CN109971413A - A kind of preparation method of high refractive index LED packaging plastic material - Google Patents
A kind of preparation method of high refractive index LED packaging plastic material Download PDFInfo
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- CN109971413A CN109971413A CN201910143460.2A CN201910143460A CN109971413A CN 109971413 A CN109971413 A CN 109971413A CN 201910143460 A CN201910143460 A CN 201910143460A CN 109971413 A CN109971413 A CN 109971413A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses a kind of preparation method of high refractive index LED packaging plastic material, the phase transfer method that the present invention uses can be used for shifting nanoparticle between two liquid phases.By using phase transfer of technology, the nanoparticle being dispersed in water phase can be transferred in organic phase, the reason is that the nano zircite particle of cladding phosphoric acid class modifying agent dissolubility in the small solvent of polarity is bigger, therefore be easy to be transferred in organic phase from water.Compared to other methods, environmental requirement needed for phase transfer method is lower, and operation is simpler, and cost is relatively low, is very suitable to largely prepare the nano zircite particles and high refractive index composite package glue material with polymolecularity.This method can prepare the small and uniform nano zircite particle of good dispersion, particle and zirconium oxide is made to be enriched with the nano zircite dispersion for forming high solids content in a solvent.And reaction condition is easily controllable, has large-scale industrial production condition.
Description
Technical field
The present invention relates to field of adhesive technology, more particularly to a kind of high refractive index, the high grade of transparency and high-adhesion LED
The preparation method of packaging plastic material.
Background technique
Zirconium dioxide is also known as zirconic anhydride or zirconium oxide, to be difficult to dissolve in water, but can be in hot concentrated sulfuric acid and hydrofluoric acid
The solid of dissolution.About 2700 DEG C of zirconium dioxide fusing point, about 4300 DEG C of boiling point, about 5000 DEG C of flash-point.Compared to rise an oxide of the same clan, two
Zirconium oxide property is stablized, and without photocatalytic, the bulk effect having due to nano material, skin effect, quantum size, quantum
The big effect of tunnel, dielectric confinement etc. five and studied and applied extensively, wherein nano zirconium dioxide particle can be applied to make
Make biomaterial, ceramic material etc., it can also be used to synthetic catalyst or co-catalyst in certain chemical reactions.Nano-silica
Change zirconium particle and be used especially for photoelectric field, such as making an addition to zirconium dioxide nanoparticles in LED light emitting device packaging plastic can be with
The refractive index for improving packaging plastic has the function that energy-saving and emission-reduction to improve the light emission rate of device.It will be appreciated that such as
Fruit is easy to reunite in organic substrate without some special surface particle modification techniques, nano zirconia particles, group
Poly- phenomenon causes local granule excessive, and dispersion is uneven, so that the transmitance of composite base material be caused to be greatly reduced, reduces instead
LED component goes out optical property.Therefore be first to prepare can be excellent in organic solvent system dispersion performance for the key of the technical field
, it is capable of the transparent zirconium dioxide dispersion of long-time stable.The dispersion again can be with simple solvent blending method and LED later
Packaging adhesive material mixing, and nano zircite particle uniformly can be scattered in organic substrate after removal of solvents, and keep high saturating
The characteristics such as bright and high refractive index.
Have described in patent certain methods and prepares the lesser nano zircite aqueous dispersions of partial size, such as patent
Heat alkaline zirconium salt solution in CN106277049B, acquired solution removes the laggard row hydro-thermal reaction of impurity through dialysis and produced
Object；Using the method that hydrogen peroxide reaction is added in strong basicity zirconium salt solution in patent CN201810836953.X, later with acid
Liquid and water wash precipitating respectively and obtain product, but LED encapsulation material is generally epoxy resin and organic silica gel class, these two types of
Organic polymer can not form the compound glue material of evenly dispersed transparent nano with hydrophilic nano zircite.Therefore one is needed
The method that its fine dispersion in organic solvent kind is realized while preparing minor diameter nano zircite particle.This method knot
Closed Aqueous dispersions Antibody Production Techniques and organic acid surface finished technology, by phase transfer method prepare high degree of dispersion, partial size it is small,
Uniform and small reunion degree transparent nano zirconium dioxide particle organic phase dispersion.Packaging plastic material is added in such dispersion
After remove solvent, can be obtained the packaging plastic of Uniform Doped nano zircite, refractive index is not compared to adding nano zircite
Packaging plastic material is obviously improved.
