CN105860087B - Cadmium metal coordination polymer having fluorescence effect and preparation method thereof - Google Patents
Cadmium metal coordination polymer having fluorescence effect and preparation method thereof Download PDFInfo
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- CN105860087B CN105860087B CN201610196540.0A CN201610196540A CN105860087B CN 105860087 B CN105860087 B CN 105860087B CN 201610196540 A CN201610196540 A CN 201610196540A CN 105860087 B CN105860087 B CN 105860087B
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Abstract
The invention discloses a cadmium metal coordination polymer having the fluorescence effect and the preparation method thereof. The molecular formula of the coordination polymer is {Cd[(C10H5N3O5(H2O)2]}n. The coordination compound belongs to a monoclinic system, and the space group thereof is C2/c. Cd atom is positioned at the center of the octahedral configuration of a hexa-coordinate. The preparation method of the coordination polymer is simple and controllable, and crystals prepared through the solvothermal method are stable in structure. The fluorescence analysis of the coordination polymer shows that, when the excitation wavelength is set at 360 nm, a strong emission band appears at 466 nm. Based on the fluorescence effect of the coordination polymer, the coordination polymer can be applied to the fields of illumination, display, solid-state laser, optical communications, optical storage, biomedical imaging, diagnosis, treatment and the like.
Description
Technical field
The invention belongs to fluorescent material technical field, and in particular to a kind of cadmium metal polycomplexation of blue-fluorescence luminescent material
Compound and preparation method thereof.
Background technology
Metal-organic framework (MOFs) is recent two decades by a kind of porous material of academia's extensive concern, this material
Material is the supramolecular network structure being self-assembly of using the metal-ligand coordinate effect between organic ligand and metal ion.
Early stage MOFs develops, the O.M.Yaghi of Univ California-Berkeley professor, Kyoto Univ Japan
S.Kitagawa teaches Wenbin professors Lin with University of North Carolina of U.S. church mountain branch school etc. it has been done specifically respectively
Definition, be defined as follows by induction and conclusion：MOFs is used as first stability, programmable, crystalline state class zeolitic material
Need to possess following condition：(1) by being coordinated bond formed rock-steady structure；(2) by design transformation organic ligand (linker) and gold
Secondary construction unit (SBU) type of category can be with the space structure of controlled material；(3) with good crystallinity thus can accurately determine
Adopted its coordination structure and steric configuration.As its name suggests, micropore metal-organic frame (MOFs) is referred to and have in framework certain quilt
The duct (aperture is within 2nm) of free solvent molecule filling simultaneously can be removed guest molecule in duct by method for subsequent processing
And do not affect the porous material of frame structure.
Heterocyclic carboxylic acid such as pyridine -2,6- dicarboxylic acids, 2,3- pyrazine acids, pyridine -3,4- dicarboxylic acids and 4,5- imidazole-2-carboxylic acid
Deng often being used for studying the structure of coordination polymer as part, however, coordinate lanthanide series and 2- (N- aoxidizes -4- pyridines) -
4,5- imidazole-2-carboxylic acid (H3DCImPyO) even less people is in research.H3DCImPyO has seven potential coordination atoms, can be formed
Higher-dimension structure, and by careful control ph, it can protonate one to three hydrogen atom and form HnDCImPyO (n=0,
1,2).Therefore, deprotonation HnDCImPyO (n=0,1,2) with flexible coodination modes.
By H3DCImPyO constitutes rimless frame system advantageously, it has been found that and selecting H with metallic element3DCImPyO is used as one
Individual organic component, attempts a kind of metal-organic framework with new architectural feature of composition and there is no research.From
H3Used as organic ligand, under the conditions of solvent-thermal method, the crystal generated with slaine or rare earth metal reaction is showed DCImPyO
Go out good heat endurance and stronger fluorescence, can be applicable to illuminate, show, solid state laser, optical communication, optical storage and
The numerous areas such as biomedical imaging, Clinics and Practices.
The content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention to provide a kind of one-dimensional { Cd
[(C10H5N3O5)(H2O)2]}nCoordination polymer and preparation method thereof, with simple controllable preparation have good heat endurance and
Stronger epipolic coordination polymer.
Technical scheme：For achieving the above object, the present invention is employed the following technical solutions：
A kind of metal cadmium coordination polymer with fluorescent effect, the general molecular formula of the coordination polymer is { Cd
[(C10H5N3O5)(H2O)2]}n.Wherein it is construction unit in braces, that is, repetitive, n repeateding unit numbers.
