CN104293249B - Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive - Google Patents
Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive Download PDFInfo
- Publication number
- CN104293249B CN104293249B CN201410570798.3A CN201410570798A CN104293249B CN 104293249 B CN104293249 B CN 104293249B CN 201410570798 A CN201410570798 A CN 201410570798A CN 104293249 B CN104293249 B CN 104293249B
- Authority
- CN
- China
- Prior art keywords
- parts
- sensitive adhesive
- pressure sensitive
- reaction
- initiator solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention provides a kind of preparation method of pressure sensitive adhesive, comprise: by after 10～30 parts of the hard monomers in parts by weight, 60～90 parts of soft monomers, 1～10 part of function monomer and 80～120 parts of Hybrid Heating of ethyl acetate, total umber of described hard monomer, described soft monomer and described function monomer is 100 parts, substep adds the first initiator solution, the second initiator solution and the reaction of the 3rd initiator solution, and then cooling discharge obtains acrylate performed polymer; After being mixed, 75～95 parts, 0.5～3 part of 0.2～0.5 part, 100 parts of described acrylate performed polymers, curing agent, silane coupler in parts by weight and ethyl acetate obtains pressure sensitive adhesive. The invention provides pressure sensitive adhesive and application thereof prepared by a kind of aforementioned preparation method. The present invention has overcome the uppity shortcoming of course of reaction, reduces the harm to human body and environment, and the pressure sensitive adhesive of preparation has good performance, and this pressure sensitive adhesive can be applied on polaroid.
Description
Technical field
The invention belongs to pressure sensitive adhesive technical field, be specifically related to a kind of pressure sensitive adhesive preparation method, pressure sensitive adhesive andIts application.
Background technology
Pressure-sensitive adhesive for polaroid is a kind of special optics pressure sensitive adhesive, the wet-hot aging performance to pressure sensitive adhesive, high temperatureDurability, optical characteristics, peeling force and peel strength etc. have special requirement, are mainly manifested in high opticsCharacteristic, good releasable energy, higher peel strength, initial bonding strength and cohesive force etc. At present at polarisationThe pressure sensitive adhesive that sheet industry is used is mainly solvent-based polyacrylate pressure sensitive adhesives, the instructions for use of Yin Qigao,At present it is produced and mainly concentrates on the ground such as Japan, Korea S, domestic to polaroid with the research of optics pressure sensitive adhesive andReport is few. Commonly using in the prior synthesizing method of polaroid use solvent type polyacrylate class optics pressure sensitive adhesiveSolvent is the mixed solvent of toluene or ethyl acetate and toluene, synthesizes and mostly on the boiling point of solvent, returnsStream reaction. The shortcoming of this technique is: 1, in course of reaction, temperature is higher, adds identical initator, instituteThe molecular weight of polymer, adhesion strength is not high, durability is bad, the wayward and energy of course of reactionConsume high; 2, in synthetic, to use the aromatic hydrocarbon solvents such as toluene, human body is had to harm, stimulate brain nervous centralis,Anesthesia stupor is also larger to the harm of environment.
Summary of the invention
The object of the embodiment of the present invention is to overcome the above-mentioned deficiency of prior art, and a kind of system of pressure sensitive adhesive is providedPreparation Method, adds initiator solution to make course of reaction be easy to control by substep.
Another object of the embodiment of the present invention is to overcome the above-mentioned deficiency of prior art, and a kind of as front institute are providedPressure sensitive adhesive prepared by the preparation method of the pressure sensitive adhesive of stating, make this pressure sensitive adhesive have good peeling force, initial bonding strength,Cohesive force, hold viscous force and durability.
The another object of the embodiment of the present invention is to overcome the above-mentioned deficiency of prior art, and a kind of as front institute are providedPressure sensitive adhesive prepared by the preparation method of the pressure sensitive adhesive of the stating application on polaroid.
In order to realize foregoing invention object, the technical scheme of the embodiment of the present invention is as follows:
A preparation method for pressure sensitive adhesive, comprising:
By 10～30 parts of the hard monomers in parts by weight, 60～90 parts of soft monomers, 1～10 part of function monomerAfter 80～120 parts of Hybrid Heating of ethyl acetate, wherein, described hard monomer, described soft monomer and described functionTotal umber of monomer is 100 parts, and substep adds the first initiator solution, the second initiator solution and the 3rd to drawSend out agent solution reaction, then cooling discharge obtains acrylate performed polymer;
By 0.2～0.5 part, 100 parts of described acrylate performed polymers, curing agent in parts by weight, silane occasionallyJoin after 75～95 parts, 0.5～3 part of agent and ethyl acetate mixes and obtain pressure sensitive adhesive.
