CN107298691B - A kind of lead source and its preparation method and application based on the double imidazole ligands of rigidity - Google Patents
A kind of lead source and its preparation method and application based on the double imidazole ligands of rigidity Download PDFInfo
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- CN107298691B CN107298691B CN201710551166.6A CN201710551166A CN107298691B CN 107298691 B CN107298691 B CN 107298691B CN 201710551166 A CN201710551166 A CN 201710551166A CN 107298691 B CN107298691 B CN 107298691B
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000003446 ligand Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- ZAUCCQHWBRVFJE-UHFFFAOYSA-N benzene 1H-imidazole Chemical compound N1C=NC=C1.N1C=NC=C1.C1=CC=CC=C1 ZAUCCQHWBRVFJE-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000002178 crystalline material Substances 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 229910002651 NO3 Inorganic materials 0.000 description 11
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 11
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 239000013256 coordination polymer Substances 0.000 description 3
- 229920001795 coordination polymer Polymers 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/24—Lead compounds
-
- 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
- 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
-
- 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)
- Materials Engineering (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Plural Heterocyclic Compounds (AREA)
Abstract
The invention discloses a kind of lead source based on the double imidazole ligands of rigidity, the chemical formula of the lead source is [Pb (BIMB) (NO3)2]n, BIMB is Isosorbide-5-Nitrae-to benzene diimidazole.The invention also discloses a kind of preparation method and application of lead source based on the double imidazole ligands of rigidity, the preparation method comprises the following steps: plumbi nitras, Isosorbide-5-Nitrae-are dissolved in water to benzene diimidazole ligand, add acid for adjusting pH to 4.8-5.2, in enclosed reaction kettle, constant temperature 70-74h carries out hydro-thermal reaction at 110-130 DEG C；Room temperature is naturally cooled to, colourless strip crystal is obtained after being filtered, washed, drying.The present invention has the advantages that (1) is first case to have the lead source functional material of right-handed helix duplex structure as ligand to benzene diimidazole；(2) synthetic method is simple, easily crystallization, yield height, reproducibility is good；(3) thermal stability of its crystalline material is high, green emitting is strong.
Description
Technical field
The present invention relates to function coordination polymer and its molecule based luminescent material technical fields, more particularly to one kind is based on rigid
Property double imidazole ligands lead source and its preparation method and application.
Background technique
Coordination polymer is because it has well-regulated cellular structure, regulatable pore size, can accommodate different guest molecules
The features such as soft permeability, unique surface area and active site and a variety of potential functions obtained by surface modification, in gas
There is unrivaled advantage in the fields such as body storage, selective catalysis, main-guest chemistry, optics and magnetics, it is considered to be most have
Desired one kind new function material.In order to obtain ideal performance, more and more metal ions are used to synthesis polycomplexation
Close object, mainly transition metal ions, rare earth ion and 3d-4f or 4d-4f mixed metal ion.In contrast, main
Race's metal ion is seldom reported, including Pb2+Ion.Compared with transition metal ions and lanthanide metal ion, main group Pb2+From
Son has bigger radius and more changeable ligancy (ligancy from 2-10 all studies have reported that), especially Pb2+Ion
It will form the active lone electron pair of spatial chemistry after 6s track and 6p orbital hybridization, and this lone electron pair is often to constructing uniqueness
Network topology structure and generate such as luminous, some performances of ion exchange and have important influence.Therefore, selection organic ligand with
Main group Pb2+Ion forms the potential source that coordination polymer is functional material.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of using Isosorbide-5-Nitrae-to benzene diimidazole as ligand,
Using lead ion as the lead source and its preparation method and application based on the double imidazole ligands of rigidity of metal ion.
The present invention is achieved by the following technical solutions: a kind of lead source based on the double imidazole ligands of rigidity, described
The chemical formula of lead source is [Pb (BIMB) (NO3)2]n, wherein BIMB is Isosorbide-5-Nitrae-to benzene diimidazole.
As one of preferred embodiment of the invention, the crystal of the lead source belongs to monoclinic system, and space group C2 is brilliant
Born of the same parents' parameter isβ=94.461 °；
A kind of preparation method of the lead source based on the double imidazole ligands of rigidity, concrete operations are as follows: by plumbi nitras, Isosorbide-5-Nitrae-
Water is dissolved in benzene diimidazole ligand, then acid adding regulation system pH to 4.8-5.2 is enclosed in reaction kettle, permanent at 110-130 DEG C
Warm 70-74h carries out hydro-thermal reaction；Room temperature is naturally cooled to after reaction, colourless strip crystal is obtained after being filtered, washed, drying, i.e.,
Chemical formula is [Pb (BIMB) (NO3)2]nLead source.
As one of preferred embodiment of the invention, the water is secondary deionized water.
