CN105566362A - Furan dicarboxylic acid and metal cadmium organic framework material and preparation method - Google Patents
Furan dicarboxylic acid and metal cadmium organic framework material and preparation method Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 25
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- DNXDYHALMANNEJ-UHFFFAOYSA-N furan-2,3-dicarboxylic acid Chemical compound OC(=O)C=1C=COC=1C(O)=O DNXDYHALMANNEJ-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910052751 metal Inorganic materials 0.000 title abstract description 5
- 239000002184 metal Substances 0.000 title abstract description 5
- 239000013384 organic framework Substances 0.000 title abstract description 3
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 27
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 7
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims abstract description 5
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 claims description 40
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 32
- -1 furandicarboxylic acid cadmium Chemical compound 0.000 claims description 23
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical group Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 230000004580 weight loss Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 239000003446 ligand Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical compound C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005260 alpha ray Effects 0.000 description 2
- 238000012926 crystallographic analysis Methods 0.000 description 2
- 238000002447 crystallographic data Methods 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SUSQOBVLVYHIEX-UHFFFAOYSA-N phenylacetonitrile Chemical compound N#CCC1=CC=CC=C1 SUSQOBVLVYHIEX-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- 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
- C07F3/08—Cadmium compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a furan dicarboxylic acid and metal cadmium organic framework material and a preparation method. The compound is a complex formed by furan dicarboxylic acid and metal cadmium for the first time, an asymmetric unit is composed of three divalent cadmium ions, four furan dicarboxylic acid negative ions, four ionized dimethylamine positive ions and a DMF solvent molecule. The dimethylamine positive ions are formed by decomposing a DMF molecule at a high temperature, and frameworks similar to the metal organic frameworks with solvolyte contained in crystals are rarely seen. The compound comprises an infinite chain-shaped structure formed by linear trinuclear secondary structural units and secondary structural units. The metal organic framework material of a network structure is formed. The material can be used for gas separation, carbon dioxide adsorption and other aspects.
Description
Technical field
The present invention relates to a kind of furandicarboxylic acid cadmium metal organic framework material and preparation method.
Background technology
Due to covalent linkage existing in metal-organic framework materials, coordinate bond, comprise molecular weak interaction again, synthetic method is imbued with designability, and research contents relates to organic chemistry (constructing part by methodology of organic synthesis), coordination chemistry (organic ligand becomes title complex with melts combine), physical chemistry (experiment and theoretical investigation to non covalent bond reactive force), biological chemistry (all substrate identification, the beginning process of bonding) and crystal engineering etc., therefore ligand polymer often shows the chemistry of some uniquenesses, physical properties, at nonlinear optical material, magneticsubstance, absorption, luminous, all many-sides such as superconducting material and catalysis have good application prospect [2].
Inorganic crystal structure is reduced to a series of node according to their topological framework by early stage A.F.Wells, and is connected to form special geometric configuration [3,4] with other node of around fixed number.
1989, R.Robson is in paper " Infinitepolymericframeworkconsistingofthree-dimensinalli nkedrod-likesegments ", the work of Wells in inorganic network structure is extended to ligand polymer field, and following imagination is proposed: with some simple monomineralic structures for web original, the node in network structure is replaced with the molecular modules geometrically mated, the single chemical bond in its prototype network is replaced with molecule link, the ligand polymer with mineral topological framework is constructed with this, and successfully synthesized by 4, 4 ', 4 ' ', 4 ' ' '-four cyano phenylmethane and Cu
+the cuprous cyano group ligand polymer [5] with diamond topology of constructing.The Fujita of Japan in 1994 finds by Cd (NO
3)
2with 4,4'-Bipyridine (4,4 '-bpy) at H
2ligand polymer [the Cd (4,4 '-bpy) with two-dimensional square lattice network structure obtained in O-EtOH mixed solvent
2(H
2o)
2] (NO
3)
2there is good catalytic activity, the silylating reaction of cyano group [6] can be accelerated.Nineteen ninety-five, the Moore of the U.S. reports Ag on Nature
+the three-dimensional coordination polymer [7] with cellular skeleton structure formed with 2,4,6-tri-(to cyanophenylethynyl) benzene, this compound has biological activity, can promote that cell increases.In the same year, O.M.Yaghi study group proposes by selecting suitable rigidity organic ligand and metal ion to construct metal-organic framework structured material on Nature, and this kind of 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 a milestone [9] in ligand polymer development history.Metal-organic framework materials develops by leaps and bounds, and metal-organic framework materials constantly novel is again found.
