CN103525342B - Preparation method for adhesive used for optical polaroid body - Google Patents
Preparation method for adhesive used for optical polaroid body Download PDFInfo
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- CN103525342B CN103525342B CN201310468434.XA CN201310468434A CN103525342B CN 103525342 B CN103525342 B CN 103525342B CN 201310468434 A CN201310468434 A CN 201310468434A CN 103525342 B CN103525342 B CN 103525342B
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Abstract
The invention discloses a preparation method for an adhesive used for an optical polaroid body. The method comprises steps of: (1) synthesizing an acrylic resin with a low molecular weight; (2) synthesizing an acrylic resin with a high molecular weight; (3) blending components; and (4) performing a bridging reaction. The adhesive has the simple preparation method and a reasonable formula. The adhesive comprises three components and the acrylic resins are the main components. The adhesive has good resistance to heat and humidity, durability, static resistance and chemical resistance, and solves a difficult binding problem between a polaroid and organic glass in a LCD panel.
Description
Technical field
The invention belongs to resin technology field, relate to a kind of preparation method of optics Polarizer body tackiness agent.
Background technology
In the epoch of 21 century, be that liquid crystal panel develops the epoch fast, as " milk of information society and bread ", liquid crystal panel is widely used in the fields such as smart mobile phone, intelligent television, panel computer in modern society.
At present, rare to optics Polarizer body tackiness agent on market, and optics Polarizer body utilizes adhesive techniques to embody a concentrated reflection of that the optics transmittance of tackiness agent, thermotolerance, humidity resistance, binding property are strong, anti-electrostatic, weather resistance, resistance to acids and bases, ageing-resistant etc. superperformance.
Summary of the invention
For solving the problems of the technologies described above, the invention provides the preparation method of a kind of physicochemical property satisfactory optics Polarizer body tackiness agent.
Technical scheme of the present invention is as follows:
The preparation method of optics Polarizer body tackiness agent, comprises the steps:
(1), low molecular weight propylene acid resin is synthesized
The component of described low molecular weight propylene acid resin comprises acrylic resin systems monomer, initiator and low boiling point solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and low boiling point solvent, heat up 82 DEG C of solvent refluxings, the mix monomer of acrylic resin systems total monomer weight 70% is dripped at 85 DEG C, reaction times is 8 ~ 9 hours, when reaction conversion ratio is greater than 98%, continues isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of low molecular weight propylene acid resin;
(2), high-molecular-weight propylene acid resin is synthesized
The component of described soft propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and high boiling solvent, heat up 120 DEG C of solvent refluxings, the mix monomer of acrylic resin systems monomer 70% is dripped at 125 DEG C, reaction times is 7 ~ 8 hours, when reaction conversion ratio is greater than 98%, continues isothermal reaction, when reaction conversion ratio reaches 99.8%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of high-molecular-weight propylene acid resin;
(3), component is blended
Get low molecular weight propylene acid resin that above-mentioned steps (1) synthesizes and the high-molecular-weight propylene acid resin that step (2) is synthesized, can be formulated after even through high-speed stirring, static 24 hours;
(4) bridge formation reaction
Use in the acrylic resin mixture in first 3 hours, specific combination polyisocyanate resin being added step (3), after stirring, froth breaking 1 hour.
On the basis of technique scheme, in described tackiness agent, the mass percent of each component is:
Low molecular weight propylene acid resin: high-molecular-weight propylene acid resin: specific combination polyisocyanate resin=40:60:1.5.
As improvement of the present invention, described in step (1), low molecular weight propylene acid resin comprises the component of following mass percent:
Methyl methacrylate monomer 40 ~ 50%, specific functional groups Acrylic Acid Monomer 5 ~ 10%, Acrylic Acid Monomer 5 ~ 10%, initiator: 0.6 ~ 2%, low boiling point solvent 40 ~ 60%.
Described in step (2), high-molecular-weight propylene acid resin comprises the component of following mass percent:
Butyl Acrylate Monomer 30 ~ 40%, methyl methacrylate monomer 5 ~ 10%, special functional acrylic monomer 10 ~ 15%, initiator 1 ~ 2%, high boiling solvent 40 ~ 60%.
As this bright further improvement, in above-mentioned steps (1), the molecular weight control of low molecular weight propylene acid resin is in Mw=10 ~ 150,000, and molecular weight distribution ratio Mw/Mn=3 ~ 5, molecular weight distribution is very narrow, and viscosity controller is at 2500 ± 500CPS.
State the molecular weight control of high-molecular-weight propylene acid resin in step (2) in Mw=100 ~ 1,500,000, molecular weight distribution ratio Mw/Mn=5 ~ 10, moderate molecular weight distribution, viscosity controller is at 7000 ± 500CPS.