Pressure sensitive adhesive prepared by a kind of preparation method of foregoing pressure sensitive adhesive.
And, pressure sensitive adhesive prepared by a kind of preparation method of the foregoing pressure sensitive adhesive application on polaroid.
The embodiment of the present invention adopts substep to drip the method for initiator solution, has overcome course of reaction waywardShortcoming, building-up process, using ethyl acetate as solvent, is not introduced aromatic hydrocarbon solvent, reduce to human body and ringThe harm in border.
The pressure sensitive adhesive that adopts the method for the embodiment of the present invention to prepare, has good peeling force, initial bonding strength, stickyKnot power, hold viscous force and durability.
The pressure sensitive adhesive that adopts the method for the embodiment of the present invention to prepare is applied to prepares polaroid, makes this polaroidCan be excellent.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment,The present invention is further elaborated. Should be appreciated that specific embodiment described herein only in order toExplain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of preparation method of pressure sensitive adhesive, comprises the steps:
Step S01: by 10～30 parts of the hard monomers in parts by weight, 60～90 parts of soft monomers, function listAfter 1～10 part of body and 80～120 parts of Hybrid Heating of ethyl acetate, substep adds the first initiator solution, secondInitiator solution and the reaction of the 3rd initiator solution, then cooling discharge obtains acrylate performed polymer;
Step S02: by 100 parts of the acrylate performed polymers in parts by weight, 0.2～0.5 part, curing agent,After mixing, 75～95 parts, 0.5～3 part of silane coupler and ethyl acetate obtains optics pressure sensitive adhesive. This acetic acidEthyl ester is to use as retarder thinner, and the ethyl acetate of 75～95 parts can be adjusted into the viscosity of pressure sensitive adhesive750～1000cP, meets the needs of technical scheme of the present invention.
The embodiment of the present invention adopts substep to drip the method for different initiator solutions, has overcome course of reaction and has been difficult forThe shortcoming of controlling, building-up process, using ethyl acetate as solvent, is not introduced aromatic hydrocarbon solvent, reduces human bodyHarm with environment.
Preferably, in step S01, hard monomer is 12～27 parts, 65～83 parts of soft monomers, function monomer 1～880～120 parts, part and ethyl acetate. In step S02,100 parts of acrylate performed polymers, curing agent 0.24～0.35Part, 83～92 parts, 0.5～1.5 part of silane coupler and ethyl acetate.
Particularly, in the above-mentioned process that obtains acrylate performed polymer (step S01), adopt and pass into inertiaThe mode of gas shield, avoids airborne oxygen to produce oxidation and inhibition etc. to this process. Preferably, shouldInert gas is nitrogen. In the above-mentioned process that obtains acrylate performed polymer, can be attended by stirring, stir speedDegree is 50～100rpm, so that each reactant fully contacts, is conducive to the raising of reaction rate.
Particularly, the process of step S01 is specially:
Step S11: by hard monomer, soft monomer, function monomer and ethyl acetate Hybrid Heating, Hybrid HeatingTemperature be 65～71 DEG C, be preferably 66～70 DEG C. Because heating-up temperature is lower, this heating can adopt waterBathe heating, can certainly adopt other mode of heating.
Step S12: to above-mentioned mixed solution and dripping the first initiator solution reaction that is heated to design temperature,Keeping the temperature of reaction is 65～72 DEG C, and the time is 4～6h. The first initiator solution is in parts by weight0.07～0.08 part of 5～20 parts, ethyl acetate and azodiisobutyronitrile. Wherein, azodiisobutyronitrile mainly playsThe effect of initator, ethyl acetate is as dissolution with solvents azodiisobutyronitrile. The first initiator solution passes through willAbove-mentioned two kinds of materials mix. Because the temperature of reaction is lower, this process can adopt heating water bath, whenSo also can adopt other mode of heating. Preferably, in the first initiator solution ethyl acetate be 12～15 parts,0.07～0.08 part of azodiisobutyronitrile, the temperature of reaction is 66～72 DEG C, the time is 4～6h.
