CN103360424A - Structure of multi-metal phosphomolybdate organic-inorganic hybrid and preparation method - Google Patents

Structure of multi-metal phosphomolybdate organic-inorganic hybrid and preparation method Download PDF

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Publication number
CN103360424A
CN103360424A CN2013102747931A CN201310274793A CN103360424A CN 103360424 A CN103360424 A CN 103360424A CN 2013102747931 A CN2013102747931 A CN 2013102747931A CN 201310274793 A CN201310274793 A CN 201310274793A CN 103360424 A CN103360424 A CN 103360424A
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bbi
organic
phosphomolybdate
thing
pmo
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曲小姝
杨艳艳
谭乃迪
金星
金刚
杨艳俊
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Jilin Institute of Chemical Technology
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Jilin Institute of Chemical Technology
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Abstract

The invention relates to a single-crystal structure of a multi-metal phosphomolybdate organic-inorganic hybrid and a preparation method. A chemical formula of the crystal is [PMo12O40]2(bbi)3 (bbi represents 1,4-diimidazole butane), and molecular weight is 2110.56; the crystal belongs to a triclinic system, the space group is P-1, and lattice parameters are as follows: a=11.8360(9) angstroms, b=12.0932(10) angstroms, c=17.7728(15) angstroms, alpha=74.0890(10) DEG, beta=70.9490(10) DEG, gamma=71.8160(10) DEG, V=2242.1(3) angstrom 3, and Z=2. The hybrid is prepared through hydro-thermal synthesis technology. The prepared compound is clear in composition and structure, being a solid material with a potential application value.

