CN103205226B - Solvent type acrylate pressure-sensitive adhesive, and preparation method and application thereof - Google Patents
Solvent type acrylate pressure-sensitive adhesive, and preparation method and application thereof Download PDFInfo
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- CN103205226B CN103205226B CN201210312005.9A CN201210312005A CN103205226B CN 103205226 B CN103205226 B CN 103205226B CN 201210312005 A CN201210312005 A CN 201210312005A CN 103205226 B CN103205226 B CN 103205226B
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Abstract
The invention relates to a solvent type acrylate pressure-sensitive adhesive and a preparation method thereof and application of the solvent type acrylate pressure-sensitive adhesive in a protective film for an ASA section bar. The pressure-sensitive adhesive comprises component A and component B, wherein the component A is an alkyl (meth)acrylate polymer, the component B is a multi-functionality aziridine cross-linking agent, and the component A is prepared through copolymerization of 2-ethylhexyl acrylate, acrylic acid and (meth)acrylate containing two double bonds under initiation of benzoyl peroxide. The pressure-sensitive adhesive prepared in the invention is coated on a substrate so as to prepare the protective film for the ASA section bar. The protective film has good resistance to aging with high temperature and high humidity; when the protective film is torn off from the surface of the ASA section bar, no residual adhesive and spots are left, so the disadvantage of great possibility of leaving of residual adhesive and spots on the ASA section bar by a conventional protective film is overcome.
Description
Technical field
The present invention relates to a kind of pressure sensitive adhesive, specifically one is applied to ASA section bar surface protective film solvent pressure-sensitive adhesive.
Background technology
Along with the raising of people's living standard, the improvement of domestic environment, the individual demand of people is more and more higher, and human oriented design and the color of building are more and more taken seriously.The appearance of colored plastic windows and doors, has not only beautified building, has manifested the theory gone back to nature, and also gives the imagination space that Designerss are larger, gives indoor dress horizontal stroke more individual color matching background, and more resident families create warm environment.
ASA section bar is exactly the one of colour section bar, and it is the section bar be co-extruded by ASA resin and conventional P VC material extending.ASA resin is a kind of ter-polymers be made up of vinyl cyanide (Acrylonitile), vinylbenzene (Styrene), vinylformic acid (Acrylate), is shortcoming for ABS weathering resistance difference and the engineering plastics developed.
ASA section bar, except bright in luster, can meet people to outside the requirement of color, compared with other section bar, also has following advantage.
(1) ASA section bar has good mechanical and physical performance
The structural similitude of ASA and ABS, is made up of acrylonitrile and butadiene rubber, and it remains the splendid mechanical and physical performance that ABS has as engineering plastics.
(2) ASA section bar has very strong weathering resistance
If containing double bond in high molecular polymer, then double bond easily open by the ultraviolet in the larger sunlight of energy intensity, the ageing-resistant performance of high molecular polymer is caused to decline thus, and ASA instead of the divinyl rubber containing unsaturated double-bond in ABS with the acrylic rubber not containing unsaturated double-bond just, therefore, not only can resist degraded that uviolizing causes, aging, fade, the decomposition simultaneously caused the high temperature in the oxidation course of processing in air or variable color have had strong guarantee, improve the anti-aging of material and weathering performance thus greatly.
(3) ASA section bar has reasonable resistance to elevated temperatures.
(4) ASA section bar is a kind of antistatic material, can make the few dust stratification dirt in surface
Because ASA section bar has above-mentioned advantage, it is in flourish period at home, and required protective membrane dimensions of market is huge; but; after existing ASA protective membrane tears from Surface of profile on the market, all fleck or cull be can leave at Surface of profile, section material appearance and final utilization effect affected.A kind of ageing-resistant performance of market demand is excellent, does not leave the ASA pressure sensitive adhesive of fleck or cull.
Summary of the invention
The object of the present invention is to provide a kind of solvent-type acrylic ester pressure-sensitive, the surface protection film made of this pressure sensitive adhesive has well attaching property to ASA section bar, does not pollute Surface of profile after stripping, can not leave fleck.
Another object of the present invention is to the preparation method that above-mentioned solvent-type acrylic ester pressure-sensitive is provided.
The present invention also aims to provide the application of solvent-type acrylic ester pressure-sensitive in ASA section bar surface protective film
In the present invention, unless otherwise stated, the ratio adopted in the present invention is weight ratio.
Object of the present invention is reached by following scheme:
Pressure sensitive adhesive of the present invention comprises composition A and composition B, it is characterized in that: composition A is (methyl) acrylate polymers; Composition B is polyfunctionality aziridine system linking agent, and consumption is 0.2 ~ 0.6% of composition A quality.
Present component B is the aziridine system linking agent of three-functionality-degree.