Step S13: cause to the above-mentioned reacted mixed solution and dripping of the first initiator solution second that addsAgent solution reaction, keeping the temperature of reaction is 72～74 DEG C, the time is 1～1.5h. The second initiator solution isIn 0.02～0.04 part of 40～45 parts, the ethyl acetate of parts by weight and azodiisobutyronitrile. Wherein, azoBis-isobutyronitrile mainly plays the effect of initator, and ethyl acetate is as dissolution with solvents azodiisobutyronitrile. SecondInitiator solution is by mixing above-mentioned two kinds of materials. Because the temperature of reaction is lower, this process canAdopt heating water bath, can certainly adopt other mode of heating.
Step S14: add the 3rd initiation of the reacted mixed solution and dripping of the second initiator solution to above-mentionedAgent solution reaction, keeping the temperature of reaction is 72～74 DEG C, is warming up to 75～76 DEG C and also protects after reaction 0.5～1hTemperature 1.5～2.5h. Wherein, azodiisobutyronitrile mainly plays the effect of initator, and ethyl acetate is as solventDissolve azodiisobutyronitrile. The 3rd initiator solution is in 10～20 parts, the ethyl acetate of parts by weight and even0.01～0.02 part of nitrogen bis-isobutyronitrile. The 3rd initiator solution is by mixing above-mentioned two kinds of materials. Due toThe temperature of reaction is lower, and this process can adopt heating water bath, can certainly adopt other mode of heating.Preferably, to the above-mentioned reacted mixed solution and dripping of the second initiator solution the 3rd initiator solution that addsReaction, keeping the temperature of reaction is 72～74 DEG C, reaction is warming up to 75～76 DEG C and be incubated 1.5～2h after 0.5～1h.
The process that obtains acrylate performed polymer of the present invention is to carry out under cryogenic conditions, can overcome existingIn technology, the high defect of synthesis temperature, has reduced energy consumption. From the concrete technology parameter of step S01, lowTemperature condition refers to that reaction temperature is under the boiling point of solvent ethyl acetate. Because initator azodiisobutyronitrile isLow activity initator, it is generally acknowledged in prior art and under low temperature, adopts the more difficult initiated polymerization of this initator, soThe temperature that prior art adopts is generally 75～80 DEG C. And technical scheme of the present invention, especially step S12Reaction temperature be 65～72 DEG C, realized the reaction of initiated polymerization at low temperatures, overcome in prior artPrejudice. It is lower that prior art is reacted the general molecular weight of copolymer obtaining under hot conditions, and molecular weight dividesCloth is wider and energy consumption is high, and the method that technical scheme of the present invention adopts cryogenic conditions and progressively heats up is passed throughRegulate temperature to control the distribution of molecular size range and the molecular weight of acrylate performed polymer. The temperature in early stageLow, make reaction condition gentleness, reaction is easy to control; The middle and later periods temperature that progressively raises, can keep system anti-Answer the stable of speed, obtain the acrylate performed polymer that molecular weight is high and molecular weight distribution is narrower (third simultaneouslyOlefin(e) acid ester copolymer), make the pressure sensitive adhesive of synthesized there is good endurance quality and hold viscosity energy; Meanwhile,Can reduce the impact of low-temp reaction on reaction rate, avoid under conventional high-temperature condition, reaction rate is too fast,React uppity problem.
