CN105061964A - Synthesis path and application of novel composite material - Google Patents
Synthesis path and application of novel composite material Download PDFInfo
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- CN105061964A CN105061964A CN201510498062.4A CN201510498062A CN105061964A CN 105061964 A CN105061964 A CN 105061964A CN 201510498062 A CN201510498062 A CN 201510498062A CN 105061964 A CN105061964 A CN 105061964A
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 36
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 34
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract 3
- 229920000642 polymer Polymers 0.000 claims description 17
- 239000011159 matrix material Substances 0.000 claims description 16
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 13
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 229920002521 macromolecule Polymers 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000004417 polycarbonate Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- -1 rare earth chloride Chemical class 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005286 illumination Methods 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims 2
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims 1
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 229910052691 Erbium Inorganic materials 0.000 claims 1
- 229910052693 Europium Inorganic materials 0.000 claims 1
- 229910052765 Lutetium Inorganic materials 0.000 claims 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 239000004793 Polystyrene Substances 0.000 claims 1
- 229910052777 Praseodymium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- 229910052769 Ytterbium Inorganic materials 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 9
- 238000010791 quenching Methods 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 3
- 239000013110 organic ligand Substances 0.000 abstract 1
- 239000002952 polymeric resin Substances 0.000 abstract 1
- 229920003002 synthetic resin Polymers 0.000 abstract 1
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- 230000007547 defect Effects 0.000 description 6
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- 230000003287 optical effect Effects 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 235000010233 benzoic acid Nutrition 0.000 description 2
- 150000001559 benzoic acids Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009415 formwork Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 101100433727 Caenorhabditis elegans got-1.2 gene Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000168254 Siro Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
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- 238000004132 cross linking Methods 0.000 description 1
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- 239000004744 fabric Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a synthesis path of a novel composite material. According to the synthesis path, firstly, a complex of rare earth and unsaturated organic carboxylic acid or derivatives of organic carboxylic acid are synthesized as a precursor, then a prepolymer of a polymer resin material is synthesized, and the complex and the prepolymer are copolymerized to form a homogeneous-phase composite material system. Compared with the prior art, a brand-new design concept is adopted, that is, a coordination compound precursor material completely formed by coordination bonds and containing a rare earth luminescent center and organic ligands is prepared by the aid of characteristics of coordination compounds, and then the precursor and the prepolymer are copolymerized to form the homogeneous-phase composite material system. The novel composite material system has processability and can be formed freely. More importantly, the proportion of the rare earth can be higher without concentration quenching, so that the fluorescence intensity of the composite material has higher application value, and the composite material can be expected to be applied to novel LED lighting and transparent display.
Description
Technical field
The invention belongs to fluorescent material technical field, relate to a kind of synthesis path and application thereof of novel matrix material
Background technology
LED (LightEmittingDiode), also known as photodiode, is born in the sixties in 20th century.Along with the continuous progress of LED manufacturing process and the exploitation of type material (element nitride crystal and fluorescent material) and application, the LED semiconductor solid-state optical source performance of coloured light of turning white the nineties in 20th century is constantly improved and enters the practical stage, makes high-brightness LED Application Areas across paramount efficiency lighting sources market.Under same illumination, the power consumption of LED is 1/10 of incandescent light, and the life-span is 20 times from vehement lamp.
In the preparation of white light LEDs, fluorescent material is a very crucial material, and its performance directly affects the brightness of white light LEDs, chromaticity coordinates, colour temperature and color developing etc.Owing to being subject to the restriction of the aspect such as patent, technology, the research and development of current fluorescent material for white light LED both at home and abroad and production are mainly in Japan, the U.S. and Taiwan, and wherein performance is it is preferred that Japan, is secondly Taiwan.How to break through the patent protection of white-light LED fluorescence material, the problem that the urgent need that entering this field has become Chinese optoelectronic industry solves.
Another problem deserving of attention is, along with the expansion of the universal of LED range of application and application scale, adopts some defects of the LED light source of existing fluorescent material and design also more and more obvious.The most outstanding defect is the homogeneity of light source, is secondly color developing.LED light source is pointolite, and no matter at lighting field or show field, pointolite all can not directly be applied.At lighting field, solution adds mat glass outside LED, and astigmatic membrane, opens make it all even soft to reach the scattering of light by pointolite as much as possible.In the display device, due to needs light source for large-area flat-panel devices provides background light source, and the intensity of light is had higher requirements, therefore have employed more complicated light guiding plate technology.Its mentality of designing is also very succinct: with polymethylmethacrylate (PMMA) for material, the light sent by LED chip is injected the total reflection being formed in PMMA inside by PMMA side, thus reaches object incident light being dispersed in whole flat board.In order to be discharged by the light of PMMA intralamellar part, must be prepared again the defect point of even compact on PMMA plate by the method for laser-induced thermal etching, the light of PMMA intralamellar part is penetrated by defect point.
