CN102191039B - Platinum compound fluorescent material - Google Patents
Platinum compound fluorescent material Download PDFInfo
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- CN102191039B CN102191039B CN 201010126977 CN201010126977A CN102191039B CN 102191039 B CN102191039 B CN 102191039B CN 201010126977 CN201010126977 CN 201010126977 CN 201010126977 A CN201010126977 A CN 201010126977A CN 102191039 B CN102191039 B CN 102191039B
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- platinum compound
- fluorescent material
- pyridine
- platinum
- compound
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Abstract
The invention discloses a platinum compound fluorescent material, and a preparation method thereof. The platinum compound fluorescent material is an ethynyl pyridine platinum compound with a certain space structure, and has a molecular formula of C40H32N2P2Pt. The preparation method of the platinum compound fluorescent material comprises the following steps of: carrying out reaction on 1,2-bis(diphenylphosphino) ethane and potassium tetrachloroplatinate under the protection of nitrogen gas to obtain a 1,2-bis(diphenylphosphino) ethane platinum compound; and carrying out chemical reaction on the 1,2-bis(diphenylphosphino) ethane platinum compound and ethynyl pyridine under the catalysis of CuI to obtain the ethynyl pyridine platinum compound. The platinum compound prepared by the preparation method has high photoelectric activity, presents good near-blue light emission performance and film forming performance, and can be used as a fluorescent material and a film material.
Description
Technical field
The invention belongs to the materials chemistry field, be specifically related to a kind of platinum compound fluorescent material.
Background technology
Fluorescent material typically refers to after having accepted outside energy, energy absorption can be stored, and is converted into luminous energy in the place of dark.The organic ligand that has optically active metal ion or contain the conjugation primitive is incorporated in fluorescent material, can greatly improves the luminescent properties of fluorescent material.The organic ligand that employing contains different conjugation primitives coordinates with metal ion, and sensitizing agent can be prepared the fluorescent material of various optical effects, and it is widely used in decorating, false proof, sign, medical treatment, the numerous areas such as commodity inspection.
Phosphor material powder was come out the earliest in 1938.The people such as early stage Stokes have synthesized the fluorescent material such as calcium wolframate and have been used for luminescent lamp.Developed phosphate phosphor in 1948, the early stage fluorescent material of this light-emitting phosphor Performance Ratio has had remarkable improvement.60～seventies of 20th century fluorescent material obtained general application.Along with deepening continuously that fluorescent material is studied, people have developed three primary colors fluorescent powder.Rare earth element is introduced in fluorescent material as activator, the luminescent properties of fluorescent material is significantly improved.The rare-earth trichromatic luminescent lamp in Europe in 1997 accounts for half of head light total amount according to statistics.The eighties in 20th century, ultrafine powder grows up gradually, increasingly becomes the emphasis of various countries' research.So-called ultrafine powder refers to yardstick between molecule, atom and bulk material, comprises metal, the multiple particulate material such as nonmetal, organic and inorganic and biological, also claims nano-particle material.Fluorescent material mainly contains sulfide-based fluorescent material in the market, aluminate fluorescent powder, phosphate-based fluorescent material, fluorescent RE powder etc.Mainly contain near ultraviolet excitated redness, green and blue colour fluorescent powder from luminous wave band.
Generally speaking, the luminous three primary colors fluorescent powder of near ultraviolet had been obtained huge progress round realizing photoluminescence in recent years, had developed the fluorescent material of many novel systems, had improved the fluorescent material performance of previous exploitation.Especially develop and improved near ultraviolet fluorescent powder, making its performance more can realize application on light emitting devices.Emerged in large numbers at present many novel systems, wherein oxynitride system and molybdenum (tungsten) silicate system etc. is very promising rouge and powder.Green powder had also been developed some novel systems in recent years.But the luminescent properties of blue powder also has many work that have much room for improvement to do, and also needs to develop more novel system, in order to improve its performance.