Technical scheme of the present invention adopts substep to add the ethyl acetate of Different Weight ratio by step S12～S14With the initiator solution of azodiisobutyronitrile composition, the ratio of ethyl acetate from low to high and reaction temperature progressivelyRaise. Step S12～S14 substep adds initiator solution to reduce and adds drawing of initator generation because of a stepSend out the impact of agent consumption on reaction rate. Step S12～S14 substep adds as the ethyl acetate of solvent also canCause hard monomer, soft monomer and function monomer concentration to reduce to reduce because ethyl acetate solvent adds, make reactionThe impact of rate reduction on reaction. In step S12, the additional proportion of ethyl acetate solvent is low, azo two isobutylsThe additional proportion of nitrile initator is relatively high, and reaction temperature is low, can ensure under the prerequisite of reaction rate,Make reaction condition gentleness, be easy to control, obtain the acrylate performed polymer of molecular weight height and narrow molecular weight distribution(being acrylate copolymer), improve synthesized pressure sensitive adhesive endurance quality and hold viscosity energy. Step S14The additional proportion of middle ethyl acetate solvent is high and temperature amplification is larger, can ensure under the prerequisite of reaction rate,Improve the conversion ratio of hard monomer, soft monomer and function monomer, under polymerization later stage hot conditions, a small amount of listBody synthetic molecular weight is relatively low, and the acrylate performed polymer that molecular weight distribution is wider is having pressure sensitive adhesiveIncreased durability and holding under the prerequisite of viscosity, has good initial cohesiveness. Wherein. Step S12 producesMolecular weight acrylate performed polymer high and narrow molecular weight distribution accounts for larger proportion, can improve the resistance to of pressure sensitive adhesiveFor a long time property, hold viscosity and peel strength, but can make tack reduce; The molecular weight that step S14 produces relativelyLow, the wider acrylate performed polymer of molecular weight distribution accounts for less ratio, can improve the tack of pressure sensitive adhesive,But can make durability, hold viscosity and peel strength declines to some extent. Therefore, drip by step S12～S14 substepThe prepared pressure sensitive adhesive of method that adds variable concentrations initiator solution and progressively heat up comprise above-mentioned two kinds differentAcrylate performed polymer, makes the existing good durability of this pressure sensitive adhesive and holds viscous force, at the beginning of also having preferablyViscosity, combination property is good.
Particularly, above-mentioned preparation process can be carried out in reactor. Certainly the application is as limit,Also can in other applicable equipment, carry out.
Particularly, the hard monomer of the embodiment of the present invention is methyl acrylate, methyl methacrylate, acetic acid secondAt least one in alkene ester, acrylonitrile, n-BMA; And/or soft monomer is acrylic acid secondAt least one in ester, butyl acrylate, Isooctyl acrylate monomer; And/or, function monomer be acrylic acid,At least one in maleic acid, acrylamide, senecioate-hydroxyl ethyl ester; And/or curing agent is in moleculeHave the compound of at least two NCOs, for example, curing agent can be 1, hexamethylene-diisocyanate,IPDI etc.; And/or silane coupler is the organosilicon with at least one alkoxylOne or more of compound, for example, silane coupler can be MTMS, dimethoxyDiethoxy silane, tetraethoxysilane etc.
Particularly, the process of step S12 at room temperature stirs.
In the process of above-mentioned steps S01 and S02, only adopt ethyl acetate as solvent, in preparation process notIntroduce aromatic hydrocarbons organic solvent, reduce pressure sensitive adhesive harm to human body and environment in preparation and use procedure,Make its environmental protection more.
The present invention adopts said method can prepare pressure sensitive adhesive, this pressure sensitive adhesive have good peeling force,Initial bonding strength, cohesive force and durability.
The present invention adopts the pressure sensitive adhesive that said method prepares on polaroid, to apply, owing to being prepared intoTo pressure sensitive adhesive there is good peeling force, initial bonding strength, cohesive force and durability, make the property of this polaroidCan be excellent.
Further illustrate technical scheme of the present invention below by specific embodiment.
In following embodiment, curing agent is selected from 1, hexamethylene-diisocyanate or IPDI,Silane coupler is selected from MTMS, dimethoxy diethoxy silane or tetraethoxysilane.
Embodiment 1
Take methyl acrylate 12g, butyl acrylate 83g, acrylic acid 5g, ethyl acetate 80g are fed intoIn reactor, start and stir and heating water bath, be heated to after 66 DEG C until system, drip 12g ethyl acetate andThe first initiator solution that 0.07g azodiisobutyronitrile mixes, regulates bath temperature, makes system temperature dimensionBe held in 66～68 DEG C, after reaction 6h, add 45g ethyl acetate and 0.04g azodiisobutyronitrile to mixThe second initiator solution and be warming up to 72 DEG C, after reaction 1.5h, add 10g ethyl acetate and 0.01g evenThe 3rd initiator solution that nitrogen bis-isobutyronitrile mixes, after 74 DEG C of reaction 1h, at 76 DEG C of insulation 2h,Then cooling discharge obtains acrylate performed polymer, whole process nitrogen protection. By pre-120g acrylateAggressiveness, 0.24g curing agent, 0.6g silane coupler and 100g ethyl acetate at room temperature mixObtain pressure sensitive adhesive.
