CN114262443A - Lanthanide metal organic framework material, and synthesis method and application thereof - Google Patents
Lanthanide metal organic framework material, and synthesis method and application thereof Download PDFInfo
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Abstract
The application relates to a lanthanide metal organic framework material, a synthesis method and application thereof, and discloses a hydrothermal method for preparing Ln (bmb)3·H2A method for preparing O (Ln ═ Tb, Eu) crystal is a high-quality way for preparing lanthanide-based novel complex scintillating material, wherein Hbmb is organic ligand 3- (benzimidazole-1-yl) benzoic acid, and the application also discloses a method for synthesizing Ln (bmb)3·H2Specific process of O (Ln ═ Tb, Eu) crystal. The scintillation crystal obtained by the method is in a monoclinic system P21The crystal in the/c space group is in a micron-scale flaky crystal shape, has good X-ray scintillation performance, and can be used as an excellent candidate material of a novel radiation detection scintillator.
Description
Technical Field
The application relates to synthesis of a lanthanide metal organic framework material, belonging to the technical field of scintillator material preparation.
Background
Scintillators are a class of materials that emit light upon absorption of high energy particles or radiation,plays an important role in the field of radiation detection, and the scintillator detector is one of the most widely used ionizing radiation detectors at present. Scintillator materials can be broadly classified as inorganic scintillators, such as CdWO4BGO, CsI, Tl, etc.; organic scintillators such as anthracene, stilbene, and the like; gas scintillators such as argon, xenon, and the like. With the development of many fields such as nuclear physics, medical diagnosis and energy detection, the requirement for scintillators is increasing day by day, and the influencing factors include chemical composition, electronic structure, chromophore interaction, crystal symmetry and atom density. Any material type currently used for radiation detection, including crystalline inorganic compounds, organic compounds, and plastics, has no inherent synthetic versatility, which can be systematically controlled. Thus, significant advances in scintillator materials may require the development of new materials outside the traditional scintillator range, and the search for new scintillating materials has become a hotspot of current research.
Lanthanide series metal organic framework materials (LnOFs) are novel scintillating materials and are special in Metal Organic Framework (MOFs) materials, and lanthanide series elements are used as metal elements in a framework structure to be coordinated with organic ligands, so that unique luminescent properties of the lanthanide series elements can be combined with flexible structural function adjustability of the MOFs, and the scintillator materials with excellent performance are designed. Lanthanide metal organic framework materials Ln (bmb) prepared by hydrothermal method in this application3·H2O (Ln ═ Tb, Eu), the preparation method is simple, and the material has good X-ray scintillation performance, and is expected to become a novel radiation detection scintillator material.
Disclosure of Invention
The lanthanide series metal organic framework material has the advantages of low production price, high yield, good X-ray scintillation performance and the like, and has a wide application value in the aspect of scintillator materials.
In order to achieve the above object, a first aspect of the present application provides a lanthanide metal-organic framework materialThe chemical formula of the lanthanide metal organic framework material is as follows: ln- (C)14N2O2H9)3·H2O，
The structural formula of the molecule is formed by that a minimum asymmetric molecular unit contains a metal Ln3+Ion, three bmb-Ligand molecule and a binding water molecule, Ln3+Ionic metal center with seven bmb-Six oxygen atoms and one nitrogen atom of the ligand are coordinated;
wherein Ln is selected from Tb and/or Eu, and bmb is 3- (benzimidazole-1-yl) benzoic acid.
Optionally, the lanthanide metal-organic framework material is monoclinic, P21The/c space group.
Alternatively, the lanthanide metal-organic framework material has a fluorescence lifetime of 1-1.5ms and 0.5-1ms, respectively, when Ln is selected from Tb and Eu.
A second aspect of the present application provides a method of lanthanide metal-organic framework material, comprising the steps of:
and (2) putting a mixture containing a lanthanide source, an organic connector, an auxiliary ligand and water into a closed container, and reacting to obtain the lanthanide metal organic framework material.
Optionally, the organic linker is 3- (benzimidazol-1-yl) benzoic acid.
