CN107056826A - A kind of rare earth Pr complexs and its preparation method and application - Google Patents
A kind of rare earth Pr complexs and its preparation method and application Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 21
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000013078 crystal Substances 0.000 claims abstract description 19
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 13
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000001632 sodium acetate Substances 0.000 claims abstract description 13
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- WYOIGGSUICKDNZ-UHFFFAOYSA-N 2,3,5,6,7,8-hexahydropyrrolizin-1-one Chemical compound C1CCC2C(=O)CCN21 WYOIGGSUICKDNZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- MUYSADWCWFFZKR-UHFFFAOYSA-N cinchomeronic acid Chemical class OC(=O)C1=CC=NC=C1C(O)=O MUYSADWCWFFZKR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 14
- 239000013110 organic ligand Substances 0.000 claims description 11
- GJAWHXHKYYXBSV-UHFFFAOYSA-N pyridinedicarboxylic acid Natural products OC(=O)C1=CC=CN=C1C(O)=O GJAWHXHKYYXBSV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- LVPMIMZXDYBCDF-UHFFFAOYSA-N isocinchomeronic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)N=C1 LVPMIMZXDYBCDF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 2
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical compound [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 36
- 239000010949 copper Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 239000013256 coordination polymer Substances 0.000 description 5
- 229920001795 coordination polymer Polymers 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- KPXRPRLCONABEG-UHFFFAOYSA-K praseodymium acetate Chemical class [Pr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O KPXRPRLCONABEG-UHFFFAOYSA-K 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- LELIWVXTBSKMRB-UHFFFAOYSA-N copper praseodymium Chemical compound [Cu].[Pr] LELIWVXTBSKMRB-UHFFFAOYSA-N 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003068 molecular probe Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229940081066 picolinic acid Drugs 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- 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
- C09K2211/182—Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide
-
- 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)
Abstract
The present invention discloses a kind of molecular structure for C16H32CuPrN2O21.5Rare earth Pr complexs, with copper acetate, 3,4 pyridinedicarboxylic acids, praseodymium acetate and sodium acetate are raw material, and rare earth Pr complexs are prepared using simple solution method.It is an advantage of the invention that：The rare earth Pr complexs prepared have unique three-dimensional structure, and have higher stability, and crystal recovery rate is high, and with preferable luminescence in visible-range.
Description
Technical field
The present invention relates to Metal-organic complex fluorescent material technical field, and in particular to a kind of rare earth Pr complexs and
Its preparation method and application.
Background technology
The synthesis of complex is the important composition of Coordinative Chemistry, is the Research foundation of Coordinative Chemistry.The preparation of this complex
Method is prepared using aqueous solution substitution reaction.Water is most common solvent, and substitution reaction in aqueous is also synthesis metal
The most common method of complex.The principle of this method is very simple, is constantly to be volatilized by solution, makes complex solution from insatiable hunger
The state of sum becomes saturation state even hypersaturated state, so as to separate out monocrystalline.This method is simple and easy to apply, and cost is low, has
Very big industrial prospect.
Transition metal-rare earth Heteronu clear metal complex shows many brand-new properties in terms of luminescent material.Nankai
The Cheng Peng seminars of university, with 2, Ln-Mn (Ln=Eu, Tb) this 2 has and received dipicolimic acid 2 (PDA) with synthesis
The complex in mitron road, and it was found that introduce very big on their prominent luminous intensity influence after transition metal ions.It is this by molecule
The chemical information of level is changed into the phenomenon of macroscopic signals (color or prominent luminous intensity change), the work with cationic fluorescent probe
With above having great importance in the application of molecular probe.In this regard, Liu Weisheng exists《Coordinative Chemistry》In also have related elaboration.Cloud
The Li Hongfang of southern university chemistry section and engineering college《Preparation, structure and the property research of rare earth/transition metal organic coordination compound》、
Shanghai Normal University Zhou Xianan《The synthesis, sign and its antibacterial activity research of rare earth (copper) complex》, Liaoning Normal University king
It is elegant gorgeous《Serial Ln-Ag/Ln-Ln matches somebody with somebody the synthesis/structure and physical property of polymers》In have related elaboration.
