CN105949845A - High-refractive-index composite coating material applied to optical thin film field - Google Patents
High-refractive-index composite coating material applied to optical thin film field Download PDFInfo
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- CN105949845A CN105949845A CN201610398273.5A CN201610398273A CN105949845A CN 105949845 A CN105949845 A CN 105949845A CN 201610398273 A CN201610398273 A CN 201610398273A CN 105949845 A CN105949845 A CN 105949845A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
Abstract
The invention discloses a high-refractive-index composite coating material applied to the optical thin film field. The composite coating material is mainly prepared from, by weight, 0.001-50% of stabilizer, 0.05-43% of a cross-linking agent, 0.5-8% of a photoinitiator, 20-30% of diluent, 0.3-5% of an inorganic modified material and the balance deionized water. According to the composite coating material, extracted ingredients in plant extract are used as the stabilizer, and the instability influence of a high-refractive-index composite coating material in the optical thin film field is eliminated.
Description
Technical field
The present invention relates to optical film technology field, particularly relate to the compound painting of a kind of high refractive index for field of optical films
Layer material.
Background technology
Indium gallium zinc oxide (IGZO) is due to its high field-effect mobility, optical clarity and machinability at low temperatures
And most promise to be the active channel material of future generation in the TFT of Flexible Displays base plate.Although there is hope in it,
But due to its sensitivity to environment, IGZO TFT stands insecure device operation.Especially, environment it is present in empty
Small-molecule substance in gas expose behind channel layer on adsorption/desorption and heliosensitivity (sub-gap photoresponse (subgap
Photoresponse)) carrier concentration in IGZO thin film can be changed.This causes turning of TFT threshold voltage (VTH)
Becoming, As time goes on it cause non-uniformity.It was demonstrated that coat with various inorganic material and organic material
IGZO channel layer is to improve device stability；But, there is the known problem relevant to state-of-the-art coating material.Such as,
The inorganic materials such as SiO deposited by plasma enhanced chemical vapor deposition method (PECVD)2And SiNxCan
The electrical characteristics of IGZOTFT are caused to be moved back due to the plasma-induced radiation damage to the behind passage area of TFT
Change.State-of-the-art organic-containing materials also will not stop surrounding (H2O、O2、O3、CO2、CO、NO、NO2)
In the chemisorbed of little molecule that contains or physical absorption, the formation of photoinduced carrier will not be stoped.
The most common ultraviolet-curing paint being applied to flat panel display backlight module field of optical films generally also exists folding
The defect that luminosity is relatively low, its index of refraction is commonly 1.5, and base material PET film 1.59 refractive power used with optical thin film refers to
Number does not mates, and causes light loss ratio during backlight module is diffused relatively big, thus affects the comprehensive effect of flat pannel display
Fruit and energy consumption.
Summary of the invention
Present invention aims to above-mentioned the deficiencies in the prior art, it is provided that a kind of high refractive power for field of optical films refers to
Number composite coating material, to overcome the defect of prior art.
The technical scheme is that and be achieved in that:
A kind of in the high refractive index composite coating material of field of optical films, mainly it is made up of the material of following weight parts: steady
Determine agent 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～30%, inorganic modified material
0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, it is characterised in that comprise following operating procedure: (a) is by the dry herb powder of Herba Crotalariae sessiliflorae
Broken, extract with 75-85% alcohol heat reflux, united extraction liquid, be concentrated into without alcohol taste, successively by petroleum ether, ethyl acetate
With water saturated n-butanol extraction, respectively obtain petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；Add
Light trigger, diluent, inorganic modified material, surplus are deionized water；Acetic acid ethyl ester extract in (b) step (a)
Use macroporous resin remove impurity, first with 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collect
75% ethanol elution, concentrating under reduced pressure obtains 75% ethanol elution thing extractum；75% ethanol elution extractum in (c) step (b)
Separate by purification on normal-phase silica gel, wash by the methylene chloride-methanol gradient that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1 successively
Take off and obtain 5 components；D in () step (c), component 4 separates further by purification on normal-phase silica gel, successively with volume ratio be 20: 1,
The methylene chloride-methanol gradient elution of 12: 1 and 5: 1 obtains 3 components；E in () step (d), component 2 uses octadecyl
The reverse phase silica gel of silane group separates, and with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collects 8-10
Column volume eluent, eluent is concentrated under reduced pressure to give pure stabilizer.
