CN104262364A - Copper-bridged flexible ligand-isopolymolybdate hybrid material structure and preparation method thereof - Google Patents
Copper-bridged flexible ligand-isopolymolybdate hybrid material structure and preparation method thereof Download PDFInfo
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- CN104262364A CN104262364A CN201410445080.1A CN201410445080A CN104262364A CN 104262364 A CN104262364 A CN 104262364A CN 201410445080 A CN201410445080 A CN 201410445080A CN 104262364 A CN104262364 A CN 104262364A
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 claims abstract 5
- 239000010949 copper Substances 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000001273 butane Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 5
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000002835 absorbance Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 125000006850 spacer group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 150000003624 transition metals Chemical class 0.000 abstract 1
- 239000003446 ligand Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000013110 organic ligand Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000013460 polyoxometalate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
- C07F1/08—Copper compounds
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- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1044—Heterocyclic compounds characterised by ligands containing two nitrogen atoms as heteroatoms
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Abstract
The invention a transition metal copper-bridged flexible organic ligand-isopolymolybdate hybrid material crystal structure and a preparation method thereof. The chemical formula of the crystal is CuI2CuII(C10N4H14)3(C3N2H)2[Mo8O26].3H2O, and the molecular weight is 2095.14; the crystal belongs to a monoclinic system, and the space group is P-1; and the cell parameters are as follows: a=12.206(4)A, b=12.569(4)A, c=12.887(8)A, alpha=97.146(6) degrees, beta=111.929(7) degrees, gamma=114.063(4) degrees, V=1582.8(12)A<3>, and Z=1. The material is synthesized by a hydrothermal process. The prepared compound has definite composition and structure, and has potential application value in the aspect of chemical sensors.
Description
Technical field
The invention belongs to inorganic polyoxometallate technical field of chemistry, relate to the synthesis of isopolymolybdate hybrid material, is Cu in particular
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2the preparation method of O compound and structure.
Background technology
Polyoxometallate, as the important inorganic building block of a class, plays very important role in the study on the synthesis of Inorganic-Organic Hybrid Material.Many new capabilities that this kind of Inorganic-Organic Hybrid Material of research display has are with a wide range of applications in fields such as catalysis, absorption, magnetics, photochemistry, host-guest chemistry, stored energy, biological chemistry and bio-pharmaceuticals.The development of this kind of material, not only constantly can create, develop new species, bring the develop rapidly of Materials science, simultaneously, also by together with the primary chemical subject convergence such as molecular engineering, organic chemistry and solid inorganic chemistry, be the new power promoting chemical science and related discipline development thereof.In the design and synthesis of polyacid Inorganic-Organic Hybrid Material, the selection of organic molecule is most important.Linear rigidity organic ligand is widely used in building polyacid Inorganic-Organic Hybrid Material.Comparatively speaking, design and synthesis, the Structure and Properties research report of the polyacid Inorganic-Organic Hybrid Material utilizing flexible organic molecule to construct are also rare.This patent selects the flexible bisglyoxaline class ligand 1 that conformation is changeable, 4-pair-(imidazoles-1-base) butane (bbi) and multi-metal oxygen cluster react under hydrothermal conditions, obtain the isopolymolybdate hybrid material of the flexible Organic ligand modification of novel structure.Compared with similar rigid ligand, flexible ligand has the constitutional features of the uniquenesses such as the strong and sterie configuration of plasticity-is changeable, thus provides colourful identification and assembling mode for constructing the Inorganic-Organic Hybrid Material with Novel Topology network structure and physical and chemical performance.
[1]?Kressge?C?T,?Leonowicz?M?E,?Roth?W?J,?et?al.?Ordered?mesoporous?molecular?sieves?synthesized?by?a?liquid-crystal?template?mechanism[J].?Nature,?1992,?359:?710-712.
[2]?Pope?M?T.?Heteropoly?and?Isopoly?Oxometalates[M].Berlin:?Springer,?1983.
[3]?Pope?M?T,?Müller?A.?Polyoxometalate?Chemistry:?An?Old?Field?with?New?Dimensions?in?Several?Disciplines[J].Angew?Chem?Int?Ed,?1991,?30:?34-38.
[4]?Hill?C?L.?Polyoxometalates?in?Medicine[J].?Chem?Rev,?1998,?98(1):?327-358。
Summary of the invention
The present invention relates to Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o(1) compound structure and preparation method thereof.
The present invention relates to the preparation method of (1) compound crystal, the research of take off data and data.
The present invention relates to Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o(1) application of compound in chemical sensor.
