CN102731537A - Zinc furandicarboxylate metal-organic framework with interpenetration structure and preparation method thereof - Google Patents
Zinc furandicarboxylate metal-organic framework with interpenetration structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a zinc furandicarboxylate metal-organic framework with an interpenetration structure and a preparation method thereof. The chemical formula of the framework is [Zn.(C6O5H2).C5H4N2].2H2O. The framework is synthesized by using a hydrothermal method with 2,5-furandicarboxylic acid as a main ligand, 4,4-dipyridine as an auxiliary ligand and zinc ions as nodes. Two ZnO3N2 form two pyramid-like 6-c nodes, a pair of 4,4-dipyridine are located at two ends, four 2,5-furandicarboxylic acid are located at central positions, and two (4,6)-meshes form the interpenetration structure due to occurrence of slip. The framework has a structure as described in the specification. The average pore size of the framework is 4.024 A degrees. The framework is applicable to the technical field of catalysis.
Description
Technical field
The present invention relates to a kind of furans dioctyl phthalate zinc metal-organic framework materials and preparation method with interspersed structure.
Technical background
Because existing covalent linkage, co-ordination bond in the metal-organic framework materials; Comprise intermolecular weak force again; On compound method, be imbued with designability; And research contents relates to organic chemistry (through methodology of organic synthesis structure part), coordination chemistry (organic ligand and metal junctions are synthesized title complex), physical chemistry (to the experiment and the theoretical investigation of non covalent bond reactive force), biological chemistry (the beginning process of all substrate identifications, bonding) and crystal engineering etc.; Therefore ligand polymer often shows some unique chemical, physical properties, good prospects for application [2] is all arranged in nonlinear optical material, magneticsubstance, absorption, luminous, superconducting material and catalysis etc. aspect many.
Early stage A.F.Wells is reduced to a series of nodes with the mineral crystal structure according to their topological framework, and is connected to form special geometric configuration [3,4] with other node of fixed number on every side.
1989, R.Robson was extended to the ligand polymer field with the work of Wells in inorganic network structure in paper " Infinite polymeric framework consisting of three-dimensinal linked rod-like segments "; And propose following imagination: the structure with some simple mineral is the network prototype; The branch submodule of going up coupling with how much replaces the node in the network structure, replaces the single chemical bond in its prototype network with the molecule link, constructs the ligand polymer with mineral topological framework with this; And successfully synthesized by 4; 4 ', 4 ", 4 " '-four cyano phenylmethane and Cu
+The cuprous cyanic acid ligand polymer [5] with diamond topology of constructing.The Fujita of Japan in 1994 finds by Cd (NO
3)
2With 4, (4,4 '-bpy) at H for 4 '-dipyridyl
2[Cd (4,4 '-bpy) for the ligand polymer with two-dimensional square lattice network structure that makes in the O-EtOH mixed solvent
2(H
2O)
2] (NO
3)
2Have good catalytic activity, can quicken cyanic acid methane glycosylation reaction [6].Nineteen ninety-five, the Moore of the U.S. has reported Ag on Nature
+With 2,4, the three-dimensional coordination polymer with cellular skeleton structure [7] that 6-three (to the cyano-phenyl ethynyl) benzene forms, this compound biologically active can promote cell to increase.In the same year, O.M.Yaghi study group has proposed on Nature through selecting appropriate rigidity organic ligand and metals ion to construct the metal-organic framework structured material, and this type material can adsorb guest molecule, is sloughing guest molecule back skeleton constant [8].This study group has synthesized very representative MOFs series ligand polymer afterwards, becomes the milestone [9] on the ligand polymer development history.
Reference:
[1]M.Eddaoudi，D.B.Moler，H.L.Li，B.L.Chen，T.M.Reineke，M.O’Keeffe，O.M.Yaghi，“Modular?Chemistry：Secondary?Building?Units?as?a?Basis?for?the?Design?of?Highly?Porous?and?Robust?Metal-Organic?Carboxylate?Frameworks”，Acc.Chem.Res.，2001，34，319-330.
[2]P.Dechambenoit?and?J.R.Long，“Microporous?magnets”，Chem.Soc.Rev.，2010，132，18115-18126.
[3]A.F.Wells，“Three?Dimensional?Nets?and?Polyhedra”，New?York，1977.