Preferably, the coordination polymer is one-dimensional catenary structure, and intermolecular there is hydrogen bond.
Preferably, the secondary building unit of the coordination polymer is：Crystal belongs to monoclinic system, and space group is C2/
C, Cd atoms are among the octoploids structure of hexa-coordinate in the structure.
Preferably, the excitation wavelength of the coordination polymer is 360nm, and launch wavelength is 466nm.It is described to imitate with fluorescence
The metal cadmium coordination polymer answered can be applicable to illuminate, show, solid state laser, optical communication, optical storage, biomedical imaging with
And Clinics and Practices field.
The preparation method of above-mentioned metal cadmium coordination polymer, from H3DCImPyO is used as part, Cd (NO3)2·4H2O makees
Slaine, is well mixed in organic solvent, and using solvent-thermal method the coordination polymer crystal is prepared, including following step
Suddenly：
Under room temperature, by part 2- (N- aoxidizes -4- pyridines) -4,5- imidazole-2-carboxylic acid H3DCImPyO and Cd (NO3)2·4H2O
It is well mixed in DMF or ethanol, is put in reactor and heats, the coordination polymer crystal is obtained after cooling.
Preferably, the H3DCImPyO and Cd (NO3)2·4H2The mol ratio 1 of O：1.
Preferably, one or both mixed liquor of the organic solvent in DMF, ethanol.
Preferably, the solvent ratio of DMF and ethanol is 1 in the mixed liquor:1(v:v).
Preferably, the condition of the heating is heated three days for 105 DEG C.
Preferably, under room temperature, by part 2- (N- aoxidizes -4- pyridines) -4,5- imidazole-2-carboxylic acid H3DCImPyO 1mmol with
Cd(NO3)2·4H2O 1mmol are well mixed in the mixed liquor of 2mLDMF and 2mL ethanol, are put into 105 DEG C of heating in reactor
Three days, the coordination polymer crystal is obtained after cooling.
Beneficial effect：Compared with prior art, the present invention provide the metal cadmium coordination polymer with fluorescent effect and
Its preparation method, with advantages below：
(1) general molecular formula of the coordination polymer is { Cd [(C10H5N3O5)(H2O)2]}n, the complex belongs to monocline
Crystallographic system, space group is C2/c；
(2) under the coordination polymer is by solvent-thermal method-high-temperature and high-pressure conditions-by solvent self assembly, coordination
Polymer architecture stability is higher, controllability is stronger, and preparation method is simple, easy to operate；
(3) fluorescence analysis of the coordination polymer shows when excitation wavelength is set at 360nm, can go out at 466nm
Now strong emission band, sends out blue-fluorescence；The strong transmitting fluorescence property that the coordination polymer possesses make its can apply to illumination,
The numerous areas such as display, solid state laser, optical communication, optical storage and biomedical imaging, Clinics and Practices.
Description of the drawings
Fig. 1 is coordination polymer { Cd [(C in embodiment 310H5N3O5)(H2O)2]}nCoordination context diagram；
Fig. 2 is coordination polymer { Cd [(C in embodiment 310H5N3O5)(H2O)2]}nChain structure containing part；
Fig. 3 is coordination polymer { Cd [(C in embodiment 310H5N3O5)(H2O)2]}nInfrared spectrogram；
Fig. 4 is coordination polymer { Cd [(C in embodiment 310H5N3O5)(H2O)2]}nThermogravimetric analysis figure；
Fig. 5 is coordination polymer { Cd [(C in embodiment 310H5N3O5)(H2O)2]}nFluorescence analysis figure.
Specific embodiment
The present invention is further explained with reference to the accompanying drawings and examples.
Embodiment 1
During room temperature, by 1mmol Cd (NO3)2·4H2O and 1mmol H3DCImPyO is thoroughly mixed in 4ml DMF,
Reactor is put into, 105 DEG C of constant temperature is heated three days in convection oven, is obtained by solvent-thermal method self assembly a kind of with fluorescence
The coordination polymer of matter.
Embodiment 2
During room temperature, by 1mmol Cd (NO3)2·4H2O and 1mmol H3DCImPyO is thoroughly mixed in 4ml ethanol,
Reactor is put into, 105 DEG C of constant temperature is heated three days in convection oven, is obtained by solvent-thermal method self assembly a kind of with fluorescence
The coordination polymer of matter.
