CN101942284A - Adhesive and manufacturing method thereof - Google Patents
Adhesive and manufacturing method thereof Download PDFInfo
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- CN101942284A CN101942284A CN2010102812388A CN201010281238A CN101942284A CN 101942284 A CN101942284 A CN 101942284A CN 2010102812388 A CN2010102812388 A CN 2010102812388A CN 201010281238 A CN201010281238 A CN 201010281238A CN 101942284 A CN101942284 A CN 101942284A
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- polymkeric substance
- sticking agent
- glass tansition
- tansition temperature
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Abstract
The invention provides an adhesive and a manufacturing method thereof. The adhesive is formed by cross-linking a first polymer and a second polymer, wherein the glass transition temperature (Tg) of the first polymer is higher than the glass transition temperature of the second polymer, and the first polymer and the second polymer are compatible. Because the adhesive of the invention is formed by cross-linking the first polymer with higher glass transition temperature and the second polymer with lower glass transition temperature, the adhesive has larger storage modulus change along with the temperature change and has good adhesion force and retention force.
Description
Technical field
The present invention is about a kind of sticking agent and manufacture method thereof; Particularly, the present invention is about a kind of sticking agent and manufacture method thereof that is used for blooming piece.
Background technology
In indicating meters such as liquid crystal or electricity slurry, storehouse has the blooming of the different functions of tool usually, for example, and optics Polarizer (TAC), phasic difference plate, EMI (hertzian wave) shielding film, antiglare film, antireflection film etc.For preventing in display production or the performance checking stage is caused these optical film surface damages, generally can paste protective membrane on the surface, when making function composite membrane or combination of liquid crystals panel, peel off removal then.Therefore, as surface protection film, the property pasted that must possess the transparency that might as well impenetrability can check and not allow to wrap into bubble etc., and with quilt body do not have the adhesion increase or have cull to residue in after pasting by situations such as surfaces.
The sticking agent that above-mentioned protective membrane is used is because be to be prerequisite being stripped from, so the adhesion of the general sticking agent of its adhesion is low.Wherein, the high glass transfer temperature of high glass transfer temperature (Tg) polymkeric substance is too high, causes almost there is not tackyness when low temperature.As for low glass transfer temperature polymkeric substance,, the insufficient problem of confining force is arranged then because of modulus is lower.
Summary of the invention
Main purpose of the present invention is providing a kind of sticking agent and manufacture method thereof, and this sticking agent has higher modulus of elasticity to be changed.
Sticking agent of the present invention is formed by first polymkeric substance and second crosslinked polymer.Wherein, the glass tansition temperature (Tg) of first polymkeric substance is higher than the glass tansition temperature of second polymkeric substance.First polymkeric substance and second polymkeric substance can dissolve each other.
Further, the glass tansition temperature of first polymkeric substance is between 0 to 150 ℃.
Further, the glass tansition temperature of first polymkeric substance is between 10 ℃ to 100 ℃.
Further, the glass tansition temperature of first polymkeric substance is between 30 ℃ to 85 ℃.
Further, the glass tansition temperature of second polymkeric substance between-100 ℃ to 0 between.
Further, the glass tansition temperature of second polymkeric substance is between-80 ℃ to-10 ℃.
Further, the glass tansition temperature of second polymkeric substance is between-60 ℃ to-20 ℃.
Further, first polymkeric substance and second polymkeric substance are the methacrylic based polyalcohol.
Further, the weight percent of this first polymkeric substance is between 0.5% to 50%, and the weight percent of this second polymkeric substance is between 99.5% to 50%.
Further, the weight percent of first polymkeric substance is between 1% to 20%, and the weight percent of second polymkeric substance is between 99% to 80%.
Further, first polymkeric substance is as the linking agent and second crosslinked polymer with isocyanic ester.
The present invention also provides a kind of sticking agent manufacture method, and the sticking agent manufacture method comprises: first polymkeric substance is provided; Second polymkeric substance is provided, and wherein the glass tansition temperature of first polymkeric substance is higher than the glass tansition temperature of second polymkeric substance, and first polymkeric substance and second polymkeric substance can dissolve each other; And make first polymkeric substance and second polymkeric substance carry out crosslinking reaction.
Further, the glass tansition temperature of first polymkeric substance is between 0 to 150 ℃.
Further, the glass tansition temperature of first polymkeric substance is between 10 ℃ to 100 ℃.
