CN107602596A - A kind of Zn MOF fluorescent sensing materials and preparation method thereof - Google Patents
A kind of Zn MOF fluorescent sensing materials and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Zn MOF fluorescent sensing materials, its chemical formula is [Zn2(L)4(DMA)(H2O)]；L is the part of the m benzene dicarboxylic acid of amido link modification（H4L）Lose obtained by four hydrogen atoms；DMA is N, N dimethyl acetamides；H2O is hydrone, and crystal parsing shows：Described Zn MOF fluorescent sensing material crystal belongs to monoclinic systemP21Space group, cell parameter are respectively：A=10.246 (2), b=16.147 (3), c=19.161 (4),α=γ=90o,β=99.98(3)o.Structure is：Its minimum asymmetric cell includes the Zn of two crystallography independence2+Ion, the ligand L of complete deprotonation, the DMA molecules and a hydrone of coordination.The porosity about 53.5% of Zn MOF fluorescent sensing materials.Fluorometric investigation shows the material to Fe3+Ion has very strong Selective recognition ability, can be used as detection Fe3+The fluorescent sensing material of ion.
Description
Technical field
The present invention relates to fluorescence MOFs field of material preparation, specially a kind of m benzene dicarboxylic acid part structure of amido link modification
The method for building fluorescence MOFs materials.
Background technology
In recent years, metal organic frame (MOFs) is as a kind of new solid material, in fluorescence, the suction of sensing, gas
It is attached that there is potential application value with the field such as separating.Up to the present, although largely luminous MOFs has been reported,
But the luminous MOFs for constructing novel structure is still the hot subject studied at present.The design synthesis of this kind of compound is with studying not
The research contents of Coordinative Chemistry is only enriched, and helps to obtain the fluorescence MOFs materials of outstanding luminescent properties.(Zhan
S.,Li M., Seik W.,et al.Chemistry-A European Journal,2013,19,10217-10225.；Liu
T.,Zhang W.,Sun W., et al.Inorganic Chemistry,2011,50,5242-5248.；Pu Y.,
Takayuki C.,Kazushige L.,et al. Advanced Materials,2015,27,1327-1332.).Isophthalic two
Carboxylic acids part has abundant coordination site, diversified coordination mode, strong coordinate bond can be formed with metal, therefore can
To construct out diversified MOFs structures.In addition, by introduce amido link functional group increase part flexibility, make part with
Configuration can be changed according to the change of coordination environment during position, add to obtain the probability of novel structure.Secondly, conjugation
Amide carboxylic acid's organic ligand can construct luminescent material, utilize such part and d10Metal constructs fluorescence MOFs materials, in fluorescence
Identification and Molecular Detection etc. have potential application. (Chen Y Q,Qu Y K,Li G R,et al.Inorganic
chemistry,2014,53(17):8842-8844.；Han,S.D.； Song,W.C.；Zhao,J.P.；Yang,Q.；Liu,
S.J.；Li,Y.；Bu X.H.Chem.Commun.,2013,49,871.； Zhang Z.,Michael J.Chemical
Society Reviews,2014,43,5444-5455.；Eddaoudi M.,Kim J., Rosi N.,et al.Science,
2002,295,469-472.；Wang Z.,Victor C.,Michael J.Angewandte Chemie International
Edition,2005,44,2877-2880.；Murat C.,Gu Z.,Martin N.,et al.Chemical
Communications,2015,51,4796-4798.)。
The synthesis and exploration of this kind of material, first the m benzene dicarboxylic acid part and d to amido link modification10Metal is constructed organic
Framework material provides reliable experimental basis, and the fluorescence identifying performance study of such compound helps to understand complex in addition
Interaction between middle metal ion and part.