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Isooctyl acrylate monomer 28.8 ~ 29.6 parts, 0.2 ~ 1 part, vinylformic acid, (methyl) acrylate 0.06 ~ 0.2 part containing two double bonds, benzoyl peroxide 0.08 ~ 0.2 part, ethyl acetate 70 parts.
Described (methyl) acrylate containing two double bonds is one or more in Ethylene glycol dimethacrylate, TEGDMA, dimethacrylate TEG ester, 1,6 hexanediol diacrylate, allyl methacrylate(AMA).
The concrete steps of the preparation method of pressure sensitive adhesive composition A of the present invention following (benzoyl peroxide is divided into two parts, portion be 75 ~ 95%, second part of total amount namely residue benzoyl peroxide be 5 ~ 25% of total amount; Ethyl acetate is divided into three parts, the 30 ~ 50%, three part of portion to be 20 ~ 40%, second part of total amount be total amount namely remaining 10 ~ 50%):
(1) take 75 ~ 95% of Isooctyl acrylate monomer, vinylformic acid, (methyl) acrylate containing two double bonds and benzoyl peroxide total amount, add mixed single still, stir obtained mix monomer;
(2) will remain benzoyl peroxide (5 ~ 25% of total amount), 40 ~ 60% of mix monomer total amount and 20 ~ 40% of ethyl acetate total amount add in reactor, stir be warming up to 60 ~ 70 DEG C after, clock reaction 1.5 ~ 2h;
(3) in residue mix monomer (i.e. total amount 40 ~ 60%), add ethyl acetate total amount 30 ~ 50%, after stirring, obtain dropping liquid;
(4), in reactor after clock reaction 1.5 ~ 2h, in reactor, drip the dropping liquid in step (3), 3 ~ 4h drips off; In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C;
(5) rear 80 DEG C ~ 90 DEG C isothermal reaction 2 ~ 3h are dripped off;
(6) by after still temperature drop to 60 DEG C, add the ethyl acetate of remaining 10 ~ 50%, discharging after stirring, obtain solvent-type acrylic ester pressure-sensitive composition A.
Pressure sensitive adhesive compound method of the present invention comprises the steps:
(1) take quality be the composition A of 100 parts in joining in glue bucket, start stirring;
(2) the composition B taking respective quality on request, in container, adds the ethyl acetate of 4 times of composition B quality, stirs;
(3) the composition B diluted slowly is added in composition A, continue stirring 15 minutes.
The solvent-type acrylic ester pressure-sensitive prepared is coated on required base material, heating, drying, after removing solvent, i.e. obtained ASA section bar protective membrane.Being coated with dry glue amount is 5 ± 1 g/m
2, initial bonding strength is 3
#~ 5
#steel ball, stripping strength is 0.1 ~ 0.3N/25mm.The surface protection film made of this pressure sensitive adhesive has well attaching property to ASA section bar, does not pollute Surface of profile after stripping, can not leave fleck.
Embodiment
Embodiment 1
Solvent-type acrylic ester pressure-sensitive of the present invention is made up of composition A and composition B;
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is by weight:
Isooctyl acrylate monomer 29.6 parts, 0.2 part, vinylformic acid, Ethylene glycol dimethacrylate 0.08 part, benzoyl peroxide 0.12 part, ethyl acetate 70 parts.
The concrete preparation process of composition A is.
(1) take whole Isooctyl acrylate monomer, vinylformic acid, Ethylene glycol dimethacrylate and 0.1 part of benzoyl peroxide, add mixed single still, stir obtained mix monomer.
(2) taking 0.02 part of benzoyl peroxide, 17 parts of mixed lists and 17 parts of ethyl acetate adds in reactor, stirs after being warming up to 70 DEG C, clock reaction 1.5h.
(3) in the mixed list of residue 13 parts, 23 parts of ethyl acetate are added, obtained dropping liquid after stirring.
(4), in reactor after clock reaction 1.5h, drip the dropping liquid in step (3), 3.5h drips off.In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C.
(5) rear 80 DEG C of isothermal reaction 2 h are dripped off.
(6) by after still temperature drop to 60 DEG C, add 30 parts of ethyl acetate, discharging after stirring, obtain the component A of solvent-type acrylic ester pressure-sensitive.
Composition B is the aziridine system linking agent of three-functionality-degree.
ASA section bar surface protective film is preparation method comprise the steps:
Taking 40 ㎏ composition A in joining in glue bucket, starting stirring.In the container taking 160g composition B, add 640g ethyl acetate, stir with glass stick, the composition B diluted slowly is added in A, continue stirring 15 minutes.Coat on base material by the pressure sensitive adhesive prepared, being coated with dry glue amount is 5 ± 1g/m
2.
Protective membrane performance: initial bonding strength (4
#steel ball); Stripping strength (0.3N/25mm); Wet and heat ageing resistant performance (72h does not fall glue, without fleck).
