CN110079306A - A kind of Mg-MOF fluorescent sensing material and preparation method thereof - Google Patents
A kind of Mg-MOF fluorescent sensing material and preparation method thereof Download PDFInfo
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- CN110079306A CN110079306A CN201910493260.XA CN201910493260A CN110079306A CN 110079306 A CN110079306 A CN 110079306A CN 201910493260 A CN201910493260 A CN 201910493260A CN 110079306 A CN110079306 A CN 110079306A
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- 239000011540 sensing material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000003446 ligand Substances 0.000 claims abstract description 48
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 42
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims abstract description 38
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 14
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 230000005855 radiation Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000005284 excitation Effects 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910020056 Mg3N2 Inorganic materials 0.000 claims abstract description 5
- -1 benzene tetramethyl carboxylic acid Chemical class 0.000 claims abstract description 5
- 239000012621 metal-organic framework Substances 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 20
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 6
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- CBEVANLIGJVSHZ-UHFFFAOYSA-N n,n'-diheptyl-n,n'-dimethylbutanediamide Chemical compound CCCCCCCN(C)C(=O)CCC(=O)N(C)CCCCCCC CBEVANLIGJVSHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910007566 Zn-MOF Inorganic materials 0.000 claims 2
- 239000013094 zinc-based metal-organic framework Substances 0.000 claims 2
- 125000003713 acetylimino group Chemical group [H]C([H])([H])C(=O)N=[*] 0.000 claims 1
- 238000005352 clarification Methods 0.000 claims 1
- 230000003760 hair shine Effects 0.000 claims 1
- 239000012046 mixed solvent Substances 0.000 claims 1
- 230000009102 absorption Effects 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 3
- 238000002447 crystallographic data Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000013384 organic framework Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- QPUMEZIFDXYGPG-UHFFFAOYSA-N piperazine 1H-pyrrole Chemical compound N1CCNCC1.N1C=CC=C1 QPUMEZIFDXYGPG-UHFFFAOYSA-N 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G83/008—Supramolecular polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/186—Metal complexes of the light metals other than alkali metals and alkaline earth metals, i.e. Be, Al or Mg
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N2021/6417—Spectrofluorimetric devices
Abstract
The invention discloses a kind of Mg-MOF fluorescent sensing material, chemical formula C24H24Mg3N2O22；Ligand is equal benzene tetramethyl carboxylic acid and pyrazine, solvent are as follows: n,N-Dimethylformamide, acetonitrile, first alcohol and water；Resulting crystal yield and purity are higher.Two Mg in structure2+Ion is hexa-coordinate, each Mg2+Ion forms coordination with four BTEC ligands respectively, and Pyromellitic Acid and Mg01 form one-dimensional layer, forms three-dimensional without limit structure by Mg02 between layers.The Mg-MOF fluorescent sensing material in the range of visible light at 200nm and 280nm there are ultraviolet radiation absorption, absorbing wavelength has certain use value within the scope of 191-325nm in terms of ultraviolet radiation absorption.Solid state fluorescence analyzes its maximum excitation wavelength and is located at 328nm, and optimum launch wavelength is 408nm, has good luminosity, can be used as fluorescent sensing material.
Description
Technical field
The present invention relates to the preparation process field of fluorescence MOFs material, specially a kind of Pyromellitic Acid ligand constructs fluorescence
Mg-MOF material and preparation method thereof.
Background technique
With the development of society, especially scientific and technical progress, is greatly facilitated the rapid development of social productive forces；Society
The progress and development of meeting, so that people's lives quality has some new of very big improvement and raising, especially chemical field
The discovery and application of material are made that contribution outstanding for the change of industry and resident living.
Metal organic frame (MOFs) has good adsorption property, catalytic property, magnetism because of its novel complicated structure
Matter, optical property etc. are a kind of important composite functional materials.Largely luminous MOFs material existing at present is reported, but structure
The luminous MOFs for building novel structure is still the hot subject studied at present.