The content of the invention
The invention provides the metal-organic framework material of a kind of " Zn-L ", L is the m benzene dicarboxylic acid of amido link modification
Part (H4L) lose obtained by four hydrogen atoms.The material crystalline is in monoclinic system P21Space group, to Fe3+Ion has very strong
Selective recognition ability, can be used as detection Fe3+The m benzene dicarboxylic acid of fluorescent sensing material and its amido link modification of ion is matched somebody with somebody
The method that body constructs fluorescence MOFs materials.
The object of the present invention is achieved like this：
A kind of Zn-MOF fluorescent sensing materials, its main body frame be represented by the chemical formula for：[Zn2(L)4(DMA)(H2O)], formula
Middle L is the part (H of the m benzene dicarboxylic acid of amido link modification4L) lose obtained by four hydrogen atoms；DMA is N, N- dimethylacetamides
Amine；H2O is hydrone.
Described Zn-MOF fluorescent sensing materials belong to monoclinic system P21Space group, cell parameter are respectively： α=γ=90 °, β=99.98 (3) °；
The structure of the Zn-MOF fluorescent sensing materials is：Its minimum asymmetric cell includes two crystallography independence
Zn2+Ion, the ligand L of complete deprotonation, DMA and hydrone of coordination；Two Zn in structure2+Ion
It is four-coordination, and double-core clusters is formed by three carboxyl bridgings, double-core cluster forms two-dimensional layer by the bridging of isophthalic acid, and two
Dimension layer connects to form the three-dimensional structure containing duct further through ligand L；Zn-MOF fluorescent sensing materials have minimum along a directions
Cross sectionPyriform duct, have along b directionsRectangle duct, the diamond hole having along c directions
The DMA molecules that road is coordinated occupy, the porosity about 53.5% of Zn-MOF fluorescent sensing materials；
The preparation method of described Zn-MOF fluorescent sensing materials is：
By zinc nitrate and part H4L is added in DMF solvent, and ultrasound becomes to solution and clarified after sealing, by gained mixture
By solvent thermal reaction, water white transparency bulk crystals are obtained after being stored at room temperature；
Described zinc nitrate and part H4L mol ratios are 1:3~1.5:5；
Described DMF/H2O solvent ratio is 3:2；
The solvent heat condition of the thermal response naturally cools to room temperature to be reacted 2-5 days at 85~115 DEG C；
Described Zn-MOF fluorescent sensing materials are in Fe3+DMA solution in fluorescence be quenched completely, work as Fe3+Concentration is 10- 4Fluorescent quenching 81% during mol/L, works as Fe3+Concentration reaches 10-3During mol/L, fluorescence is quenched completely.Fluorometric investigation shows the material
To Fe3+Ion has very strong Selective recognition ability, can be used as detection Fe3+The fluorescent sensing material of ion.
Positive beneficial effect：
The invention discloses a kind of Zn-MOF fluorescent sensing materials, its chemical formula is [Zn2(L)4(DMA)(H2O)]；H4L is
A kind of m benzene dicarboxylic acid class part of amido link modification, solvent are：DMAC N,N' dimethyl acetamide and water；The crystal yield of gained and
Purity is higher.Crystal parsing shows：The Zn-MOF fluorescent sensing materials crystal belongs to monoclinic system P21Space group, structure cell
Parameter is respectively：α=γ=90 °, β=99.98 (3) °；
Structure is：Its minimum asymmetric cell of described Zn-MOF fluorescent sensing materials includes the Zn of two crystallography independence2+Ion,
The ligand L of one complete deprotonation, a DMA molecule and a hydrone being coordinated；Two Zn in structure2+Ion is
Four-coordination, and double-core cluster is formed by three carboxyl bridgings, double-core cluster forms two-dimensional layer, two-dimensional layer by the bridging of isophthalic acid
Connect to form the three-dimensional structure containing duct further through ligand L；Zn-MOF fluorescent sensing materials have minimum transversal along a directions
FacePyriform duct, have along b directionsRectangle duct, the rhombus duct quilt having along c directions
The DMA molecules of coordination occupy.Highly unordered solvent molecule passes through SQUEEZE journeys in the duct of Zn-MOF fluorescent sensing materials
Sequence carries out desolvation processing, and porosity about 53.5% is calculated through PLATON.Fluorometric investigation shows the material to Fe3+Ion has
There is very strong Selective recognition ability, detection Fe can be used as3+The fluorescent sensing material of ion.
Brief description of the drawings
Fig. 1 is the metal Zn of the present invention2+Coordination mode；
Fig. 2 is the two-dimensional layer structure chart of the present invention；
Fig. 3 is the tomograph along a directions of the present invention；
Fig. 4 is the powder PXRD figures of the present invention；
Fig. 5 is the IR figures of the present invention；
Fig. 6 is the present invention (10 in different nitrate solutions-3Mol/L fluorescence intensity)；
Fig. 7 is Fe of the present invention in various concentrations3+Fluorescence intensity in solution.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is described further：
A kind of Zn-MOF fluorescent sensing materials, its main body frame be represented by the chemical formula for：[Zn2(L)4(DMA)(H2O)], formula
Middle L is the part (H of the m benzene dicarboxylic acid of amido link modification4L) lose obtained by four hydrogen atoms；DMA is N, N- dimethylacetamides
Amine；H2O is hydrone；
Described Zn-MOF fluorescent sensing material crystal monoclinic systems P21Space group, cell parameter are respectively： α=γ=90 °, β=99.98 (3) °；
The structure of the Zn-MOF fluorescent sensing materials is：Minimum asymmetric cell includes the Zn of two crystallography independence2+
Ion, the ligand L of complete deprotonation, the DMA molecules and a hydrone of coordination；Two Zn in structure2+From
Son is four-coordination, and forms double-core cluster by three carboxyl bridgings, and double-core cluster forms two-dimensional layer by the bridging of isophthalic acid,
Two-dimensional layer connects to form the three-dimensional structure containing duct further through ligand L；Zn-MOF fluorescent sensing materials have most along a directions
Small cross sectionPyriform duct, have along b directionsRectangle duct, the rhombus having along c directions
The DMA molecules that duct is coordinated occupy.The porosity of Zn-MOF fluorescent sensing materials about 53.5%.
The preparation method of described Zn-MOF fluorescent sensing materials is：
By zinc nitrate and part H4L is added in DMF solvent, and ultrasound becomes to solution and clarified after sealing, by gained mixture
By solvent thermal reaction, water white transparency bulk crystals are obtained after being stored at room temperature；
Described zinc nitrate and part H4L mol ratios are 1:3~1.5:5；
Described DMF/H2O solvent ratio is 3:2；
The solvent heat condition of the thermal response naturally cools to room temperature to be reacted 2-5 days at 85~115 DEG C；
Described Zn-MOF fluorescent sensing materials are in Fe3+DMA solution in fluorescence be quenched completely, work as Fe3+Concentration is 10- 4Fluorescent quenching 81% during mol/L, works as Fe3+Concentration reaches 10-3During mol/L, fluorescence is quenched completely.Fluorometric investigation shows the material
To Fe3+Ion has very strong Selective recognition ability, can be used as detection Fe3+The fluorescent sensing material of ion.
Embodiment 1
The preparation of Zn-MOF fluorescent sensing materials：
Weigh zinc nitrate 0.07mmol and part H4L0.21mmol is placed in 10mL bottles, adds 3mL N, N- dimethyl
Formamide and 2 milliliters of water, it is sealed at 95 DEG C and reacts 3 days, water white transparency bulk crystals are obtained after being stored at room temperature.
To the sign of embodiment 1：
(1) crystal structure determination
As Figure 1-4, select that size is suitable, the preferable monocrystalline of crystal mass under the microscope, in Saturn70
Tested on (4x4bin mode) type Advances in crystal X-ray diffraction instrument, with the Mo K alpha rays through graphite monochromator monochromatizationWithMode collects diffraction data.All diffraction datas carry out semiempirical using SADABS programs and absorb school
Just.Cell parameter determines that data convert and structure elucidation use Crystalclear and SHELXTL respectively with least square method
Program is completed.Crystal structure is solved with direct method, first determines that whole non-hydrogen atoms are sat with difference function method and least square method
Mark, and hydrogen atom position is obtained with theoretical hydrogenation method, refine then is carried out to crystal structure with least square method.Predominant crystal
Parameter is learned to see the table below：
(2) powder diffraction characterizes phase purity：
As shown in figure 5, the powder diffraction data of embodiment 1 is collected on Rigaku D/Max-2500X- x ray diffractometer xs
Complete.
(3) IR Characterization：
The IR Characterization of embodiment 1 is collected by Tensor 27OPUS (Bruker) FT-IR radar stealthy materials, KBr tablettings, knot
Fruit is as shown in Figure 6.
(4) photoluminescent property of embodiment 1 is studied：
3mg embodiments 1 after grinding are added to 10-3In the mol/L DMA solution containing different cation nitrate,
Suspension is obtained after ultrasonic 30min, then its fluorescence is tested respectively by Hitachi F-4500 types XRF,
As a result it is as shown in Figure 7.After weighing the grinding of 3mg embodiments 1,10 are added to-3The DMA of mol/L different cation mixed nitrates
In solution, suspension is obtained after ultrasonic 30min, analyzes the anti-interference recognition capability of Zn-MOF fluorescent sensing materials.
The invention discloses a kind of Zn-MOF fluorescent sensing materials, its chemical formula is [Zn2(L)4(DMA)(H2O)]；H4L is
A kind of m benzene dicarboxylic acid class part of amido link modification, solvent are：DMAC N,N' dimethyl acetamide and water；The crystal yield of gained and
Purity is higher.Crystal parsing shows：The Zn-MOF fluorescent sensing materials crystal belongs to monoclinic system P21Space group, structure cell
Parameter is respectively：α=γ=90 °, β=99.98 (3) °；
Structure is：Its minimum asymmetric cell of described Zn-MOF fluorescent sensing materials includes the Zn of two crystallography independence2+Ion,
The ligand L of one complete deprotonation, a DMA molecule and a hydrone being coordinated；Two Zn in structure2+Ion is
Four-coordination, and double-core cluster is formed by three carboxyl bridgings, double-core cluster forms two-dimensional layer, two-dimensional layer by the bridging of isophthalic acid
Connect to form the three-dimensional structure containing duct further through ligand L；Zn-MOF fluorescent sensing materials have minimum transversal along a directions
FacePyriform duct, have along b directionsRectangle duct, the rhombus duct quilt having along c directions
The DMA molecules of coordination occupy.The porosity of Zn-MOF fluorescent sensing materials about 53.5%.Fluorometric investigation shows the material in Fe3+
DMA solution in fluorescence be quenched completely, work as Fe3+Concentration is 10-4Fluorescent quenching 81% during mol/L, works as Fe3+Concentration reaches 10- 3During mol/L, fluorescence is quenched completely.Fluorometric investigation shows the material to Fe3+Ion has very strong Selective recognition ability, can
As detection Fe3+The fluorescent sensing material of ion.
Above case study on implementation is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the field those of ordinary skill possessed knowledge, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., it is regarded as the protection domain of the application.
Claims (8)
- A kind of 1. Zn-MOF fluorescent sensing materials, it is characterised in that：Main body frame be represented by the chemical formula for：[Zn2(L)4(DMA) (H2O)], L is the part of the m benzene dicarboxylic acid of amido link modification in formula（H4L）Lose obtained by four hydrogen atoms；DMA is N, N- bis- Methylacetamide；H2O is hydrone.