As one of preferred embodiment of the invention, the plumbi nitras and Isosorbide-5-Nitrae-are 1:1 to the molar ratio of benzene diimidazole ligand.
As one of preferred embodiment of the invention, the system pH adjusts the HNO that acid-specific used is 1M3。
As one of preferred embodiment of the invention, the hydro-thermal reaction uses liner for the stainless steel reaction of polytetrafluoroethylene (PTFE)
Kettle carries out.
As one of preferred embodiment of the invention, the hydro-thermal reaction controls temperature using electric heating constant-temperature blowing drying box.
As one of preferred embodiment of the invention, the room temperature is 23-25 DEG C.
A kind of application of the lead source based on the double imidazole ligands of rigidity, the crystalline material of the lead source can be used as green
Color luminescent material is applied.
The present invention compared with prior art the advantages of be:
It (1) is first case to have to benzene diimidazole as ligand the present invention is based on lead source of the 1,4- to benzene diimidazole ligand
There is the lead source functional material of right-handed helix duplex structure；
(2) synthetic method is simple, easily crystallization, synthetic yield height, reproducibility is good；
(3) crystalline material of lead source of the present invention shows high thermal stability and strong green emitting property；
(4) it is studied through light and heat property, can be used as green luminescent material and applied in molecule based luminescent material field.
Detailed description of the invention
Fig. 1 be in embodiment 5 1,4- to the crystal structure figure of the lead source of benzene diimidazole ligand；
Fig. 2 be in embodiment 5 1,4- to the one-dimensional right-handed helix duplex structure figure of the lead source of benzene diimidazole ligand；
Fig. 3 be in embodiment 5 1,4- to the two-dimensional layer figure of the lead source of benzene diimidazole ligand；
Fig. 4 be in embodiment 5 1,4- to the thermogravimetric analysis figure of the lead source of benzene diimidazole ligand；
Fig. 5 be in embodiment 5 1,4- to the fluorescence spectra of the lead source of benzene diimidazole ligand.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of lead source based on the double imidazole ligands of rigidity of the present embodiment, using Isosorbide-5-Nitrae-to benzene diimidazole as ligand, with
Lead ion is metal ion.The chemical formula of the lead source is [Pb (BIMB) (NO3)2]n, BIMB is Isosorbide-5-Nitrae-to benzene diimidazole.
Embodiment 2
A kind of method preparing the lead source based on the double imidazole ligands of rigidity in above-described embodiment 1 of the present embodiment, tool
Gymnastics is made as follows: by Pb (NO3)2, BIMB ligand according to molar ratio 1:1 be dissolved in H2In O (secondary deionized water), add the HNO tune of 1M
Then section system pH to 4.8 is enclosed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), constant temperature 70h carries out water at 110 DEG C
Thermal response, wherein the temperature of hydro-thermal reaction is controlled using electric heating constant-temperature blowing drying box；23 DEG C are naturally cooled to after reaction, mistake
Colourless strip crystal is obtained after filter, washing, drying, i.e. chemical formula is [Pb (BIMB) (NO3)2]nLead source.
Embodiment 3
A kind of method preparing the lead source based on the double imidazole ligands of rigidity in above-described embodiment 1 of the present embodiment, tool
Gymnastics is made as follows: by Pb (NO3)2, BIMB ligand according to molar ratio 1:1 be dissolved in H2In O (secondary deionized water), add the HNO tune of 1M
Then section system pH to 5.2 is enclosed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), constant temperature 74h carries out water at 130 DEG C
Thermal response, wherein the temperature of hydro-thermal reaction is controlled using electric heating constant-temperature blowing drying box；24 DEG C are naturally cooled to after reaction, mistake
Colourless strip crystal is obtained after filter, washing, drying, i.e. chemical formula is [Pb (BIMB) (NO3)2]nLead source.
Embodiment 4
A kind of method preparing the lead source based on the double imidazole ligands of rigidity in above-described embodiment 1 of the present embodiment, tool
Gymnastics is made as follows: by the Pb (NO of 0.4mmol3)2, the miscible H in 10mL of the BIMB ligand of 0.4mmol2O (secondary deionized water)
In, add the HNO of 1M3Regulation system pH is 5, is encapsulated into after stirring 30min at room temperature at 25 DEG C in polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, 72 hours progress hydro-thermal reactions of constant temperature at 120 DEG C, wherein the temperature of hydro-thermal reaction utilizes electricity
Hot constant temperature blast drying oven control；It after naturally cooling to 25 DEG C of room temperatures, is filtered, washed, dries, obtain colourless strip crystal,
I.e. chemical formula is [Pb (BIMB) (NO3)2]nLead source.Based on Pb (NO3)2The yield of calculating is 78%.