Description

Structure and the preparation method of the organic-inorganic hybridized thing of a kind of many metals phosphomolybdate
Affiliated technical field
The invention belongs to inorganic polyoxometallate technical field of chemistry, relate to the synthetic of the organic-inorganic hybridized thing of many metals phosphomolybdate, say so more specifically [PMo 12O 40] 2(bbi) 3Preparation method and the structure of (bbi=Isosorbide-5-Nitrae-two imidazolyl butane) compound.
Background technology
Materials science is the forward position of current scientific research, the exploitation of novel material has caused chemist and material scholar's extensive concern with development, particularly in recent years along with high-tech fast development, synthetic have novel texture and new functional materials has become the essential of social development.In the research of novel material, shown unique advantage take polyoxometallate as main solid material at aspects such as light, electricity, magnetic and catalytic performances.The research of synthesizing, preparing and assembling of this class inorganic materials will have extremely profound significance to the creation exploitation of new species, novel material [1,2]Meanwhile, based on polyacid building block and flexible ligand inorganic-research of organic Hybrid Materials become an extremely important part of new function material, its development more and more is subject to chemist and material scholar's attention.This patent adopts flexible organic ligand bbi and many metals phosphomolybdate to construct an organic-inorganic hybrid [PMo 12O 40] 2(bbi) 3, utilize X-ray single crystal diffraction and infrared spectra that its structure is characterized, next step will continue research its electrochemical properties, fluorescence property and catalytic performance, expect that it has using value in the solid material field.
Reference
[1] Jin Yanan. take the hybrid inorganic-organic materials [D] of polyoxometallate as constructing piece. Zhengzhou: He'nan University, 2008.
[2] Shi Zhenyu, Peng Jun. Magnetic Properties of Three-Dimensional Supramolecular Complex compound (H 2Bimb) 2(SiW 12O 40) Hydrothermal Synthesis and crystalline structure [J]. molecular science journal, 2011,27 (3): 161-165.
Summary of the invention
The present invention relates to [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane) (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 [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane) (1) compound application aspect solid material.
For achieving the above object, the invention provides following technical scheme:
The organic-inorganic hybridized thing of many metals phosphomolybdate with following chemical general formula: [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane)
The organic-inorganic hybridized thing of many metals phosphomolybdate of the present invention, wherein monocrystalline is collected with Bruker Smart CCD Apex (II) diffractometer, adopt Mo-K α (λ=0.71073), room temperature 296 K, use SHELX 97 programs to resolve and the correction crystalline structure by direct method and complete matrix method of least squares, record main crystal data as follows: chemical formula is [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane), molecular weight is 2110.56, belongs to triclinic(crystalline)system, spacer P-1, unit cell parameters a=11.8360 (9), b=12.0932 (10), c=17.7728 (15), α=74.0890 (10), β=70.9490 (10), γ=71.8160 (10), V=2242.1 (3) 3, Z=2, R1=0.035, wR2=0.0468.
The present invention further discloses [PMo 12O 40] 2(bbi) 3The preparation method of (bbi=Isosorbide-5-Nitrae-two imidazolyl butane) (1) compound: with K 6[α-P 2W 18O 62] nH 2O (0.32g, 0.07mmol), CoCl 2(0.12g, 0.12 mmol), bbi (0.12g, 0.63mmol) and water 6mL mixing, transfer pH to 3.5～4.5 with rare HCl, dilute NaOH solution, then join 10mL with in the teflon-lined stainless steel cauldron, be heated to 160 ° of C from 25 ° of C, constant temperature 82 hours with the mean rate of 22.5 ° of C/h, then be down to 25 ° of C with the mean rate of 11.25 ° of C/h, at the bottom of still, get yellow tetragon crystal.
Description of drawings
Fig. 1 is [PMo 12O 40] 2(bbi) 3The molecular structure of (bbi=Isosorbide-5-Nitrae-two imidazolyl butane) (1).
Fig. 2 is [PMo 12O 40] 2(bbi) 3The Magnetic Properties of Three-Dimensional Supramolecular Complex structure iron (polyhedron/bat) of (bbi=Isosorbide-5-Nitrae-two imidazolyl butane) (1).
Embodiment
Organic-inorganic hybridized thing [the PMo of a kind of many metals phosphomolybdate 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane) and preparation method thereof and condition: with K 6[α-P 2W 18O 62] nH 2O (0.32g, 0.07mmol), CoCl 2(0.12g, 0.12 mmol), bbi (0.12g, 0.63mmol) and the mixing of 6mL water, transfer pH to 3.5～4.5 with rare HCl, dilute NaOH solution, then join 10mL with in the teflon-lined stainless steel cauldron, be heated to 160 ° of C from 25 ° of C, constant temperature 82 hours with the mean rate of 22.5 ° of C/h, then be down to 25 ° of C with the mean rate of 11.25 ° of C/h, at the bottom of still, get yellow tetragon crystal.
This crystal records its structure by X-single crystal diffractometer and corresponding software.The X-radiocrystallography studies show that, compound 1 is by α -Polyanionic [the PMo of Keggin structure 12O 40] 3-Consist of with protonated bbi positively charged ion.Polyanionic [PMo 12O 40] 3-Between be connected to form one-dimensional chain by end oxygen hydrogen bond action, infinitely extend at the b direction of principal axis; Pass through the flexible organic ligand bbi of bidentate and polyanionic [PMo between the one-dimensional chain 12O 40] 3-The hydrogen bond of upper end oxygen is connected to form in the unlimited two-dimentional corrugated layer of extending of c-axis direction; Pass through again polyanionic [PMo between the two-dimensional layer 12O 40] 3-On end oxygen hydrogen bond action connect, form the Magnetic Properties of Three-Dimensional Supramolecular Complex structure in a direction of principal axis infinite expanding.
Compound [PMo 12O 40] 2(bbi) 3The IR collection of illustrative plates at 1062.1,963.8,886.4,795.7 cm -1The strong absorption peak at place is attributed to respectively same polyanionic [PMo 12O 40] 3-Middle ν (P=O a), ν (Mo-O d), ν (Mo-O b-Mo) and ν (Mo-O c-Mo) the stretching vibration of key.At 1273.2cm -1～1635.2cm -1C=N, C-N appear in the place, C-C absorption band is the characteristic peak of organic ligand bbi.
Embodiment
With K 6[α-P 2W 18O 62] nH 2O (0.32g, 0.07mmol), CoCl 2(0.12g, 0.12 mmol), bbi (0.12g, 0.63mmol) and the mixing of 6mL water, transfer pH to 3.5～4.5 with rare HCl, dilute NaOH solution, then join 10mL with in the teflon-lined stainless steel cauldron, be heated to 160 ° of C from 25 ° of C, constant temperature 82 hours with the mean rate of 22.5 ° of C/h, then be down to 25 ° of C with the mean rate of 11.25 ° of C/h, at the bottom of still, get yellow tetragon crystal.This crystal records its structure by X-single crystal diffractometer and corresponding software.