In described step (a), extract with 80% alcohol heat reflux, united extraction liquid.
Described macroporous resin is AB-8 type macroporous adsorbent resin.
Described cross-linking agent is polymerisable monomer, 2-acrylamide-2-methyl propane sulfonic sodium, Sodium styrene sulfonate, metering system
Acid dimethylaminoethyl, acrylamide, DMAA, divinylbenzene and diisocyanate, N, N-methylene
One or more in bisacrylamide.
The preparation method of the described high refractive index composite coating material in field of optical films, it is characterised in that comprise with
Lower method step: the preparation of S1: stabilizer；The preparation of S2: cross-linking agent: being dropped to by the aqueous solution containing initiator can
In the aqueous solution of polymerizable monomer compound, dripping complete, adjustment system pH is 7-8, and system is heated to 30-100 DEG C,
Continuing to system temperature, stand 10-200min, constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3:
Stabilizer aqueous solution prepared by described step S1 is added dropwise in described step S2, temperature: 5-35 DEG C, vacuum:
0.06-0.095MPa, mixing speed: 2-15r/min, mixing time: 45-130min.
The thickness of described compositions spraying is 0.01-15mm.
The thickness of described compositions spraying is 0.5-10mm.
Use magnetically controlled sputter method film forming.
Described diluent comprises the one in isopropanol, n-butyl alcohol, ethyl acetate or ethylene glycol bis glycidyl ether or many
The mixture planted.
Described light trigger comprises 1-oxybenzone, 2-hydroxy-2-methyl-1-phenyl-propan-1-ketone.
Described inorganic modified material is mainly rare earth fluoride materials, comprises such as lanthanum fluoride, neodymium fluoride, gadolinium fluoride, fluorination
One or more mixture in aluminum or cryolite.
Beneficial effects of the present invention: the extract component in plant extraction liquid is used for stabilizer by the present invention, eliminates for light
The performance of the high refractive index composite coating material learning film applications causes unstability to affect.
Heat stability increases, and nano inorganic material itself has excellent heat stability, and this is that compound system heat stability improves
One of reason.When, after material modified being doped, inorganic nano material of the present invention joins in organic facies, a side
In the face of organic segment produces sterically hindered, on the other hand and forming certain interaction between organic segment, these all limit
The motion of organic segment when material is heated, thus improve the heat stability of product.In compound system, nanoparticle energy
Conduction of heat played retardation and playing to external diffusion of thermal degradation products is adsorbed and inhibition, also making compound system
Heat stability improves.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but is not intended that any limit to the present invention
System.
Industrial chemicals illustrates: chemical reagent is purchased from traditional Chinese medicines group, and all industrial chemicals are process, directly use.
Embodiment 1
1. for a high refractive index composite coating material for field of optical films, mainly by the material group of following weight parts
Become: stabilizer 0.001-50%, cross-linking agent 0.05-430%, light trigger 0.5～8%, diluent 20～30%, inorganic change
Property material 0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, it is characterised in that comprise following operating procedure: the dry herb (10kg) of Herba Crotalariae sessiliflorae
Pulverize, extract (25L × 3 time) with 80% alcohol heat reflux, united extraction liquid, it is concentrated into without alcohol taste (3L), uses successively
Petroleum ether (3L × 3 time), ethyl acetate (3L × 3 time) and water saturated n-butyl alcohol (3L × 3 time) extraction, respectively
Obtain petroleum ether extract, acetic acid ethyl ester extract (398g) and n-butyl alcohol extract；Add light-initiated according to aforementioned proportion
Agent, diluent, inorganic modified material, surplus are deionized water；Acetic acid ethyl ester extract AB-8 in (b) step (a)
Type macroporous resin remove impurity, first with 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collects
75% ethanol elution, concentrating under reduced pressure obtains 75% ethanol elution thing extractum (163g)；C in () step (b), 75% ethanol is washed
De-extractum 200-300 mesh purification on normal-phase silica gel separates, and is 85: 1 (8 column volumes), 40: 1 (8 cylinders by volume ratio successively
Long-pending), 20: 1 (8 column volumes), 12: 1 (10 column volumes) and 1: 1 (5 column volumes) methylene chloride-methanol terraced
Degree affords 5 components；D in () step (c), component 4 (49g) 200-300 mesh purification on normal-phase silica gel separates further,
It is 20: 1 (8 column volumes), 12: 1 (10 column volumes) and the dichloromethane of 5: 1 (5 column volumes) by volume ratio successively
Alkane-methanol elution gradient obtains 3 components；E in () step (d), component 2 (25g) is bonded by octadecylsilane
Reverse phase silica gel ODS-C18 separates, and with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collects 8～10
Column volume eluent, eluent is concentrated under reduced pressure to give pure compound (I) (44mg).