The main performance index method for measuring of this pressure sensitive adhesive is as follows:
It is that the PETG of 38 μ m is release that prepared pressure sensitive adhesive is evenly coated to thicknessOn film, gluing thickness is about 22 μ m, is 32 DEG C in temperature, humidity be under 65% condition solidify after 7 days byProperties according to following method of testing test pressure sensitive adhesive:
180 ° of peel test forces: according to GB/T2792-1998, survey with desktop tensile testing machineExamination.
Initial bonding strength test: will be coated with this pressure sensitive adhesive, be of a size of the strip polaroid sample of 25 × 300mm,Adopt the accurate test of 2kg standard pressure roller labeling steel plate, roll once, at room temperature place 30min and carry out 180 °Peel off, peeling rate is 300mm/min.
Cohesive force test: will be coated with this pressure sensitive adhesive, be of a size of the strip sample polaroid product of 25 × 300mm,Adopt the accurate test of 2kg standard pressure roller labeling steel plate, roll once, at 50 DEG C, under 5kg/f pressure, deaerationAfter 20min, room temperature placement 24h carries out 90 ° and peels off, and peeling rate is 300mm/min.
Hold viscous force test: according to GB/T4851-1988, carry out with baking oven type adhesive tape retention testing machineTest.
Durability test: will be coated with this pressure sensitive adhesive, be of a size of the polaroid sample of 50mm × 75mm, and useIt is on glass that hand push roller attaches to LCD, and at 50 DEG C, under 5kg/f pressure condition, deaeration 20min, makes resistance toProperty test sample, carries out respectively 80 DEG C × 500h of high temperature, 60 DEG C × 90%RH × 500h of constant temperature and humidity, low temperature for a long time-40 DEG C × 500h and thermal shock-40 DEG C × 30min～80 DEG C × 30min, 100 circulations, four durability are surveyedExamination, watches after 500h test the outward appearance of pressure-sensitive adhesive layer.
Embodiment 2
Take methyl methacrylate 27g, Isooctyl acrylate monomer 72g, acrylic acid 1g, ethyl acetate 90gBe fed in reactor, start and stir and heating water bath, be heated to after 68 DEG C until system, drip 15g acetic acidThe first initiator solution that ethyl ester and 0.07g azodiisobutyronitrile mix, regulates bath temperature, makes bodyBe that temperature maintains 68～70 DEG C, after reaction 5h, add 40g ethyl acetate and 0.03g azodiisobutyronitrileThe second initiator solution mixing is also warming up to 74 DEG C, reaction 1h after, add 20g ethyl acetate andThe 3rd initiator solution that 0.02g azodiisobutyronitrile mixes, after 74 DEG C of reaction 0.5h, at 75 DEG CLower insulation 2h, then cooling discharge obtains acrylate performed polymer, whole process nitrogen protection. By 120gAcrylate performed polymer, 0.36g curing agent and 1.2g silane coupler and 110g ethyl acetate are at room temperature mixedClose and evenly can obtain pressure sensitive adhesive. Carry out properties test according to the coating in embodiment 1 and method of testing.
Embodiment 3
Take methyl methacrylate 5g, methyl acrylate 22g, butyl acrylate 65g, acrylamide 8g,Ethyl acetate 120g is fed in reactor, starts and stirs and heating water bath, be heated to after 70 DEG C until system,Drip the first initiator solution that 12g ethyl acetate and 0.08g azodiisobutyronitrile mix, regulate waterBath temperature, makes system temperature maintain 70～72 DEG C, after reaction 4h, adds 43g ethyl acetate and 0.02gThe second initiator solution that azodiisobutyronitrile mixes is also warming up to 73 DEG C, after reaction 1h, adds 15gThe 3rd initiator solution that ethyl acetate and 0.02g azodiisobutyronitrile mix, at 72 DEG C of reaction 1hAfter, at 76 DEG C of insulation 1.5h, then cooling discharge obtains acrylate performed polymer, and whole process is protected with nitrogenProtect. By 120g acrylate performed polymer, 0.42g curing agent and 1.8g silane coupler and 100g acetic acid secondEster at room temperature mixes and can obtain pressure sensitive adhesive. Carry out according to the coating in embodiment 1 and method of testingProperties test.