It, can be by using the surface of end You Jian functional group when preparing transparent nano zirconia particles organic phase dispersion
Modifying agent by the chemical bond of Zirconium oxide nano grain in conjunction with modifying agent, to increase its dispersibility in dispersate, therefore
Selecting a kind of suitable modifying agent is an extremely crucial step.Some modifying agent are selectively used in research before
It is modified that surface is carried out to nano zircite.Patent CN102448888A is using aryl-sulfonyl oxygen modifying agent to nano zircite
Grain is modified, and the method raw material technique that is easy to get is simpler, but there is a defect is the general mistake of aryl-sulfonyl oxygen organic matter
It is difficult to remove in stabilization, impurity in product may be made excessive；Patent CN102031026A is by amino silane to nano oxidized
Zirconium is modified, and can obtain the preferable zirconia dispersion of dispersibility, but since its dispersant is single, preparation process is multiple
It is miscellaneous, and reaction condition is more demanding, therefore, it is difficult to realize industrial a large amount of preparations.
The present invention has selected be modified the surface of Zirconium oxide nano grain using phosphoric acid as a kind of organic acid of representative, this
Class organic acid has as a kind of new untapped modifying agent compared to the more superior property of other modifying agent.With phosphoric acid
For modifying agent, method of modifying be zirconium surface formed Zr-O-P key, due to the phosphate radical thermal stability in phosphoric acid compared with
Height effectively hinders the contact between zirconia particles, so that the length of Zirconium oxide nano grain is inhibited in phase transfer reaction
Big and reunion, to increase the dispersion degree of nano particle.
The phase transfer method that the present invention uses can be used for shifting nanoparticle between two liquid phases.By using phase transfer skill
Art, the nanoparticle being dispersed in water phase can be transferred in organic phase, the reason is that cladding phosphoric acid class modifying agent is nano oxidized
Zirconium particle dissolubility in the small solvent of polarity is bigger, therefore is easy to be transferred in organic phase from water.Compared to its other party
Method, environmental requirement needed for phase transfer method is lower, operates simpler, and cost is relatively low, and being very suitable to largely prepare has polymolecularity
Nano zircite particle and high refractive index composite package glue material.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of transparent organic phase nano zircite particle dispersion
The preparation method of body.First with the nano zircite aqueous dispersions of the preparations such as hydro-thermal method, then pass through has the preparation method
The modified method of machine acid makes zirconium surface bonding, so that phase transfer reaction occur, nano zircite particle is enriched in organic phase
Middle formation transparent zirconium oxide nanoparticle dispersion.This method can prepare the small and uniform nano oxygen of good dispersion, particle
Change zirconium particle, and zirconium oxide can be made to be enriched with the nano zircite dispersion for forming high solids content in a solvent.And reaction condition is easy
In control, has large-scale industrial production condition.
Second technical problem to be solved by this invention is to provide a kind of transparent organic phase nano zircite particle point
Granular media.The transparent organic phase dispersion solid content is 0.01-50wt%, and crystal of zirconium oxide partial size is small, is evenly distributed, average grain diameter
6.23 nanometer；In addition, the liquid dispersion stable dispersion effect is good, liquid dispersion solid content is higher, is suitable for placing for a long time
It saves, industrial production can be widely used in.
Third technical problem to be solved by this invention is to provide a kind of transparent organic phase nano zircite particle point
The application description of granular media.
In order to solve the first technical problem mentioned above, the technical solution adopted by the present invention is that providing a kind of transparent organic phase nanometer
The preparation method of zirconia particles dispersion, the preparation method include the following steps:
Step 1) prepares the modified nano zircite particle dispersion in the non-surface of water phase；Nano zircite particle dispersion root
It is prepared according to the methods of patent CN106277049B and CN201810836953.X.