Described cross-linking agent is polymerisable monomer, 2-acrylamide-2-methyl propane sulfonic sodium.
The described high refractive index composite coating material for field of optical films, it is characterised in that comprise following methods step
Rapid: S1: the preparation of stabilizer；The preparation of S2: cross-linking agent: the aqueous solution containing initiator is dropped to polymerisable monomer
In the aqueous solution of compound, dripping complete, adjusting system pH is 7, system is heated to 30 DEG C, continues to system
Temperature, stands 10min, and constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3: described step S1 system
Standby stabilizer aqueous solution is added dropwise in described step S2, temperature: 5 DEG C, vacuum: 0.06MPa, mixing speed: 2r/min,
Mixing time: 45min.
The thickness of described compositions spraying is 0.01mm.
Use magnetically controlled sputter method film forming.
Described diluent comprises the one in isopropanol, n-butyl alcohol, ethyl acetate or ethylene glycol bis glycidyl ether or many
The mixture planted.
Described light trigger comprises 1-oxybenzone, 2-hydroxy-2-methyl-1-phenyl-propan-1-ketone.
Embodiment 2
1. for a high refractive index composite coating material for field of optical films, mainly by the material group of following weight parts
Become: stabilizer 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～30%, inorganic change
Property material 0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, it is characterised in that comprise following operating procedure: (a) is by the dry herb powder of Herba Crotalariae sessiliflorae
Broken, with 85% alcohol heat reflux extract, united extraction liquid, be concentrated into without alcohol taste, successively use petroleum ether, ethyl acetate and
Water saturated n-butanol extraction, respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；According to upper
Ratio of stating adds light trigger, diluent, inorganic modified material；Acetic acid ethyl ester extract macropore in (b) step (a)
Resin remove impurity, first with 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collects 75% second
Alcohol eluen, concentrating under reduced pressure obtains 75% ethanol elution thing extractum；75% ethanol elution extractum positive in (c) step (b)
Silica gel separates, and obtains with the methylene chloride-methanol gradient elution that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1 successively
5 components；D in () step (c), component 4 separates further by purification on normal-phase silica gel, be 20: 1,12: 1 by volume ratio successively
With 5: 1 methylene chloride-methanol gradient elution obtain 3 components；E in () step (d), component 2 uses octadecylsilane
The reverse phase silica gel of bonding separates, and with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collects 10 column volumes
Eluent, eluent is concentrated under reduced pressure to give pure stabilizer.
Described cross-linking agent is polymerisable monomer, 2-acrylamide-2-methyl propane sulfonic sodium, Sodium styrene sulfonate, metering system
Acid dimethylaminoethyl, acrylamide, DMAA, divinylbenzene and diisocyanate, N, N-methylene
Bisacrylamide, its mass ratio is 1: 2: 0.1: 1: 0.5: 0.3: 1.5: 0.8.
The described high refractive index composite coating material for field of optical films, comprises following methods step: S1: steady
Determine the preparation of agent；The preparation of S2: cross-linking agent: the aqueous solution containing initiator is dropped to the water of polymerisable monomer compound
In solution, dripping complete, adjusting system pH is 8, system is heated to 100 DEG C, continues to system temperature, quiet
Putting 200min, constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3: prepared by described step S1 stablizes
Agent aqueous solution is added dropwise in described step S2, temperature: 35 DEG C, vacuum: 0.095MPa, and mixing speed: 15r/min stirs
Mix the time: 130min.
The thickness of described compositions spraying is 15mm.Described diluent comprises isopropanol, n-butyl alcohol, ethyl acetate or second
One or more mixture in glycol bisglycidyl ether.
Described light trigger comprises 1-oxybenzone, 2-hydroxy-2-methyl-1-phenyl-propan-1-ketone.