Comparative example 1
Hard monomer 33.6g, soft monomer 80.4g, function monomer 6g and ethyl acetate 120g are fed into nitrogen and protectIn the reactor protecting, stir for subsequent use. 96g ethyl acetate and 0.144g azodiisobutyronitrile are mixed allThe even initiator solution that obtains is added dropwise to 1/3 above-mentioned initiator solution in the time of 75～80 DEG C, in 0.5～1h, drips.Continue backflow 3h and be added dropwise to again 1/3 above-mentioned initiator solution, in 0.5～1h, drip, continue after backflow 2hBe added dropwise to remaining above-mentioned initiator solution, in 0.5～1h, drip. Under reflux state, continue polymerisation2～3h, obtains acrylate performed polymer after cooling. By 100g acrylate performed polymer, 0.35g curing agent and1.5g silane coupler and appropriate ethyl acetate mix and can obtain pressure sensitive adhesive. According in embodiment 1Coating and method of testing are carried out properties test.
The performance of the pressure sensitive adhesive that embodiment 1～3 and comparative example 1 obtain is respectively as shown in table 1.
The performance of table 1 pressure sensitive adhesive
Note: durability is the result of test 500h; Zero: represent without peeling off without water wave; △: representative is slightly peeled off or water wave; ×:Representative is seriously peeled off or water wave.
As can be seen from Table 1, the initator adding due to comparative example 1 substep is identical with the temperature of every step,And temperature is higher, the molecular weight distribution of low molecular weight of acrylate performed polymer is narrow, therefore comparative example 1 obtainsThe initial bonding strength of optics pressure sensitive adhesive is better. Although the initial bonding strength of comparative example 1 is better than optics pressure sensitive adhesive of the present invention,But other performance is all poor than optics pressure sensitive adhesive of the present invention, and particularly comparative example 1 does not have durability, makesIts application is greatly limited. In embodiment 1～3, reaction temperature in early stage is controlled at lower scope, and monomer concentrationHeight, the first initiator concentration is lower, the acrylate performed polymer molecular weight that obtains is higher, molecular weight distributionNarrow. Reaction mid-term, adds the second initator after suitably improving temperature, continue maintenance system reaction rate andThe HMW of performed polymer and Narrow Molecular Weight Distribution, thus the peeling force of the optics pressure sensitive adhesive obtaining, hold viscous force,Cohesive force and durability are better. Reaction the later stage, continue improve temperature and amplification larger, obtain molecular weight low,The performed polymer that molecular weight distribution is wide, provides the initial bonding strength that optics pressure sensitive adhesive is good.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, not all at thisAny amendment of doing within bright spirit and principle, be equal to and replace and improvement etc., all should be included in the present inventionProtection domain within.
Claims (6)
1. a preparation method for pressure sensitive adhesive, is characterized in that, comprising:
By 10～30 parts of the hard monomers in parts by weight, 60～90 parts of soft monomers, 1～10 part of function monomer andAfter 80～120 parts of Hybrid Heating of ethyl acetate, wherein, described hard monomer, described soft monomer and described function listTotal umber of body is 100 parts, and substep adds the first initiator solution, the second initiator solution and the 3rd initiationAgent solution reaction, then cooling discharge obtains acrylate performed polymer;
By 0.2～0.5 part, 100 parts of described acrylate performed polymers, curing agent in parts by weight, silane occasionallyJoin after 75～95 parts, 0.5～3 part of agent and ethyl acetate mixes and obtain pressure sensitive adhesive;
Wherein,
Described the first initiator solution is 5～20 parts, ethyl acetate and the azodiisobutyronitrile in parts by weight0.07～0.08 part; While adding described the first initiator solution reaction, keeping the temperature of reaction is 65～72 DEG C,Time is 4～6h;
Described the second initiator solution is 40～45 parts, ethyl acetate and the azodiisobutyronitrile in parts by weight0.02～0.04 part; While adding described the second initiator solution reaction, keeping the temperature of reaction is 72～74 DEG C,Time is 1～1.5h;
Described the 3rd initiator solution is 10～20 parts, ethyl acetate and the azodiisobutyronitrile in parts by weight0.01～0.02 part; While adding described the 3rd initiator solution reaction, keeping the temperature of reaction is 72～74 DEG C,Reaction is warming up to 75～76 DEG C and be incubated 1.5～2.5h after 0.5～1h.