Further, the glass tansition temperature of first polymkeric substance is between 30 ℃ to 85 ℃.
Further, the glass tansition temperature of second polymkeric substance between-100 ℃ to 0 between.
Further, the glass tansition temperature of second polymkeric substance is between-80 ℃ to-10 ℃.
Further, the glass tansition temperature of second polymkeric substance is between-60 ℃ to-20 ℃.
Further, first polymkeric substance and second polymkeric substance are the methacrylic based polyalcohol.
Further, the weight percent of this first polymkeric substance is between 0.5% to 50%, and the weight percent of this second polymkeric substance is between 99.5% to 50%.
Further, the weight percent of first polymkeric substance is between 1% to 20%, and the weight percent of second polymkeric substance is between 99% to 80%.
Further, first polymkeric substance is as the linking agent and second crosslinked polymer with isocyanic ester.
Compared with prior art, sticking agent of the present invention is formed by first polymkeric substance with higher glass tansition temperature and second crosslinked polymer with low glass tansition temperature, can have higher storage modulus with temperature and change, and have good adhesion and confining force.
Can be about the advantages and spirit of the present invention by following detailed Description Of The Invention and appended graphic being further understood.
Description of drawings
Fig. 1 is an embodiment of the invention schema.
Embodiment
Sticking agent of the present invention is formed by first polymkeric substance and second crosslinked polymer.Wherein, the glass tansition temperature (Tg) of first polymkeric substance is higher than the glass tansition temperature of second polymkeric substance.First polymkeric substance and second polymkeric substance can dissolve each other.
First polymkeric substance is preferably the methacrylic based polyalcohol.Particularly, can use that to have the alkyl carbon number be 1 to 12, based on the monomer of methacrylic, for example methyl methacrylate, the methacrylic acid ethyl ester, the methacrylic acid n-butyl, methacrylic acid sec-butyl ester, the methacrylic acid tertiary butyl ester, the methacrylic acid isobutyl, the methacrylic acid polyhexamethylene, methacrylic acid 2-second polyhexamethylene, methacrylic acid n-octyl ester, the methacrylic acid isooctyl acrylate, methacrylic acid n-nonyl ester, the different nonyl ester of methacrylic acid, the positive decyl ester of methacrylic acid, methacrylic acid isodecyl ester, positive ten dicarbonyl esters of methacrylic acid or similar person.Wherein, the weight percent of first polymkeric substance is preferable between 0.5% to 50%, and is better between 1% to 20%, and molecular-weight average is preferable between 100,000 to 5,000, between 000, is more preferred from 500,000 to 2,000, between 000.The weight percent of second polymkeric substance is preferable between 99.5% to 50%, and is better between 99% to 80%, and molecular-weight average is preferable between 2,000 to 800,000, is more preferred between 200,000 to 400,000.
First polymkeric substance is preferable but do not limit with isocyanic ester as the linking agent and second crosslinked polymer.The method of crosslinking polymerization is selected solution polymerization, emulsion polymerization, suspension polymerization or overall polymerization etc. for use.Wherein, the glass tansition temperature of first polymkeric substance is between 0 to 150 ℃, and is preferable between 10 ℃ to 100 ℃, better between 30 ℃ to 85 ℃.The glass tansition temperature of second polymkeric substance between-100 ℃ to 0 between, preferable between-80 ℃ to-10 ℃, better between-60 ℃ to-20 ℃.
As shown in Figure 1, sticking agent manufacture method of the present invention comprises: step 1010 provides aforementioned first polymkeric substance; Step 1030 provides aforementioned second polymkeric substance, and wherein the glass tansition temperature of first polymkeric substance is higher than the glass tansition temperature of second polymkeric substance, and first polymkeric substance and second polymkeric substance can dissolve each other; And step 1050, make first polymkeric substance and second polymkeric substance carry out crosslinking reaction.
Below by different embodiment the effect of sticking agent of the present invention is described.Wherein, embodiment A to the raw material that D reaches embodiment 1 to 5 as a comparative example uses.