Step 2) nano zircite particle dispersion and inorganic acid, organic acid that the non-surface of the water phase of preparation is modified
Surface modifier and organic solvent are mixed to get acid stratified liquid by proper proportion；
Acid stratified liquid is placed in progress appropriate time phase transfer reaction in stirred reactor by step 3), reacted to obtain
The transparent organic phase nano zircite particle dispersion of product；
Step 4) is by transparent organic phase nano zircite particle dispersion obtained and packaging plastic organic substrate by certain ratio
Example uniformly mixing, removes solvent therein, both obtains final product high refractive index LED packaging plastic material.
Preferably, in step 2), the organic acid surface modifying agent is the mixed of the one or more selected from following substance
Close object: ethylhexyl dihydrogen phosphate, diisobutyl phosphate, hexadecanol phosphate, double hexadecyl acid ester, Dan Zhengshi bis-
Alkyl phosphate, cetostearyl alcohol phosphate, dimethyl hydrogen phosphate, bis- (fourth oxygen ethyl) phosphates, two (2- ethylhexyls)
Phosphate, normal-butyl phosphate, ethylhexyl dihydrogen phosphate, iso octyl ester of phosphoric acid, 9- octadecene-1-ol phosphate；It is highly preferred that
Select one kind or several of ethylhexyl dihydrogen phosphate, single dodecyl phosphate, normal-butyl phosphate, hexadecanol phosphate
Kind.
Preferably, in step 2), the inorganic acid is the one or more selected from following substance: hydrochloric acid, nitric acid, boron
Acid, hydrogen cyanide, hydrogen fluorine (halogen) acid, nitrous acid, high hydracid, hydracid, halous acid, hypohalogenous acids and meta-aluminic acid.
Preferably, step 3) the stirred reactor purpose is sufficiently mixed to the substance for participating in chemical reaction, is stirred
Mixing reactor includes airflow stirring reactor, jet mixing reactor, static pipeline stirred reactor, electromagnetic agitation reactor
Deng.The reaction revolving speed turns for 50-300, it is highly preferred that reaction revolving speed turns for 70-150；Most preferably, reaction revolving speed is 100
Turn.
Preferably, in step 3), the organic solvent is selected from one of following substance or a variety of: benzene, toluene, diformazan
Benzene, phenol, aniline, benzoic acid, nitrobenzene, ether, petroleum ether, tetrahydrofuran, methylene chloride, chloroform, carbon tetrachloride, just
Amylalcohol, methyl acetate, ethyl acetate, phenylacetate, methyl benzoate, butyl acetate, 2-ethyl hexyl acrylate, isoamyl acetate, benzene
Methyl formate, gaultherolin, glyceride.
Preferably, in step 4), the organic substrate is selected from one of following substance or a variety of: methyl system organosilicon
Glue, phenyl system organic silica gel, glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidol amine epoxy
Resin, linear aliphatic epoxy resin, alicyclic based epoxy resin.
To solve above-mentioned second technical problem, the present invention is adopted the following technical solutions: a kind of transparent organic phase nano oxygen
Change zirconium particle dispersion, including organic phase medium and nano zircite particle, the nano zircite particle is transparent organic phase
The nano zircite particle that the preparation method of nano zircite particle dispersion obtains；The solid content of the dispersion is 0.01-
50wt%；The nano zircite particle it is one-dimensional having a size of 6.2nm；The liquid phase medium be benzene,toluene,xylene, phenol,
Aniline, benzoic acid, nitrobenzene, ether, petroleum ether, tetrahydrofuran, methylene chloride, chloroform, carbon tetrachloride, n-amyl alcohol, second
Sour methyl esters, ethyl acetate, phenylacetate, methyl benzoate, butyl acetate, 2-ethyl hexyl acrylate, isoamyl acetate, benzoic acid first
One or more of ester, gaultherolin, glyceride.
The invention solves third technical problem be to provide a kind of transparent organic phase nano zircite particle dispersion
Application.Transparent organic phase nano zirconium oxide dispersion is since with good dispersibility, stablizing effect is good, solution dispersion
Body solid content is higher, is suitable for placing to save for a long time, can be widely used in industrial production, therefore may be used as ceramic material
Material, such as dental material, joint prosthesis, lambda sensor, ceramic insertion core, sensor material, polishing material, fuel cell, structural wood
Material etc.；Or it is used for synthetic catalyst component part, such as major catalyst, co-catalyst；The water phase of this method preparation is utilized simultaneously
Nano zircite in nano zircite dispersion has the characteristics that refractive index is high, so that the big important use of one is to keep resin
The refractive index that composite material is improved under the premise of the original high light transmittance of material, especially has Zhuo in the manufacture application aspect of optical element
Performance more.