For achieving the above object, the invention provides following technical scheme:
There is the isopolymolybdate hybrid material of following chemical general formula:
Isopolymolybdate hybrid material of the present invention, wherein monocrystalline Bruker Smart CCD Apex (II) diffractometer is collected, and adopts Mo-K α (λ=0.71073), room temperature 296 (2) K.SHELX 97 program is used to be resolved by direct method and complete matrix method of least squares and revise crystalline structure.Record predominant crystal data as follows: molecular formula C
36h
48cu
3mo
8n
16o
26, molecular weight 2095.14, monocline, spacer
p-1,a=12.206 (4), b=12.569 (4), c=12.887 (8), α=97.146 (6),
β=111.929 (7), γ=114.063 (4),
v=1582.8 (12)
3, the molecule number 1 in unit cell, specific absorbance (mm
-1) 2.601, weighting factor 1.059, the consistence factor final R1=0.0363 of point diffraction, the consistence factor w of point diffraction
r2
=0.0410.
The present invention further discloses Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o(1) preparation method of compound: take H
3pMo
12o
40nH
2o (0.11g, 0.06mmol), Cu (CH
3cOO)
2h
2o (0.07g, 0.35mmol), Isosorbide-5-Nitrae-bis--(imidazoles-1-base) butane (0.095g, 0.5mmol) and water 6mL mix, and use 0.5mol/LH
2sO
4pH to 5.32 is adjusted with 0.5mol/LnaOH, then 10mL is joined with in teflon-lined stainless steel cauldron, 150 DEG C are heated to from 25 DEG C with the mean rate of 22.5 DEG C/h, constant temperature 82 hours, then be down to 25 DEG C with the mean rate of 11.25 DEG C/h, at the bottom of still, obtain purple powder Polygons bulk crystals.
Accompanying drawing explanation
Fig. 1 is Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o(1) molecular structure (mallet)
Fig. 2 is Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o(1) two-dimensional network structure figure (polyhedron/mallet).
Embodiment
The structure of the flexible ligand-isopolymolybdate hybrid material of copper bridging and preparation method
Its preparation method and condition: take H
3pMo
12o
40nH
2o (0.11g, 0.06mmol), Cu (CH
3cOO)
2h
2o (0.07g, 0.35mmol), Isosorbide-5-Nitrae-bis--(imidazoles-1-base) butane (0.095g, 0.5mmol) and water 6mL mix, and use 0.5mol/LH
2sO
4pH to 5.32 is adjusted with 0.5mol/LnaOH, then 10mL is joined with in teflon-lined stainless steel cauldron, 150 DEG C are heated to from 25 DEG C with the mean rate of 22.5 DEG C/h, constant temperature 82 hours, then be down to 25 DEG C with the mean rate of 11.25 DEG C/h, at the bottom of still, obtain purple powder Polygons bulk crystals.
This crystal records its structure by X-single crystal diffractometer and corresponding software.The research of X-radiocrystallography shows, compound 1 is by [Mo
8o
26]
4-polyoxoanion, Ni metal
, Ni metal
and organic ligand bbi and imidazoles are formed.[Mo
8o
26]
4-bunch by the MoO on 6 altogether limits
6octahedra composition, and present classical α-[Mo
8o
26]
4-structure.Bond valence sum shows that all Mo atoms are in highest oxidation state, and mean value is 6.108, demonstrates all Mo and presents+6 oxidation state.This is consistent with X-ray single crystal diffraction test result.BVS also shows, the mean value of all O atoms is similar to-2 for-1.9.This illustrates that O atoms all on polyanionic is all not protonated.
The Cu of two kinds of coordination environments is had in crystal.Cu1 is monovalence, three-fold coordination tetrahedral configuration, respectively with 2 atom N in 2 bbi molecules and [Mo
8o
26]
4-the oxygen coordination of 1 end.Atoms metal Cu2 is divalence, hexa-coordinate octoploids structure, respectively with 2 atom N in 2 bbi molecules, 2 atom N in 2 imidazole molecules and [Mo
8o
26]
4-the oxygen coordination of 2 ends.Polyoxoanion becomes two-dimensional network structure by Cu2 with bidentate flexible ligand bbi bridging, in addition, polyacid bunch is also connected with Cu1-bbi ligand polymer chain.
In the IR spectrum of compound, at 503.2 cm
-1~ 953.9cm
-1the absorption band occurred in scope is the characteristic peak of molybdenum bunch, wherein 953.9cm
-1and 919.2cm
-1the characteristic peak that place occurs can be summed up as ν in polyanionic (Mo=Ot), the vibration of ν (Mo-O-Mo).At 1099.4cm
-1~ 1635.4cm
-1the absorption band occurred in scope is the characteristic peak of organic ligand bbi, imidazoles, wherein at 1524.9cm
-1and 1448.1cm
-1the absorption peak that place occurs belongs to ν (CH
2) and δ (CH
2), at 1635.4cm
-1, 1246.0cm
-1, 1099.4cm
-1c=N, C-N, C-C absorption band is there is in scope.At 3460.9cm
-1the broad peak at place is the characteristic peak of water molecules.
