CN107384373A - One kind has selectivity detection Fe3+Luminescent crystal material of ion and preparation method thereof - Google Patents
One kind has selectivity detection Fe3+Luminescent crystal material of ion and preparation method thereof Download PDFInfo
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- CN107384373A CN107384373A CN201710543173.1A CN201710543173A CN107384373A CN 107384373 A CN107384373 A CN 107384373A CN 201710543173 A CN201710543173 A CN 201710543173A CN 107384373 A CN107384373 A CN 107384373A
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- 239000000463 material Substances 0.000 title claims abstract description 56
- 239000013078 crystal Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 150000002500 ions Chemical class 0.000 title claims abstract description 23
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 32
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011701 zinc Substances 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 17
- WVDRSXGPQWNUBN-UHFFFAOYSA-N 4-(4-carboxyphenoxy)benzoic acid Chemical class C1=CC(C(=O)O)=CC=C1OC1=CC=C(C(O)=O)C=C1 WVDRSXGPQWNUBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 2
- 150000000178 1,2,4-triazoles Chemical class 0.000 abstract 1
- UOFDVLCOMURSTA-UHFFFAOYSA-N 2-(2-carboxyphenoxy)benzoic acid Chemical class OC(=O)C1=CC=CC=C1OC1=CC=CC=C1C(O)=O UOFDVLCOMURSTA-UHFFFAOYSA-N 0.000 abstract 1
- 150000003852 triazoles Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 150000001768 cations Chemical class 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 11
- 238000002189 fluorescence spectrum Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 125000002091 cationic group Chemical group 0.000 description 6
- 150000002460 imidazoles Chemical class 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000002178 crystalline material Substances 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 206010022971 Iron Deficiencies Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
-
- 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
- C07F3/06—Zinc compounds
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- 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
- C09K2211/188—Metal complexes of other metals not provided for in one of the previous groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses one kind to have selectivity detection Fe3+Luminescent crystal material of ion and preparation method thereof, the chemical formula of the luminescent crystal material is [Zn (OBA) (3 abit)]n, belong to anorthic system, space group is P 1, and cell parameter is α=73.382 (2) °, β=76.088 (2) °, γ=80.229 (2) °, Z=2.Its preparation process comprises the following steps：By zinc nitrate and 4,4 ' oxydibenzoic acids, which are added in the aqueous solution, to be stirred, by 4 amino 3,5 two (imidazolmethyls) 1,2,4 triazoles, which are added in methanol solution, to be stirred, by zinc nitrate obtained above and 4, the aqueous solution of 4 ' oxydibenzoic acids is placed in reaction tube and adds buffer solvent, again by (imidazolmethyl) 1,2 of 4 amino 3,5 two, the methanol solution of 4 triazoles is slowly added into reaction tube, through crystallizing, filtering, washing, drying to obtain luminescent crystal material [Zn (OBA) (3 abit)] after sealingn.Luminescent crystal material prepared by the present invention is to Fe3+The selective Effect on Detecting of ion, and the chemistry of luminescent crystal material, optical stability are good.
Description
Technical field
The present invention relates to the preparation of metal cation detection material, and in particular to one kind has selectivity detection Fe3+Ion
Luminescent crystal material and preparation method thereof.
Background technology
With the fast development of global industry, iron and its alloy have become in the world using most a kind of metal materials
Material, because it has numerous good performances, makes it be widely used in the national economy such as machinework, catalyst, metallurgical product
Every field, provide strong favourable support for economic development.Meanwhile ferro element is also the essential element for forming human body
One of, it is not only the pith of hemoglobin, or many enzymes and the composition of immune system compound, and can participate in
The transport and storage of oxygen, have the function that important to health.However, the fast development of industry result in substantial amounts of Fe3+From
Son is discharged into environment water, and serious threat is caused to environment etc.；Simultaneously in human body, iron deficiency and Fe supply can be to them
Cause very big injury, such as anaemia, heart and liver diseases, diabetes.Therefore effective detection Fe3+Ion pair environment and
Health is extremely important.In the various Detection Techniques reported, the chemistry based on fluorescence coordination polymer
Sensing is because it has the characteristics that high sensitivity and high selectivity, cheap and easy to get, easy has flexibly turned into current numerous scientific research people
The emphasis of member's research.Such as document Dalton Trans., 2013,42,12403-12409 and Inorg.Chem.2016,55,
3952-3959 is reported with Fe3+The luminous complex of ion detection performance.
The content of the invention
In order to solve the above technical problems, the present invention, which provides one kind, has selectivity detection Fe3+The luminescent crystal material of ion
And preparation method thereof；Used technical scheme is：
It is described that there is selectivity detection Fe3+The luminescent crystal material of ion, its chemical formula are [Zn (OBA) (3-abit)]n,
Belong to anorthic system, space group P-1, cell parameter isα=
73.382 (2) °, β=76.088 (2) °, γ=80.229 (2) °, Z=2.The crystalline material structure is as shown in figure 1, be by four
A kind of one-dimensional trapezoidal skeleton structure that the Zn of connection and two kinds of bridge ligand OBA, 3-abit constructions form.