The beneficial effects of the present invention are:
1. the nano zircite particle modified that the present invention prepares has polymolecularity, high stable in organic phase
The features such as property and high solids content.Compared to use Aqueous dispersions nano zircite particle before, the zirconium oxide that such method obtains
Nano particle diameter is smaller, is evenly distributed, one-dimensional to have widened the use scope of nano zircite having a size of 6.2nm, can
It is used to prepare high refractive index LED packaging adhesive material.
2. the dispersing agent of the transparent organic phase nano zirconium oxide liquid dispersion of gained of the invention select gas chromatography or its
Mixture makes it have bigger selectivity in preparation, has better adaptability to all kinds of organic solvents in dispersion process,
It can be preferably applied for industrial production.
3. refractive index is obviously mentioned after LED packaging plastic is added to modified zirconia nano particle obtained by the present invention
It rises.
4. preparation process of the present invention is simple, product quality is preferable, and raw material type used is easy to get extensively, simple process, just
In control condition, products obtained therefrom is pure, is easy to largely prepare, has the potentiality of large-scale industrial production.
Detailed description of the invention
Fig. 1 is the dynamic light scattering laser particle figure of modified nano zircite particle in embodiment 1；
Fig. 2 is the dynamic light scattering laser particle figure of modified nano zircite particle in embodiment 2；
Fig. 3 is the transmission electron microscope picture of modified nano zircite particle in embodiment 1；
Fig. 4 is the transmission electron microscope picture of modified nano zircite particle in embodiment 2；
Fig. 5 is the transmission electron microscope picture of modified nano zircite particle in embodiment 3；
Fig. 6 is the transmission electron microscope picture of modified nano zircite particle in embodiment 4；
Fig. 7 is the pictorial diagram of modified nano zircite dispersion in embodiment 1；
Fig. 8 is the refractive index for being added to the silica gel of modified nano zircite in embodiment 1；
Fig. 9 is the refractive index for being added to the epoxy resin of modified nano zircite in embodiment 1；
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and embodiments, but the contents of the present invention are not merely limited to
In the following examples or other similar example.
Embodiment 1
1) the modified nano zircite particle in the non-surface of water phase is prepared according to patent CN201810836953.X the method
Dispersion；
2) taking solid content is 5 milliliters of 1wt% Zirconium oxide nano grain aqueous dispersion liquid, 2 milliliters of chloroform, 2- ethyl hexyl
.5 milliliters of base phosphoesterase 30 are put into bottle, stand to its layering.
3) bottom of bottle is placed on magnetic stirring apparatus after adding magneton, carries out phase transfer reaction with 100 rpms of speed stirring,
Reaction time is 1 hour, obtains the transparent organic phase nano zircite particle dispersion of final product.Wherein nanoparticle is in Electronic Speculum
Under granular size be 3-8 nanometers.It is 6.23 nanometers that dynamic light scattering laser particle, which analyzes nano particle average grain diameter,.
4) transparent organic phase nano zircite particle dispersion is mixed with pure glue material, wherein modified nano oxidized
The weight of zirconium accounts for 50 percent (not including solvent portion) of total solid weight, and spin coating is rolled at its refractive index is surveyed after glue film
Rate curve is penetrated, obtaining its refractive index in 633 nanometers is 1.558, and keeping transmitance is 98%.
Embodiment 2
1) the modified nano zircite particle point in the non-surface of the water phase obtained according to patent CN106277049B the method
Granular media；
2) taking solid content is 5 milliliters of 1wt% Zirconium oxide nano grain aqueous dispersion liquid, 2 milliliters of chloroform, Dan Zhengshi bis-
0.5 milliliter of alkyl phosphate is put into bottle, stands to its layering.
3) bottom of bottle is placed on magnetic stirring apparatus after adding magneton, carries out phase transfer reaction with 100 rpms of speed stirring,
Reaction time is 1 hour, obtains the transparent organic phase nano zircite particle dispersion of final product.Wherein nanoparticle is in Electronic Speculum
Under granular size be 2-7 nanometers.It is 5.17 nanometers that dynamic light scattering laser particle, which analyzes nano particle average grain diameter,.