Picolinic acid coordination polymer has following obviously advantage：(1) metal ion can provide particular geometric
Coordination atom in coordination configuration, with organic ligand has adhesion from weak to strong, is matched somebody with somebody so as to be formed by unstable to stable
Position polymer；Also, the characteristics such as electricity, optics, magnetochemistry and the reduction of oxidation one of metal ion may all be embodied in design and close
Into coordination polymer in.(2) diversity of organic ligand, modifiability and the different coordination sides between different metal ions
Formula, possibility is provided for design synthesis controlled shape, the coordination polymer that size is controllable and property is controllable.Meanwhile, metal from
The properties such as son exclusive light, electricity, magnetic, can knifeedge be regulated and controled, and matched somebody with somebody by metal ion with organic in ligand field
Different coordination mode between body, can produce the peculiar property that one pack system does not have.Hebei Normal University's LI Yajuan exists《It is based on
Synthesis, structure and the performance study of the coordination polymer of asymmetric ligand 3,4- pyridinedicarboxylic acids》In mention, because metal is organic
Coordination polymer is to be formed by metal ion and organic ligand by self assembling process, therefore combines organic ligand and metal
The characteristics of both ions, not only with charming topological structure, such as：One-dimensional straight-chain, word chain, two-dimensional lattice shape, it is netted,
Stratiform, cellular, brick wall shape, three dimensional diamond shape etc., but also other unique properties may be shown, in nonlinear optical
The aspects such as, magnetics superconduction, adsorbing separation, catalysis all have good potential application foreground.But, reasonably select organic
Part and metal ion, and the condition of reaction is controlled, NW-TFT expected structure is still challenging.
The content of the invention
In order to solve the above technical problems, the present invention is original with copper acetate, 3,4- pyridinedicarboxylic acids, praseodymium acetate and sodium acetate
Material, a kind of rare earth Pr complexs are prepared using simple solution method, the three-dimensional structure with uniqueness, and have higher stability,
Crystal recovery rate is high, and with preferable luminescence in visible-range.
Concrete technical scheme is as follows：
A kind of rare earth Pr complexs, chemical formula is C16H32CuPrN2O21.5, monoclinic system, P1 space groups, cell parameter isα=90 °, β=102.445 (4) °, γ=90 °,Wherein a, b, c refer to a axles, b axles, c-axis respectively, and α, β, γ are space angle, and V is unit cell volume,For
Long measure,
A kind of preparation method of rare earth Pr complexs, is original with copper acetate, 3,4- pyridinedicarboxylic acids, praseodymium acetate and sodium acetate
Material, Cu-Pr complexs are prepared using simple solution method, and specific preparation process is as follows：
(1) copper acetate, praseodymium acetate are dissolved in distilled water, are prepared into solution A；By the pyridinedicarboxylic acid of organic ligand 3,4
It is dissolved in distilled water, is prepared into solution B；Wherein, copper acetate, praseodymium acetate, 3, the mole ratio of 4 pyridinedicarboxylic acids is 1:1:2,
Distillation water consumption is 20~40 times of mixed liquor mole；
(2) solution A, B are mixed, adds the NaOH solution that concentration is 1mol/L, adjustment pH value to 9~11 is added simultaneously
Sodium acetate, is prepared into solution C；The consumption of sodium acetate is 0.5~3 times of 3,4 pyridinedicarboxylic acids；
(3) ethanol solution is added in solution C, 24~72h is stood after filtering, the complex crystal is obtained；Ethanol is molten
The consumption of liquid is 5~10 times of mixed liquor mole.
The rare earth Pr complexs are applied to fluorescent material field.
This method have the advantage that：
1st, rare earth Pr complexs prepared by the present invention have unique three-dimensional structure, and have higher stability, pass through
The consumption of sodium acetate and ethanol is adjusted, crystal recovery rate can be improved, it is environmentally safe.
2nd, rare earth Pr complexs prepared by the present invention can light at room temperature, fluorometric investigation be carried out to it, in 298nm wavelength
Excite down, two fluorescence emission peaks are presented in the emission spectrum of complex copper-praseodymium, right respectively respectively at 600nm and 640nm
Answer Pr3+Characteristic emission transition peak.
Brief description of the drawings
Fig. 1 is the molecular structure of complex；
Fig. 2 is the structure cell accumulation graph of complex；
Fig. 3 is the space structure figure of Cu complexs；
Fig. 4 is the space structure figure of Pr complexs；
Fig. 5 is complex exciting light spectrogram；
Fig. 6 is complex launching light spectrogram；
Fig. 7 is the infrared spectrum of complex.