The metal organic micromolecule compound that Recent study finds to have optically active metal ion and the organic ligand assembling that contains the conjugation primitive demonstrates good luminescent properties.Such research has significant novelty: organic composition and inorganic components can be carried out autotelic screening and regulation and control, by the size of screening metal ion or conjugation primitive, realize the regulation and control to emission wavelength; In addition, can the design to material synthesize on molecular level, be conducive to the relation of research structure and performance, explore the luminescence mechanism of material, thereby provide theoretical foundation for designing advanced luminescent material.Use two (diphenyl phosphine oxide) platinic compound of 1.2-and acetylene pyridine to carry out chemical reaction, we have prepared a kind of Novel ethyne pyridine platinic compound, and this compound has potential application prospect as nearly blue light emitting material.
Summary of the invention
Primary technical problem to be solved by this invention is for prior art, and a kind of platinum compound fluorescent material with good blue emission performance is provided.
The present invention for the technical scheme that solves above-mentioned primary technical problem and take is: a kind of platinum compound fluorescent material, it is characterized in that this platinum compound fluorescent material is a kind of acetylene pyridine platinic compound with certain space structure, and its molecular formula is C
40H
32N
2P
2Pt.Crystallographic system is monocline, and spacer is Cc, unit cell parameters
α=γ=90 °, β=108.98 °, platinum ion is planar shape coordination mode, and two phosphorus ligating atoms come from 1.2-two (diphenyl phosphine oxide), and two carbon ligating atoms come from 4-pyridine acetylene.
Described platinum compound fluorescent material is a kind of pale yellow crystals.
The present invention for the technical scheme that solves above-mentioned second technical problem and take is: a kind of preparation method of platinum compound fluorescent material is characterized in that comprising the following steps:
1) take appropriate 1.2-two (diphenyl phosphine oxide) (being called for short dppe) and add in the vacuum system of nitrogen protection, add appropriate CH
2Cl
2/ C
2H
5OH (volume ratio 1: 0.8-1.2, preferred 1: 1) mixing solutions, heated and stirred makes its dissolving, then adds equimolar K
2PtCl
4The aqueous solution, reacting by heating 20-50min, temperature of reaction is 50-70 ℃, filters to get white powder, rinses with ethanol and ether, obtains initial product PtCl
2(dppe);
2) get PtCl
2(dppe) 0.15-0.30g is added to dry 10-15mLN, in N '-dimethyl formamide (being called for short DMF), stirs, once add the 10-15mL triethylamine, 0.15-0.25g hydrochloric acid 4-pyridine acetylene, 10-15mg CuI, heating reflux reaction 6-12h, temperature is 50-70 ℃; Then cooling, filtration is rinsed with normal hexane and ether respectively, gets light yellow solid.
3) with the light yellow solid recrystallization in the mixing solutions of chloroform and methyl alcohol (volume ratio is 1: 0.8-1.2 is preferably 1: 1) that makes, obtain pale yellow crystals, be described platinic compound, after measured, the molecular formula of this platinic compound is C
40H
32N
2P
2Pt.
Described CH
2Cl
2/ C
2H
5The CH of OH mixed solution
2Cl
2With C
2H
5The OH volume ratio is 1: 1.
Described N, N '-dimethyl formamide are dry deoxidations, and described potassium tetrachloroplatinate is analytical pure, and the purity of described 1.2-two (diphenyl phosphine oxide) is 99.5%.
Compared with prior art, the invention has the advantages that: potassium tetrachloroplatinate and the 1.2-two (diphenyl phosphine oxide) that will have optical property make two (diphenyl phosphine oxide) platinic compound of 1.2-for raw material, carry out chemical reaction with the acetylene pyridine again and make Novel ethyne pyridine platinic compound, this compound has space structure (Fig. 1) and molecular formula accurately accurately as nearly blue light emitting material; The triple bond (alkynyl) that contains insatiable hunger has and enriches optically active Pt (II) ion, the pyridine imine base, and the large π key of conjugation etc., be conducive to transition of electron and transmission ofenergy, thereby make compound have good photoelectric activity.Prepared material has good nearly blue emission performance and film forming properties, has potential application prospect as fluorescent material and thin-film material.
Description of drawings
Fig. 1 is the structural unit figure of platinic compound of the present invention;
Fig. 2 is platinic compound fluorescence emission spectrum of the present invention.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Take 0.8g 1.2-two (diphenyl phosphine oxide) and add in the vacuum system of nitrogen protection, add the CH of 50 milliliters with syringe
2Cl
2/ ethanol (1: 1), heated and stirred makes its dissolving, then adds equimolar K
2PtCl
4The aqueous solution, reacting by heating 30min, temperature of reaction is 60 ℃, filters to get white powder, rinses with ethanol and ether, obtains initial product PtCl
2(dppe).
With above-mentioned initial product PtCl
2(dppe) 0.20g is added in nitrogen atmosphere in dry 12mL DMF, stirs, and once adds 12mL NEt3,0.2g hydrochloric acid 4-pyridine acetylene (being called for short ccpy), and 12mg CuI, heating reflux reaction 9h, temperature is 50-70 ℃.Cooling, filtration are rinsed with normal hexane and ether respectively, get light yellow solid.
With the pale yellow crystals of light yellow solid recrystallization in the mixing solutions of chloroform and methyl alcohol (volume ratio 1: 1) of making, be described platinic compound at last, advancing to measure its molecular formula is C
40H
32N
2P
2P, crystallographic system is monocline, spacer is Cc, unit cell parameters
α=γ=90 °, β=108.98 °, platinum ion is planar shape coordination mode, and two phosphorus ligating atoms come from 1.2-two (diphenyl phosphine oxide), and two carbon ligating atoms come from 4-pyridine acetylene, and its crystalline structure figure is as shown in Figure 1.
With prepared platinic compound C
40H
32N
2P
2P carries out the fluorescence property test, and this compound demonstrates good nearly blue emission performance (as Fig. 2), and has good film forming properties.
Claims (1)
1. a platinum compound fluorescent material, is characterized in that this platinum compound fluorescent material is a kind of acetylene pyridine platinic compound with certain space structure, and its molecular formula is C
40H
32N
2P
2Pt, crystallographic system is monocline, spacer is Cc, unit cell parameters
α=γ=90 °, β=108.98 °, platinum ion is planar shape coordination mode, and two phosphorus ligating atoms come from 1.2-two (diphenyl phosphine oxide), and two carbon ligating atoms come from 4-pyridine acetylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010126977 CN102191039B (en) | 2010-03-17 | 2010-03-17 | Platinum compound fluorescent material |
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|---|---|---|---|
| CN 201010126977 CN102191039B (en) | 2010-03-17 | 2010-03-17 | Platinum compound fluorescent material |
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|---|---|
| CN102191039A CN102191039A (en) | 2011-09-21 |
| CN102191039B true CN102191039B (en) | 2013-11-06 |
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| CN 201010126977 Expired - Fee Related CN102191039B (en) | 2010-03-17 | 2010-03-17 | Platinum compound fluorescent material |
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| CN103122243B (en) * | 2013-01-28 | 2015-01-28 | 宁波大学 | Platinum compound fluorescent material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6610848B1 (en) * | 1998-07-27 | 2003-08-26 | Lumet Llc | Platinum complex dioxygen sensors |
-
2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6610848B1 (en) * | 1998-07-27 | 2003-08-26 | Lumet Llc | Platinum complex dioxygen sensors |
Non-Patent Citations (8)
| Title |
|---|
| Electrospray mass spectrometric analysis of transition-metal halide complexes;William Henderson等;《Inorganica Chimica Acta》;19991231;第294卷;183–192 * |
| Guest Chemistry of Mixed, Neutral-Charged, Pt− |
| Jeffery A. Whiteford等.Molecular Architecture via Coordination:  |
| Jeffery A. Whiteford等.Molecular Architecture via Coordination: Self-Assembly, Characterization, and Host−Guest Chemistry of Mixed, Neutral-Charged, Pt−Pt and Pt−Pd Macrocyclic Tetranuclear Complexes. X-ray Crystal Structure of Cyclobis[[cis-Pt(dppp)(4-ethynylpyridine)2.《J. Am. Chem. Soc.》.1997,第119卷2524-2533. * |
| Pd Macrocyclic Tetranuclear Complexes. X-ray Crystal Structure of Cyclobis[[cis-Pt(dppp)(4-ethynylpyridine)2.《J. Am. Chem. Soc.》.1997,第119卷2524-2533. |
| Pt and Pt− |
| Self-Assembly, Characterization, and Host− |
| William Henderson等.Electrospray mass spectrometric analysis of transition-metal halide complexes.《Inorganica Chimica Acta》.1999,第294卷183–192. |
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