[4]A.F.Wells，“Structrual?Inorganic?Chemistry”，5
th?ed.，Oxford?Univ.Press，1983.
[5]F.Hoskins，R.Robson，“Infinite?polymeric?frameworks?consisting?of?three?dimensionally?linked?rod-like?segments”，J.Am.Chem.Soc.，1989，111，5962-5964.
[6]M.Fujita，Y.J.Kwon，M.Miyazawa，K.Ogura，“One-dimensional?coordinate?polymer?involving?heptacoordinate?cadmium(II)?ions”，Chem.Commun.，1994，1977-1978.
[7]G.B.Gardner，D.Venkaraman，J.S.Moore，S.Lee，“Spontaneous?assembly?of?a?hinged?coordination?network”，Nature，1995，374，792-794.
[8]O.M.Yaghi，G.M.Li，H.L.Li，“Selective?binding?and?removal?of?guests?in?a?microporous?metal-organic?framework”，Nature，1995，378，703-706.
[9]H.Li，M.Eddaoudi，M.O’keeffe，O.M.Yaghi，“Design?and?synthesis?of?an?exceptionally?stable?and?highly?porous?metal-organic?framework”，Nature，1999，402，276-279.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure.
A kind of furans dioctyl phthalate zinc metal-organic framework materials with interspersed structure, its chemical formula is [Zn (C
6O
5H
2) C
5H
4N
2] 2H
2O belongs to rhombic system, Pcc2 spacer, unit cell parameters a=18.298 (4)
B=11.405 (2)
C=15.185 (3)
α=90 °, β=90 °, γ=90 °, μ=1.582 unit cell volume V=3168.9 (1)
Z=4, Dc=1.595Mg/m
3This framework material is two ZnO
3N
2Form two triangular pyramidal 6-c nodes, a pair of 4, the 4-dipyridyl is positioned at two ends, and four 2,5-furans dioctyl phthalate is positioned at the mid-way, and two (4,6)-nets intert mutually, have formed the metal-organic framework materials with interspersed structure; Its structure is as shown in Figure 1.
A kind of preparation method with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure of the present invention comprises the steps and condition: according to proportioning, add ethanol and N; The mixed solvent that dinethylformamide is formed under agitation adds zinc source, main part, inferior part in order, stirred 5 hours, and polytetrafluoroethyllining lining is put into reaction kettle; 90 ℃ of isothermal reactions are 24 hours then; Take out cool to room temperature, drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1～3: 0.5～2: 0.5～2: 50～70: 20～40; Described zinc source is zinc oxide, zinc hydroxide, zinc chloride or zinc nitrate hexahydrate; Described main part is 2, and 5-furans dioctyl phthalate, inferior part are 4, the 4-dipyridyl.
With following instrument and method product is characterized:
1. select a perfect crystal and be used for the single crystal structure analysis, the single crystal diffraction data are collected on Rigaku R-AXIS RAPID diffractometer, with MoK alpha-ray (λ=0.71073 of graphite monochromator monochromatization
), belonging to rhombic system, spacer is pcc2, unit cell parameters: a=18.298 (4)
B=11.405 (2)
C=15.185 (3)
α=90 °, β=90 °, γ=90 °, V=3168.9 (1)
Z=4, Dc=1.595Mg/m
3, μ=1.582mm
-1, R
1=0.0927.Monocrystalline data and parameter are seen table 1,2.
A kind of two (4,6)-reticulated structure figure crystalline structure that intert mutually with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure of the present invention are seen Fig. 1.A kind of furans dioctyl phthalate zinc metal-organic framework materials topology diagram with interspersed structure of the present invention is seen Fig. 2.Fig. 1, Fig. 2 draw by Diamond2.1 software.
2. use Pyris Diamond TG/DTA analyser that product is carried out thermogravimetric analysis; Example weight 4.2mg; TR: 30～700 ℃, temperature rise rate: 10 ℃/min, a kind of furans dioctyl phthalate zinc metal-organic framework materials thermogravimetric analysis figure with interspersed structure of the present invention sees Fig. 3.This metal-organic framework materials is divided into from 150 ℃ to 450 ℃ slowly and rapid two stage weightlessness, 150 ℃ to 450 ℃ weightlessness 62.8% (2,5-furans dioctyl phthalate and 4,4-dipyridyl).
Beneficial effect: the present invention has obtained first and has had the furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure, and this framework material is two ZnO
3N
2Form two triangular pyramidal 6-c nodes, a pair of 4, the 4-dipyridyl is positioned at two ends, and four 2,5-furans dioctyl phthalate is positioned at the mid-way, and two (4,6)-nets intert mutually, have formed the metal-organic framework materials with interspersed structure.The mean pore size of this compound be 4.024
can be applied to catalysis technical field.
Description of drawings
Fig. 1 is a kind of two (4,6)-reticulated structure figure that intert mutually with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure of the present invention.
Fig. 2 is a kind of furans dioctyl phthalate zinc metal-organic framework materials topology diagram with interspersed structure of the present invention.
Fig. 3 is a kind of furans dioctyl phthalate zinc metal-organic framework materials thermogravimetric analysis figure with interspersed structure of the present invention.
Embodiment
Embodiment 1 takes out the polytetrafluoroethyllining lining of reaction kettle and is placed on the magnetic stirring apparatus, is to add ethanol and N at 56: 32 according to mol ratio, and the mixed solvent that dinethylformamide is formed under agitation adds zinc nitrate hexahydrate 2mmol in order; 2,5-furans dioctyl phthalate 1mmol, 4,4-dipyridyl 1mmol; Stirred 5 hours, polytetrafluoroethyllining lining is put into reaction kettle, 90 ℃ of isothermal reactions are 24 hours then; Take out cool to room temperature, drying obtains title product;
Use following instrument and method that product is characterized:
1. select a perfect crystal and be used for the single crystal structure analysis, the single crystal diffraction data are collected on Rigaku R-AXIS RAPID diffractometer, with MoK alpha-ray (λ=0.71073 of graphite monochromator monochromatization
), belonging to rhombic system, spacer is pcc2, unit cell parameters: a=18.298 (4)
B=11.405 (2)
C=15.185 (3)
α=90 °, β=90 °, γ=90 °, V=3168.9 (1)
Z=4, Dc=1.595Mg/m
3, μ=1.582mm
-1, R
1=0.0927.Monocrystalline data and parameter are seen table 1,2, and crystalline structure is seen Fig. 1-2 (drafting of Diamond2.1 software).
2. use Pyris Diamond TG/DTA analyser that product is carried out thermogravimetric analysis, example weight 4.2mg, TR: 30～700 ℃, temperature rise rate: 10 ℃/min, see Fig. 4.This metal-organic framework materials is divided into from 150 ℃ to 450 ℃ slowly and rapid two stage weightlessness, 150 ℃ to 450 ℃ weightlessness 62.8% (2,5-furans dioctyl phthalate and 4,4-dipyridyl).
Table 1: monocrystalline data
Table 2: atomic coordinate and equivalence are respectively to displacement parameter
Condition such as the table 3 of embodiment 2-8, remaining is with embodiment 1.
Table 3
Preparing method of the present invention comprises the steps and condition: according to proportioning, add ethanol and N, the mixed solvent that dinethylformamide is formed; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, then 90-120 ℃ isothermal reaction 24-96 hour, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1～3: 0.5～2: 0.5～2: 50～70: 20～40; Described zinc source is zinc oxide, zinc hydroxide, zinc chloride or zinc nitrate hexahydrate; Described main part is 2, and 5-furans dioctyl phthalate, inferior part are 4, the 4-dipyridyl.