Embodiment
With reference to specific embodiment, the present invention is described in detail, but protection scope of the present invention is not by embodiment institute
Limit.
Embodiment 1
Weigh 1mmol copper acetates, 1mmol praseodymium acetates to be dissolved in 10ml distilled water, be prepared into solution A；Weigh 2mmol
The pyridinedicarboxylic acid of organic ligand 3,4, is dissolved in 10ml distilled water, is prepared into solution B；
A, B are mixed, the NaOH that concentration is 1mol/L, stirring is added until dissolving, adjustment pH value to 9, are added simultaneously
2mmol sodium acetate, is prepared into solution C；Solution C is added to 20ml ethanol solution, filtering, standing 24h obtain the cooperation
Thing crystal, crystal recovery rate is 60%.
Single crystal diffraction is carried out to the crystal using Germany's production Bruker P4 single crystal diffractometers.Detailed axonometry data
It is shown in Table 1, table 2 and table 3.
The predominant crystal data of table 1Cu-Pr monocrystal
The main atom bonding lengths of table 2Cu-Pr monocrystal
Table 3Cu-Pr monocrystal Cu2+, Pr3+Ionogenic linkage bond angle
Embodiment 2
Weigh 2mmol copper acetates, 2mmol praseodymium acetates to be dissolved in 15ml distilled water, be prepared into solution A；Weigh 4mmol
The pyridinedicarboxylic acid of organic ligand 3,4, is dissolved in 15ml distilled water, is prepared into solution B；
A, B are mixed, the NaOH that concentration is 1mol/L, stirring is added until dissolving, adjustment pH value to 10, are added simultaneously
8mmol sodium acetate, is prepared into solution C；Solution C is added to 40ml ethanol solution, filtering, standing 36h obtain the cooperation
Thing crystal.Crystal recovery rate is 80%.The molecular structure of complex as shown in figure 1, complex structure cell accumulation as shown in Fig. 2
As seen from Figure 1, each repeat unit contains the Pr of non-equivalence3+Unit and Cu2+Unit is constituted.
Embodiment 3
Weigh 2mmol copper acetates, 2mmol praseodymium acetates to be dissolved in 10ml distilled water, be prepared into solution A；Weigh 4mmol
The pyridinedicarboxylic acid of organic ligand 3,4, is dissolved in 15ml distilled water, is prepared into solution B；
A, B are mixed, the NaOH that concentration is 1mol/L, stirring is added until dissolving, adjustment pH value to 10, are added simultaneously
12mmol sodium acetate, is prepared into solution C；Solution C is added to 60ml ethanol solution, filtering, standing 36h obtain described match somebody with somebody
Solvate crystal.Crystal recovery rate is 85%, and the space structure of complex is as shown in Figure 3, Figure 4.Cu spatial coordination as seen from Figure 3
Structure, Cu2+Unit be 5 coordination structures, wherein equatorial plane by two N (N1, N2) with two from four different 3,4-pdc
O (O3, O6) atom of part is occupied.Pr as seen from Figure 43+Unit is 9 coordination structures, wherein the oxygen atom of four coordinations comes from two
Individual 3,4-pdc parts, two oxygen atoms come from water of coordination molecule, and three coordinating oxygen atoms are from two acetate parts.
Embodiment 4
Weigh 3mmol copper acetates, 3mmol praseodymium acetates to be dissolved in 15ml distilled water, be prepared into solution A；Weigh 6mmol
The pyridinedicarboxylic acid of organic ligand 3,4, is dissolved in 15ml distilled water, is prepared into solution B；A, B are mixed, adding concentration is
1mol/L NaOH, stirring are until dissolving, adjustment pH value to 11, while adding 12mmol sodium acetate, are prepared into solution C；Will
Solution C adds 80ml ethanol solution, and filtering, standing 72h obtain the complex crystal, and crystal recovery rate is 88%.Coordinate
Thing Pr-Cu excitation spectrums are as shown in Figure 5；Complex Pr-Cu emission spectrum, as shown in Figure 6.In the case where the wavelength is excited, coordinate
Two fluorescence emission peaks are presented in thing Pr-Cu emission spectrum, at 600nm and 640nm, it was demonstrated that it has in visible-range
Luminescence.