4) transparent organic phase nano zircite particle dispersion is mixed with pure glue material, wherein modified nano oxidized
The weight of zirconium accounts for 50 percent (not including solvent portion) of total solid weight, and spin coating is rolled at its refractive index is surveyed after glue film
Rate curve is penetrated, is 1.543 in 633 nanometers refractive index, transmitance 97%.
Embodiment 3
1) the modified nano zircite particle in the non-surface of water phase is prepared according to patent CN201810836953.X the method
Dispersion；
2) taking solid content is 5 milliliters of 1wt% Zirconium oxide nano grain aqueous dispersion liquid, 2 milliliters of chloroform, normal-butyl phosphorus
0.5 milliliter of acid esters is put into bottle, stands to its layering.
3) bottom of bottle is placed on magnetic stirring apparatus after adding magneton, carries out phase transfer reaction with 100 rpms of speed stirring,
Reaction time is 10 hours, obtains the transparent organic phase nano zircite particle dispersion of final product.Wherein nanoparticle is in electricity
Granular size under mirror is 4-6 nanometers.It is 5.98 nanometers that dynamic light scattering laser particle, which analyzes nano particle average grain diameter,.
4) transparent organic phase nano zircite particle dispersion is mixed with pure glue material, wherein modified nano oxidized
The weight of zirconium accounts for 40 percent (not including solvent portion) of total solid weight, and spin coating is rolled at its refractive index is surveyed after glue film
Rate curve is penetrated, is 1.542 in 633 nanometers refractive index, transmitance 97%.
Embodiment 4
1) the modified nano zircite particle in the non-surface of water phase is prepared according to patent CN106277049B the method to disperse
Body；
2) taking solid content is 5 milliliters of 1wt% Zirconium oxide nano grain aqueous dispersion liquid, 2 milliliters of toluene, normal-butyl phosphate
0.5 milliliter is put into bottle, stands to its layering.
3) bottom of bottle is placed on magnetic stirring apparatus after adding magneton, carries out phase transfer reaction with 100 rpms of speed stirring,
Reaction time is 10 hours, obtains the transparent organic phase nano zircite particle dispersion of final product.Wherein nanoparticle is in electricity
Granular size under mirror is 3-9 nanometers.It is 6.77 nanometers that dynamic light scattering laser particle, which analyzes nano particle average grain diameter,.
4) transparent organic phase nano zircite particle dispersion is mixed with pure glue material, wherein modified nano oxidized
The weight of zirconium accounts for 30 percent (not including solvent portion) of total solid weight, and spin coating is rolled at its refractive index is surveyed after glue film
Rate curve is penetrated, is 1.531 in 633 nanometers refractive index, transmitance 98%.
Embodiment 5
1) the modified nano zircite particle in the non-surface of water phase is prepared according to patent CN201810836953.X the method
Dispersion；
2) taking solid content is 5 milliliters of 1wt% Zirconium oxide nano grain aqueous dispersion liquid, 2 milliliters of tetrahydrofuran, hexadecanol
.5 milliliters of phosphoesterase 30 are put into bottle, stand to its layering.
3) bottom of bottle is placed on magnetic stirring apparatus after adding magneton, carries out phase transfer reaction with 200 rpms of speed stirring,
Reaction time is 5 hours, obtains the transparent organic phase nano zircite particle dispersion of final product.Wherein nanoparticle is in Electronic Speculum
Under granular size be 2-6 nanometers.It is 5.41 nanometers that dynamic light scattering laser particle, which analyzes nano particle average grain diameter,.
4) transparent organic phase nano zircite particle dispersion is mixed with pure glue material, wherein modified nano oxidized
The weight of zirconium accounts for 20 percent (not including solvent portion) of total solid weight, and spin coating is rolled at its refractive index is surveyed after glue film
Rate curve is penetrated, is 1.529 in 633 nanometers refractive index, transmitance 96%.