[embodiment A]
The hydroxyethyl methylacrylate (HEMA) of the positive butyl ester of 98.5 parts by weight of acrylic (n-BA), 1.0 parts by weight of acrylic (AA), 0.5 weight part, the vinyl acetic monomer of 150 weight parts and the Diisopropyl azodicarboxylate (AIBN) of 0.06 weight part are put into the four-hole reaction vessel, behind the air in the nitrogen replacement reaction vessel, in nitrogen environment, stir, reaction soln is warming up to 60 ℃, reacted 8 hours.After reaction finishes, be diluted to the acrylate copolymer solution of solid content 20% with vinyl acetic monomer, it is 1,500,000 that the copolymer solution of gained acrylate is recorded weight average molecular weight (Mw) by GPC device (600 Controller are made by Waters company).Wherein, measuring condition is as follows: sample concentration is 0.2Wt% tetrahydrofuran (THF) (THF) solution, sample injection volume 200 μ L, towards extract is tetrahydrofuran solution, the sample tubing string is Shodex KF803 (tubing string 1), Shodex KF804 (tubing string 2), Shodex KF805 (tubing string 3) and Shodex KF806 (tubing string 4), detector is RI-detector (RI), and molecular weight gets according to polystyrene.
[Embodiment B]
Methacrylic acid the 3rd butene esters (t-BMA), the positive butyl ester of 20 parts by weight of acrylic (n-BA), 10 parts by weight of acrylic (AA), the hydroxyethyl methylacrylate (HEMA) of 10 weight parts, the acetone of 150 weight parts and the Diisopropyl azodicarboxylate (AIBN) of 0.5 weight part of 60 weight parts are put into the four-hole reaction vessel, behind the air in the nitrogen replacement reaction vessel, in nitrogen environment, stir, reaction soln is warming up to backflow (reflux temperature series solvent boiling temperature, for example the acetone boiling temperature is 57 ℃), reacted 12 hours.After reaction finishes, be diluted to the acrylate copolymer solution of solid content 20% with vinyl acetic monomer, it is 400,000 that the copolymer solution of gained acrylate is recorded weight average molecular weight (Mw) by the GPC device.The glass tansition temperature that is recorded by DSC device (DSC Q100, TA Instruments makes) is 61.3 ℃.
[Embodiment C]
Methacrylic acid the 3rd butene esters (t-BMA), the positive butyl ester of 35 parts by weight of acrylic (n-BA), 10 parts by weight of acrylic (AA), the hydroxyethyl methylacrylate (HEMA) of 10 weight parts, the acetone of 150 weight parts and the Diisopropyl azodicarboxylate (AIBN) of 0.5 weight part of 45 weight parts are put into the four-hole reaction vessel, behind the air in the nitrogen replacement reaction vessel, in nitrogen environment, stir, reaction soln is warming up to backflow, reacted 12 hours.After reaction finishes, be diluted to the acrylate copolymer solution of solid content 20% with vinyl acetic monomer, it is 400,000 that the copolymer solution of gained acrylate is recorded weight average molecular weight (Mw) by the GPC device.The glass tansition temperature that is recorded by the DSC device is 30.7 ℃.
[embodiment D]
Methacrylic acid the 3rd butene esters (t-BMA), the positive butyl ester of 12 parts by weight of acrylic (n-BA), 10 parts by weight of acrylic (AA), the hydroxyethyl methylacrylate (HEMA) of 10 weight parts, the acetone of 150 weight parts and the Diisopropyl azodicarboxylate (AIBN) of 0.5 weight part of 68 weight parts are put into the four-hole reaction vessel, behind the air in the nitrogen replacement reaction vessel, in nitrogen environment, stir, reaction soln is warming up to backflow, reacted 12 hours.After reaction finishes, be diluted to the acrylate copolymer solution of solid content 20% with vinyl acetic monomer, it is 400,000 that the copolymer solution of gained acrylate is recorded weight average molecular weight (Mw) by the GPC device.The glass tansition temperature that is recorded by the DSC device is 80.3 ℃.
Embodiment A to the polymer weight of D is formed whole shown in following table one.To D, embodiment A generates second polymkeric substance in embodiment A, and Embodiment B, C, D generate first polymkeric substance.
