a 23mL polytetrafluoroethylene tube, sealing the polytetrafluoroethylene tube in a stainless steel reaction kettle, heating at 160 ℃ for 72 hours, naturally cooling, standing overnight, and observing that no crystal is separated out from a colorless clear solution. As can be seen from comparative examples 1 to 3, the coordination polymer of the present invention can be obtained only under the conditions of the solvent and the compounding ratio thereof defined in the present invention, and the metal salt, the ligand and the molar ratio thereof.
Claims (4)
1. A mononuclear manganese coordination polymer is characterized by having a structural formula: [ Mn (5-Hctmia) (H)2O)2]n，Wherein 5-H3ctmia is 5- ((3-carboxy-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid; the structural formula is as follows:
the coordination polymer belongs to a monoclinic system and has a space group of P21C, unit cell parameters:
α＝90°,β＝102.742(4)°,γ＝90°。
2. the method of claim 1, comprising the steps of:
1) MnCl with a molar ratio of 1:12·4H2Adding O and 5- ((3-carboxyl-1, 2, 4-triazol-1-yl) methyl) -isophthalic acid into a polytetrafluoroethylene tube containing a mixed solvent of water and acetonitrile in a volume ratio of 5: 2;
2) the polytetrafluoroethylene tube is placed in a stainless steel reaction kettle to be sealed, the temperature is increased to 160 ℃, the reaction lasts for 60 to 90 hours, the temperature is naturally reduced to the room temperature, colorless blocky crystals are obtained, and the crystals are washed by distilled water for a plurality of times and then are dried in vacuum.
3. The method of claim 2, wherein the reaction time of step 2) is 72 hours.
4. The mononuclear manganese coordination polymer according to claim 1 for use as a molecular magnetic material.
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| CN104844657A (en) * | 2015-04-09 | 2015-08-19 | 山西大学 | Manganese metal polymer and preparation method and application thereof |
| CN106543142A (en) * | 2016-10-09 | 2017-03-29 | 洛阳师范学院 | A kind of complex of (3 (3 yl of pyridine) 1,2,4 triazoles of 1H, 5 yl) benzoic acid cadmium and preparation method thereof |
| WO2017184991A1 (en) * | 2016-04-22 | 2017-10-26 | The Regents Of The University Of California | Post-synthetically modified metal-organic frameworks for selective binding of heavy metal ions in water |
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| CN104844657A (en) * | 2015-04-09 | 2015-08-19 | 山西大学 | Manganese metal polymer and preparation method and application thereof |
| WO2017184991A1 (en) * | 2016-04-22 | 2017-10-26 | The Regents Of The University Of California | Post-synthetically modified metal-organic frameworks for selective binding of heavy metal ions in water |
| CN106543142A (en) * | 2016-10-09 | 2017-03-29 | 洛阳师范学院 | A kind of complex of (3 (3 yl of pyridine) 1,2,4 triazoles of 1H, 5 yl) benzoic acid cadmium and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| A Novel Three-dimensional Mn(II) Coordination Polymer Constructed from Biphenyl-3,3΄,5,5΄-tetracarboxylic Acid and Water;LI Shao-Dong等;《结构化学》;20161215;第35卷(第12期);第1920-1928页 * |
| M2+ and Ln3+-catalyzed synthesis of a [1,2,4]triazine core via intramolecular C–H/N–H functionalization and C–N bond formation (M = Mn, Zn, Cd;Ln = Dy, Tb);Wen-Bin Chen等;《New J. Chem.,》;20141125;第39卷(第2期);第1222-1227页 * |
| Magnetic metal–organic frameworksw;Mohamedally Kurmoo;《Chem. Soc. Rev.,》;20090224;第38卷;第1353-1379页 * |
| 一维链式三唑锰晶体的结构及磁性能研究;闫娟枝等;《人工晶体学报》;20140815;第43卷(第8期);第2164-2169页 * |
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