The design synthesis of Mg-MOF material enriches the research of metal coordination chemistry with research, helps to obtain beneficial hair
Optical property fluorescent material, equal benzene tertacarbonic acid's class ligand have coordination site abundant, and diversified coordination mode can be with alkaline earth gold
Belong to magnesium atom and form stronger coordinate bond, therefore diversified Mg-MOF structure can be constructed out.Secondly, carboxylic acids organic ligand
Conjugation help to prepare advanced luminescent material, facilitated using the fluorescent material that such ligand is constructed with alkaline-earth metal magnesium
Understand the interaction in complex between alkaline-earth metal ions and ligand, fluorescence identifying and in terms of have it is latent
Application.
The synthesis and exploration of this kind of material, constructing organic framework material offer to equal benzene tertacarbonic acid's ligand and alkaline-earth metal can
The experimental basis leaned on, in addition the fluorescence identifying performance study of such compound helps to understand metal ion and ligand in complex
Between interaction.
Therefore, the preparation method for studying Mg-MOF fluorescent sensing material, is a urgent problem needed to be solved.
Summary of the invention
In order to solve above-mentioned problems of the prior art, the present invention provides a kind of Pyromellitic Acid ligand construct it is glimmering
The method of light Mg-MOF material, the material are a kind of with Mg-MOF " Mg1.5(BTEC) (C2H7N)•(H2O alkaline earth gold) "
Belong to organic framework materials.The material crystalline is in orthorhombic systemPbcnSpace group, in the range of visible light at 200nm and 280nm
There are ultraviolet radiation absorption, absorbing wavelength has certain use value within the scope of 191-325nm in terms of ultraviolet radiation absorption.
The object of the present invention is achieved like this:
A kind of Mg-MOF fluorescent sensing material, chemical formula C24H24Mg3N2O22；Wherein ligand choose equal benzene tetramethyl carboxylic acid and
Pyrazine, solvent are as follows: n,N-Dimethylformamide, acetonitrile (C2H3N), first alcohol and water (H2O)；
The Mg-MOF fluorescent sensing material belongs to monoclinic systemPbcnSpace group, cell parameter are respectively as follows: a=18.854
(4), b=9.5088 (19), c=17.382 (4),α=β=γ=90o；
The structure of the Mg-MOF fluorescent sensing material is: its minimum asymmetric cell includes two Mg2+Ion, four ligands.
Two Mg in structure2+Ion is hexa-coordinate, each Mg2+Ion forms coordination, equal benzene tetramethyl with four BTEC ligands respectively
Acid forms one-dimensional layer with Mg01, forms three-dimensional without limit structure by Mg02 between layers；Ligand Pyromellitic Acid takes one
The monodentate ligand of carboxyl oxygen atom, the Bidentate State of neighbored carboxyl groups oxygen atom, two ligands provide the three of three oxygen atoms
Tooth coordination mode；
The Mg-MOF fluorescent sensing material the preparation method comprises the following steps:
It is molten that magnesium nitrate and ligand Pyromellitic Acid, pyrazine are added to N,N-dimethylformamide, acetonitrile, the mixing of first alcohol and water
Ultrasound becomes to solution in agent, after the sealing of glass bottle closure clarifies, by gained mixture by solvent thermal reaction, after being stored at room temperature
To white needle-like crystals；
Ligand Pyromellitic Acid, pyrazine and the magnesium nitrate molar ratio is 1: 1.5: 1.5~1.5: 5: 5；
The DMF/ C2H3N / H2O or DMF/ CH3OH / H2The solvent ratio of O is 4: 3: 1；
It is described by glass bottle closure it is closed after 5 ~ 10min of ultrasonic oscillation；
The solvent heat condition of the thermal response is 90~115oIt is reacted 3-5 days under C, cooled to room temperature；
The application of the Mg-MOF fluorescent sensing material, there are ultraviolet light suctions at 200nm and 280nm in the range of visible light
It receives, absorbing wavelength has certain use value within the scope of 191-325nm in terms of ultraviolet radiation absorption；Solid state fluorescence analyzes it
Maximum excitation wavelength is located at 328nm, and optimum launch wavelength is 408nm, has good luminosity, can be used as fluorescence sense
Material.