The purpose of using 3- (benzimidazol-1-yl) benzoic acid as organic ligand is that only 3- (benzimidazol-1-yl) benzoic acid is able to successfully synthesize Tb (bmb) when the organic ligand is selected3·H2O and Eu (bmb)3·H2O two lanthanide metal organic frameworks, successfully found new ligands for these two lanthanide metals, an effect that could not be achieved with other organic ligands.
Optionally, the reaction temperature is 100-160 ℃, and the reaction time is 24-72 h.
Preferably, the reaction temperature is 140-160 ℃ and the reaction time is 48-72 h.
Optionally, the molar ratio of the auxiliary ligand to the lanthanide contained in the lanthanide source is 1 (1-3).
Preferably, the ancillary ligand is 2,2' -bipyridine.
The reason for adopting the preferable conditions is that 2,2' -bipyridyl is used as the auxiliary ligand, although the auxiliary ligand does not directly perform the complex reaction with lanthanide during the synthesis process, the reaction is promoted to be more complete, and larger Tb (bmb) can be obtained3·H2O and Eu (bmb)3·H2And (4) O yield.
Optionally, the lanthanide source is selected from Tb, Eu-containing compounds.
Alternatively, the ratio of the lanthanide source, organic linker, and water is (1-3mmol):1mmol:33 mL.
A third aspect of the present application provides the use of the material prepared according to the above-described material and preparation method as a radiation detecting scintillator material.
Through the technical scheme, the lanthanide metal organic framework material obtained by the method at least has the following beneficial effects:
(1) by using the method for producing a lanthanide metal-organic framework material described herein, the resulting lanthanide metal-organic framework material has a fluorescence lifetime on the order of at least milliseconds;
(2) two new lanthanide metal-organic framework materials were successfully synthesized by using 3- (benzimidazol-1-yl) benzoic acid as the ligand for the lanthanide metal element;
(3) by using the method for producing the lanthanide metal organic framework material, the yield of the obtained lanthanide metal organic framework material is more than or equal to 35%, and is improved by 10% compared with the method without using an auxiliary ligand;
(4) by using the production method disclosed by the application, the obtained lanthanide metal organic framework material shows strong characteristic emission peaks of respective metal centers under ultraviolet light and X-rays;
drawings
FIG. 1 shows a molecular structure of a sample in example 1 of the present application;
FIG. 2 shows a crystal structure of a sample in example 1 of the present application;
FIG. 3 shows an optical micrograph of a sample prepared in the present application, wherein FIG. (a) is Tb (bmb) described in example 13·H2O, FIG. b is Eu (bmb) described in example 43·H2Optical microscopy pictures of O;
FIG. 4 shows experimental and simulated powder XRD patterns of samples from example 1 of the present application;
FIG. 5 shows the hydrothermal preparation of a lanthanide metal organic framework material Ln (bmb)3·H2A flow chart of O (Ln ═ Tb, Eu);
FIG. 6 shows a fluorescence lifetime spectrum (PL) of a sample prepared in the present application, wherein FIG. (a) is Tb (bmb) described in example 13·H2O fluorescence lifetime spectrum, FIG. b shows Eu (bmb) described in example 43·H2A fluorescence lifetime map of O;
FIG. 7 shows an X-ray excitation emission spectrum of a sample prepared in the present application, wherein FIG. (a) is Tb (bmb) described in example 13·H2X-ray excitation emission spectrum of O, FIG. (b) is Eu (bmb) described in example 43·H2X-ray excitation emission spectrum of O.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The present application will be described in more detail with reference to the following embodiments and the accompanying drawings, but the present application is not limited to the following embodiments.
Starting materials used in examples and comparative examples, TbCl used3·H2O was purchased from Shanghai Aladdin Biotechnology, Inc. under the model number T100634. Eucl used3·H2O from Shanghai Aladdin Biotechnology LtdNumber E119161. 3- (benzimidazol-1-yl) benzoic acid was purchased from Jinan Heng Biotech, Inc. The deionized water is prepared by a water purifier Smart-Q30UT, and the ion rejection rate is 97-99%.
In the present application, the fluorescence lifetime is measured by a steady-state/transient fluorescence spectrometer of the type FLS1000, manufactured by edinburgh corporation, uk, under room temperature.