Embodiment 5
The present embodiment carries out the lead source based on the double imidazole ligands of rigidity obtained in above-described embodiment further
Characterization, process are as follows:
(1) single crystal structure determination of the 1,4- to the lead source of benzene diimidazole ligand
Single crystal data is to collect on Bruker Smart APEX II CCD single crystal diffractometer at room temperature, using through graphite
The Mo-K alpha ray of monochromator monochromatizationMake incident light source, withScanning mode collects point diffraction,
Then data convert is carried out by SAINT program.The position of metallic atom Pb is first determined with direct method, then is schemed from poor Fourier
In find out corresponding C, N atom, and complete matrix least square method amendment is carried out to their coordinate and its anisotropy thermal parameter.
H atom in ligand is then to add hydrogen to obtain by geometry.All calculating is carried out using SHELXTL program bag.Crystallography number
It is shown in Table 1 according to structure refinement parameter, the bond distance of selection and bond angle data are shown in Table 2, and crystal structure is as shown in Fig. 1,2 and Fig. 3.
Predominant crystal data and refined parameters of 1 1,4- of table to the lead source of benzene diimidazole ligand
R1=∑ | | Fo |-| Fcs | |/∑ | Fo | wR2=∑ [w (Fo2-Fc2)2]/∑[w(Fo2)2]1/2
Selection bond distance of 2 1,4- of table to the lead source of benzene diimidazole ligandWith bond angle (°)
Symmetry transformations used to generate equivalent atoms:#1-x+1/2,y
+1/2,-z#2-x+1/2,y-1/2,-z#3-x+1,y+1,-z+1#4-x+1,y-1,-z+1
It is analyzed by the result of table 1, table 2 and Fig. 1,2,3, it can be gathered that the structure feature of the lead source are as follows:
Belong to monoclinic system, space group C2, cell parameter isB=9.409 (5)β=94.461 °.The asymmetric cell of the complex contains 1 independent Pb2+Ion, in 1
The BIMB ligand of property, 2 coordinated nitrates ions.As shown in Figure 1, center Pb2+Ion takes the hemispherical geometry structure of pentacoordinate
Type is mutually coordinated with the O atom on the imidazoles N atom and two nitrate anions on 2 BIMB respectively, and wherein Pb-N bond distance is
2.502 andPb-O bond distance is 2.655,2.549 HesCenter Pb2+The hemispherical coordination geometry of ion
Configuration is due to ligand BIBM, and nitrate anion is unevenly distributed around it and causes.When Pb-O bond distance fromIt expands toWhen, there are four Pb-O weak bonds for discovery Due to the presence of weak bond, cause in center Pb2+Do not match significantly around ion
The blanking bar of bit space distribution, illustrates that the center Pb (II) does not have the active lone electron pair of spatial chemistry.In ligand BIMB, phenyl ring and
Not in the same plane, corresponding dihedral angle is respectively 32.47 ° and 45.76 ° to two imidazole rings.Due to there is torsion angle,
BIMB connects two Pb of equal value as bridging ligand2+Ion forms an one-dimensional spiral by nitrate anion decoration in two sides
Chain, the distance between Pb ... Pb areSuch antiparallel to be formed similar to DNA one of spiraling of two coiled strands
A double-spiral structure, as shown in Figure 2.Adjacent double helix chain further is extended to two by Pb-O weak bond present in structure
Oversubscription sublayer structure is tieed up, as shown in Figure 3.
(2) 1,4- analyzes the elemental analysis of the lead source of benzene diimidazole ligand and infrared spectrometer
Lead of the Isosorbide-5-Nitrae-to benzene diimidazole ligand is matched using VARIO EL III elemental analyser (Germany, Elementar)
It closes object and carries out elemental analysis: calculated value C12H10N6O6Pb:C, 26.62；H, 1.86；N, 15.52；Measured value: C, 26.17；H,
1.22；N, 14.93%.
Using AVATAR-360 infrared spectrometer (U.S., Nicolet) to Isosorbide-5-Nitrae-to the lead source of benzene diimidazole ligand
Carry out infrared spectrum analysis: its characteristic IR absorbance peaks is (KBr, cm-1): 3129 (m), 1750 (w), 1522 (s), 1387 (s),
1300 (s), 1116 (m), 1068 (s), 928 (m), 827 (m), 644 (w), 554 (w).
(3) 1,4- studies the thermal stability of the lead source of benzene diimidazole ligand
It is washed, be dried after complex crystal sample under the conditions of air atmosphere with the rate of 10 DEG C/min from room
Temperature is progressively heated at 800 DEG C, heat analysis is carried out to it by STA-409PC synthesis thermal analyzer (Germany, Netzsch), heat
It is as shown in Figure 4 to analyze curve.Complex crystalline material complex skeleton at 260 DEG C just starts to decompose, until 450 DEG C
Complex skeletal disintegration is complete, weight loss 63.4%, the mistake corresponding to 1 BIMB ligand and 2 nitrate anions in crystal structure
Go (theoretical value 61.7%).It should be the experimental results showed that gained complex thermodynamic stability with higher, be it as function
The development and application of energy material provide reliable thermal stability guarantee.