Claims (7)
1. a kind of preparation method of high refractive index LED packaging plastic material, it is characterised in that: the preparation method includes the following steps,
Step 1) prepares the modified nano zircite particle dispersion in the non-surface of water phase；
Step 2) nano zircite particle dispersion and inorganic acid, organic acid surface that the non-surface of the water phase of preparation is modified
Modifying agent and organic solvent are mixed to get acid stratified liquid by proper proportion；
Acid stratified liquid is placed in progress appropriate time phase transfer reaction in stirred reactor by step 3), reacted to obtain product
Transparent organic phase nano zircite particle dispersion；
Step 4) is equal by a certain percentage by transparent organic phase nano zircite particle dispersion obtained and packaging plastic organic substrate
Even mixing removes solvent therein, both obtains final product high refractive index LED packaging plastic material.
2. a kind of preparation method of high refractive index LED packaging plastic material according to claim 1, it is characterised in that: step
2) in, the organic acid surface modifying agent is one or more kinds of mixtures selected from following substance: 2- ethylhexyl phosphoric acid
Ester, diisobutyl phosphate, hexadecanol phosphate, double hexadecyl acid ester, single dodecyl phosphate, 16
Alcohol phosphate, dimethyl hydrogen phosphate, biphosphonate, bisphosphate, normal-butyl phosphate, ethylhexyl dihydrogen phosphate, phosphoric acid
Different monooctyl ester, 9- octadecene-1-ol phosphate.
3. a kind of preparation method of high refractive index LED packaging plastic material according to claim 1, it is characterised in that: step
2) in, the inorganic acid is the one or more selected from following substance: hydrochloric acid, nitric acid, boric acid, hydrogen cyanide, hydrofluoric acid, nitrous
Sour, high hydracid, hydracid, halous acid, hypohalogenous acids and meta-aluminic acid.
4. a kind of preparation method of high refractive index LED packaging plastic material according to claim 1, it is characterised in that: step
3) the stirred reactor purpose is sufficiently mixed to the substance for participating in chemical reaction, and stirred reactor includes airflow stirring
Reactor, jet mixing reactor, static pipeline stirred reactor, electromagnetic agitation reactor；The reaction revolving speed is 50-300
Turn.
5. a kind of preparation method of high refractive index LED packaging plastic material according to claim 1, it is characterised in that: step
3) in, the organic solvent is selected from one of following substance or a variety of: benzene,toluene,xylene, phenol, aniline, benzoic acid,
Nitrobenzene, ether, petroleum ether, tetrahydrofuran, methylene chloride, chloroform, carbon tetrachloride, n-amyl alcohol, methyl acetate, acetic acid second
Ester, phenylacetate, methyl benzoate, butyl acetate, 2-ethyl hexyl acrylate, isoamyl acetate, methyl benzoate, gaultherolin,
Glyceride.
6. a kind of preparation method of high refractive index LED packaging plastic material according to claim 1, it is characterised in that: step
4) in, the organic substrate is selected from one of following substance or a variety of: methyl system organic silica gel, phenyl system organic silica gel, contracting
Water glycerol ether type epoxy resins, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic class epoxy
Resin, alicyclic based epoxy resin.
7. a kind of transparent organic phase nano zircite particle dispersion, it is characterised in that: including organic phase medium and nano oxidized
Zirconium particle, the nano zircite particle are the nanometer that the preparation method of transparent organic phase nano zircite particle dispersion obtains
Zirconia particles；The solid content of the dispersion is 0.01-50wt%；The nano zircite particle it is one-dimensional having a size of
6.2nm；The liquid phase medium is benzene,toluene,xylene, phenol, aniline, benzoic acid, nitrobenzene, ether, petroleum ether, tetrahydro furan
It mutters, methylene chloride, chloroform, carbon tetrachloride, n-amyl alcohol, methyl acetate, ethyl acetate, phenylacetate, methyl benzoate, second
One or more of acid butyl ester, 2-ethyl hexyl acrylate, isoamyl acetate, methyl benzoate, gaultherolin, glyceride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116445030A (en) * | 2023-03-14 | 2023-07-18 | 北京化工大学 | Transparent nano-oxide aqueous dispersion, nano-composite polyurethane coating adhesive, and preparation methods and applications thereof |
| WO2023216486A1 (en) * | 2022-05-07 | 2023-11-16 | 山东国瓷功能材料股份有限公司 | Zirconia resin type dispersion liquid, uv curing glue, and preparation method therefor and application thereof |
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