Embodiment
Take H
3pMo
12o
40nH
2o (0.11g, 0.06mmol), Cu (CH
3cOO)
2h
2o (0.07g, 0.35mmol), Isosorbide-5-Nitrae-bis--(imidazoles-1-base) butane (0.095g, 0.5mmol) and water 6mL mix, and use 0.5mol/LH
2sO
4pH to 5.32 is adjusted with 0.5mol/LnaOH, then 10mL is joined with in teflon-lined stainless steel cauldron, 150 DEG C are heated to from 25 DEG C with the mean rate of 22.5 DEG C/h, constant temperature 82 hours, then be down to 25 DEG C with the mean rate of 11.25 DEG C/h, at the bottom of still, obtain purple powder Polygons bulk crystals.This crystal records its structure by X-single crystal diffractometer and corresponding software.
Claims (4)
1. flexible organic ligand-isopolymolybdate hybrid material of transition metal copper bridging, its chemical formula is Cu
i 2cu
iI(C
10n
4h
14)
3(C
3n
2h)
2[Mo
8o
26] 3H
2o, molecular weight is 2095.14.
2. the flexible organic ligand-isopolymolybdate hybrid material of transition metal copper bridging according to claim 1, wherein monocrystalline Bruker Smart CCD Apex (II) diffractometer is collected, adopt Mo-K α (λ=0.71073), room temperature 296 (2) K, use SHELX 97 program resolved by direct method and complete matrix method of least squares and revise crystalline structure, record predominant crystal data as follows: molecular formula C
36h
48cu
3mo
8n
16o
26, molecular weight 2095.14, monocline, spacer
p-1,a=12.206 (4), b=12.569 (4), c=12.887 (8), α=97.146 (6),
β=111.929 (7), γ=114.063 (4),
v=1582.8 (12)
3, the molecule number 1 in unit cell, specific absorbance (mm
-1) 2.601, weighting factor 1.059, the consistence factor final R1=0.0363 of point diffraction, the consistence factor w of point diffraction
r2
=0.0410.
3. prepare a method for the flexible organic ligand-isopolymolybdate hybrid material of transition metal copper bridging described in claim 1, it is characterized in that: take H
3pMo
12o
40nH
2o (0.11g, 0.06mmol), Cu (CH
3cOO)
2h
2o (0.07g, 0.35mmol), Isosorbide-5-Nitrae-bis--(imidazoles-1-base) butane (0.095g, 0.5mmol) and water 6mL mix, and use 0.5mol/LH
2sO
4pH to 5.32 is adjusted with 0.5mol/LnaOH, then 10mL is joined with in teflon-lined stainless steel cauldron, 150 DEG C are heated to from 25 DEG C with the mean rate of 22.5 DEG C/h, constant temperature 82 hours, then be down to 25 DEG C with the mean rate of 11.25 DEG C/h, at the bottom of still, obtain purple powder Polygons bulk crystals.
4. the application being prepared in electrochemical sensor and luminescent material aspect of the flexible organic ligand-isopolymolybdate hybrid material of transition metal copper bridging described in claim 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153203A (en) * | 2015-08-28 | 2015-12-16 | 太原科技大学 | Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof |
| US20230173469A1 (en) * | 2021-12-03 | 2023-06-08 | Changzhou University | Isopoly-molybdic acid coordination polymer catalyst, method of manufacturing the same and application thereof |
Citations (1)
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|---|---|---|---|---|
| CN103360424A (en) * | 2013-07-03 | 2013-10-23 | 吉林化工学院 | Structure of multi-metal phosphomolybdate organic-inorganic hybrid and preparation method |
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2014
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103360424A (en) * | 2013-07-03 | 2013-10-23 | 吉林化工学院 | Structure of multi-metal phosphomolybdate organic-inorganic hybrid and preparation method |
Non-Patent Citations (3)
| Title |
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| KAN W Q. ET AL: ""pH-Dependent assembly of two octamolybdate hybrid materials: A self-threading CdSO4-type framework and a 3D 4-connected framework"", 《CRYSTENGCOMM》 * |
| ZHANG C J. ET AL: ""Tailoring microstructures of isopolymolybdates: regular tuning of the ligand spacer length and metal coordination preferences"", 《DALTON TRANSACTIONS》 * |
| 丁艳等: ""基于八钼酸盐杂化网络的离子热合成、晶体结构和光催化性质"", 《高等学校化学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105153203A (en) * | 2015-08-28 | 2015-12-16 | 太原科技大学 | Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof |
| US20230173469A1 (en) * | 2021-12-03 | 2023-06-08 | Changzhou University | Isopoly-molybdic acid coordination polymer catalyst, method of manufacturing the same and application thereof |
| US11878288B2 (en) * | 2021-12-03 | 2024-01-23 | Changzhou University | Isopoly-molybdic acid coordination polymer catalyst, method of manufacturing the same and application thereof |
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Application publication date: 20150107 |