(4) solid fluorescence performance study of the 1,4- to the lead source of benzene diimidazole ligand
Complex crystal sample passes through FLS920 type stable state transient state fluorescence light through being fully ground after washed, drying process
Spectrometer (Britain, Edinburgh) carries out the test of solid luminescence at room temperature, and excitation and emission spectra is as shown in figure 5, Fig. 5
In, compoud 1 (ex) is excitation wavelength light map of the Isosorbide-5-Nitrae-to the lead source of benzene diimidazole ligand, compoud 1 (em)
It is 1,4- to the launch wavelength light map of the lead source of benzene diimidazole ligand.1,4- exists to the lead source of benzene diimidazole ligand
Strong green emitting property is showed under the light excitation that wavelength is 448nm, emission peak is located at 562nm.It is in green emitting material
Material aspect has potential application.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of lead source based on the double imidazole ligands of rigidity, which is characterized in that the chemical formula of the lead source is [Pb
(BIMB)(NO3)2]n, wherein BIMB is Isosorbide-5-Nitrae-to benzene diimidazole；
The crystal of the lead source belongs to monoclinic system, space group C2, and cell parameter is β=94.461 °；
2. the preparation method of the lead source according to claim 1 based on the double imidazole ligands of rigidity, which is characterized in that tool
Gymnastics is made as follows: plumbi nitras, Isosorbide-5-Nitrae-being dissolved in water to benzene diimidazole ligand, then acid adding regulation system pH to 4.8-5.2 is enclosed
In reaction kettle, constant temperature 70-74h carries out hydro-thermal reaction at 110-130 DEG C；Room temperature is naturally cooled to after reaction, be filtered, washed,
Colourless strip crystal is obtained after drying, i.e. chemical formula is [Pb (BIMB) (NO3)2]nLead source.
3. the preparation method of the lead source according to claim 2 based on the double imidazole ligands of rigidity, which is characterized in that institute
Stating water is secondary deionized water.
4. the preparation method of the lead source according to claim 2 based on the double imidazole ligands of rigidity, which is characterized in that institute
Stating plumbi nitras and 1,4- is 1:1 to the molar ratio of benzene diimidazole ligand.
5. the preparation method of the lead source according to claim 3 based on the double imidazole ligands of rigidity, which is characterized in that institute
It states system pH and adjusts the HNO that acid-specific used is 1M3。
6. the preparation method of the lead source according to claim 2 based on the double imidazole ligands of rigidity, which is characterized in that institute
Stating hydro-thermal reaction uses liner to carry out for the stainless steel cauldron of polytetrafluoroethylene (PTFE).
7. the preparation method of the lead source according to claim 2 based on the double imidazole ligands of rigidity, which is characterized in that institute
It states hydro-thermal reaction and controls temperature using electric heating constant-temperature blowing drying box.
8. the preparation method of the lead source according to claim 2 based on the double imidazole ligands of rigidity, which is characterized in that institute
Stating room temperature is 23-25 DEG C.
9. the application of the lead source according to claim 1 based on the double imidazole ligands of rigidity, which is characterized in that the lead
The crystalline material of complex can be used as green luminescent material and be applied.
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| CN113024597B (en) * | 2021-03-23 | 2023-06-27 | 陕西科技大学 | Lead-based inorganic anion complex fluorescent color-changing material, and preparation method and application thereof |
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| CN103539805A (en) * | 2013-11-03 | 2014-01-29 | 安庆师范学院 | Flexible dual-triazole ligand based CuCN complex and preparation method thereof |
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| Title |
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| An Infinite 2D Polyrotaxane Network in Ag2(bix)3(NO3)2 (bix ) ,4-Bis(imidazol-1-ylmethyl)benzene);Bernard F. Hoskins et al.;《J.Am.Chem.Soc.》;19971231;第119卷;第2952-2953页 * |
| Novel Pb(II) coordination frameworks: synthesis, crystal structures and unusual third-order nonlinear optical properties;Bin Sui et al.;《J.Mater.Chem.》;20040422;第14卷;摘要，scheme 1，第1632页左栏第2段 * |
| The Structure of [Zn(bix)2(NO3)2]4.5H20 (bix = 1,4-Bis(irnidazol-l-ylmethyl)benzene): A New Type of Two-Dimensional Polyrotaxane;Bernard F. Hoskins et al.;《Angew. Chem. Int. Ed. Engl.》;19971231;第36卷;第2336-2337页 * |
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