Positive beneficial effect: the invention discloses Mg-MOF fluorescent sensing material ligand be equal benzene tetramethyl carboxylic acid and pyrrole
Piperazine, solvent are as follows: n,N-Dimethylformamide, acetonitrile, first alcohol and water；Resulting crystal yield and purity are higher；Crystal parsing
Show: its minimum asymmetric cell includes two Mg2+Ion, four ligands；Two Mg in structure2+Ion is hexa-coordinate, often
A Mg2+Ion forms coordination with four BTEC ligands respectively, and Pyromellitic Acid and Mg01 form one-dimensional layer, lead between layers
It crosses Mg02 and forms three-dimensional without limit structure；Ligand Pyromellitic Acid takes the monodentate ligand of a carboxyl oxygen atom, neighbored carboxyl groups oxygen
The Bidentate State of atom, two ligands provide the tridentate ligand mode of three oxygen atoms；The Mg-MOF fluorescent sensing material
There are ultraviolet radiation absorption at 200nm and 280nm in the range of visible light, absorbing wavelength is within the scope of 191-325nm, ultraviolet
There is certain use value in terms of line absorption；Solid state fluorescence analyzes its maximum excitation wavelength and is located at 328nm, optimum launch wavelength
For 408nm, there is good luminosity, can be used as fluorescent sensing material.
Detailed description of the invention
Fig. 1 is metal Mg of the invention2+Coordination mode；
Fig. 2 is three-dimension layer structure chart of the invention；
Fig. 3 is that powder IR of the invention schemes；
Fig. 4 is that TG of the invention schemes.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is described further:
A kind of Mg-MOF fluorescent sensing material, chemical formula C24H24Mg3N2O22；Ligand is Pyromellitic Acid and pyrazine, solvent
Are as follows: N,N-dimethylformamide, acetonitrile, first alcohol and water；
The Mg-MOF fluorescent sensing material belongs to monoclinic systemPbcnSpace group, cell parameter are respectively as follows: a=18.854
(4), b=9.5088 (19), c=17.382 (4),α=β=γ=90o；
The structure of the Mg-MOF fluorescent sensing material is: its minimum asymmetric cell includes two Mg2+Ion, four ligands；
Two Mg in structure2+Ion is hexa-coordinate, each Mg2+Ion forms coordination, equal benzene tetramethyl with four BTEC ligands respectively
Acid forms one-dimensional layer with Mg01, forms three-dimensional without limit structure by Mg02 between layers；Ligand Pyromellitic Acid takes one
The monodentate ligand of carboxyl oxygen atom, the Bidentate State of neighbored carboxyl groups oxygen atom, two ligands provide the three of three oxygen atoms
Tooth coordination mode；
The Mg-MOF fluorescent sensing material the preparation method comprises the following steps:
It is molten that magnesium nitrate and ligand Pyromellitic Acid, pyrazine are added to N,N-dimethylformamide, acetonitrile, the mixing of first alcohol and water
In agent, ultrasound becomes to solution and clarifies after sealing, by gained mixture by solvent thermal reaction, obtains white needles after being stored at room temperature
Crystal；
Ligand Pyromellitic Acid, pyrazine and the magnesium nitrate molar ratio is 1: 1.5: 1.5~1.5: 5: 5；
The DMF/ C2H3N / H2O or DMF/ CH3OH / H2The solvent ratio of O is 4: 3: 1；
It is described by glass bottle closure it is closed after ultrasonic oscillation 5min；
The solvent heat condition of the thermal response is 90~115oIt is reacted 3-5 days under C, cooled to room temperature；
There are ultraviolet radiation absorptions at 200nm and 280nm in the range of visible light for the Mg-MOF fluorescent sensing material, absorb
Wavelength has certain use value within the scope of 191-325nm in terms of ultraviolet radiation absorption；Solid state fluorescence analyzes its maximum excitation
Wavelength is located at 328nm, and optimum launch wavelength is 408nm, has good luminosity, can be used as fluorescent sensing material.
Embodiment 1
The preparation of Mg-MOF fluorescent sensing material:
Weigh 0.2 mmol of 0.3 mmol of zinc nitrate and ligand Pyromellitic Acid, 0.3 mmol of pyrazine is placed in 10mL bottle, add
Enter 4 mL n,N-Dimethylformamide, 3 mL acetonitriles or methanol and 1 mL water, ultrasonic vibration 6min are sealed in 95oIt is anti-under C
72 h are answered, obtain white needle-like crystals after being stored at room temperature.