Reference:
[1]M.Eddaoudi,D.B.Moler,H.L.Li,B.L.Chen,T.M.Reineke,M.O’Keeffe,O.M.Yaghi,“ModularChemistry:SecondaryBuildingUnitsasaBasisfortheDesignofHighlyPorousandRobustMetal-OrganicCarboxylateFrameworks”,Acc.Chem.Res.,2001,34,319-330.
[2]P.DechambenoitandJ.R.Long,“Microporousmagnets”,Chem.Soc.Rev.,2010,132,18115-18126.
[3]A.F.Wells,“ThreeDimensionalNetsandPolyhedra”,NewYork,1977.
[4]A.F.Wells,“StructrualInorganicChemistry”,5
thed.,OxfordUniv.Press,1983.
[5]F.Hoskins,R.Robson,“Infinitepolymericframeworksconsistingofthreedimensionallylinkedrod-likesegments”,J.Am.Chem.Soc.,1989,111,5962-5964.
[6]M.Fujita,Y.J.Kwon,M.Miyazawa,K.Ogura,“One-dimensionalcoordinatepolymerinvolvingheptacoordinatecadmium(II)ions”,Chem.Commun.,1994,1977-1978.
[7]G.B.Gardner,D.Venkaraman,J.S.Moore,S.Lee,“Spontaneousassemblyofahingedcoordinationnetwork”,Nature,1995,374,792-794.
[8]O.M.Yaghi,G.M.Li,H.L.Li,“Selectivebindingandremovalofguestsinamicroporousmetal-organicframework”,Nature,1995,378,703-706.
[9]H.Li,M.Eddaoudi,M.O’keeffe,O.M.Yaghi,“Designandsynthesisofanexceptionallystableandhighlyporousmetal-organicframework”,Nature,1999,402,276-279.。
Summary of the invention
In order to abundant and expansion metal-organic framework materials, the invention provides a kind of furandicarboxylic acid cadmium metal organic framework material and preparation method.
A kind of furandicarboxylic acid cadmium metal organic framework material provided by the invention is first with the title complex that furandicarboxylic acid is formed with cadmium metal.Containing the dimethylamine cation produced by solvent DMF decomposes in the structure of this material.This phenomenon is comparatively rare in the synthesis of metal-organic framework materials.
A kind of furandicarboxylic acid cadmium metal organic framework material, its chemical formula is (HDMA)
2cd
3(FDA)
4dMF, wherein, HDMA is dimethylamine, and FDA is FDCA, and DMF is DMF;
Its structural formula is:
This compound asymmetric cell is by three divalent cadmium ions, four 2,5-furandicarboxylic acid negatively charged ion and Ionized dimethylamine cation and a N, dinethylformamide molecule, compound comprises the unlimited chain-like structure of linear three core secondary structure units and secondary structure unit formation, defines the metal-organic framework materials with network structure.
This compound belongs to triclinic(crystalline)system, P1 spacer, unit cell parameters a=9.4378 (19), b=10.192 (2), c=11.234 (2), α=64.11(3) °, β=73.10(3) °, γ=83.18(3) °, unit cell volume V=930.2 (3)
3, Z=1, Dc=1.997mg/m
3;
The preparation method of a kind of furandicarboxylic acid cadmium metal organic framework material provided by the invention, comprise the steps and condition: the polytetrafluoroethyllining lining of reactor is taken out and is placed on magnetic stirring apparatus, solvent is added according to proportioning, under agitation add cadmium source, main part, triethylene diamine in turn, stir, all reactants dissolved;
Polytetrafluoroethyllining lining is put into reactor, and then, 130-150 DEG C of isothermal reaction 24-48 hour, then naturally cools to room temperature, filtering separation, with DMF washing, dry in vacuum drying oven, obtains target product; Described cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1-2:2-3:0.5-1:300-500, and described cadmium source is Cadmium chloride fine powder, and main part is FDCA, and solvent is DMF.
With following instrument and method, product is characterized:
Ray crystallographic analysis: single crystal diffraction data are collected on RigakuR-AXISRAPID diffractometer, with the MoK alpha-ray of graphite monochromator monochromatization, λ=0.71073, belongs to triclinic(crystalline)system, P1 spacer, unit cell parameters a=9.4378 (19), b=10.192 (2), c=11.234 (2), α=64.11(3) °, β=73.10(3) °, γ=83.18(3) °, unit cell volume V=930.2 (3)
3, Z=1, Dc=1.997mg/m
3, R
1=0.0452.
Single crystal data and parameter are in table 1,2,3,4,5,6.