The synthesis used in the present application is summarized in FIG. 5.
Example 1
Weighing TbCl3·6H2O (0.1119g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. The filtered product is put into a drying oven to be dried for 6 hours at 65 ℃, and finally colorless and transparent flaky crystals Tb (bmb) are obtained3·H2O, yield of 36%, the molecular structure of the prepared crystalline material is shown in FIG. 1, and the molecular structure is represented by a formula in which a minimum asymmetric molecular unit contains a metal Ln3+Ion, three bmb-Ligand molecule and a binding water molecule, Ln3+Ionic metal center with seven bmb-Six oxygen atoms and one nitrogen atom of the ligand are coordinated. The arrangement of the overall crystals is shown in FIG. 2, and FIG. 2 shows a crystal composed of a plurality of molecules Ln (bmb)3·H2Crystal structure of O. An optical microscope photograph of the bulk crystal is shown in fig. 3 (a).
Example 2
Weighing TbCl3·6H2O (0.1119g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. Poly (IV) will be polymerizedAnd (3) ultrasonically treating the vinyl fluoride inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting into a drying oven. The drying oven was heated to 160 ℃ and kept at this temperature for 48 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. The filtered product is put into a drying oven to be dried for 6 hours at 65 ℃, and finally colorless and transparent flaky crystals Tb (bmb) are obtained3·H2O。
Example 3
Weighing TbCl3·6H2O (0.0373g, 0.1mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. The filtered product is put into a drying oven to be dried for 6 hours at 65 ℃, and finally colorless and transparent flaky crystals Tb (bmb) are obtained3·H2O。
Example 4
Weighing EuCl3·6H2O (0.1098g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. Drying the filtered product in a drying oven at 65 ℃ for 6 hours to finally obtain colorless and transparent flaky crystal Eu (bmb)3·H2O, yield 38%. An optical microscope photograph of the bulk crystal is shown in fig. 3 (b).
Example 5
Weighing EuCl3·6H2O (0.1098g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 160 ℃ and kept at this temperature for 48 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. Drying the filtered product in a drying oven at 65 ℃ for 6 hours to finally obtain colorless and transparent flaky crystal Eu (bmb)3·H2O。
Example 6
Weighing EuCl3·6H2O (0.0366g, 0.1mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. Drying the filtered product in a drying oven at 65 ℃ for 6 hours to finally obtain colorless and transparent flaky crystal Eu (bmb)3·H2O。
Example 7
Weighing Tb (NO)3)3·6H2O (0.1359g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying cabinet is heated to 140 ℃ and kept at this temperature for 72 hours, and then heatedThe temperature was decreased to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. The filtered product is put into a drying oven to be dried for 6 hours at 65 ℃, and finally colorless and transparent flaky crystals Tb (bmb) are obtained3·H2O。
Tb (bmb) obtained in the above manner3·H2O and Eu (bmb)3·H2The crystal of O was subjected to X-ray powder diffraction measurement, and Tb (bmb) obtained in example 1 was selected3·H2O and Eu (bmb) prepared in example 43·H2O as an example, the test results are shown in FIG. 4, and Eu/Tb (bmb) obtained by simulation3·H2The X-ray diffraction pattern of O is the same as that obtained in the examples of the present application, indicating that the target product can be successfully synthesized using the method of the present application.
For the synthesized Eu/Tb (bmb)3·H2Fluorescence lifetime and X-ray excitation tests were performed and are shown in fig. 6 and 7, respectively. In FIG. 6, (a) corresponds to Tb (bmb)3·H2O, (b) corresponds to Eu (bmb)3·H2And O. Fluorescence test finding, Tb (bmb)3·H2Fluorescence lifetime of O has exceeded 1ms, Eu (bmb)3·H2The fluorescence lifetime of O also reaches 0.8 ms; the X-ray excitation test chart shown in FIG. 7 reveals that Tb (bmb)3·H2O has a very good excitation response around a wavelength of 540nm, Eu (bmb)3·H2O also has a very good excitation response near a wavelength of 610 nm.