Embodiment 3
A kind of high refractive index composite coating material for field of optical films, is mainly made up of the material of following weight parts:
Stabilizer 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～30%, inorganic change
Property material 0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, comprises following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), with 80%
Alcohol heat reflux extracts, and united extraction liquid is concentrated into without alcohol taste, successively by petroleum ether, ethyl acetate and water saturated positive fourth
Alcohol extracts, and respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；Light is added according to aforementioned proportion
Initiator, diluent, inorganic modified material；Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a), first
With 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collect 75% ethanol elution, subtract
Pressure is concentrated to give 75% ethanol elution thing extractum；C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel separates, depend on
Secondary volume ratio be 85: 1,40: 1,20: 1,12: 1 and 1: 1 methylene chloride-methanol gradient elution obtain 5 components；(d)
In step (c), component 4 separates further by purification on normal-phase silica gel, successively with the dichloromethane that volume ratio is 20: 1,12: 1 and 5: 1
Alkane-methanol elution gradient obtains 3 components；E reverse phase silica gel that in () step (d), component 2 is bonded by octadecylsilane
Separate, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 9 column volume eluents, eluent
It is concentrated under reduced pressure to give pure stabilizer.
Described macroporous resin is AB-8 type macroporous adsorbent resin.
Described cross-linking agent is polymerisable monomer, divinylbenzene and diisocyanate, N,N methylene bis acrylamide,
Mass ratio 3: 4.
The preparation method of the described high refractive index composite coating material for field of optical films, it is characterised in that comprise
The preparation of following methods step: S1: stabilizer；The preparation of S2: cross-linking agent: the aqueous solution containing initiator is dropped to
In the aqueous solution of polymerisable monomer compound, dripping complete, adjusting system pH is 7, system is heated to 40 DEG C, continues
Continuous maintenance system temperature, stands 50min, and constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3: described
Stabilizer aqueous solution prepared by step S1 is added dropwise in described step S2, temperature: 20 DEG C, and vacuum: 0.075MPa stirs
Mix speed: 12r/min, mixing time: 105min.
The thickness of described compositions spraying is 0.5mm.
Use magnetically controlled sputter method film forming.
Embodiment 4
A kind of high refractive index composite coating material for field of optical films, is mainly made up of the material of following weight parts:
Stabilizer 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～30%, inorganic change
Property material 0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, comprises following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), with 78%
Alcohol heat reflux extracts, and united extraction liquid is concentrated into without alcohol taste, successively by petroleum ether, ethyl acetate and water saturated positive fourth
Alcohol extracts, and respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；Light is added according to aforementioned proportion
Initiator, diluent, inorganic modified material；Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a), first
With 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collect 75% ethanol elution, subtract
Pressure is concentrated to give 75% ethanol elution thing extractum；C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel separates, depend on
Secondary volume ratio be 85: 1,40: 1,20: 1,12: 1 and 1: 1 methylene chloride-methanol gradient elution obtain 5 components；(d)
In step (c), component 4 separates further by purification on normal-phase silica gel, successively with the dichloromethane that volume ratio is 20: 1,12: 1 and 5: 1
Alkane-methanol elution gradient obtains 3 components；E reverse phase silica gel that in () step (d), component 2 is bonded by octadecylsilane
Separate, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8-10 column volume eluent, eluting
Liquid is concentrated under reduced pressure to give pure stabilizer.
Described macroporous resin is AB-8 type macroporous adsorbent resin.
Described cross-linking agent is polymerisable monomer, divinylbenzene and diisocyanate,.
The preparation method of the described high refractive index composite coating material for field of optical films, comprises following methods step
Rapid: S1: the preparation of stabilizer；The preparation of S2: cross-linking agent: the aqueous solution containing initiator is dropped to polymerisable monomer
In the aqueous solution of compound, dripping complete, adjusting system pH is 8, system is heated to 80 DEG C, continues to system
Temperature, stands 168min, and constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3: described step S1
The stabilizer aqueous solution of preparation is added dropwise in described step S2, temperature: 35 DEG C, vacuum: 0.085MPa, mixing speed:
12r/min, mixing time: 104min.
The thickness of described compositions spraying is 10mm.
Use magnetically controlled sputter method film forming.
Embodiment 5
A kind of high refractive index composite coating material for field of optical films, is mainly made up of the material of following weight parts:
Stabilizer 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～30%, inorganic change
Property material 0.3～5%, surplus be deionized water.