Embodiment 3
During room temperature, by 1mmol Cd (NO3)2·4H2O and 1mmol H3DCImPyO is abundant in 2ml DMF and 2ml ethanol
Stirring mixing, is put into reactor, and 105 DEG C of constant temperature is heated three days in convection oven, and one kind is obtained by solvent-thermal method self assembly
Coordination polymer with photoluminescent property.
By contrast above-described embodiment 1-3, under the conditions of temperature and part and slaine identical, only solvent DMF with
In the case of the volume ratio difference of EtOH, in solvent volume 1 is compared:Under the conditions of 1, i.e. embodiment 3, resulting crystal is optimum
's.This material is that, by passing through solvent self assembly under solvent-thermal method-high-temperature and high-pressure conditions, material structure stability is higher,
And the structural controllability of this material is stronger, preparation method is simple, easy to operate.
Coordination polymer crystal in embodiment 3 is analyzed, the monocrystalline of suitable size, room temperature are chosen under the microscope
When with Jing graphite monochromatised Mo K alpha raysMonocrystalline is determined on Bruker Apex II CCD diffractometers
X-ray diffraction structure, the results are shown in Table 1.Semiempirical absorption correction, cell parameter least square method are carried out with SADABS methods
It is determined that, data convert and structure elucidation are completed respectively using SAINT and SHELXL program bags, and all non-hydrogen atoms complete matrix is most
Little square law carries out anisotropy refine, and the coordination context diagram of coordination polymer is as shown in figure 1, the N of Cd (II) and two imidazoles
Atom and two carboxylate oxygen atoms and two O atoms provided by two lattice watters are coordinated, and are somewhat distorted so as to constitute
Octahedral environment.
The crystallographic data of coordination polymer prepared by 1 embodiment of table 3
Fig. 2 is one-dimensional catenary structure figure of the coordination polymer containing part：Central atom Cd atoms in structure are in six
Among the octoploids structure of coordination；Cd atoms and N atoms, are connected with each other by N-Cd-N keys, form chain structure.
Infrared spectrum characterization to the coordination polymer in embodiment 3, as shown in Figure 3.In 845cm-1Place, has one strongly
Absworption peak, be benzene contraposition replace absworption peak；In 1198cm-1There is a strong absworption peak, be C=O double bond stretching vibrations
Absworption peak；In 1275cm-1There is a strong absworption peak, be C-N key stretching vibration absworption peaks；In 1560cm-1Place, there is one
Strong absworption peak, is the absworption peak of phenyl ring；In 2357cm-1Place, is the absworption peak of carboxylic acid；In 3361cm-1Place, has one by force
Strong absworption peak, is the absworption peak of O-H keys.
Thermogravimetric analysis to the coordination polymer in embodiment 3 is characterized, as shown in figure 4, can be seen that from thermogravimetric analysis
Coordination polymer has two obvious weight loss processes.It is the loss of lattice watter in coordination polymer at wherein first, the
It is that disintegrating for the coordination polymer structure is caved at two.
Fig. 5 is analyzed for the solid fluorescence of coordination polymer, and the fluorescence analysis of the coordination polymer shows when excitation wavelength quilt
When being set in 360nm, can 466nm at the strong emission band of appearance, and the blue-fluorescence effect that it has, can be applicable to illumination,
The numerous areas such as display, solid state laser, optical communication, optical storage and biomedical imaging, Clinics and Practices.
Above example simply plays explanation example effect to the technology design of the present invention, can not limit the present invention with this
Protection domain, those skilled in the art modify and are equal in the spirit and scope without departing from technical solution of the present invention
Replace, all should fall within the scope and spirit of the invention.
Claims (10)
1. a kind of metal cadmium coordination polymer with fluorescent effect, it is characterised in that：The general molecular formula of the coordination polymer
For { Cd [(C10H5N3O5)(H2O)2]}n；The preparation method of the coordination polymer prepares coordination polymer using solvent-thermal method
Crystal, comprises the steps：Under room temperature, by part 2- (N- aoxidizes -4- pyridines) -4,5- imidazole-2-carboxylic acid H3DCImPyO and Cd
(NO3)2·4H2O is well mixed in organic solvent, is put in reactor and heats, and the coordination polymer is obtained after cooling brilliant
Body；The H3DCImPyO and Cd (NO3)2·4H2The mol ratio 1 of O：1.
2. the metal cadmium coordination polymer with fluorescent effect according to claim 1, it is characterised in that：The polycomplexation
Compound is one-dimensional catenary structure, and intermolecular there is hydrogen bond.