Clearly, the light that LED light source sends is penetrated by defect point through light guiding plate scattering the shortcoming of this method again, is still pointolite in essence, only defines the pointolite array of very dense regular.Can not need light guiding plate completely in theory, directly LED light source is arranged into array, its light efficiency is much higher; But in technique, because highdensity LED chip flocks together the heating problem caused and the difficulty of the process implementing aspect that may bring, directly adopt LED light source array as backlight more problems.In addition, even if the decay of PMMA material on incident light is lower, but still there is loss to a certain degree.This have impact on Energy Efficiency Ratio to a certain extent.
No matter be illumination or display, the fundamental design idea of LED is all consistent: use as luminescence unit by LED chip, and it is large that the volume due to chip itself can not do, and has naturally just occurred that LED is the result of pointolite.Follow-up series of problems and solution are all formed based on the defect of LED point light source.
The key solved the problem is to prepare a kind of novel fluorescent material.This type material should possess following features:
1: higher Energy Efficiency Ratio, namely can provide higher lumen under identical power.
2: easily machine-shaping, can be prepared into the luminescence unit of arbitrary shape.
Reach this object, method feasible is at present by inorganic fluorescent material and organic polymer formation homogeneous phase compound.This compound system had both remained the optical characteristics of fluorescent material, can have again the machinable characteristic of polymkeric substance.Meanwhile, this compound system does not need the problem considering concentration quenching, fluorescence intensity can be improved by the ratio improving fluorescent material.
Patent CN201210016027.0 (week gathers around son, Du Fazhao, Wang Kefeng) provides a kind of good light stability, and light decay is little, and luminous efficiency is high, the white light LEDs rare-earth fluorescent PC (polycarbonate) that transmittance is high and mist degree is high.By PC, combined fluorescent RE powder, compatilizer, oxidation inhibitor, gained mixture evenly, then is put into twin screw extruder melt blending by lubricant and dispersant, obtains white light LEDs rare-earth fluorescent PC.
Patent CN201320646310.1 (stone light, Wang Zezhong, Hou Qiong) invent a kind of fluorescence LED device, it comprises light diffusion lampshade, rare-earth fluorescent resin sheet, LED condensing lens, LED chip and Combined type reflection cup, described Combined type reflection cup comprises outside reflection cup and inner reflection cup, inner reflection cup back-off shape is combined with outside reflection cup, the first enclosed space is formed after the cup bottom opening place of inner reflection cup and rare-earth fluorescent resin sheet combine, LED condensing lens and LED chip are in the first enclosed space, LED chip is in below LED condensing lens, above outside reflection cup, the second enclosed space formed after outside reflection cup and light diffusion lampshade compact siro spinning technology, the first enclosed space is positioned at the second enclosed space.Fluorescent material is separated with LED chip, is conducive to the heat radiation of chip and maintains the stability in use of fluorescent material; Light conversion range is limited in a pocket, the consumption of fluorescence resin sheet can be reduced, reduce costs; The protection of light diffusion lampshade is inner, makes light soft, specious simultaneously.
Patent No. CN200810204416.X (Yan Bing contains triumphant) adopts the method for colloidal sol-gel that obtained material is obtained xerogel through polyreaction, the organic high molecular polymer with Long carbon chain is embedded in silica network matrix by covalent linkage, and obtain chemistry by dry weathering process and thermodynamic property is stablized, surface topography is regular, have characteristic fluorescence launch polymer composite.
Patent 200910217728.9 discloses a kind of preparation method of rare earth fluorescence micro/nano fibers array, by mass ratio be 1: 5 ~ 40 rare earth compounding and macromolecular material to be dissolved in respectively in organic solvent and to stir, prepared rare earth compounding/macromolecule material solution; Described solution is got 1 ~ 5 microlitre drop on slide glass, then be that the porous alumina formwork of 50 ~ 800 nanometers is placed on drop by aperture, solvent dissolves alumina formwork after naturally volatilizing, just the regular nanofiber array of array.Rare earth compounding/macromolecular material composite micro-nano rice fiber prepared by this invention and array thereof are due to the stable workability of the photoluminescence property and macromolecular material with rare earth material, can be used for following field: micro-nano luminescent device, optical sensor, micro Nano material mark, used for solar batteriesly turn optical assembly, false proof or Noctilucent safety sign fabrics, safety check and security detection etc.
Patent 02134788.3 (Zhang Xiuju Chen Ming) is thiazolinyl organic acid rare earth compound and the high molecular graft copolymer of synthesis, and scion grafting rate is 1 ~ 20%.Its synthetic method adopts the method for fusion-grafting by thiazolinyl organic acid rare earth compound fusion-grafting in synthesis macromolecule matrix, and reaction product is dissolved through aromatic hydrocarbon solvent again, and acetone precipitation, drying forms.This luminescent material good stability, applies face width, cost is low, method is easy, is easy to suitability for industrialized production, and this material fluorescence intensity is high, purity of color is high, has widened the use face of photoluminescence rareearth polymer material, can be widely used in luminous and display field.
Patent 201410673863.5 (western Peng Zhao Fu Laiguxiao China builds Cheng Bowen) discloses nano phase change energy storage luminescent fibre, comprising: polyurethanes solid-solid phase transition material 50%-100%; Polymethylmethacrylate 0%-50%, above constituent mass content is 100%; With said components total amount, benzoic acids ternary RE luminescent material accounts for the 10%-30% of above-mentioned total mass.Invention also discloses the preparation method of nano phase change energy storage luminescent fibre, with polyurethanes solid-solid phase transition material for fibre-forming polymer, with benzoic acids ternary rare earth complex for luminescent material, with ethyl acetate and N, dinethylformamide is double solvents, is prepared the phase-change accumulation energy luminescent fibre of diameter 30-100nm by electrostatic spinning technique.The features such as the phase in version enthalpy that this phase transformation luminescent fibre has thermal energy storage and release is high, and phase transition rate is fast, stable luminescent property, and fluorescence lifetime is long, can be widely used in the field such as medical and health, electronic information clothes.
Summary of the invention
The object of the invention is for the problems referred to above, a kind of synthesis path of the novel matrix material that can solve the problems of the technologies described above is provided.
In order to reach above-mentioned goal of the invention, have employed following technical proposal: the present invention adopts coordination high polymer to be the presoma of matrix material, with the linear performed polymer of synthesized polymer material for reactant, using coordination compound as linking agent, be cross-linked with tridimensional network by the linear molecule chain of performed polymer, being formed with rare earth compounding is the three-dimensional netted polymer composite system of node.Be specially the title complex forming polyfunctionality with RE (rare earth element) and vinylformic acid and acrylic acid derivative coordination, then the monomer of macromolecule resin to be synthesized be polymerized in advance the linear performed polymer of distribution of low molecular weight.In performed polymer, add rare earth compounding cause the polymer composite system that crosslinking reaction formation has tridimensional network.
Compared with prior art, the present invention, have employed a kind of brand-new mentality of designing.Namely utilize the feature of coordination compound, prepare completely with the coordination compound persursor material containing rare-earth luminescent center and organic phase part that coordinate bond is formed, then presoma and polymer performed polymer are carried out copolymerization form homogeneous phase composite system.This advanced composite material system possesses machinable ability, can random molding.Prior thing, can do higher of the ratio due to rare earth and concentration quenching can not occur, the fluorescence intensity of this matrix material embodies higher using value, is expected to apply in Novel LED illuminating and Transparence Display.
Embodiment
The preparation of title complex:
RE2O3 (a gram), adds 20ml water, drips concentrated hydrochloric acid under magnetic agitation, when becoming clear to liquid.Be heated to 100 degrees Celsius, keep 10-20 minute.Be cooled to room temperature, now have and precipitate generation in a large number.Filter, dry.Add ethanol 10ml, stir as settled solution.Methacrylic acid (MMA) 20ml is altogether dripped under whipped state.Then at room temperature stir 48 hours.Alcohol solvent steams by products therefrom under 75-78 degree Celsius, is the mixture of RE/MMA title complex and MMA.Be product I.
The synthesis of PMMA performed polymer:
First class methyl acrylate (MMA) 50 grams, adds Diisopropyl azodicarboxylate 0.3 gram, shakes up and melt.Water-bath 75 degrees Celsius reaction 30 minutes-60 minutes.Control performed polymer viscosity between 1000-3000.Be product II.
The preparation of RE/PMMA compound system:
Under product II ice-water bath whipped state, drip product I, after dropwising, mixture is moved in mould, according to the condition of temperature rise rate 1 °/min, by the temperature of reaction system to 50 degrees Celsius, insulation 1-3 hour.Be warmed up to 95 degrees Celsius, insulation 1-3 hour.Be product III.This is final product.
Matrix material is applied in Novel LED illuminating and Transparence Display.
Claims (7)
1. the synthesis path of a novel matrix material, it is characterized in that, namely now the title complex of synthesizing rare-earth and unsaturated organic carboxyl acid or derivatives thereof is as presoma, and the performed polymer of resynthesis macromolecule resin material, then forms homogeneous phase composite system by title complex and performed polymer copolymerization.
2. the synthesis path of novel matrix material according to claim 1, is characterized in that, the title complex of described rare earth and unsaturated organic carboxyl acid, and the composition of its rare earth is Ce, Eu, Yb, Er, Lu, Dy, Dm, Ho, Sm, Tb, La, Pr, Nd, Y; Valence state is trivalent; The kind of unsaturated organic carboxyl acid is vinylformic acid, methacrylic acid and corresponding derivative methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate etc.
3. the synthesis path of novel matrix material according to claim 1, it is characterized in that, the kind of described synthetic macromolecule resin material is polymethylmethacrylate (PMMA), polystyrene (PS), polycarbonate (PC).
4. the synthesis path of novel matrix material according to claim 1, is characterized in that, the synthetic method of the title complex of described rare earth and unsaturated organic carboxyl acid is as follows: be synthesize starting point with rare earth oxide, obtain the muriate of rare earth with dissolving with hydrochloric acid; The saturated alcohol solution of rare earth chloride is obtained with dissolve with ethanol rare earth chloride; Under agitation, room temperature drips unsaturated carboxylic acid and enters rare earth saturated alcohol solution; At the uniform velocity stirring reaction 48 hours under room temperature; Heating evaporation solvent obtains the xln of title complex; Filter, with methanol wash xln three times, after drying, be title complex.
5. the synthesis path of novel matrix material according to claim 1, is characterized in that, the macromolecule resin material of described synthesis, and the viscosity controller of its performed polymer is at 1000-5000C.P.S.
6. the synthesis path of novel matrix material according to claim 1, is characterized in that, is 1-10:100 (weight percent) in the ratio of complex precursors and synthetic macromolecule resin material.
7. according to the application of matrix material in illumination and display that the synthesis path of the novel matrix material of claim 1-6 any one obtains.
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CN201510498062.4A CN105061964A (en) | 2015-08-13 | 2015-08-13 | Synthesis path and application of novel composite material |
CN201610010254.0A CN105693751B (en) | 2015-08-13 | 2016-01-06 | A kind of RE@MMA linear fit object and its application |
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CN201510498062.4A CN105061964A (en) | 2015-08-13 | 2015-08-13 | Synthesis path and application of novel composite material |
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CN201610010254.0A Active CN105693751B (en) | 2015-08-13 | 2016-01-06 | A kind of RE@MMA linear fit object and its application |
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CN105693751A (en) * | 2015-08-13 | 2016-06-22 | 嘉善镭铈光电科技有限公司 | RE@MMA linear complex and application thereof |
CN108822266A (en) * | 2018-05-31 | 2018-11-16 | 合肥昂诺新材料有限公司 | A kind of preparation method of polyurethane photo-induced luminescent material |
CN109762088A (en) * | 2018-12-27 | 2019-05-17 | 帝斯曼先达合成树脂(佛山)有限公司 | A kind of preparation method for the cross-linked network intermediate being used to prepare aqueous dual-component system acrylic resin |
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CN103755864B (en) * | 2014-01-20 | 2016-06-22 | 扬州大学 | A kind of preparation method of fluorescence lucite |
CN104558383B (en) * | 2015-01-06 | 2017-05-10 | 湖北鼎龙控股股份有限公司 | Fluorescent complex containing carboxylic acid type high polymer and rare earth, preparation method of fluorescent complex, fluorescent chemical carbon powder and preparation method of fluorescent chemical carbon powder |
CN105061964A (en) * | 2015-08-13 | 2015-11-18 | 嘉善镭铈光电科技有限公司 | Synthesis path and application of novel composite material |
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CN105693751A (en) * | 2015-08-13 | 2016-06-22 | 嘉善镭铈光电科技有限公司 | RE@MMA linear complex and application thereof |
CN105693751B (en) * | 2015-08-13 | 2019-05-10 | 嘉善镭铈光电科技有限公司 | A kind of RE@MMA linear fit object and its application |
CN108822266A (en) * | 2018-05-31 | 2018-11-16 | 合肥昂诺新材料有限公司 | A kind of preparation method of polyurethane photo-induced luminescent material |
CN109762088A (en) * | 2018-12-27 | 2019-05-17 | 帝斯曼先达合成树脂(佛山)有限公司 | A kind of preparation method for the cross-linked network intermediate being used to prepare aqueous dual-component system acrylic resin |
CN109762088B (en) * | 2018-12-27 | 2021-07-27 | 帝斯曼先达合成树脂(佛山)有限公司 | Preparation method of crosslinked network intermediate for preparing acrylic resin of aqueous bi-component system |
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