CN117801337A - PDLC spacer material with high transmittance and preparation method thereof - Google Patents
PDLC spacer material with high transmittance and preparation method thereof Download PDFInfo
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- CN117801337A CN117801337A CN202311843082.1A CN202311843082A CN117801337A CN 117801337 A CN117801337 A CN 117801337A CN 202311843082 A CN202311843082 A CN 202311843082A CN 117801337 A CN117801337 A CN 117801337A
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- 125000006850 spacer group Chemical group 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 50
- 239000004983 Polymer Dispersed Liquid Crystal Substances 0.000 title claims abstract description 45
- 238000002834 transmittance Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000004005 microsphere Substances 0.000 claims abstract description 29
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 18
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000007720 emulsion polymerization reaction Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 230000008961 swelling Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 28
- 238000009826 distribution Methods 0.000 description 9
- 239000003292 glue Substances 0.000 description 8
- 239000004973 liquid crystal related substance Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 239000005264 High molar mass liquid crystal Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 229920002125 Sokalan® Polymers 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000004584 polyacrylic acid Substances 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000005340 laminated glass Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 239000000113 methacrylic resin Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
-
- 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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
-
- 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
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1334—Constructional arrangements; Manufacturing methods based on polymer dispersed liquid crystals, e.g. microencapsulated liquid crystals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nonlinear Science (AREA)
- Mathematical Physics (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Liquid Crystal (AREA)
Abstract
The invention discloses a PDLC spacer material with high light transmittance and a preparation method thereof. The PDLC spacer material is resin microsphere, the grain diameter is 6-20 μm, CV value is less than or equal to 4%, light transmittance is more than or equal to 85%, recovery rate is 70% -85% under 10mN pressure, and thermal decomposition temperature is more than or equal to 300 ℃. The PDLC spacer material with high transmittance has excellent miscibility, excellent hardness and recovery rate, excellent monodispersity, light transmittance and high temperature resistance, and can be applied to different scenes.
Description
Technical Field
The invention belongs to the technical field of light-adjusting film spacing materials, and particularly relates to a PDLC spacing material with high light transmittance and a preparation method thereof.
Background
The electronic curtain PDLC (Polymer Dispersed Liquid Crystal), also called intelligent dimming film, is a polymer dispersed liquid crystal, and is prepared by mixing polymer liquid crystal with prepolymer, attaching the mixture onto transparent conductive substrate, and using dielectric anisotropy of polymer liquid crystal to make the polymer liquid crystal have excellent photoelectric property after UV photopolymerization. When no external voltage electric field is applied, a regular electric field cannot be formed in the dimming film, rod-shaped polymer liquid crystal molecules are arranged in a disordered way, incident light is strongly scattered, and the dimming film is in a white opaque state; after the electric field is applied, the polymer liquid crystal molecules are arranged perpendicular to the surface and are consistent with the direction of the electric field, so that incident light is effectively transmitted out, and the dimming film is in a transparent state.
The mixture of the high molecular liquid crystal prepolymer refers to a mixture of a photo-curing material (glue monomer), a photoinitiator, a liquid crystal material and a spacer material.
Unlike traditional display screen, PDLC intelligent dimming film does not need to coat PI orientation layer and paste polaroid, and preparation process is simple, can prepare large tracts of land flexible display screen, has simultaneously the characteristics such as protection privacy, energy-concerving and environment-protective, safety concurrently, consequently is widely used in fields such as hotel isolation, projection display, car door window, electronic book, automatically controlled glass, artwork show. However, in practical use, the conventional PDLC dimming film has the defects of poor heat resistance, low transmittance, insufficient haze and the like, and a product with better high temperature resistance and better haze needs to be developed by a smart dimming film manufacturer.
Currently, each manufacturer mainly depends on preparing high-temperature liquid crystal and adjusting a PDLC material composition, namely liquid crystal molecules, glue monomer components or formulas. In fact, along with localization of liquid crystal glue and continuous adjustment and upgrading of the formula, the existing spacer particles are generally suitable for the LCD industry, and have defects of agglomeration, flocculation, separation of light-adjusting film edge spheres and glue and the like in actual use and coating. It is therefore an urgent need to prepare PDLC spacer materials that have better dispersibility in glues and meet the requirements of excellent hardness and recovery.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides a PDLC spacer material with high light transmittance and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a PDLC spacer material with high transmittance is resin microsphere, the particle size is 6-20 μm, CV value is less than or equal to 4%, light transmittance is more than or equal to 85%, recovery rate is 70% -85% under 10mN pressure, and thermal decomposition temperature is more than or equal to 300 ℃.
Further, the surface of the resin microsphere is modified with an acrylic acid functional group.
A preparation method of the PDLC spacer material with high transmittance,
(1) One or more than two of acrylic acid monomer, styrene monomer and divinylbenzene monomer are used as monomers, and emulsion polymerization is adopted to prepare seed microspheres;
(2) Preparing a polymer mother sphere by continuously adopting a seed polymerization method between the seed microsphere and one or more than two monomers of an acrylic monomer, a styrene monomer and a divinylbenzene monomer;
(3) The surface of the polymer mother sphere is modified with acrylic acid functional groups to obtain the PDLC spacer material with high transmittance.
Further, the initiator of emulsion polymerization in the step (1) adopts azodiisobutyronitrile and benzoyl peroxide, and the addition amount is 0.5-5% of the total mass of the monomers.
Further, the reaction temperature of the emulsion polymerization in the step (1) is 50-80 ℃ and the reaction time is 8-24 h.
Further, the addition amount of the swelling agent in the seed polymerization method in the step (2) is 1-10 times of the mass of the seed microsphere, and the addition amount of the monomer is 30-500 times of the mass of the seed microsphere.
Further, the addition amount of the dispersing agent in the seed polymerization method in the step (2) is 1-5% of the mass of the seed microsphere.
Further, the surface of the polymer mother sphere in the step (3) is modified by specifically adopting the following steps: dispersing polymer mother balls in a sodium dodecyl benzene sulfonate aqueous solution by ultrasonic, stirring and reacting for 6-12 h, adding an ethanol solution of methyl methacrylate, stirring and reacting for 5-10 h at room temperature, adding potassium persulfate, heating to 50-80 ℃ and reacting for 8-12 h, centrifuging and cleaning the reaction solution with absolute ethanol or deionized water for 3-5 times after the reaction is finished, and vacuum drying for 8-12 h to obtain the PDLC spacer material with high transmittance.
The high-transmittance PDLC spacer material disclosed by the application is different from the conventional LCD spacer particles in that the structural unit of the spacer material contains an acrylic monomer so as to achieve the aim of achieving excellent miscibility with polar groups in glue by forming intermolecular forces in consideration of the fact that the glue formulation contains at least one of methacrylic resin oligomer, polyurethane acrylic resin oligomer and dimethyl acrylic resin.
Unlike common polyacrylic acid branch microspheres, the spacer material has excellent hardness and recovery rate, the recovery rate is generally 70-85%, and the spacer material is operated by common workers, so that the defects of up-down short circuit, screen burning and the like caused by poor sphere support in the preparation of laminated glass are effectively avoided.
Unlike common polyacrylic acid microsphere, the spacer material has the particle size of 6-20 microns, excellent monodispersity and CV value less than or equal to 4%, and the uniform particle size is favorable for keeping the thickness of the liquid crystal box and realizing good waviness of the dimming film.
The PDLC spacer material is different from a conventional LCD spacer material, has more excellent transmittance, and the actual transmittance is more than or equal to 85%, so that the transparency of the dimming film after being electrified is higher, and the experience feeling of scenes such as electric control glass, artwork display, projection display and the like is better.
The PDLC spacer material is subjected to surface modification, modified particles are different from conventional spacers, and the PDLC spacer material has better haze and ensures the experience of privacy protection, automobile windows, electronic books and other scenes.
The PDLC spacer material has excellent high temperature resistance, and the thermal decomposition temperature is more than or equal to 300 ℃.
Drawings
FIG. 1 shows particle size and particle size distribution of seed microspheres of examples.
FIG. 2 is a surface topography of example seed microspheres.
FIG. 3 shows the particle size and particle size distribution of the example pellets.
Fig. 4 is a graph showing hardness and recovery of the PDLC spacer material of the example.
Fig. 5 shows particle size and particle size distribution of the PDLC spacer of example.
Fig. 6 is a surface topography of an example PDLC spacer material.
Fig. 7 is a DSC/TG thermal performance analysis of the example PDLC spacer.
Fig. 8 is a comparison of performance index of dimming films of the PDLC spacer material of example.
Detailed Description
In order to enable those skilled in the art to better understand the present application, the following description will make clear and complete descriptions of the technical solutions in the embodiments of the present application with reference to the accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are merely some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
It should be noted that the terms "comprises" and "comprising," and any variations thereof, in the description and claims of the present application and in the foregoing figures, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or apparatus.
The PDLC spacer material is prepared by a seed polymerization method, and the preparation process comprises three steps: preparing seed microspheres; preparing a mother ball; and (5) surface modification.
Unlike common polyacrylic acid microsphere, the spacer material has excellent hardness and recovery rate, the recovery rate is generally 70-85%, and the spacer material is operated by common workers, so that the defects of up-down short circuit, screen burning and the like caused by poor sphere support during the preparation of laminated glass are effectively avoided.
Unlike common polyacrylic acid microsphere, the spacer material has particle size of 6-20 microns, excellent monodispersity, CV value less than or equal to 4%, homogeneous particle size favorable to maintaining the thickness of the liquid crystal cell and excellent ripple degree of the light regulating film.
The PDLC spacer material is different from the conventional LCD spacer material, has more excellent transmittance, and the actual transmittance is more than or equal to 85%, so that the transparency of the dimming film after being electrified is higher, and the experience of scenes such as electric control glass, artwork display, projection display and the like is better.
The PDLC spacer material is subjected to surface modification, modified particles are different from conventional spacers, and the PDLC spacer material has better haze, so that the experience of privacy protection, automobile windows, electronic books and other scenes is ensured.
The PDLC spacer material has excellent high temperature resistance, and the thermal decomposition temperature is more than or equal to 300 ℃.
The seed microsphere is prepared by emulsion polymerization, and the reaction monomer can be one or more copolymers of different types of acrylic acid monomers, styrene monomers and divinylbenzene monomers.
The seed microsphere can adopt conventional initiators such as azodiisobutyronitrile, benzoyl peroxide and the like, and the addition amount of the initiator is 0.5-5%.
The mother balls are prepared by a seed polymerization method, and the polymer monomers are one or more of acrylic monomers, styrene monomers and divinylbenzene monomers of different types.
The addition of the mother ball swelling agent is generally 1-10 times of the mass of the seeds, and the addition of the monomer is 30-500 times of the mass of the seeds. The addition amount of the mother ball dispersing agent is generally 1-5%.
The surface modification in the preparation method generally refers to a block reaction, the reaction monomers are acrylic acid monomers of different types, and the miscibility with the liquid crystal glue is realized by modifying more acrylic acid functional groups on the surface.
Examples
100g of absolute ethanol, 10g of PVP and 1.5L of sodium dodecyl benzene sulfonate aqueous solution were taken and added to a 2.5L four-necked flask equipped with a mechanical stirring and condensing tube, the stirring speed being 100rpm/min and the temperature being 50 ℃. 200g of styrene and 10g of azobisisobutyronitrile were added to another beaker, after being sufficiently dissolved, the mixture was added to the flask, stirred at 100rpm/min at 50℃for 30 minutes, then heated to 70℃and reacted for 20 hours, followed by cooling to obtain an emulsion. And (3) centrifugally cleaning the emulsion by absolute ethyl alcohol/deionized water for 3-5 times, and then drying in vacuum for 10 hours to obtain the polystyrene seed microspheres.
Mixing 10g of the seed microsphere, 25 g of dimethyl phthalate and 1L of sodium dodecyl benzene sulfonate aqueous solution, emulsifying for 3-10 min by a cell homogenizer after ultrasonic treatment, and transferring into a three-mouth bottle to swell for 12 hours at 30 ℃; then adding an aqueous emulsion containing 100g of methyl methacrylate/divinylbenzene monomer and 1g of benzoyl peroxide, and continuing swelling at 30 ℃; after swelling for 6 hours, adding 5g of dispersing agent polyvinylpyrrolidone, heating to 70 ℃, stirring and reacting for 12 hours, centrifugally cleaning with absolute ethyl alcohol/deionized water for 3-5 times, and vacuum drying for 10 hours to obtain the polymer mother ball.
Taking 100g of the polymer mother ball, adding 1L of sodium dodecyl benzene sulfonate aqueous solution into a three-mouth bottle provided with a mechanical stirring and condensing tube after ultrasonic dispersion, and stirring and reacting for 10 hours at room temperature; 10g of methyl methacrylate/50 g of ethanol was added to the above mixture, followed by stirring at room temperature for 10 hours, then 1g of potassium persulfate was added thereto, and the temperature was raised to 70℃for 10 hours. After the reaction is finished, the reaction solution is centrifugally washed for 3 to 5 times by absolute ethyl alcohol/deionized water, and then is dried in vacuum for 10 hours, so that the PDLC spacer material with high transmittance is obtained.
FIG. 1 shows the particle size and particle size distribution of the seed microspheres prepared, the particle size and particle size distribution being 2.10 μm,2.52%;
FIG. 2 is a surface morphology of seed microspheres, from which it can be seen that the seed microspheres have smooth surfaces and excellent homogeneity;
FIG. 3 is a particle size and particle size distribution of the cue ball, the particle size and particle size distribution being 20.00 μm,2.46%;
FIG. 4 is a plot of hardness and recovery of PDLC spacer material, recovery 83% at 10mN pressure;
FIG. 5 is a particle size and particle size distribution of PDLC spacer material, particle size and particle size distribution of 20.03 μm,2.48%;
FIG. 6 is a surface topography of a PDLC spacer material with burrs on the surface showing successful cladding, successful blocking of the monomer;
FIG. 7 is a DSC/TG thermal performance analysis of the example PDLC spacer material, from which it can be seen that the thermal decomposition temperature is greater than or equal to 300 ℃;
fig. 8 shows that the dimming film performance index of the PDLC spacer according to the embodiment is better than that of the other agents, and the particles have better light shielding degree, light transmittance and haze, so that more excellent experience feeling of projection display, hotel isolation, automobile sunroof and the like can be realized.
The above description of the present invention is further illustrated in detail and should not be taken as limiting the practice of the present invention. It is within the scope of the present invention for those skilled in the art to make simple deductions or substitutions without departing from the concept of the present invention.
Claims (8)
1. A high transmittance PDLC spacer material, characterized by: the PDLC spacer material is resin microsphere, the grain diameter is 6-20 μm, CV value is less than or equal to 4%, light transmittance is more than or equal to 85%, recovery rate is 70% -85% under 10mN pressure, and thermal decomposition temperature is more than or equal to 300 ℃.
2. The high transmittance PDLC spacer material of claim 1, wherein: the surface of the resin microsphere is modified with an acrylic acid functional group.
3. A method for preparing the high transmittance PDLC spacer material of claim 1 or 2, wherein:
(1) One or more than two of acrylic acid monomer, styrene monomer and divinylbenzene monomer are used as monomers, and emulsion polymerization is adopted to prepare seed microspheres;
(2) Preparing a polymer mother sphere by continuously adopting a seed polymerization method between the seed microsphere and one or more than two monomers of an acrylic monomer, a styrene monomer and a divinylbenzene monomer;
(3) The surface of the polymer mother sphere is modified with acrylic acid functional groups to obtain the PDLC spacer material with high transmittance.
4. A method of preparation according to claim 3, characterized in that: the initiator of emulsion polymerization in the step (1) adopts azodiisobutyronitrile and benzoyl peroxide, and the addition amount is 0.5-5% of the total mass of the monomers.
5. A method of preparation according to claim 3, characterized in that: the reaction temperature of the emulsion polymerization in the step (1) is 50-80 ℃ and the reaction time is 8-24 h.
6. A method of preparation according to claim 3, characterized in that: the addition of the swelling agent in the seed polymerization method in the step (2) is 1-10 times of the mass of the seed microsphere, and the addition of the monomer is 30-500 times of the mass of the seed microsphere.
7. A method of preparation according to claim 3, characterized in that: the addition amount of the dispersing agent in the seed polymerization method in the step (2) is 1-5% of the mass of the seed microsphere.
8. A method of preparation according to claim 3, characterized in that: the surface of the polymer mother sphere in the step (3) is modified by the following steps: dispersing polymer mother balls in a sodium dodecyl benzene sulfonate aqueous solution by ultrasonic, stirring and reacting for 6-12 h, adding an ethanol solution of methyl methacrylate, stirring and reacting for 5-10 h at room temperature, adding potassium persulfate, heating to 50-80 ℃ and reacting for 8-12 h, centrifuging and cleaning the reaction solution with absolute ethanol or deionized water for 3-5 times after the reaction is finished, and vacuum drying for 8-12 h to obtain the PDLC spacer material with high transmittance.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311843082.1A CN117801337A (en) | 2023-12-29 | 2023-12-29 | PDLC spacer material with high transmittance and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311843082.1A CN117801337A (en) | 2023-12-29 | 2023-12-29 | PDLC spacer material with high transmittance and preparation method thereof |
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| CN117801337A true CN117801337A (en) | 2024-04-02 |
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| CN202311843082.1A Pending CN117801337A (en) | 2023-12-29 | 2023-12-29 | PDLC spacer material with high transmittance and preparation method thereof |
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| Country | Link |
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| CN (1) | CN117801337A (en) |
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