Comparative example 1
Weighing TbCl3·6H2O (0.1119g, 0.3mmol), 2- (2-Carboxylic acid phenyl) imidazole (4,5-f) (1,10) O-phenanthroline (Hnpc,0.1020g, 0.3mmol), 2' -bipyridine (0.0468g, 0.3mmol) were placed in a 25ml Teflon liner, and 10ml deionized water was added. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. Filtering the obtained product with filter paper whileWashing with deionized water. The filtered product was dried in a drying oven at 65 ℃ for 6 hours to obtain the final product.
Comparative example 2
Weighing TbCl3·6H2O (0.1119g, 0.3mmol), 3- (benzimidazol-1-yl) benzoic acid (Hbmb,0.0714g, 0.3mmol) were placed in a 25ml Teflon liner, followed by 10ml deionized water. And (3) carrying out ultrasonic treatment on the polytetrafluoroethylene inner container in an ultrasonic cleaning machine for 10 minutes, then putting the polytetrafluoroethylene inner container into a stainless steel water heating tank, screwing and putting the polytetrafluoroethylene inner container into a drying box. The drying oven was heated to 140 ℃ and kept at this temperature for 72 hours, and then cooled to room temperature at a rate of 3 ℃/h. The resulting product was filtered through filter paper while being washed with deionized water. The filtered product is put into a drying oven to be dried for 6 hours at 65 ℃, and finally colorless and transparent flaky crystals Tb (bmb) are obtained3·H2O, yield 25% (based on Tb).
From the above examples and comparative examples, it is considered that the lanthanide metal organic frameworks Ln (bmb) described in the present application can be successfully prepared using Hbmb as an organic ligand3·H2And O. The addition of the auxiliary ligand 2,2' -bipyridine in the preparation process effectively promotes the production of the product and improves the yield by at least 10%.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (9)
1. A lanthanide metal-organic framework material, wherein the lanthanide metal-organic framework material has the formula: ln- (C)14N2O2H9)3·H2O, the structural formula of the molecule is formed by that a minimum asymmetric molecular unit contains a metal Ln3+Ion, three bmb-Ligand moietyA molecule of a binding water, Ln3+Ionic metal center with seven bmb-Six oxygen atoms and one nitrogen atom of the ligand are coordinated;
wherein Ln is selected from Tb and/or Eu, and bmb is 3- (benzimidazole-1-yl) benzoic acid.
2. The lanthanide metal-organic framework material of claim 1, wherein the lanthanide metal-organic framework material is monoclinic, P21The/c space group.
3. The lanthanide metal-organic framework material of claim 2, wherein the lanthanide metal-organic framework material has a fluorescence lifetime of 1-1.5ms and 0.5-1ms, respectively, when Ln is selected from Tb and Eu.
4. A method for preparing a lanthanide metal-organic framework material as defined in any one of claims 1-3, comprising the steps of:
putting a mixture containing a lanthanide source, an organic connector, an auxiliary ligand and water into a closed container, and reacting to obtain the lanthanide metal organic framework material;
the organic linker is 3- (benzimidazol-1-yl) benzoic acid.
5. The method of claim 4, wherein the ratio of lanthanide source, organic linker, and water is (1-3mmol):1mmol:33 mL;
wherein, the lanthanide source is used in a molar ratio based on the lanthanide contained therein.
6. The method of claim 4, wherein the ancillary ligand is 2,2' -bipyridine;
preferably, the molar ratio of the auxiliary ligand to the lanthanide contained in the lanthanide source is 1 (1-3).
7. The method according to claim 4, wherein the lanthanide source is selected from soluble salts corresponding to the Tb element and/or soluble salts corresponding to the Eu element;
preferably, the soluble salt corresponding to Tb is TbCl3；
The soluble salt corresponding to Eu element is EuCl3。
8. The method according to claim 4, characterized in that the reaction conditions are: the reaction temperature is 100-160 ℃, and the reaction time is 24-72 h;
preferably, the reaction temperature is 140-160 ℃, and the reaction time is 48-72 h.
9. Use of a lanthanide metal-organic framework material as defined in any one of claims 1-3 and/or a lanthanide metal-organic framework material prepared according to the method defined in claims 4-8 as a radiation-detecting scintillator material.
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