Further, the preparation method of the luminescent crystal material comprises the following steps：
(1) zinc nitrate and 4,4 '-oxydibenzoic acid (OBA) are added in the aqueous solution, stir 3-6 minutes, and add
Alkaline solution adjusts pH to 6-8；
(2) (the imidazolmethyl) -1,2,4- triazoles (3-abit) of 4- amino -3,5- two are added in methanol solution and stirred
Mix 5-7 minutes；
(3) obtained solution in step (1) is placed in reaction tube, and adds buffer solvent, be slowly added in step (2)
Obtained solution, through crystallizing, filtering, washing, drying to obtain luminescent crystal material [Zn (OBA) (3-abit)] after sealingn。
Further, it is provided by the invention that there is selectivity detection Fe3+In the preparation method of the luminescent crystal material of ion,
Start material zinc nitrate, 4,4 '-oxydibenzoic acid, 4- amino -3,5- bis- (imidazolmethyl) -1, mole of 2,4- triazoles
Than for 1：0.5~1：0.5~1.
Further, it is provided by the invention that there is selectivity detection Fe3+The preparation method of the luminescent crystal material of ion
In, the buffer solvent is CH3OH and H2O mixed solution, wherein CH3OH and H2O volume ratio is 1：0.5~1.
By luminescent crystal material provided by the invention not only to Fe3+The selective Effect on Detecting of ion, it is produced
Fluorescence intensity obvious quenching effects occur, and effect is not quenched to the fluorescence intensity of other metal cations significantly then
Fruit, and the chemistry of luminescent crystal material, optical stability are good；Not only reacted in the preparation process of luminescent crystal material simultaneously
Beginning thing is cheap and easy to get, and cost is relatively low, and preparation condition is gentle, easily controllable.Detected by X-ray diffraction pattern, the present invention
Prepared luminescent crystal material [Zn (OBA) (3-abit)]nPowder x-ray diffraction pattern and theoretical calculation X-ray
Diffraction pattern is basically identical, illustrates the crystalline material [Zn (OBA) (3-abit)] prepared by the present inventionnWith very high purity.
Brief description of the drawings
Fig. 1 is the luminescent crystal material [Zn (OBA) (3-abit)] of the present inventionnOne-dimentional structure figure；
Fig. 2 is the luminescent crystal material [Zn (OBA) (3-abit)] of the present inventionnOne-dimentional structure figure partial enlarged drawing；
Fig. 3 is 1 milligram of luminescent crystal material [Zn (OBA) (3-abit)]nVolume be 3 milliliters, solubility be 0.01 to rub
You/liter the metal cation aqueous solution in fluorescence spectra (excitation wavelength 350nm)；
Fig. 4 is fluorescence column diagram corresponding to Fig. 3 fluorescence spectras；
Fig. 5 is the luminescent crystal material [Zn (OBA) (3-abit)] of the present inventionnPowder X-ray diffractogram.
Embodiment
Preparation method of the present invention is described further with specific embodiment below in conjunction with accompanying drawing.
Embodiment 1：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.1mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 4 minutes in liquid, and add sodium hydroxide solution regulation pH to 6；(2) by 0.1mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 6 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：1, then obtained solution in step (2) is added in reaction tube, after sealing through crystallizing, filtering, washing, drying to obtain is sent out
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
As shown in Figure 3 and Figure 4, luminescent crystal material provided by the invention is each not to the fluorescence spectrum of different metal cation
It is identical, wherein to Fe3+Ion is far below other metal cations, selective Effect on Detecting, its caused fluorescence intensity
The obvious quenching effects of generation, and there is no obvious quenching effects then to the fluorescence intensity of other metal cations.
3rd, X-ray diffraction is analyzed：The powder of the luminescent crystal material (5mg) of preparation is put into X-ray diffractometer and carried out
Diffraction pattern is analyzed.
As shown in figure 5, detected by X-ray diffraction pattern, the luminescent crystal material [Zn (OBA) prepared by the present invention
(3-abit)]nX-ray diffraction pattern and theoretical calculation X-ray diffraction pattern it is basically identical, illustrate prepared by the present invention
Crystalline material [Zn (OBA) (3-abit)]nWith very high purity.
Embodiment 2：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.05mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 5 minutes in liquid, and add sodium hydroxide solution regulation pH to 6；(2) by 0.05mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 5 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：0.5, then obtained solution in step (2) is added in reaction tube, through crystallizing, filtering, washing, drying to obtain after sealing
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
3rd, X-ray diffraction is analyzed：Luminescent crystal material (5mg) powder of preparation is put into X-ray diffractometer and spread out
Penetrate Interferogram Analysis.
Embodiment 3：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.05mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 5 minutes in liquid, and add sodium hydroxide solution regulation pH to 7；(2) by 0.1mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 5 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：1, then obtained solution in step (2) is added in reaction tube, after sealing through crystallizing, filtering, washing, drying to obtain is sent out
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
3rd, X-ray diffraction is analyzed：Luminescent crystal material (5mg) powder of preparation is put into X-ray diffractometer and spread out
Penetrate Interferogram Analysis.