To the characterization of embodiment 1:
(1) crystal structure determination:
Select that size is suitable, the preferable monocrystalline of crystal quality under the microscope, in Saturn70 (4x4 bin mode) type list
Tested on brilliant x-ray diffractometer, with through graphite monochromator monochromatization Mo K alpha ray (λ=0.71073), withφ-ωMode
Collect diffraction data；All diffraction datas carry out semiempirical absorption correction using SADABS program；Cell parameter least square
Method determines that data convert and structure elucidation use Crystalclear and SHELXTL program to complete respectively；Crystal structure is with directly
Method solves, and first determines whole non-hydrogen atom coordinates with difference function method and least square method, and obtain hydrogen original with theoretical hydrogenation method
Then sub- position carries out refine to crystal structure with least square method；Predominant crystal parameter is shown in such as table 1:
(2) powder diffraction characterizes phase purity:
As shown in table 1, the powder diffraction data of embodiment 1 is collected complete on Rigaku D/Max-2500 x-ray diffractometer
At.
(3) IR Characterization:
The IR Characterization of embodiment 1 is collected by 27 OPUS of Tensor (Bruker) FT-IR radar stealthy materials, KBr tabletting, as a result
As shown in Figure 3；
The present invention discloses Mg-MOF fluorescent sensing material, chemical formula C24H24Mg3N2O22；Ligand be equal benzene tetramethyl carboxylic acid and
Pyrazine, solvent are as follows: n,N-Dimethylformamide, acetonitrile, first alcohol and water；Resulting crystal yield and purity are higher；Crystal solution
Analysis shows: its minimum asymmetric cell includes two Mg2+Ion, four ligands；Two Mg in structure2+Ion is hexa-coordinate,
Each Mg2+Ion forms coordination with four BTEC ligands respectively, and Pyromellitic Acid and Mg01 form one-dimensional layer, between layers
Three-dimensional is formed without limit structure by Mg02；Ligand Pyromellitic Acid takes the monodentate ligand of a carboxyl oxygen atom, neighbored carboxyl groups
The Bidentate State of oxygen atom, two ligands provide the tridentate ligand mode of three oxygen atoms；The Mg-MOF fluorescence sense material
Material in the range of visible light at 200nm and 280nm there are ultraviolet radiation absorption, absorbing wavelength is within the scope of 191 ~ 325nm, in purple
Outside line absorption aspects have certain use value；Solid state fluorescence analyzes its maximum excitation wavelength and is located at 328nm, optimum transmitted wave
A length of 408nm has good luminosity, can be used as fluorescent sensing material；
The above case study on implementation is merely to illustrate the preferred embodiment of the present invention, but present invention is not limited to the embodiments described above,
The field those of ordinary skill within the scope of knowledge, it is made within the spirit and principles in the present invention any to repair
Change, equivalent substitute and improvement etc., is regarded as the protection scope of the application.
Claims (9)
1. a kind of Mg-MOF fluorescent sensing material, it is characterised in that: chemical formula C24H24Mg3N2O22；Ligand is equal benzene tetramethyl carboxylic
Acid and pyrazine, solvent are as follows: n,N-Dimethylformamide, acetonitrile, first alcohol and water.
2. a kind of Mg-MOF fluorescent sensing material according to claim 1, it is characterised in that: the Zn-MOF fluorescence passes
The crystal of sense material belongs to monoclinic systemPbcnSpace group, cell parameter are respectively as follows: a=18.854 (4), b=9.5088
(19), c=17.382 (4),α=β =γ =90o。
3. a kind of Mg-MOF fluorescent sensing material according to claim 1, it is characterised in that: the Zn-MOF fluorescence passes
The structure of sense material is: its minimum asymmetric cell includes two Mg2+Ion, four ligands；Two Mg in structure2+Ion is equal
It is hexa-coordinate, each Mg2+Ion forms coordination with four BTEC ligands respectively, and Pyromellitic Acid and Mg01 form one-dimensional layer, layer
Three-dimensional is formed without limit structure by Mg02 between layer；Ligand Pyromellitic Acid takes the monodentate ligand of a carboxyl oxygen atom,
The Bidentate State of neighbored carboxyl groups oxygen atom, two ligands provide the tridentate ligand mode of three oxygen atoms.