Table one
[comparative example]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds the isocyanate-based linking agent (peace peak corporate system AD-75) that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
[embodiment 1]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds product 10 weight parts of Embodiment B gained, add the isocyanate-based linking agent that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
[embodiment 2]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds product 5 weight parts of Embodiment B gained, add the isocyanate-based linking agent that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
[embodiment 3]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds product 1.0 weight parts of Embodiment B gained, add the isocyanate-based linking agent that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
[embodiment 4]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds product 10 weight parts of Embodiment C gained, add the isocyanate-based linking agent that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
[embodiment 5]
The acrylate copolymer solution of embodiment A gained solid content 20% is used as 100 weight parts, adds product 10 weight parts of embodiment D gained, add the isocyanate-based linking agent that is equivalent to 0.15 weight part, can get sticking agent behind the thorough mixing.The gained sticking agent is coated through on the PET film of shape processing,, formed adhesive layer behind the solvent flashing,, make the sample of assessment usefulness 50 ℃ of following maturations 20 hours 90 ℃ of oven dry 3 minutes.
The sticking agent of comparative example and embodiment 1 to 5 is formed whole shown in following table two.
Table two
| Embodiment A | Embodiment B | Embodiment C | Embodiment D | |
| Comparative example | 100 | 0 | 0 | 0 |
| Embodiment 1 | 100 | 10 | 0 | 0 |
| Embodiment 2 | 100 | 5 | 0 | 0 |
| Embodiment 3 | 100 | 1 | 0 | 0 |
| Embodiment 4 | 100 | 0 | 10 | 0 |
| Embodiment 5 | 100 | 0 | 0 | 10 |
Then, the sticking agent sample to comparative example and embodiment 1 to 5 carries out adhesion, confining force respectively and stores the modulus test.Wherein, the adhesion test is to use puller system (Dachang, make by wide rhenium instrument), the PET adhesive film of coating sticking agent is cut into 2.5 centimeters wide long strip shape test piece, after fractal film in the test piece removed, make test piece stick together face through 2kg spreading roller and stick on the SUS316 standard surface of steel plate, under 23 ± 1 ℃/50 ± 2%RH (relative humidity) environment, use puller system to measure test piece and stick together 180 degree adhesions in the face of steel plate to draw high speed 300mm/min.
Confining force test be will the coating sticking agent the PET adhesive film cut into 2.5 centimeters wide long strip type test piece, after fractal film in the test piece removed, the area of applying 2.5mmx2.5mm on SUS316 standard steel plate, making test piece stick together face through 2kg spreading roller sticks on the SUS316 standard surface of steel plate, in 70 ℃ circulation baking oven, placed 20 minutes earlier, and then hang up the counterweight 40 minutes of 1kg, confining force is meant that test piece till the time that begins to be measured to weights and drop, then writes down the distance (unit: mm) of test piece displacement through 40 minutes counterweight persons of not dropping.
Storing the modulus test is to use the rotary type rheology to move (AR2000ex is made by TA) to carry out.Measure and use diameter 25mm flat board, spacing 1mm, stress 2000Pa, frequency 10Hz, 25 ℃ to 100 ℃ of temperature ranges.
The sticking agent rerum natura of comparative example and embodiment 1 to 5 is whole shown in following table three.
Table three
By table three as can be seen, the embodiment 1 to 5 that adds high glass tansition temperature (30 ℃-80 ℃) material is arranged, its comparative example that does not add high glass tansition temperature material at 30 ℃ storage modulus (G ') for high, does not then have apparent variation at 80 ℃ storage moduluses at 30 ℃ storage modulus.That is by first polymkeric substance and have the sticking agent of the present invention that second crosslinked polymer of low glass tansition temperature forms, can have higher storage modulus with temperature and change, and have good adhesion and confining force with higher glass tansition temperature.
Though aforesaid description and graphicly disclosed preferred embodiment of the present invention, must recognize variously increase, many modifications and replace and may be used in preferred embodiment of the present invention, and can not break away from the spirit and the scope of the principle of the invention that claim defines.The general skill person who is familiar with the technical field of the invention can know from experience, and the present invention can be used in the modification of many forms, structure, layout, ratio, material, assembly and assembly.Therefore, this paper should be regarded as in order to explanation the present invention in the embodiment that this disclosed, but not in order to restriction the present invention.Scope of the present invention should be defined by claim, and contains its legal equivalents, is not limited to previous description.
Claims (20)
1. sticking agent, it is characterized in that, this sticking agent is formed by first polymkeric substance and second crosslinked polymer, and wherein the glass tansition temperature of this first polymkeric substance is higher than the glass tansition temperature of this second polymkeric substance, and this first polymkeric substance and this second polymkeric substance can dissolve each other.
2. sticking agent as claimed in claim 1, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 0 to 150 ℃.
3. sticking agent as claimed in claim 2, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 10 ℃ to 100 ℃.
4. sticking agent as claimed in claim 3, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 30 ℃ to 85 ℃.
5. sticking agent as claimed in claim 1, the glass tansition temperature that it is characterized in that this second polymkeric substance between-100 ℃ to 0 between.
6. sticking agent as claimed in claim 5, the glass tansition temperature that it is characterized in that this second polymkeric substance is between-80 ℃ to-10 ℃.
7. sticking agent as claimed in claim 6, the glass tansition temperature that it is characterized in that this second polymkeric substance is between-60 ℃ to-20 ℃.
8. sticking agent as claimed in claim 1 is characterized in that this first polymkeric substance and this second polymkeric substance are the methacrylic based polyalcohol.
9. sticking agent as claimed in claim 1, the weight percent that it is characterized in that this first polymkeric substance is between 0.5% to 50%, and the weight percent of this second polymkeric substance is between 99.5% to 50%.
10. sticking agent as claimed in claim 9, the weight percent that it is characterized in that this first polymkeric substance is between 1% to 20%, and the weight percent of this second polymkeric substance is between 99% to 80%.
11. sticking agent as claimed in claim 1, it is characterized in that this first polymkeric substance with isocyanic ester as linking agent and this second crosslinked polymer.
12. a sticking agent manufacture method is characterized in that this sticking agent manufacture method comprises:
First polymkeric substance is provided;
Second polymkeric substance is provided, and wherein the glass tansition temperature of this first polymkeric substance is higher than this second polymkeric substance
The glass tansition temperature, this first polymkeric substance and this second polymkeric substance can dissolve each other; And
Make this first polymkeric substance and this second polymkeric substance carry out crosslinking reaction.
13. sticking agent manufacture method as claimed in claim 12, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 0 to 150 ℃.
14. sticking agent manufacture method as claimed in claim 13, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 10 ℃ to 100 ℃.
15. sticking agent manufacture method as claimed in claim 14, the glass tansition temperature that it is characterized in that this first polymkeric substance is between 30 ℃ to 85 ℃.
16. sticking agent manufacture method as claimed in claim 12, the glass tansition temperature that it is characterized in that this second polymkeric substance between-100 ℃ to 0 between.
17. sticking agent manufacture method as claimed in claim 16, the glass tansition temperature that it is characterized in that this second polymkeric substance is between-80 ℃ to-10 ℃.
18. sticking agent manufacture method as claimed in claim 17, the glass tansition temperature that it is characterized in that this second polymkeric substance is between-60 ℃ to-20 ℃.
19. sticking agent manufacture method as claimed in claim 12, the weight percent that it is characterized in that this first polymkeric substance is between 0.5% to 50%, and the weight percent of this second polymkeric substance is between 99.5% to 50%.
20. sticking agent manufacture method as claimed in claim 19, the weight percent that it is characterized in that this first polymkeric substance is between 1% to 20%, and the weight percent of this second polymkeric substance is between 99% to 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102812388A CN101942284A (en) | 2010-09-05 | 2010-09-05 | Adhesive and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102812388A CN101942284A (en) | 2010-09-05 | 2010-09-05 | Adhesive and manufacturing method thereof |
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| CN101942284A true CN101942284A (en) | 2011-01-12 |
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| CN2010102812388A Pending CN101942284A (en) | 2010-09-05 | 2010-09-05 | Adhesive and manufacturing method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284977A (en) * | 2007-04-10 | 2008-10-15 | 琳得科株式会社 | Adhesion agent for optical functional film, optical functional film and preparation thereof |
| CN101573409A (en) * | 2006-12-26 | 2009-11-04 | 综研化学株式会社 | Binder resin for near-infrared absorbing film, and near-infrared absorbing filter using the same |
-
2010
- 2010-09-05 CN CN2010102812388A patent/CN101942284A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101573409A (en) * | 2006-12-26 | 2009-11-04 | 综研化学株式会社 | Binder resin for near-infrared absorbing film, and near-infrared absorbing filter using the same |
| CN101284977A (en) * | 2007-04-10 | 2008-10-15 | 琳得科株式会社 | Adhesion agent for optical functional film, optical functional film and preparation thereof |
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Application publication date: 20110112 |