2. the preparation method of pressure sensitive adhesive as claimed in claim 1, is characterized in that: by described hard monomer,The temperature of described soft monomer, described function monomer and described ethyl acetate Hybrid Heating is 65～71 DEG C.
3. the preparation method of pressure sensitive adhesive as claimed in claim 1, is characterized in that: described in obtain acrylic acidIn the process of ester performed polymer, pass into inert gas shielding.
4. the preparation method of pressure sensitive adhesive as claimed in claim 1, is characterized in that:
Described hard monomer is methyl acrylate, methyl methacrylate, vinylacetate, acrylonitrile, methylAt least one in n-butyl acrylate; And/or,
Described soft monomer is at least one in ethyl acrylate, butyl acrylate, Isooctyl acrylate monomer; With/Or,
Described function monomer is at least one in acrylic acid, maleic acid, acrylamide, senecioate-hydroxyl ethyl esterKind; And/or,
Described curing agent is the compound in molecule with at least two NCOs; And/or,
Described silane coupler is one or more of organo-silicon compound with at least one alkoxyl.
5. the pressure sensitive adhesive that prepared by the preparation method of the pressure sensitive adhesive as described in claim 1～4 any one.
6. the pressure sensitive adhesive that prepared by the preparation method of the pressure sensitive adhesive as described in claim 1～4 any one is partiallyApplication on mating plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410570798.3A CN104293249B (en) | 2014-10-23 | 2014-10-23 | Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410570798.3A CN104293249B (en) | 2014-10-23 | 2014-10-23 | Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104293249A CN104293249A (en) | 2015-01-21 |
| CN104293249B true CN104293249B (en) | 2016-05-04 |
Family
ID=52313213
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410570798.3A Active CN104293249B (en) | 2014-10-23 | 2014-10-23 | Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104293249B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI642753B (en) * | 2015-07-27 | 2018-12-01 | 住華科技股份有限公司 | Optical adhesive product and touch display module and adhering method thereof |
| CN106832101A (en) * | 2017-01-05 | 2017-06-13 | 无锡海特新材料研究院有限公司 | A kind of acrylic pressure-sensitive adhesivee of removable labeling and preparation method thereof |
| CN106832103B (en) * | 2017-01-05 | 2019-02-19 | 无锡海特新材料研究院有限公司 | A kind of acrylate pressure-sensitive adhesive and preparation method thereof of strong adherence PC substrate |
| CN110462473B (en) * | 2017-03-29 | 2021-12-21 | 日东电工株式会社 | Adhesive layer-attached single-sided protective polarizing film, image display device, and continuous production method therefor |
| CN109762493A (en) * | 2019-02-12 | 2019-05-17 | 上海巍盛化工科技有限公司 | A kind of acrylate pressure sensitive adhesive and preparation method thereof being used in body of a motor car pad pasting |
| CN111410928A (en) * | 2020-05-08 | 2020-07-14 | 绿色轻化科技发展(北京)有限公司 | High-temperature-resistant acrylic pressure-sensitive adhesive and preparation process thereof |
| CN112708008B (en) * | 2020-12-07 | 2022-08-16 | 苏州赛伍应用技术股份有限公司 | Acrylic copolymer, pressure-sensitive adhesive, preparation method and application in polarizer |
| CN112646515A (en) * | 2020-12-22 | 2021-04-13 | 深圳市益达兴科技股份有限公司 | High-temperature-resistant solvent type acrylate pressure-sensitive adhesive and preparation method thereof |
| CN113322030A (en) * | 2021-05-24 | 2021-08-31 | 深圳市通泰盈科技股份有限公司 | High-performance acrylic acid adhesive, preparation method thereof and pressure-sensitive adhesive tape |
| CN113637436B (en) * | 2021-09-06 | 2022-09-16 | 合肥工业大学 | Acrylate pressure-sensitive adhesive, preparation method thereof and polarizer protective film |
| CN115386034A (en) * | 2021-12-02 | 2022-11-25 | 广东邦固化学科技有限公司 | Acrylate pressure-sensitive adhesive with high humidity and heat resistance and water whitening resistance and preparation method thereof |
| CN114823956B (en) * | 2022-05-19 | 2024-04-05 | 常州百佳年代薄膜科技股份有限公司 | Composite material for solar cell light component and preparation method thereof |