3. the metal cadmium coordination polymer with fluorescent effect according to claim 1, it is characterised in that：The polycomplexation
The secondary building unit of compound is：Crystal belongs to monoclinic system, and space group is C2/c, and Cd atoms are in six in the structure
Among the octoploids structure of coordination.
4. the metal cadmium coordination polymer with fluorescent effect according to claim 1, it is characterised in that：The polycomplexation
The excitation wavelength of compound is 360nm, and launch wavelength is 466nm.
5. a kind of preparation method of the metal cadmium coordination polymer with fluorescent effect as described in any one of claim 1-4,
It is characterized in that：The preparation method prepares the coordination polymer crystal using solvent-thermal method, comprises the steps：
Under room temperature, by part 2- (N- aoxidizes -4- pyridines) -4,5- imidazole-2-carboxylic acid H3DCImPyO and Cd (NO3)2·4H2O is having
It is well mixed in machine solvent, is put in reactor and heats, the coordination polymer crystal is obtained after cooling.
6. the preparation method of the metal cadmium coordination polymer with fluorescent effect according to claim 5, it is characterised in that：
The H3DCImPyO and Cd (NO3)2·4H2The mol ratio 1 of O：1.
7. the preparation method of the metal cadmium coordination polymer with fluorescent effect according to claim 5, it is characterised in that：
One or both mixed liquor of the organic solvent in DMF, ethanol.
8. the preparation method of the metal cadmium coordination polymer with fluorescent effect according to claim 7, it is characterised in that：
The solvent ratio of DMF and ethanol is 1 in the mixed liquor:1(v:v).
9. the preparation method of the metal cadmium coordination polymer with fluorescent effect according to claim 5, it is characterised in that：
The condition of the heating is 105 DEG C and heats three days.
10. the preparation method of the metal cadmium coordination polymer with fluorescent effect according to any one of claim 5-9, its
It is characterised by：Under room temperature, by part 2- (N- aoxidizes -4- pyridines) -4,5- imidazole-2-carboxylic acid H3DCImPyO 1mmol and Cd
(NO3)2·4H2O 1mmol are well mixed in the mixed liquor of 2mLDMF and 2mL ethanol, are put into 105 DEG C of heating three in reactor
My god, the coordination polymer crystal is obtained after cooling.
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| CN108676171B (en) * | 2018-04-28 | 2023-08-15 | 镇江市高等专科学校 | Olefin copper coordination polymer with orange fluorescence effect and preparation method thereof |
| CN109467711B (en) * | 2018-11-01 | 2021-06-08 | 陕西科技大学 | Cd coordination polymer iodine vapor load material and preparation method and application thereof |
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| CN103450234A (en) * | 2013-07-29 | 2013-12-18 | 南开大学 | Cadmium coordination polymer and preparation method thereof |
| CN103554083A (en) * | 2013-11-11 | 2014-02-05 | 吉林化工学院 | Monocrystal structure of cadmium coordination compound with blue light performance and preparation method thereof |
| CN103880871A (en) * | 2014-04-03 | 2014-06-25 | 哈尔滨工业大学 | Cadmium coordination polymer with 0D-to-2D double-interpenetration structure, and synthesis method thereof |
| CN103980301A (en) * | 2014-05-22 | 2014-08-13 | 洛阳师范学院 | 2,3',5,5'-diphenyl tetracarboxylic acid cadmium complex and preparation method thereof |
| CN104610310A (en) * | 2015-02-04 | 2015-05-13 | 河南工业职业技术学院 | Benzimidazole derivative namely cadmium (II) complex with fluorescence property and synthetic method of benzimidazole derivative |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103450234A (en) * | 2013-07-29 | 2013-12-18 | 南开大学 | Cadmium coordination polymer and preparation method thereof |
| CN103554083A (en) * | 2013-11-11 | 2014-02-05 | 吉林化工学院 | Monocrystal structure of cadmium coordination compound with blue light performance and preparation method thereof |
| CN103880871A (en) * | 2014-04-03 | 2014-06-25 | 哈尔滨工业大学 | Cadmium coordination polymer with 0D-to-2D double-interpenetration structure, and synthesis method thereof |
| CN103980301A (en) * | 2014-05-22 | 2014-08-13 | 洛阳师范学院 | 2,3',5,5'-diphenyl tetracarboxylic acid cadmium complex and preparation method thereof |
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