Claims (4)

1. the organic-inorganic hybridized thing of metal phosphomolybdate more than a kind, its chemical formula is [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane), molecular weight is 2110.56.
2. the organic-inorganic hybridized thing of many metals phosphomolybdate claimed in claim 1, wherein monocrystalline is collected with Bruker Smart CCD Apex (II) diffractometer, adopt Mo-K α (λ=0.71073), room temperature 296 K, use SHELX 97 programs to resolve and the correction crystalline structure by direct method and complete matrix method of least squares, record main crystal data as follows: chemical formula is [PMo 12O 40] 2(bbi) 3(bbi=Isosorbide-5-Nitrae-two imidazolyl butane), molecular weight is 2110.56, belongs to triclinic(crystalline)system, spacer P-1, unit cell parameters a=11.8360 (9), b=12.0932 (10), c=17.7728 (15), α=74.0890 (10), β=70.9490 (10), γ=71.8160 (10), V=2242.1 (3) 3, Z=2, R1=0.035, wR2=0.0468.
3. a method for preparing the organic-inorganic hybridized thing of the described many metals phosphomolybdate of claim 1 is characterized in that: with K 6[α-P 2W 18O 62] nH 2O (0.32g, 0.07mmol), CoCl 2(0.12g, 0.12 mmol), bbi (0.12g, 0.63mmol) and the mixing of 6mL water, transfer pH to 3.5～4.5 with rare HCl, dilute NaOH solution, then join 10mL with in the teflon-lined stainless steel cauldron, be heated to 160 ° of C from 25 ° of C, constant temperature 82 hours with the mean rate of 22.5 ° of C/h, then be down to 25 ° of C with the mean rate of 11.25 ° of C/h, at the bottom of still, get yellow tetragon crystal.
4. the application of the organic-inorganic hybridized thing preparation of the described many metals phosphomolybdate of claim 1 aspect solid material.
CN2013102747931A 2013-07-03 2013-07-03 Structure of multi-metal phosphomolybdate organic-inorganic hybrid and preparation method Pending CN103360424A (en)

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CN104262364A (en) * 2014-09-03 2015-01-07 吉林化工学院 Copper-bridged flexible ligand-isopolymolybdate hybrid material structure and preparation method thereof
CN106948009A (en) * 2017-05-24 2017-07-14 合肥学院 A kind of molybdenum copper crystalloid material of organic inorganic hybridization and preparation method thereof
CN107130297A (en) * 2017-05-24 2017-09-05 合肥学院 Silver-colored crystalloid material of the molybdenum of a kind of organic inorganic hybridization and preparation method thereof
CN107141259A (en) * 2017-05-12 2017-09-08 昆明学院 A kind of imidazoles with many wolframic acid cocrystallization super molecular compounds and preparation method thereof
CN107652327A (en) * 2017-10-30 2018-02-02 济南大学 A kind of preparation method of more molybdophosphate azacyclo- salt super molecular compounds
CN107827932A (en) * 2017-10-30 2018-03-23 济南大学 A kind of more molybdophosphate azacyclo- salt super molecular compounds
CN107884464A (en) * 2017-10-30 2018-04-06 济南大学 A kind of preparation method of more molybdophosphate azacyclo- salt super molecular compound modified electrodes

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104262364A (en) * 2014-09-03 2015-01-07 吉林化工学院 Copper-bridged flexible ligand-isopolymolybdate hybrid material structure and preparation method thereof
CN107141259A (en) * 2017-05-12 2017-09-08 昆明学院 A kind of imidazoles with many wolframic acid cocrystallization super molecular compounds and preparation method thereof
CN106948009A (en) * 2017-05-24 2017-07-14 合肥学院 A kind of molybdenum copper crystalloid material of organic inorganic hybridization and preparation method thereof
CN107130297A (en) * 2017-05-24 2017-09-05 合肥学院 Silver-colored crystalloid material of the molybdenum of a kind of organic inorganic hybridization and preparation method thereof
CN107652327A (en) * 2017-10-30 2018-02-02 济南大学 A kind of preparation method of more molybdophosphate azacyclo- salt super molecular compounds
CN107827932A (en) * 2017-10-30 2018-03-23 济南大学 A kind of more molybdophosphate azacyclo- salt super molecular compounds
CN107884464A (en) * 2017-10-30 2018-04-06 济南大学 A kind of preparation method of more molybdophosphate azacyclo- salt super molecular compound modified electrodes
CN107884464B (en) * 2017-10-30 2020-02-18 济南大学 Preparation method of multi-molybdophosphoric acid-nitrogen heterocyclic salt supermolecular compound modified electrode

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