PyrisDiamondTG/DTA analyser is used to carry out thermogravimetric analysis to product: example weight 8.349893mg, temperature range: 30 ~ 900 DEG C, temperature rise rate: 10 DEG C/min, see Fig. 1.Weight after sample weight loss is 1.741704mg, and rate of weight loss is about 79%, is the theoretical value approximate (calculated value is 76%) that CdO calculates with final product.Before about 240 DEG C, Cd title complex slightly weight loss.This may be the weight loss owing to leaving title complex in heat-processed at the object DMF in title complex duct or surface.After 240 DEG C, Cd title complex weight loss is obvious, and illustrate that Cd complex structure starts to be damaged at such a temperature, along with the rising of temperature, title complex decomposes gradually.
Beneficial effect: the invention provides a kind of furandicarboxylic acid cadmium metal organic framework material and preparation method.This compound is first with the title complex that furandicarboxylic acid is formed with cadmium metal, asymmetric cell is by three divalent cadmium ions, four furandicarboxylic acid negatively charged ion and Ionized dimethylamine cation and a DMF solvent molecule, dimethylamine cation is wherein due to DMF molecular breakdown gained under high temperature, and the metal organic frame containing solvolyte in similar this crystal is comparatively rare.Compound comprises the unlimited chain-like structure of linear three core secondary structure units and secondary structure unit formation.Define the metal-organic framework materials with network structure.May be used for the aspect such as the separation of gas and the absorption of carbonic acid gas.
Accompanying drawing explanation
Fig. 1 is a kind of furandicarboxylic acid cadmium metal of the present invention organic framework material thermogravimetric analysis figure.
Embodiment
Embodiment 1 one kinds of furandicarboxylic acid cadmium metal organic framework materials, its chemical formula is (HDMA)
2cd
3(FDA)
4dMF, wherein, HDMA is dimethylamine, and FDA is FDCA, and DMF is DMF;
Its structural formula is:
This compound asymmetric cell is by three divalent cadmium ions, four 2,5-furandicarboxylic acid negatively charged ion and Ionized dimethylamine cation and a N, dinethylformamide molecule, compound comprises the unlimited chain-like structure of linear three core secondary structure units and secondary structure unit formation, defines the metal-organic framework materials with network structure.
This compounds process for production thereof comprises the steps and condition:
The polytetrafluoroethyllining lining of reactor is taken out to be placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1:2:0.5:300, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.1mmol (25mg)
22.5H
2the FDCA of O, 0.20mmol (42mg), the triethylene diamine of 0.05mmol (13mg), under agitation join 300mmol(3mL in turn) N, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 130 DEG C, keep isothermal reaction 48h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
The preparation method of embodiment 2 one kinds of furandicarboxylic acid cadmium metal organic framework materials is as follows: the polytetrafluoroethyllining lining of reactor is taken out and is placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 2:3:1:500, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.2mmol (50mg)
22.5H
2the FDCA of O, 0.3mmol (63mg), the triethylene diamine of 0.1mmol (25mg), under agitation join 500mmol(5mL in turn) N, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 140 DEG C, keep isothermal reaction 24h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
The preparation method of embodiment 3 one kinds of furandicarboxylic acid cadmium metal organic framework materials is as follows: the polytetrafluoroethyllining lining of reactor is taken out and is placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1:3:0.5:400, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.1mmol (25mg)
22.5H
2the FDCA of O, 0.3mmol (63mg), the triethylene diamine of 0.05mmol (13mg), under agitation join 400mmol(5mL in turn) N of 5mL, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 150 DEG C, keep isothermal reaction 36h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
Following instrument and method is used to characterize product:
Ray crystallographic analysis: single crystal diffraction data are collected on RigakuR-AXISRAPID diffractometer, with the MoK alpha-ray of graphite monochromator monochromatization, λ=0.71073, belongs to triclinic(crystalline)system, P1 spacer, unit cell parameters a=9.4378 (19), b=10.192 (2), c=11.234 (2), α=64.11(3) °, β=73.10(3) °, γ=83.18(3) °, unit cell volume V=930.2 (3)
3, Z=1, Dc=1.997mg/m
3, R
1=0.0452.
Single crystal data and parameter are in table 1,2,3,4,5,6.
PyrisDiamondTG/DTA analyser is used to carry out thermogravimetric analysis to product: example weight 8.349893mg, temperature range: 30 ~ 900 DEG C, temperature rise rate: 10 DEG C/min, see Fig. 1.Weight after sample weight loss is 1.741704mg, and rate of weight loss is about 79%, is the theoretical value approximate (calculated value is 76%) that CdO calculates with final product.Before about 240 DEG C, Cd title complex slightly weight loss.This may be the weight loss owing to leaving title complex in heat-processed at the object DMF in title complex duct or surface.After 240 DEG C, Cd title complex weight loss is obvious, and illustrate that Cd complex structure starts to be damaged at such a temperature, along with the rising of temperature, title complex decomposes gradually.