| CN115044330A (en) * | 2022-07-11 | 2022-09-13 | 惠州华星光电显示有限公司 | Preparation method of pressure-sensitive adhesive, polaroid and application method of polaroid |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4913937B2 (en) * | 2000-08-01 | 2012-04-11 | 日東電工株式会社 | Fixing method of pressure-sensitive adhesive sheets and functional films |
| CN101993675A (en) * | 2010-11-02 | 2011-03-30 | 北京高盟新材料股份有限公司 | Silane coupling agent modified acrylic pressure sensitive adhesive and preparation method thereof |
| CN102533171B (en) * | 2010-12-20 | 2015-02-11 | 常州化学研究所 | Solid cleaning adhesive and preparation method thereof |
| CN102504732B (en) * | 2011-11-29 | 2013-09-04 | 广东达美新材料有限公司 | Solvent-based reticulated pressure-sensitive adhesive for polyethylene protective film and preparation method thereof |
| CN103571367B (en) * | 2013-11-08 | 2014-10-22 | 烟台德邦科技有限公司 | Pressure-sensitive adhesive for wafer grinding and preparation method thereof |
| CN103725231B (en) * | 2013-12-24 | 2015-07-01 | 四川东材科技集团股份有限公司 | Adhesive material for adhesive tapes and preparation method thereof |
| CN103952104A (en) * | 2014-03-28 | 2014-07-30 | 广东达美新材料有限公司 | Solvent type pressure-sensitive adhesive used for polyethylene electronic protection film, and preparation method thereof |
-
2014
- 2014-10-23 CN CN201410570798.3A patent/CN104293249B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104293249A (en) | 2015-01-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104293249B (en) | Preparation method, pressure sensitive adhesive and the application thereof of pressure sensitive adhesive | |
| CN101974299B (en) | High temperature-resistant polyacrylate pressure-sensitive adhesive emulsion and preparation method and application thereof | |
| CN103140517B (en) | Adhesive sheet | |
| CN103937429A (en) | High temperature resistant non-yellowing high stripping strength pressure-sensitive adhesive and preparation method thereof | |
| CN102732176A (en) | Peelable polyacrylate pressure-sensitive adhesive film with controllable peeling force | |
| CN106632818A (en) | High-permeability and high-temperature-resistant type acrylate pressure-sensitive adhesive and preparation method thereof | |
| KR20110042330A (en) | Composite article | |
| Lu et al. | Viscoelastic and adhesive properties of single‐component thermo‐resistant acrylic pressure sensitive adhesives | |
| JPWO2014002203A1 (en) | Adhesive composition and adhesive tape using the same | |
| WO2012026456A1 (en) | Adhesive agent composition | |
| CN105593328B (en) | Pressure-sensitive adhesive composition | |
| CN106832103A (en) | A kind of acrylate pressure-sensitive adhesive of strong adherence PC base materials and preparation method thereof | |
| CN110387199B (en) | Preparation method and application of acrylate pressure-sensitive adhesive for bathroom toughened glass safety film | |
| JP2014205834A (en) | Silane primer for improving adhesion of adhesive tape on hydrophilic surface, especially glass surface | |
| JP2014205835A (en) | Black silane primer for improving adhesion of adhesive tape to glass surface | |
| CN104152084A (en) | High temperature-resistant low viscosity pressure-sensitive adhesive used for protection films, and preparation method and application thereof | |
| JP5128960B2 (en) | Pressure sensitive adhesive composition, method of applying it and method for preparing it | |
| CN105593256A (en) | Block copolymer | |
| TWI553024B (en) | Process for the preparation of radiation curable compositions | |
| WO2017138609A1 (en) | Uv curable acrylic polymer and method for producing same, and uv curable hot melt adhesive | |
| Chen et al. | Improvement in mechanical properties and thermal stability of solvent‐based pressure‐sensitive adhesives based on triazine heterocyclic monomer | |
| CN109536085B (en) | Preparation method of organic silicon modified polyacrylate pressure-sensitive adhesive and pressure-sensitive adhesive prepared by preparation method | |
| JP7130302B2 (en) | Adhesive composition and baseless adhesive tape | |
| CN114891447B (en) | Acrylate/polyisobutylene rubber hybrid pressure-sensitive adhesive composition | |
| TW202302787A (en) | Curable composition and use thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |