CN105801745B - A kind of preparation method for the iridium europium bimetallic polymerization matter fluorescent powder for sending out bright red - Google Patents

A kind of preparation method for the iridium europium bimetallic polymerization matter fluorescent powder for sending out bright red Download PDF

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CN105801745B
CN105801745B CN201610167598.2A CN201610167598A CN105801745B CN 105801745 B CN105801745 B CN 105801745B CN 201610167598 A CN201610167598 A CN 201610167598A CN 105801745 B CN105801745 B CN 105801745B
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iridium
europium
bright red
fluorescent powder
water
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CN105801745A (en
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张爱琴
侯哲寓
贾虎生
许并社
杨亚敏
赵希瑾
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • 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
    • C09K2211/14—Macromolecular compounds

Abstract

The present invention relates to a kind of preparation method for the iridium europium bimetallic polymerization matter fluorescent powder for sending out bright red,It is to prepare hardly possible for hair bright red iridium europium bimetallic polymerization thing,Purity is low,The situation of poor performance,Using iridium europium complex,Dimethyl sulfoxide (DMSO),Methyl methacrylate,Absolute methanol and azodiisobutyronitrile are raw material,It is configured solution,Synthetic polymer,Precipitation,Washing,Filter,Vacuum freeze drying,It is prepared into the iridium europium bimetallic polymerization matter fluorescent powder of hair bright red,This preparation method technique is advanced,Data are accurately full and accurate,Obtained iridium europium bimetallic polymerization thing is powder,Powder granule diameter≤0.2 μm,Product purity is good,Up to 99.4%,Chromaticity coordinates is X=0.627,Y=0.331,Send out bright red,Can be with indigo plant,Green fluorescence powder synthesizes white fluorescence film,It is the fast preparation method of the advanced iridium europium bimetallic polymerization matter fluorescent powder to glow,Can be in 3D printing technique field application.

Description

A kind of preparation method for the iridium-europium bimetallic polymerization matter fluorescent powder for sending out bright red
Technical field
The present invention relates to a kind of fast preparation method for the fluorescent material for sending out bright red, belongs to what luminescent material was prepared and applied Technical field.
Background technology
White light emitting diode LED has the advantages of little power consumption, fast response time, long lifespan, small volume, is most prospect Solid-state illumination light source, be a problem for needing to study because complex manufacturing, cost are high.
The main flow for realizing white light is fluorescent material conversion, mainly there is blue chip+yellow fluorescent powder, black light chip+three Two methods of primary colours fluorescent material；The former colour rendering index is low, color-match is poor, bias light be present；The latter's white color quality depends on In fluorescent material, colour rendering index is high, can obtain the white light LEDs of stronger color；Ultraviolet light does not influence on illuminant colour, and colourity is by temperature Degree, curent change influence it is smaller, the problem of in the absence of bias light；Therefore, near ultraviolet excited white light LED is increasingly by luminous photograph The attention in bright field.
Black light LED red light fluorescent powder primarily serves regulation colour temperature and improves the effect of colour rendering index, to obtain The warm white of stronger color reproduction；Simultaneously in order to shorten the production time of LED component, simplify technique, research and develop near ultraviolet The red light fluorescent powder excited is highly important.
The content of the invention
Goal of the invention
The purpose of the present invention is the situation for background technology, with iridium-europium complex, dimethyl sulfoxide (DMSO), methacrylic acid Methyl esters, absolute methanol, azodiisobutyronitrile are raw material, and it is cold to be configured solution, synthetic polymer, precipitation, washing, suction filtration, vacuum It is lyophilized dry, iridium-europium bimetallic polymerization matter fluorescent powder of hair bright red is made, to improve the purity of white light emitting material, luminescent properties, It can be applied in 3D printing technique.
Technical scheme
The chemical substance material that the present invention uses is：It is iridium-europium complex, dimethyl sulfoxide (DMSO), methyl methacrylate, anhydrous Methanol, azodiisobutyronitrile, nitrogen, it is as follows that it combines preparation dosage：With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows：
(1) selected chemical substance material
To preparation, required chemical substance material will be carried out selected, and carry out quality purity control：
(2) solution is prepared
Iridium-europium complex 0.1905g ± 0.0001g is weighed, dimethyl sulfoxide (DMSO) 10mL ± 0.0001mL is measured, measures methyl Methyl acrylate 1.6mL ± 0.0001mL；
It is added in beaker, stirs 30min, make its dissolving, into：0.01mol/L iridium-europium complex solution；
(3) azodiisobutyronitrile solution is prepared
Azodiisobutyronitrile 0.0148g ± 0.0001g is weighed, measures dimethyl sulfoxide (DMSO) 2mL ± 0.0001mL；
Add in beaker, stir 5min, make its dissolving, into：0.05mol/L azodiisobutyronitrile solution；
(4) iridium-europium bimetallic polymerization thing is prepared
The preparation of iridium-europium bimetallic polymerization thing is carried out in four-hole boiling flask, be heating water bath, stirring, logical nitrogen, Completed under water circulation condensing state；
1. four-hole boiling flask is placed on cleansing bath tub, cleansing bath tub is placed on electric heater, is water-bath water in cleansing bath tub, water-bath Water will flood the 4/5 of four-hole boiling flask volume；
Four-hole boiling flask top sets gradually nitrogen tube, agitator, addition funnel, water circulation condenser pipe from left to right；
2. the iridium of configuration-europium complex solution, azodiisobutyronitrile solution are added in four-hole boiling flask, into mixed solution；
Opening electric heater, heat mixed solution, 78 DEG C ± 1 DEG C of heating-up temperature, heat time 12h；
Nitrogen tube is opened, nitrogen, nitrogen input speed 20cm are inputted into four-hole boiling flask3/ min, input time 12h；
Agitator is stirred, and water circulation condenser pipe is condensed；
Mixed solution will chemically react under heating water bath, stirring, nitrogen protection, water circulation condensation, reactional equation Formula is as follows：
In formulaIridium-europium bimetallic gathers Compound, polymerization degree n=18000；
After reaction terminates, stop heating, stop logical nitrogen, stop stirring, stop water circulation condensation, make mixed solution with bottle It is cooled to 25 DEG C；
(5) precipitate
Reacted mixed solution is poured into beaker, then adds absolute methanol 100mL, carries out precipitation process, is stood 1h, white flock precipitate thing is generated, is then shredded sediment with scissors；
(6) absolute methanol washing, suction filtration
The white flock precipitate thing shredded is placed in beaker, adds absolute methanol 100mL, agitator treating 5min, then Filtered with miillpore filter, retain filter cake, discard cleaning solution；
Washing, suction filtration repeat 5 times；
(7) vacuum freeze drying
Product cake is placed in silica dish, is subsequently placed in vacuum freezing drying oven and is dried, drying temperature -80 DEG C, vacuum 6Pa, drying time 480min, red light fluorescent powder is obtained after drying；
(8) grind, sieve
Dried red light fluorescent powder is ground with agate mortar, pestle, then sieved with 650 mesh filter screens, grinding, Sieving is repeated；Obtain iridium-europium bimetallic polymerization matter fluorescent powder of end-product hair bright red；
(9) test, analysis and characterization
To the pattern of iridium-europium bimetallic polymerization matter fluorescent powder of the hair bright red of preparation, color and luster, purity, chemical composition, Luminescent properties and chromaticity coordinates are detected, analyzed and characterized；
Fluorescence excitation, emission spectrographic analysis are carried out to product with XRF；
Product morphology analysis is carried out to product with ESEM；
Mutation analysis of the differential heat flow with temperature and time is carried out to product with differential scanning calorimeter；
Conclusion：Iridium-europium bimetallic polymerization matter fluorescent powder of hair bright red is white powder, the μ of powder granule diameter≤0.2 M, product purity 99.4%, send out bright red, chromaticity coordinates：X=0.627, Y=0.331；
(10) product storage
The glass container of amber transparent is stored in iridium-europium bimetallic polymerization matter fluorescent powder of the hair bright red of preparation In, closed to be kept in dark place, moistureproof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, is to be directed to bright red iridium-europium bimetallic polymerization thing Preparation is difficult, purity is low, poor performance situation, using iridium-europium complex, dimethyl sulfoxide (DMSO), methyl methacrylate, absolute methanol It is raw material with azodiisobutyronitrile, is configured solution, synthetic polymer, precipitation, washing, suction filtration, vacuum freeze drying, is prepared into Iridium-europium bimetallic polymerization matter fluorescent powder of bright red is sent out, this preparation method technique is advanced, and data are accurately full and accurate, obtained iridium- Europium bimetallic polymerization thing is powder, and powder granule diameter≤0.2 μm, product purity is good, up to 99.4%, chromaticity coordinates X= 0.627, Y=0.331, send out bright red, can with it is blue, green fluorescence powder synthesizes white fluorescence film, be the advanced iridium-europium to glow The fast preparation method of bimetallic polymerization matter fluorescent powder, can be in 3D printing technique field application.
Brief description of the drawings
Fig. 1, prepare iridium-europium bimetallic polymerization thing polymerization state figure
Fig. 2, the iridium-europium bimetallic polymerization thing exciting light spectrogram for sending out bright red
Fig. 3, the iridium-europium bimetallic polymerization thing fluorescence spectra for sending out bright red
Fig. 4, the iridium-europium bimetallic polymerization matter fluorescent powder chromaticity coordinates figure for sending out bright red
Fig. 5, the iridium-europium bimetallic polymerization matter fluorescent powder shape appearance figure for sending out bright red
Fig. 6, the iridium-europium bimetallic polymerization matter fluorescent powder means of differential scanning calorimetry figure for sending out bright red
Fig. 7, the iridium-europium bimetallic polymerization matter fluorescent powder diffracted intensity collection of illustrative plates for sending out bright red
Shown in figure, list of numerals is as follows：
1 electric heater, 2 electric cabinets, 3 display screens, 4 indicator lamps, 5 power switches, 6 cleansing bath tubs, 7 four-hole boiling flasks, 8 water circulations Condenser pipe, 9 gas outlets, 10 water inlets, 11 delivery ports, 12 addition funnels, 13 control valves, 14 agitators, 15 nitrogen valves, 16 nitrogen Pipe, 17 nitrogen cylinders, 18 resistance heaters, 19 heating temperature controls, 20 agitator controllers, 21 nitrogen, 22 water-bath waters, 23 is mixed Close solution, 24 fixed seats.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described：
Shown in Fig. 1, to send out iridium-europium bimetallic polymerization thing polymerization state figure of bright red, each portion position, annexation will Correctly, match, sequentially operate according to quantity.
The value for preparing each chemical substance used is determined by the scope pre-set, with gram, milliliter, centimetre3For Measurement unit.
The synthesis of iridium-europium bimetallic polymerization thing for sending out bright red is carried out in four-hole boiling flask, be prepare solution, Completed under heating water bath, stirring, nitrogen protection, water circulation condensing state；
The top of electric heating agitator 1 is cleansing bath tub 6；Four-hole boiling flask 7 is installed on the top of cleansing bath tub 6, and is fixed by fixed seat 24；Water It is water-bath water 22 in bathtub 6, water-bath water 22 will flood the 4/5 of four-hole boiling flask volume；Nitrogen is set from left to right on the top of four-hole boiling flask 7 Tracheae 16, agitator 14, addition funnel 12 and control valve 13, water circulation condenser pipe 8 and gas outlet 9, water inlet 10, delivery port 11；Resistance heater 18 is provided with electric heater 1；Nitrogen cylinder 17 is provided with the left part of electric heater 1, the top of nitrogen cylinder 17 is set There are nitrogen valve 15, nitrogen tube 16, and nitrogen 21 is inputted into four-hole boiling flask 7；The right part of electric heater 1 is provided with electric cabinet 2, automatically controlled Case 2 is provided with display screen 3, indicator lamp 4, power switch 5, heating temperature control 19, agitator controller 20.
Shown in Fig. 2, to send out iridium-europium bimetallic polymerization thing exciting light spectrogram of bright red, shown in figure, the double gold of iridium-europium Category polymer fluorescent powder can be excited at black light 390nm, and it is a kind of to be excited available near ultraviolet chip to illustrate it Red fluorescence powder.
Shown in Fig. 3, to send out iridium-europium bimetallic polymerization thing fluorescence spectra of bright red, shown in figure, the double gold of iridium-europium Category polymer shows sharp strong emission peak at 612nm, is the characteristic emission peak of europium ion, shows that iridium-europium bimetallic gathers Compound successful polymerization.
Shown in Fig. 4, to send out iridium-europium bimetallic polymerization matter fluorescent powder chromaticity coordinates figure of bright red, shown in figure, iridium-europium The chromaticity coordinates of bimetallic polymerization thing is X=0.627, Y=0.331, positioned at red light district.
Shown in Fig. 5, to send out iridium-europium bimetallic polymerization matter fluorescent powder shape appearance figure of bright red, shown in figure, complex list Body is uniformly distributed in polymer matrix, and scattered hole shape, grain diameter≤0.2 μm is presented.
Shown in Fig. 6, to send out iridium-europium bimetallic polymerization matter fluorescent powder means of differential scanning calorimetry figure of bright red, shown in figure, The melting temperature of polymer is 133 DEG C, and 3D printing technique can be used under melting temperature, is printed as with blue, green light fluorescent powder white Light fluorescent film, prepare the LED component to emit white light.
Shown in Fig. 7, to send out iridium-europium bimetallic polymerization matter fluorescent powder diffracted intensity collection of illustrative plates of bright red, shown in figure, indulge Coordinate is diffracted intensity index, and abscissa is the θ of the angle of diffraction 2, and iridium-europium bimetallic fluorescent material steamed bun type occurs in 14 ° and 30 ° Diffraction maximum, show that iridium-europium bimetallic polymerization matter fluorescent powder shows non-crystalline.