Bian gets technique scheme, and the beneficial effect that the present invention has is:
Preparation method of the present invention is simple, can prepare without the need to specific installation, formula rationally, tackiness agent is three components, take acrylic resin as main ingredient, tackiness agent has good humidity resistance, weather resistance, resistance to electrostatic and chemical-resistant characteristic, the difficult problem that the Polarizer solving liquid crystal panel inside combines with synthetic glass.
Accompanying drawing explanation
Fig. 1 is the structural representation of the tackiness agent prepared of the present invention for liquid crystal panel.
Reference numeral is:
1-backlight, 2-first Polarizer, 3-transistor substrate, 4-crystal liquid substrate, 5-optical filtering substrate, 6-second Polarizer.
Embodiment
The preparation method of optics Polarizer body tackiness agent, comprises the steps:
(1), low molecular weight propylene acid resin is synthesized
The component of described low molecular weight propylene acid resin comprises acrylic resin systems monomer, initiator and low boiling point solvent;
During preparation, take methyl methacrylate monomer 800.0g, specific functional groups Acrylic Acid Monomer (hydroxyethyl methylacrylate) 85.0g, Acrylic Acid Monomer 56.5g; Initiator Diisopropyl azodicarboxylate 21.0g, solvent uses the mixed solvent 1250.0g that ethyl acetate and toluene mass ratio are 3:1;
The total monomer weight 30% i.e. mix monomer bed material of 282.5g is first added in the jacket reactor of Dropping feeder that condensation reflux unit and flow control are housed, heat up 82 DEG C of solvent refluxings, at 85 DEG C, drip the total monomer weight 70% i.e. mix monomer bed material of 659.0g, the reaction times is 8 ~ 9 hours, when reaction conversion ratio is greater than 98%, continue isothermal reaction, reaction conversion ratio reaches 99%, adds solvent cut cooling fluid, is cooled within 30 DEG C, filter, the discharging of low molecular weight propylene acid tackiness agent;
(2), high-molecular-weight propylene acid resin is synthesized
The component of described soft propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent;
During preparation, take Butyl Acrylate Monomer 750.0g, methyl methacrylate monomer 75g, specific functional groups Acrylic Acid Monomer (HPMA) 135.0g; Initiator is benzoyl peroxide tert-butyl ester 18.5g, and solvent uses the mixed solvent 1300.0g that dimethylbenzene and toluene mass ratio are 3:1;
The total monomer weight 30% i.e. mix monomer bed material of 288.0g is first added in the jacket reactor of Dropping feeder that condensation reflux unit and flow control are housed, heat up 120 DEG C of solvent refluxings, drips the monomer weight 70% i.e. mix monomer bed material of 672.0g that bed material is left at 125 DEG C; Reaction times is 7 ~ 8 hours, when reaction conversion ratio is greater than 98%, and continue isothermal reaction, reaction conversion ratio reaches 99.8%, adds solvent cut cooling fluid, is cooled within 30 DEG C, filters, the discharging of high-molecular-weight propylene acid adhesive resin;
(3), component is blended
In mass ratio for 60:40 takes low molecular weight propylene acid resin that above-mentioned steps (1) synthesizes and the high-molecular-weight propylene acid resin that step (2) is synthesized, can be formulated after even through high-speed stirring, static 24 hours;
(4) bridge formation reaction
Use in first 3 hours and incite somebody to action, in mass ratio for 1.5:100 takes the acrylic resin mixture of specific combination polyisocyanate resin and step (3) respectively, after stirring, froth breaking 1 hour.
Tackiness agent prepared by the present invention in use, coating method routinely.
As shown in Figure 1, display panels is from inside to outside followed successively by: backlight 1, first Polarizer 2, transistor substrate 3, crystal liquid substrate 4, optical filtering substrate 5 and the second Polarizer 6, when the first Polarizer 2 and transistor substrate 3 and optical filtering substrate 5 and the second Polarizer 6 bond, tackiness agent the present invention can prepared carries out use ordinary method and coats between the two.
Applicant states, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thus the new numerical range produced, also be one of record scope of the present invention, the application, for making specification sheets simple and clear, no longer enumerates these numerical ranges
.
Claims (6)
1. the preparation method of optics Polarizer body tackiness agent, is characterized in that, comprise the steps:
(1), low molecular weight propylene acid resin is synthesized
The component of described low molecular weight propylene acid resin comprises acrylic resin systems monomer, initiator and low boiling point solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and low boiling point solvent, heat up 82 DEG C of solvent refluxings, at 85 DEG C, drip the mix monomer of acrylic resin systems total monomer weight 70%, the reaction times is 8 ~ 9 hours, when reaction conversion ratio is greater than 98%, continue isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter, the discharging of low molecular weight propylene acid resin;
(2), high-molecular-weight propylene acid resin is synthesized
The component of described high-molecular-weight propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and high boiling solvent, heat up 120 DEG C of solvent refluxings, at 125 DEG C, drip the mix monomer of acrylic resin systems monomer 70%, the reaction times is 7 ~ 8 hours, when reaction conversion ratio is greater than 98%, continue isothermal reaction, when reaction conversion ratio reaches 99.8%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter, the discharging of high-molecular-weight propylene acid resin;
(3), component is blended
Get low molecular weight propylene acid resin that above-mentioned steps (1) synthesizes and the high-molecular-weight propylene acid resin that step (2) is synthesized, can be formulated after even through high-speed stirring, static 24 hours;
(4) bridge formation reaction
Use in the acrylic resin mixture in first 3 hours, specific combination polyisocyanate resin being added step (3), after stirring, froth breaking 1 hour.
2. the preparation method of optics Polarizer body tackiness agent according to claim 1, it is characterized in that, in described tackiness agent, the mass percent of each component is:
Low molecular weight propylene acid resin: high-molecular-weight propylene acid resin: specific combination polyisocyanate resin=40:60:1.5.
3. the preparation method of optics Polarizer body tackiness agent according to claim 1, it is characterized in that, described in step (1), low molecular weight propylene acid resin comprises the component of following mass percent:
Methyl methacrylate monomer 40 ~ 50%, specific functional groups Acrylic Acid Monomer 5 ~ 10%, Acrylic Acid Monomer 5 ~ 10%, initiator: 0.6 ~ 2%, low boiling point solvent 40 ~ 60%, each constituent mass per-cent sum is 100%.
4. the preparation method of optics Polarizer body tackiness agent according to claim 1, it is characterized in that, described in step (2), high-molecular-weight propylene acid resin comprises the component of following mass percent:
Butyl Acrylate Monomer 30 ~ 40%, methyl methacrylate monomer 5 ~ 10%, special functional acrylic monomer 10 ~ 15%, initiator 1 ~ 2%, high boiling solvent 40 ~ 60%, each constituent mass per-cent sum is 100%.
5. the preparation method of optics Polarizer body tackiness agent according to claim 1, it is characterized in that: in described step (1), the molecular weight control of low molecular weight propylene acid resin is in Mw=10 ~ 150,000, molecular weight distribution ratio Mw/Mn=3 ~ 5, viscosity controller is at 2500 ± 500CPS.
6. the preparation method of optics Polarizer body tackiness agent according to claim 1, it is characterized in that: in described step (2), the molecular weight control of high-molecular-weight propylene acid resin is in Mw=100 ~ 1,500,000, molecular weight distribution ratio Mw/Mn=5 ~ 10, viscosity controller is at 7000 ± 500CPS.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310468434.XA CN103525342B (en) | 2013-10-10 | 2013-10-10 | Preparation method for adhesive used for optical polaroid body |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310468434.XA CN103525342B (en) | 2013-10-10 | 2013-10-10 | Preparation method for adhesive used for optical polaroid body |
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| CN103525342A CN103525342A (en) | 2014-01-22 |
| CN103525342B true CN103525342B (en) | 2015-07-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057505B (en) * | 2019-12-25 | 2021-12-24 | 常州华日升反光材料有限公司 | Special pressure-sensitive adhesive for cement surface prism film and preparation method thereof |
| CN111117532A (en) * | 2020-01-06 | 2020-05-08 | 镝普材料(深圳)有限公司 | Optical-grade acrylate adhesive glue for 3D hot bending hardening film interlayer |
| CN113025213A (en) * | 2021-03-18 | 2021-06-25 | 东莞市清鸿新材料科技有限公司 | High-durability intelligent wearable sealant and preparation method thereof |
| CN115710477A (en) * | 2022-08-16 | 2023-02-24 | 昆山石梅新材料科技有限公司 | OCA optical cement for flexible folding screen and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445709A (en) * | 2007-11-28 | 2009-06-03 | 第一毛织株式会社 | Adhesive compostion for die-bonding in semiconductor assembly and adhesive film prepared therefrom |
| CN103030914A (en) * | 2012-12-31 | 2013-04-10 | 宁波大榭开发区综研化学有限公司 | Acrylic ester composition, preparation method of acrylic ester composition, and adhesive tape applying composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008101183A (en) * | 2006-09-20 | 2008-05-01 | Hitachi Chem Co Ltd | Pressure-sensitive adhesive sheet, semiconductor device produced by using the same and method for producing the semiconductor device |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445709A (en) * | 2007-11-28 | 2009-06-03 | 第一毛织株式会社 | Adhesive compostion for die-bonding in semiconductor assembly and adhesive film prepared therefrom |
| CN103030914A (en) * | 2012-12-31 | 2013-04-10 | 宁波大榭开发区综研化学有限公司 | Acrylic ester composition, preparation method of acrylic ester composition, and adhesive tape applying composition |
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