Embodiment 4：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.05mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 5 minutes in liquid, and add sodium hydroxide solution regulation pH to 7；(2) by 0.05mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 5 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：0.5, then obtained solution in step (2) is added in reaction tube, through crystallizing, filtering, washing, drying to obtain after sealing
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
3rd, X-ray diffraction is analyzed：Luminescent crystal material (5mg) powder of preparation is put into X-ray diffractometer and spread out
Penetrate Interferogram Analysis.
Embodiment 5：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.1mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 3 minutes in liquid, and add sodium hydroxide solution regulation pH to 8；(2) by 0.05mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 7 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：0.5, then obtained solution in step (2) is added in reaction tube, through crystallizing, filtering, washing, drying to obtain after sealing
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
3rd, X-ray diffraction is analyzed：Luminescent crystal material (5mg) powder of preparation is put into X-ray diffractometer and spread out
Penetrate Interferogram Analysis.
Embodiment 6：
1st, the preparation of luminescent crystal material：Comprise the following steps：
(1) 0.1mmol zinc nitrate and 0.05mmol 4,4 '-oxydibenzoic acid (OBA) are added to the water-soluble of 5mL
Stirred 5 minutes in liquid, and add sodium hydroxide solution regulation pH to 8；(2) by 0.05mmol (the imidazoles first of 4- amino -3,5- two
Base) -1,2,4- triazoles (3-abit) are added in 5mL methanol solution, are stirred 5 minutes；(3) will be obtained in step (1)
Solution is placed in reaction tube and adds 3mL CH3OH and H2The CH of O buffer solvents, wherein buffer solvent3OH and H2O volume ratio
For 1：0.5, then obtained solution in step (2) is added in reaction tube, through crystallizing, filtering, washing, drying to obtain after sealing
Luminescent crystal material [Zn (OBA) (3-abit)] n；
2、Fe3+Ion selectivity detection performance is tested：The luminescent crystal material (1 milligram) of preparation is added to volume as 3
In milliliter, the metal cation aqueous solution that solubility is 0.01 mol/L, ultrasonic two hours obtained stable suspensions, Ran Hou
The fluorescence spectrum of different cationic aqueous solutions is determined under 350nm exciting lights.
3rd, X-ray diffraction is analyzed：Luminescent crystal material (5mg) powder of preparation is put into X-ray diffractometer and spread out
Penetrate Interferogram Analysis.
Above-mentioned embodiment is used for illustrative purposes only, and is not limitation of the present invention, relevant technical field
Those of ordinary skill, can be so that various changes can be made and modification without departing from the spirit and scope of the present invention, therefore institute
There is equivalent technical scheme also to belong to scope of the invention.
Claims (4)
1. one kind has selectivity detection Fe3+The luminescent crystal material of ion, it is characterised in that：The change of the luminescent crystal material
Formula is [Zn (OBA) (3-abit)]n, belong to anorthic system, space group P-1, cell parameter is α=73.382 (2) °, β=76.088 (2) °, γ=
80.229 (2) °, Z=2.
2. there is selectivity detection Fe described in a kind of claim 13+The preparation method of the luminescent crystal material of ion, including with
Lower step：
(1) zinc nitrate and 4,4 '-oxydibenzoic acid are added in the aqueous solution, stir 3-6 minutes, and add alkaline solution tune
Save pH to 6-8；
(2) 4- amino -3,5- two (imidazolmethyl) -1,2,4- triazoles are added in methanol solution and stirred 5-7 minutes；
(3) obtained solution in step (1) is placed in reaction tube, and adds buffer solvent, be slowly added to obtain in step (2)
Solution, through crystallizing, filtering, washing, drying to obtain luminescent crystal material [Zn (OBA) (3-abit)] after sealingn。
3. according to claim 2 have selectivity detection Fe3+The preparation method of the luminescent crystal material of ion, its feature
It is that zinc nitrate, 4,4 '-oxydibenzoic acid, the mol ratio of 4- amino -3,5- two (imidazolmethyl) -1,2,4- triazoles are 1：
0.5~1：0.5~1.
4. according to claim 2 there is selectivity detection to detect Fe3+The preparation method of the luminescent crystal material of ion, its
It is characterised by, the buffer solvent is CH3OH and H2O mixed solution, wherein CH3OH and H2O volume ratio is 1：0.5~1.
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| CN106866989A (en) * | 2017-01-20 | 2017-06-20 | 江南大学 | One kind has selectivity detection Fe3+The preparation method of the luminescent crystal material of ion |
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| CN108034990A (en) * | 2017-12-08 | 2018-05-15 | 江南大学 | Can highly sensitive detection 2,4,6- trinitrophenols luminescent crystal material preparation |
| CN108034990B (en) * | 2017-12-08 | 2019-08-06 | 江南大学 | Can it is highly sensitive detection 2,4,6- trinitrophenol luminescent crystal material preparation |
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