Claims (4)

  1. A kind of 1. preparation method for the iridium-europium bimetallic polymerization matter fluorescent powder for sending out bright red, it is characterised in that：
    The chemical substance material used is：Iridium-europium complex Eu (C28H16N3O2F4Ir)2(C12H8N2)(C11H19O2), dimethyl it is sub- Sulfone, methyl methacrylate, absolute methanol, azodiisobutyronitrile, nitrogen；
    Preparation method is as follows：
    (1) selected chemical substance material
    To preparation, required chemical substance material will be carried out selected, and carry out quality purity control：
    (2) solution is prepared
    Iridium-europium complex 0.1905g ± 0.0001g is weighed, dimethyl sulfoxide (DMSO) 10mL ± 0.0001mL is measured, measures metering system Sour methyl esters 1.6mL ± 0.0001mL, is added in beaker, stirs 30min, makes its dissolving, into iridium-europium complex solution；
    (3) azodiisobutyronitrile solution is prepared
    Azodiisobutyronitrile 0.0148g ± 0.0001g is weighed, measures dimethyl sulfoxide (DMSO) 2mL ± 0.0001mL；
    Add in beaker, stir 5min, make its dissolving, into azodiisobutyronitrile solution；
    (4) iridium-europium bimetallic polymerization thing is prepared
    The preparation of iridium-europium bimetallic polymerization thing is carried out in four-hole boiling flask, is followed in heating water bath, stirring, logical nitrogen gas and water Completed under ring condensing state；
    1. four-hole boiling flask is placed on cleansing bath tub, cleansing bath tub is placed on electric heater, is water-bath water in cleansing bath tub, water-bath water will Flood the 4/5 of four-hole boiling flask volume；
    Four-hole boiling flask top sets gradually nitrogen tube, agitator, addition funnel, water circulation condenser pipe from left to right；
    2. the iridium of configuration-europium complex solution, azodiisobutyronitrile solution are added in four-hole boiling flask, into mixed solution；
    Opening electric heater, heat mixed solution, 78 DEG C ± 1 DEG C of heating-up temperature, heat time 12h；
    Nitrogen tube is opened, nitrogen, nitrogen input speed 20cm are inputted into four-hole boiling flask3/ min, input time 12h；
    Agitator is stirred, and water circulation condenser pipe is condensed；
    Mixed solution will chemically react under heating water bath, stirring, nitrogen protection, water circulation condensation；
    After reaction terminates, stop heating, stop logical nitrogen, stop stirring, stop water circulation condensation, mixed solution is cooled down with bottle To 25 DEG C；
    (5) precipitate
    Reacted mixed solution is poured into beaker, then adds absolute methanol 100mL, carries out precipitation process, stands 1h, it is raw Into white flock precipitate thing, then sediment is shredded with scissors；
    (6) absolute methanol washing, suction filtration
    The white flock precipitate thing shredded is placed in beaker, absolute methanol 100mL, agitator treating 5min are added, then with micro- Hole filter membrane is filtered, and is retained filter cake, is discarded cleaning solution；
    Washing, suction filtration repeat 5 times；
    (7) vacuum freeze drying
    Product cake is placed in silica dish, is subsequently placed in vacuum freezing drying oven and is dried, -80 DEG C of drying temperature, very Reciprocal of duty cycle 6Pa, drying time 480min, red light fluorescent powder is obtained after drying；
    (8) grind, sieve
    Dried red light fluorescent powder is ground with agate mortar, pestle, then sieved with 650 mesh filter screens, grinding, sieving It is repeated；Obtain iridium-europium bimetallic polymerization matter fluorescent powder of end-product hair bright red；
    Conclusion：Iridium-europium bimetallic polymerization matter fluorescent powder of hair bright red is white powder, powder granule diameter≤0.2 μm, is produced Thing purity 99.4%, send out bright red, chromaticity coordinates：X=0.627, Y=0.331.
  2. 2. a kind of preparation method of iridium-europium bimetallic polymerization matter fluorescent powder for sending out bright red according to claim 1, its It is characterised by：
    The synthesis for sending out iridium-europium bimetallic polymerization thing of bright red is carried out in four-hole boiling flask, is to prepare solution, water-bath Completed under heating, stirring, logical nitrogen, water circulation condensing state；
    Electric heater (1) top is cleansing bath tub (6)；Cleansing bath tub (6) top installation four-hole boiling flask (7), and it is solid by fixed seat (24) It is fixed；It is water-bath water (22) in cleansing bath tub (6), water-bath water (22) will flood the 4/5 of four-hole boiling flask volume；On four-hole boiling flask (7) Portion sets nitrogen tube (16), agitator (14), addition funnel (12) and control valve (13) thereon, water circulation condenser pipe from left to right (8) gas outlet (9) and thereon, water inlet (10), delivery port (11)；Resistance heater (18) is provided with electric heater (1)； Nitrogen cylinder (17) is provided with the left part of electric heater (1), nitrogen cylinder (17) top is provided with nitrogen valve (15), nitrogen tube (16), and Input nitrogen (21) in four-hole boiling flask (7)；Electric heater (1) right part is provided with electric cabinet (2), is provided with electric cabinet (2) aobvious Display screen (3), indicator lamp (4), power switch (5), heating temperature control (19), agitator controller (20).
  3. 3. a kind of preparation method of iridium-europium bimetallic polymerization matter fluorescent powder for sending out bright red according to claim 1, its It is characterised by：Iridium-europium bimetallic polymerization matter fluorescent powder can be excited at black light 390nm.
  4. 4. a kind of preparation method of iridium-europium bimetallic polymerization matter fluorescent powder for sending out bright red according to claim 1, its It is characterised by：The melting temperature of its polymer is 133 DEG C.
CN201610167598.2A 2016-03-23 2016-03-23 A kind of preparation method for the iridium europium bimetallic polymerization matter fluorescent powder for sending out bright red Active CN105801745B (en)

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CN101367826A (en) * 2008-09-24 2009-02-18 上海大学 Linking type Eu3+ organic conjunction, its copolymer red luminescent material and method of preparing the same
CN104498032A (en) * 2014-12-16 2015-04-08 武汉工程大学 Side-hanging type polymethyl methacrylate rare earth complex luminescent material and preparation method thereof
CN105061481B (en) * 2015-08-26 2017-03-22 重庆理工大学 Preparation method of ternary terbium complex monomer and copolymer luminescent material of ternary terbium complex monomer and MMA
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