Embodiment 2
Solvent-type acrylic ester pressure-sensitive of the present invention is made up of composition A and composition B;
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is by weight:
Isooctyl acrylate monomer 28.8 parts, 0.84 part, vinylformic acid, Ethylene glycol dimethacrylate 0.2 part, benzoyl peroxide 0.16 part, ethyl acetate 70 parts.The concrete preparation process of composition A is.
(1) take whole Isooctyl acrylate monomer, vinylformic acid, Ethylene glycol dimethacrylate and 0.12 part of benzoyl peroxide, add mixed single still, stir obtained mix monomer.
(2) taking 0.04 part of benzoyl peroxide, 14 parts of mixed lists and 14 parts of ethyl acetate adds in reactor, stirs after being warming up to 65 DEG C, clock reaction 2h.
(3) in the mixed list of residue 16 parts, 24 parts of ethyl acetate are added, obtained dropping liquid after stirring.
(4), after reactor clock reaction 2h, drip the dropping liquid in step (3), 3h drips off.In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C.
(5) rear 80 DEG C of isothermal reaction 2 h are dripped off.
(6) by after still temperature drop to 60 DEG C, add 32 parts of ethyl acetate, discharging after stirring, obtain the component A of solvent-type acrylic ester pressure-sensitive.
Composition B is the aziridine system linking agent of three-functionality-degree.
ASA section bar surface protective film is preparation method comprise the steps:
Taking 40 ㎏ composition A in joining in glue bucket, starting stirring, in the container taking 80g composition B, adding 320g ethyl acetate, stir with glass stick, the composition B diluted slowly is added in A, continue stirring 15 minutes.Coat on base material by the pressure sensitive adhesive prepared, being coated with dry glue amount is 5 ± 1g/m
2.
Protective membrane performance: initial bonding strength (4
#steel ball); Stripping strength (0.25N/25mm); Wet and heat ageing resistant performance (72h does not fall glue, without fleck).
Embodiment 3
Solvent-type acrylic ester pressure-sensitive of the present invention is made up of composition A and composition B;
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is by weight:
Isooctyl acrylate monomer 29.44 parts, 0.32 part, vinylformic acid, Ethylene glycol dimethacrylate 0.16 part, benzoyl peroxide 0.08 part, ethyl acetate 70 parts.
The concrete preparation process of composition A is.
(1) take whole Isooctyl acrylate monomer, vinylformic acid, Ethylene glycol dimethacrylate and 0.06 part of benzoyl peroxide, add mixed single still, stir obtained mix monomer.
(2) taking 0.02 part of benzoyl peroxide, 14 parts of mixed lists and 14 parts of ethyl acetate adds in reactor, stirs after being warming up to 70 DEG C, clock reaction 2h.
(3) in the mixed list of residue 16 parts, 24 parts of ethyl acetate are added, obtained dropping liquid after stirring.
(4), after reactor clock reaction 2h, drip the dropping liquid in step (3), 3h drips off.In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C.
(5) rear 80 DEG C of isothermal reaction 2h are dripped off.
(6) by after still temperature drop to 60 DEG C, add 32 parts of ethyl acetate, discharging after stirring, obtain the component A of solvent-type acrylic ester pressure-sensitive.
Composition B is the aziridine system linking agent of three-functionality-degree.
ASA section bar surface protective film is preparation method comprise the steps:
Taking 40 ㎏ composition A in joining in glue bucket, starting stirring, in the container taking 200g composition B, adding 800g ethyl acetate, stir with glass stick, the composition B diluted slowly is added in A, continue stirring 15 minutes.Coat on base material by the pressure sensitive adhesive prepared, being coated with dry glue amount is 5 ± 1g/m
2.
Protective membrane performance: initial bonding strength (5
#steel ball); Stripping strength (0.2N/25mm); Wet and heat ageing resistant performance (72h does not fall glue, without fleck).
Embodiment 4
Solvent-type acrylic ester pressure-sensitive of the present invention is made up of composition A and composition B;
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is by weight:
Isooctyl acrylate monomer 29.5 parts, 0.22 part, vinylformic acid, dimethacrylate TEG ester 0.08 part, benzoyl peroxide 0.2 part, ethyl acetate 70 parts.
The concrete preparation process of composition A is.
(1) take whole Isooctyl acrylate monomer, vinylformic acid, dimethacrylate TEG ester and 0.18 part of benzoyl peroxide, add mixed single still, stir obtained mix monomer.
(2) taking 0.02 part of benzoyl peroxide, 14 parts of mixed lists and 14 parts of ethyl acetate adds in reactor, stirs after being warming up to 70 DEG C, clock reaction 2h.
(3) in the mixed list of residue 16 parts, 26 parts of ethyl acetate are added, obtained dropping liquid after stirring.