Claims (5)
1. a furandicarboxylic acid cadmium metal organic framework material, is characterized in that, its chemical formula is (HDMA)
2cd
3(FDA)
4dMF, wherein, HDMA is dimethylamine, and FDA is FDCA, and DMF is DMF;
Its structural formula is:
This compound asymmetric cell is by three divalent cadmium ions, four 2,5-furandicarboxylic acid negatively charged ion and Ionized dimethylamine cation and a N, dinethylformamide molecule, compound comprises the unlimited chain-like structure of linear three core secondary structure units and secondary structure unit formation, defines the metal-organic framework materials with network structure.
2. a kind of furandicarboxylic acid cadmium metal organic framework material as claimed in claim 1, it is characterized in that, its preparation method comprises the steps and condition: the polytetrafluoroethyllining lining of reactor is taken out and is placed on magnetic stirring apparatus, solvent is added according to proportioning, under agitation add cadmium source, main part, triethylene diamine in turn, stir, all reactants dissolved;
Polytetrafluoroethyllining lining is put into reactor, and then, 130-150 DEG C of isothermal reaction 24-48 hour, then naturally cools to room temperature, filtering separation, with DMF washing, dry in vacuum drying oven, obtains target product; Described cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1-2:2-3:0.5-1:300-500, and described cadmium source is Cadmium chloride fine powder, and main part is FDCA, and solvent is DMF.
3. the preparation method of a kind of furandicarboxylic acid cadmium metal organic framework material as claimed in claim 2, is characterized in that, comprise the steps and condition:
The polytetrafluoroethyllining lining of reactor is taken out to be placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1:2:0.5:300, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.1mmol (25mg)
22.5H
2the FDCA of O, 0.20mmol (42mg), the triethylene diamine of 0.05mmol (13mg), under agitation join 300mmol(3mL in turn) N, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 130 DEG C, keep isothermal reaction 48h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
4. the preparation method of a kind of furandicarboxylic acid cadmium metal organic framework material as claimed in claim 2, is characterized in that, comprise the steps and condition:
The polytetrafluoroethyllining lining of reactor is taken out to be placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 2:3:1:500, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.2mmol (50mg)
22.5H
2the FDCA of O, 0.3mmol (63mg), the triethylene diamine of 0.1mmol (25mg), under agitation join 500mmol(5mL in turn) N, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 140 DEG C, keep isothermal reaction 24h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
5. the preparation method of a kind of furandicarboxylic acid cadmium metal organic framework material as claimed in claim 2, is characterized in that, comprise the steps and condition:
The polytetrafluoroethyllining lining of reactor is taken out to be placed on magnetic stirring apparatus, add solvent, according to cadmium source: main part: triethylene diamine: the mol ratio of solvent is 1:3:0.5:400, described cadmium source is Cadmium chloride fine powder, main part is FDCA, and solvent is N, dinethylformamide, by the CdCl of 0.1mmol (25mg)
22.5H
2the FDCA of O, 0.3mmol (63mg), the triethylene diamine of 0.05mmol (13mg), under agitation join 400mmol(5mL in turn) N of 5mL, in dinethylformamide, stir, all reactants dissolved, polytetrafluoroethyllining lining is put into reactor, then, is heated to 150 DEG C, keep isothermal reaction 36h, cool to room temperature, filtering separation, washs with DMF, dry in vacuum drying oven, obtain target product.
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| CN105833662A (en) * | 2016-05-17 | 2016-08-10 | 浙江大学 | Method for adsorbing and separating sulfur-containing acid gas |
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| CN106496282A (en) * | 2016-09-13 | 2017-03-15 | 桂林理工大学 | 2 hydroxyacetophenone derivative Schiff base nickel complex Ni (dcah) DMA and synthetic method |
| CN108998007A (en) * | 2018-08-02 | 2018-12-14 | 江西省科学院应用化学研究所 | A kind of preparation method of rare earth metal organic framework materials |
| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
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| CN105833662B (en) * | 2016-05-17 | 2018-08-31 | 浙江大学 | A kind of method of adsorbing separation sulfuric acid gas |
| CN106496282A (en) * | 2016-09-13 | 2017-03-15 | 桂林理工大学 | 2 hydroxyacetophenone derivative Schiff base nickel complex Ni (dcah) DMA and synthetic method |
| 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 |
| CN108998007A (en) * | 2018-08-02 | 2018-12-14 | 江西省科学院应用化学研究所 | A kind of preparation method of rare earth metal organic framework materials |
| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
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