4. the preparation method of Mg-MOF fluorescent sensing material as described in claim 1, it is characterised in that: by magnesium nitrate and ligand
Pyromellitic Acid, pyrazine are added to the in the mixed solvent of n,N-Dimethylformamide, acetonitrile, first alcohol and water, after sealing ultrasound extremely
Solution becomes clarification, by gained mixture by solvent thermal reaction, obtains white needle-like crystals after being stored at room temperature.
5. a kind of preparation method of Mg-MOF fluorescent sensing material according to claim 4, it is characterised in that: described matches
Body Pyromellitic Acid, pyrazine and magnesium nitrate molar ratio are 1: 1.5: 1.5~1.5: 5: 5.
6. a kind of preparation method of Mg-MOF fluorescent sensing material according to claim 4, it is characterised in that: DMF/
C2H3N / H2O or DMF/ CH3OH / H2The solvent ratio of O is 4: 3: 1.
7. a kind of preparation method of Mg-MOF fluorescent sensing material according to claim 4, it is characterised in that: the heat is anti-
The solvent heat condition answered is 90~115oIt is reacted 3-5 days under C, cooled to room temperature.
8. a kind of preparation method of Mg-MOF fluorescent sensing material according to claim 4, it is characterised in that: the general
5 ~ 10min of ultrasonic oscillation after glass bottle closure is closed.
9. the application of Mg-MOF fluorescent sensing material as described in claim 1, it is characterised in that: in the range of visible light
There are ultraviolet radiation absorption at 200nm and 280nm, absorbing wavelength has use within the scope of 191 ~ 325nm in terms of ultraviolet radiation absorption
Value；Solid state fluorescence analyzes its maximum excitation wavelength and is located at 328nm, and optimum launch wavelength is 408nm, has and shines well
Property can be used as fluorescent sensing material.
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| CN201910493260.XA Pending CN110079306A (en) | 2019-06-07 | 2019-06-07 | A kind of Mg-MOF fluorescent sensing material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942605A (en) * | 2019-03-08 | 2019-06-28 | 河南城建学院 | A kind of Magnesium Complex, preparation method and applications |
| CN111825851A (en) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
| CN113861434A (en) * | 2021-09-14 | 2021-12-31 | 南开大学 | Novel magnesium-based MOF material and solution processing method of MOF material |
| CN114276367A (en) * | 2021-12-30 | 2022-04-05 | 郑州大学 | Bispyrazine macrocyclic compound, preparation method and application thereof in construction of fluorescent powder |
-
2019
- 2019-06-07 CN CN201910493260.XA patent/CN110079306A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| CALDERONE, PAUL J. ET AL: "Temperature dependent structure formation and photoluminescence studies of a series of magnesium-based coordination networks", 《INORGANICA CHIMICA ACTA》 * |
| LIU, HSIN-KUAN ET AL: "Microwave synthesis and single-crystal-to-single-crystal transformation of magnesium coordination polymers exhibiting selective gas adsorption and luminescence properties", 《CRYSTENGCOMM》 * |
| ZHANG, DAO-JUN ET AL: "Solvothermal synthesis, crystal structure and photoluminescent property of a novel 3-D magnesium metal-organic framework[Mg1.5(μ5-btec)(H2O)2][H2N(CH3)2].H2O", 《INORGANIC CHEMISTRY COMMUNICATIONS》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942605A (en) * | 2019-03-08 | 2019-06-28 | 河南城建学院 | A kind of Magnesium Complex, preparation method and applications |
| CN111825851A (en) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
| CN111825851B (en) * | 2020-08-11 | 2022-04-05 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
| CN113861434A (en) * | 2021-09-14 | 2021-12-31 | 南开大学 | Novel magnesium-based MOF material and solution processing method of MOF material |
| CN113861434B (en) * | 2021-09-14 | 2022-10-21 | 南开大学 | Novel magnesium-based MOF material and solution processing method of MOF material |
| CN114276367A (en) * | 2021-12-30 | 2022-04-05 | 郑州大学 | Bispyrazine macrocyclic compound, preparation method and application thereof in construction of fluorescent powder |
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