- A kind of 2. Zn-MOF fluorescent sensing materials according to claim 1, it is characterised in that：Described Zn-MOF fluorescence passes Sense material crystals belong to monoclinic systemP21Space group, cell parameter are respectively：A=10.246 (2), b=16.147 (3), c =19.161 (4),α=γ =90o,β=99.98(3)o。
- A kind of 3. Zn-MOF fluorescent sensing materials according to claim 1, it is characterised in that：The Zn-MOF fluorescence senses Its structure of material is：Its minimum asymmetric cell includes the Zn of two crystallography independence2+Ion, complete deprotonation are matched somebody with somebody Body L, a DMA molecule and a hydrone being coordinated；Two Zn in structure2+Ion is four-coordination, and passes through three carboxyls Bridging forms double-core cluster, and double-core cluster forms two-dimensional layer by the bridging of isophthalic acid, and two-dimensional layer connects to be formed further through ligand L to be contained There is the three-dimensional structure in duct；Zn-MOF fluorescent sensing materials edgeaDirection has the pyriform duct of minimum cross-section 4 × 14, edgeb Direction has 3 × 12 rectangle duct, edgecThe DMA molecules that the rhombus duct that direction has is coordinated occupy, Zn-MOF The porosity of fluorescent sensing material about 53.5%.
- 4. the preparation method of Zn-MOF fluorescent sensing materials as claimed in claim 1, it is characterised in that：By zinc nitrate and part H4L is added in DMF solvent, and ultrasound becomes to solution and clarified after sealing, by gained mixture by solvent thermal reaction, is stored at room temperature After obtain water white transparency bulk crystals.
- A kind of 5. preparation method of Zn-MOF fluorescent sensing materials according to claim 4, it is characterised in that：Described nitre Sour zinc and part H4L mol ratios are 1:3~1.5:5.
- A kind of 6. preparation method of Zn-MOF fluorescent sensing materials according to claim 4, it is characterised in that：Described DMF/H2O solvent ratio is 3:2.
- A kind of 7. preparation method of Zn-MOF fluorescent sensing materials according to claim 1, it is characterised in that：The heat is anti- The solvent heat condition answered is 85~115oReacted 2-5 days under C, naturally cool to room temperature.
- 8. the Zn-MOF fluorescent sensing materials prepared such as claim 4, it is characterised in that：Fluorometric investigation shows the material to Fe3+ Ion has very strong Selective recognition ability, can be used as detection Fe3+The fluorescent sensing material of ion.
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| CN108586764A (en) * | 2018-05-04 | 2018-09-28 | 淮南师范学院 | A kind of zinc-base fluorescent material and preparation method thereof synthesized by solvent-induced strategy |
| CN110776649B (en) * | 2019-11-11 | 2021-10-26 | 重庆师范大学 | Cadmium-organic supramolecular polymer containing anthracene group and preparation method and application thereof |
| CN110776649A (en) * | 2019-11-11 | 2020-02-11 | 重庆师范大学 | Cadmium-organic supramolecular polymer containing anthracene group and preparation method and application thereof |
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| CN111662320B (en) * | 2020-06-03 | 2023-05-09 | 陕西科技大学 | Pb-MOF integrated fluorescence sensor and preparation method thereof |
| CN112142764A (en) * | 2020-09-30 | 2020-12-29 | 渤海大学 | Zinc complex and synthesis and fluorescent recognition of Fe thereof3+Method of ionizing |
| CN112142764B (en) * | 2020-09-30 | 2023-09-05 | 渤海大学 | Zinc complex and synthesis and fluorescence recognition Fe thereof 3+ Method for ion |
| CN114716879A (en) * | 2022-03-10 | 2022-07-08 | 华中科技大学 | Intelligent coating material for early warning of damage perception corrosion and application thereof |
| CN114716879B (en) * | 2022-03-10 | 2023-01-24 | 华中科技大学 | Intelligent coating material for early warning of damage perception corrosion and application thereof |
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