The structural formula of described stabilizer is:
The preparation method of described stabilizer, comprises following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), with 82%
Alcohol heat reflux extracts, and united extraction liquid is concentrated into without alcohol taste, successively by petroleum ether, ethyl acetate and water saturated positive fourth
Alcohol extracts, and respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；Light is added according to aforementioned proportion
Initiator, diluent, inorganic modified material；Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a), first
With 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collect 75% ethanol elution, subtract
Pressure is concentrated to give 75% ethanol elution thing extractum；C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel separates, depend on
Secondary volume ratio be 85: 1,40: 1,20: 1,12: 1 and 1: 1 methylene chloride-methanol gradient elution obtain 5 components；(d)
In step (c), component 4 separates further by purification on normal-phase silica gel, successively with the dichloromethane that volume ratio is 20: 1,12: 1 and 5: 1
Alkane-methanol elution gradient obtains 3 components；E reverse phase silica gel that in () step (d), component 2 is bonded by octadecylsilane
Separate, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8-10 column volume eluent, eluting
Liquid is concentrated under reduced pressure to give pure stabilizer.
In described step (a), extract with 80% alcohol heat reflux, united extraction liquid.
Described macroporous resin is AB-8 type macroporous adsorbent resin.
Described cross-linking agent is polymerisable monomer, 2-acrylamide-2-methyl propane sulfonic sodium, Sodium styrene sulfonate, metering system
Acid dimethylaminoethyl, acrylamide, DMAA, divinylbenzene and diisocyanate, N, N-methylene
One or more in bisacrylamide.
The preparation method of the described high refractive index composite coating material for field of optical films, comprises following methods step
Rapid: S1: the preparation of stabilizer；The preparation of S2: cross-linking agent: the aqueous solution containing initiator is dropped to polymerisable monomer
In the aqueous solution of compound, dripping complete, adjusting system pH is 8, system is heated to 95 DEG C, continues to system
Temperature, stands 175min, and constant temperature stands after terminating, and is cooled to room temperature, obtains cross-linking agent solution；S3: described step S1
The stabilizer aqueous solution of preparation is added dropwise in described step S2, temperature: 10 DEG C, vacuum: 0.065MPa, mixing speed:
5r/min, mixing time: 55min.
The thickness of described compositions spraying is 6mm.
Use magnetically controlled sputter method film forming.
Test 1: adhere to test: prepared solution is rotated under 1000rpm 90s and rotary coating on ITO substrate.
Immediately sample is bakeed at 100 DEG C 60s, and is then used by Model 2000Dymax photocuring system 3000mJ/cm2
UV-A flood exposure solidify, the most under atmospheric pressure in tube furnace, sample is bakeed at 220 DEG C 1h.
Sample it is placed in the plane of rigidity and edge adhesive tape is fixed, preparing that to be penetrated into 6 of substrate surface parallel
Cutting, at a distance of 1mm.Carry out the other parallel cutting of equal number, make original cutting intersect with shape with them with 90 °
Become lattice pattern.Adhesive tape (3M 600 or TQC adhesive tape) is positioned over by the direction being parallel to one group of cutting lattice it
Upper and adhesive tape flattened to suitable position and the distance beyond at least 20mm with finger on the region of lattice.
Go through cutting zone and compare to specify in six kinds of classification with the classification chart of offer in ASTM D3359
Kind, repeat at least three times.Whole coated films of the present invention meet B classification, it was demonstrated that fabulous viscous to ITO substrate
Attached power.
Test 2: use Keithley 4200 Semiconductor Parameter Analyzer to measure electrical characteristics, the results are shown in Table 1.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, therefore all
It is without departing from technical solution of the present invention content, any is simply repaiied according to what above example made by the technical spirit of the present invention
Change, equivalent variations and modification, all still fall within the range of technical solution of the present invention.
Claims (10)
1. the high refractive index composite coating material for field of optical films, it is characterised in that: main by following heavy
The material composition of amount part: stabilizer 0.001-50%, cross-linking agent 0.05-43%, light trigger 0.5～8%, diluent 20～
30%, inorganic modified material 0.3～5%, surplus be deionized water.
2. require a kind of high refractive index composite coating material for field of optical films described in 1, its feature according to power
It is: the structural formula of described stabilizer is:
3. the high refractive index composite coating material for field of optical films described in claim 2, it is characterised in that:
The preparation method of described stabilizer, comprises following operating procedure: the dry herb of Herba Crotalariae sessiliflorae is pulverized by (a), uses 75-85%
Alcohol heat reflux extracts, and united extraction liquid is concentrated into without alcohol taste, successively by petroleum ether, ethyl acetate and water saturated positive fourth
Alcohol extracts, and respectively obtains petroleum ether extract, acetic acid ethyl ester extract and n-butyl alcohol extract；Add light trigger, dilution
Agent, inorganic modified material, surplus are deionized water；Acetic acid ethyl ester extract macroporous resin remove impurity in (b) step (a),
First with 8 column volumes of 10% ethanol elution, then with 10 column volumes of 75% ethanol elution, collect 75% ethanol elution, subtract
Pressure is concentrated to give 75% ethanol elution thing extractum；C in () step (b), 75% ethanol elution extractum purification on normal-phase silica gel separates, successively
5 components are obtained with the methylene chloride-methanol gradient elution that volume ratio is 85: 1,40: 1,20: 1,12: 1 and 1: 1；(d)
In step (c), component 4 separates further by purification on normal-phase silica gel, successively with the dichloromethane that volume ratio is 20: 1,12: 1 and 5: 1
Alkane-methanol elution gradient obtains 3 components；E reverse phase silica gel that in () step (d), component 2 is bonded by octadecylsilane
Separate, with the methanol aqueous solution isocratic elution that concentration expressed in percentage by volume is 70%, collect 8-10 column volume eluent, eluting
Liquid is concentrated under reduced pressure to give pure stabilizer.
The preparation side of the high refractive index composite coating material for field of optical films the most according to claim 3
Method, it is characterised in that: in step (a), extract with 80% alcohol heat reflux, united extraction liquid.
The preparation side of the high refractive index composite coating material for field of optical films the most according to claim 3
Method, it is characterised in that: described macroporous resin is AB-8 type macroporous adsorbent resin.
6. require the high refractive index composite coating material for field of optical films described in 1 according to power, it is characterised in that:
Described cross-linking agent is polymerisable monomer, 2-acrylamide-2-methyl propane sulfonic sodium, Sodium styrene sulfonate, methacrylic acid
Dimethylaminoethyl, acrylamide, DMAA, divinylbenzene and diisocyanate, N, N-di-2-ethylhexylphosphine oxide third
One or more in acrylamide.
High refractive index composite coating material for field of optical films the most according to claim 1, its feature exists
In, comprise the preparation of following methods step: S1: stabilizer；The preparation of S2: cross-linking agent: by the aqueous solution containing initiator
Dropping to, in the aqueous solution of polymerisable monomer compound, drip complete, adjustment system pH is 7-8, system is heated to
30-100 DEG C, continuing to system temperature, stand 10-200min, constant temperature stands after terminating, and is cooled to room temperature, obtains crosslinking
Agent solution；S3: stabilizer aqueous solution prepared by described step S1 is added dropwise in described step S2, temperature: 5-35 DEG C, very
Empty: 0.06-0.095MPa, mixing speed: 2-15r/min, mixing time: 45-130min.
High refractive index composite coating material for field of optical films the most according to claim 1, its feature exists
In: the thickness of described compositions spraying is 0.01-15mm.
High refractive index composite coating material for field of optical films the most according to claim 1, its feature exists
The one in isopropanol, n-butyl alcohol, ethyl acetate or ethylene glycol bis glycidyl ether or many is comprised in: described diluent
The mixture planted.
High refractive index composite coating material for field of optical films the most according to claim 1, its feature exists
In: described light trigger comprises 1-oxybenzone, 2-hydroxy-2-methyl-1-phenyl-propan-1-ketone.
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|---|---|---|---|---|
| CN102199376A (en) * | 2011-04-02 | 2011-09-28 | 焦虑凡 | Novel UV solidified composite coating material with high refractive index applied to optical film field and its preparation method |
| CN104641471A (en) * | 2012-07-11 | 2015-05-20 | 破立纪元有限公司 | Coating materials for oxide thin film transistors |
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| CN105544306A (en) * | 2015-11-26 | 2016-05-04 | 张建刚 | Making method of graphene oxide-containing antibiosis and mildew prevention wallpaper |
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| CN102199376A (en) * | 2011-04-02 | 2011-09-28 | 焦虑凡 | Novel UV solidified composite coating material with high refractive index applied to optical film field and its preparation method |
| CN104641471A (en) * | 2012-07-11 | 2015-05-20 | 破立纪元有限公司 | Coating materials for oxide thin film transistors |
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