Embodiment 5
Weigh 3mmol copper acetates, 3mmol praseodymium acetates to be dissolved in 15ml distilled water, be prepared into solution A；Weigh 6mmol
The pyridinedicarboxylic acid of organic ligand 3,4, is dissolved in 15ml distilled water, is prepared into solution B；A, B are mixed, adding concentration is
1mol/L NaOH, stirring are until dissolving, adjustment pH value to 11, while adding 18mmol sodium acetate, are prepared into solution C；Will
Solution C adds 80ml ethanol solution, and filtering, standing 72h obtain the complex crystal.Crystal recovery rate is 90%.
Complex Pr-Cu infrared spectrum is as shown in Figure 7, it can be clearly seen that in wave number 3448.5cm-1There are O-H in place
The characteristic absorption peak of key, illustrates to contain hydrone in complex Pr-Cu, and forms between complex hydrogen bond, this and list
The structure of complex is completely the same determined by brilliant analysis result.3,4- pyridinedicarboxylic acids are in 1716cm-1Neighbouring feature
Absworption peak disappears.Wave number 1627cm-1There is very strong absworption peak, C-O asymmetric stretching vibration absworption peak can be attributed to,
1400cm-1The strong absworption peak at place is C=O symmetrical stretching vibration absworption peak, and wave number is 1045cm-1Absworption peak be C-N keys
Vibration absorption peak.In 686.6cm-1The absworption peak at place can be attributed to the absorption vibration peak of Pr-O keys.C-O in complex Pr-Cu
The eigen vibration of key, C-N keys and these keys in 3,4- pyridinedicarboxylic acid is compared, and occurs red shift, illustrates 3,4- pyridine dicarboxyls
N and O in acid are coordinated with metal Pr and Cu.
Claims (3)
1. a kind of rare earth Pr complexs, it is characterised in that：The rare earth Pr coordination chemistries formula is C16H32CuPrN2O21.5, monocline
Crystallographic system, P1Space group, cell parameter is α=
90 °, β=102.445 (4) °, γ=90 °,
2. a kind of preparation method of rare earth Pr complexs, it is characterised in that：With copper acetate, 3,4- pyridinedicarboxylic acids, praseodymium acetate and
Sodium acetate is raw material, and rare earth Pr complexs are prepared using simple solution method, and specific preparation process is as follows：
(1) copper acetate, praseodymium acetate are dissolved in distilled water, are prepared into solution A；By the dissolving of the pyridinedicarboxylic acid of organic ligand 3,4
In distilled water, solution B is prepared into；Wherein, copper acetate, praseodymium acetate, 3, the mole ratio of 4 pyridinedicarboxylic acids is 1:1:2, distillation
Water consumption is 20~40 times of mixed liquor mole；
(2) solution A, B are mixed, adds the NaOH solution that concentration is 1mol/L, adjustment pH value to 9~11, while adding acetic acid
Sodium, is prepared into solution C；The consumption of sodium acetate is 0.5~3 times of 3,4 pyridinedicarboxylic acids；
(3) ethanol solution is added in solution C, 24~72h is stood after filtering, the complex crystal is obtained；Ethanol solution
Consumption is 5~10 times of mixed liquor mole.
3. the preparation method of rare earth Pr complexs according to claim 2, it is characterised in that：The rare earth Pr complex applications
In fluorescent material field.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478947A (en) * | 2014-11-28 | 2015-04-01 | 东北大学 | Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof |
| CN104610382A (en) * | 2015-01-06 | 2015-05-13 | 东北大学 | Green fluorescent complex containing terbium and preparation method and application thereof |
-
2017
- 2017-05-22 CN CN201710362269.8A patent/CN107056826A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478947A (en) * | 2014-11-28 | 2015-04-01 | 东北大学 | Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof |
| CN104610382A (en) * | 2015-01-06 | 2015-05-13 | 东北大学 | Green fluorescent complex containing terbium and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| XUAN-WEN LIU,ET AL.: ""Two series of novel 3D potentially porous heterometallic Cu–Ln coordination frameworks assembled by 3,4-pyridinedicarboxylic acid with different topologies and channels: syntheses, structures, luminescence and magnetic properties"", 《RSC ADV.》 * |
| ZHENG-QIANG XIA ET AL.: ""Copper(II)–lanthanide(III) coordination polymers constructed from pyridine-2,5-dicarboxylicacid: Preparation,crystal structure and photoluminescence"", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
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