Claims (9)
1. the furans dioctyl phthalate zinc metal-organic framework materials with interspersed structure is characterized in that its chemical formula is [Zn (C
6O
5H
2) C
5H
4N
2] 2H
2O belongs to rhombic system, Pcc2 spacer, unit cell parameters a=18.298 (4)
B=11.405 (2)
C=15.185 (3)
α=90 °, β=90 °, γ=90 °, μ=1.582 unit cell volume V=3168.9 (1)
Z=4, Dc=1.595Mg/m
3This compound is two ZnO
3N
2Form two triangular pyramidal 6-c nodes, a pair of 4, the 4-dipyridyl is positioned at two ends, and four 2,5-furans dioctyl phthalate is positioned at the mid-way, and two (4,6)-nets intert mutually, have formed the metal-organic framework materials with interspersed structure; Its structure is following:
2. according to the said a kind of preparation method of claim 1, it is characterized in that, comprise the steps and condition: be placed on the taking-up of the polytetrafluoroethyllining lining of reaction kettle on the magnetic stirring apparatus with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; According to proportioning; In polytetrafluoroethyllining lining, add mixed solvent, under agitation add zinc source, main part, inferior part in order, stirred 5 hours, polytetrafluoroethyllining lining is put into reaction kettle; Then 90-120 ℃ isothermal reaction 24-96 hour; Take out cool to room temperature, drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1～3: 0.5～2: 0.5～2: 50～70: 20～40; Described zinc source is zinc oxide, zinc hydroxide, zinc chloride or zinc nitrate hexahydrate; Described main part is 2, and 5-furans dioctyl phthalate, inferior part are 4, the 4-dipyridyl; Described mixed solvent is to be 50～70: 20～40 by ethanol and N according to mol ratio, and dinethylformamide is formed.
3. according to the said a kind of preparation method of claim 2 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 56: 32; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 90 ℃ of isothermal reactions are 24 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 2: 1: 1: 56: 32; Described zinc source is a zinc nitrate hexahydrate; Described main part is 2, and 5-furans dioctyl phthalate, inferior part are 4, the 4-dipyridyl.
4. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 56: 32; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 90 ℃ of isothermal reactions are 24 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 2: 1: 0.5: 56: 32; Remaining is with claim 3.
5. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 50: 20; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 100 ℃ of isothermal reactions are 48 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1: 2: 1.5: 50: 20; Described zinc source is a zinc oxide; Remaining is with claim 3.
6. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 70: 20; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 90 ℃ of isothermal reactions are 72 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 3: 1.5: 2: 70: 20; Described zinc source is a zinc hydroxide; Remaining is with claim 3.
7. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 50: 40; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 120 ℃ of isothermal reactions are 24 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1.5: 0.5: 2: 50: 40; Described zinc source is a zinc nitrate hexahydrate; Remaining is with claim 3.
8. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 56: 32; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 120 ℃ of isothermal reactions are 72 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 1.5: 2: 1: 56: 32; Described zinc source is a zinc chloride; Remaining is with claim 3.
9. according to the said a kind of preparation method of claim 3 with furans dioctyl phthalate zinc metal-organic framework materials of interspersed structure; It is characterized in that, comprise the steps and condition: according to mol ratio is to add ethanol and N, the mixed solvent that dinethylformamide is formed at 56: 32; Under agitation add zinc source, main part, inferior part in order, stirred 5 hours; Polytetrafluoroethyllining lining is put into reaction kettle, and 120 ℃ of isothermal reactions are 72 hours then, take out cool to room temperature; Drying obtains title product; Described zinc source: main part: inferior part: ethanol: N, the mol ratio of dinethylformamide is 2: 1: 1.5: 56: 32; Described zinc source is a zinc oxide; Remaining is with claim 3.
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| CN106432342A (en) * | 2016-09-18 | 2017-02-22 | 长春工业大学 | Furan dioctyl phthalate manganese metal organic skeleton material and preparation method |
| CN109942606A (en) * | 2019-04-28 | 2019-06-28 | 北京石油化工学院 | A kind of 3,3- bipyridyl Zn complex and the preparation method and application thereof |
| CN109970772A (en) * | 2019-04-28 | 2019-07-05 | 北京石油化工学院 | A kind of 3,3- bipyridyl complex and the preparation method and application thereof |
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| US20110319604A1 (en) * | 2008-11-18 | 2011-12-29 | Universite De Versailles-Saint Quentin En Yvelines | Method for preparing metal-organic framework crystallised and porous aluminium aromatic azocarboxylates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106432342A (en) * | 2016-09-18 | 2017-02-22 | 长春工业大学 | Furan dioctyl phthalate manganese metal organic skeleton material and preparation method |
| CN109942606A (en) * | 2019-04-28 | 2019-06-28 | 北京石油化工学院 | A kind of 3,3- bipyridyl Zn complex and the preparation method and application thereof |
| CN109970772A (en) * | 2019-04-28 | 2019-07-05 | 北京石油化工学院 | A kind of 3,3- bipyridyl complex and the preparation method and application thereof |
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