(4), after reactor clock reaction 2h, drip the dropping liquid in step (3), 3h drips off.In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C.
(5) rear 80 DEG C of isothermal reaction 2h are dripped off.
(6) by after still temperature drop to 60 DEG C, add 30 parts of ethyl acetate, discharging after stirring, obtain the component A of solvent-type acrylic ester pressure-sensitive.
Composition B is the aziridine system linking agent of three-functionality-degree.
ASA section bar surface protective film is preparation method comprise the steps:
Taking 40 ㎏ composition A in joining in glue bucket, starting stirring, in the container taking 160g composition B, adding 640g ethyl acetate, stir with glass stick, the composition B diluted slowly is added in A, continue stirring 15 minutes.Coat on base material by the pressure sensitive adhesive prepared, being coated with dry glue amount is 5 ± 1g/m
2.
Protective membrane performance: initial bonding strength (4
#steel ball); Stripping strength (0.15N/25mm); Wet and heat ageing resistant performance (72h does not fall glue, without fleck).
Embodiment 5
Solvent-type acrylic ester pressure-sensitive of the present invention is made up of composition A and composition B;
Composition A is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is by weight:
Isooctyl acrylate monomer 29 parts, 0.6 part, vinylformic acid, allyl methacrylate(AMA) 0.2 part, benzoyl peroxide 0.2 part, ethyl acetate 70 parts.
The concrete preparation process of composition A is.
(1) take whole Isooctyl acrylate monomer, vinylformic acid, allyl methacrylate(AMA) and 0.18 part of benzoyl peroxide, add mixed single still, stir obtained mix monomer.
(2) taking 0.02 part of benzoyl peroxide, 15 parts of mixed lists and 15 parts of ethyl acetate adds in reactor, stirs after being warming up to 70 DEG C, clock reaction 2h.
(3) in the mixed list of residue 15 parts, 20 parts of ethyl acetate are added, obtained dropping liquid after stirring.
(4), after reactor clock reaction 2h, drip the dropping liquid in step (3), 3.5h drips off.In dropping process, controlling temperature in reactor is 78 DEG C ~ 82 DEG C.
(5) rear 80 DEG C of isothermal reaction 2h are dripped off.
(6) by after still temperature drop to 60 DEG C, add 35 parts of ethyl acetate, discharging after stirring, obtain the component A of solvent-type acrylic ester pressure-sensitive.
Composition B is the aziridine system linking agent of three-functionality-degree.
ASA section bar surface protective film is preparation method comprise the steps:
Taking 40 ㎏ composition A in joining in glue bucket, starting stirring, in the container taking 240g composition B, adding 960g ethyl acetate, stir with glass stick, the composition B diluted slowly is added in A, continue stirring 15 minutes.Coat on base material by the pressure sensitive adhesive prepared, being coated with dry glue amount is 5 ± 1g/m
2.
Protective membrane performance: initial bonding strength (3
#steel ball); Stripping strength (0.15N/25mm); Wet and heat ageing resistant performance (72h does not fall glue, without fleck).
Claims (5)
1. a preparation method for solvent-type acrylic ester pressure-sensitive, is characterized in that: solvent-type acrylic ester pressure-sensitive comprises composition A and composition B, and composition A comprises (methyl) acrylate polymers; Composition B is polyfunctionality aziridine system linking agent, and consumption is 0.2 ~ 0.6% of composition A quality;
Described composition A causes copolymerization by following component raw material through benzoyl peroxide and obtains, and its composition and ratio is as follows by weight: Isooctyl acrylate monomer 28.8 ~ 29.6 parts, 0.2 ~ 1 part, vinylformic acid, (methyl) acrylate 0.06 ~ 0.2 part containing two double bonds, benzoyl peroxide 0.08 ~ 0.2 part, ethyl acetate 70 parts;
The preparation of described composition A comprises following operation, and the ratio of the following stated is all weight percentage:
(1) take 75 ~ 95% of Isooctyl acrylate monomer, vinylformic acid, (methyl) acrylate containing two double bonds and benzoyl peroxide total amount, add mixed single still, stir obtained mix monomer;
(2) by residue benzoyl peroxide, 40 ~ 60% of mix monomer total amount and 20 ~ 40% of ethyl acetate total amount add in reactor, stir be warming up to 60 ~ 70 DEG C after, clock reaction 1.5 ~ 2h;
(3) in residue mix monomer, ethyl acetate total amount 30 ~ 50% is added, obtained dropping liquid after stirring;
(4) in reactor, drip the dropping liquid in step (3), 3 ~ 4h drips off, and during dropping, controlling temperature in reactor is 78 DEG C ~ 82 DEG C;
(5) rear 80 DEG C ~ 90 DEG C isothermal reaction 2 ~ 3h are dripped off;
(6) by after still temperature drop to 60 DEG C, add remaining ethyl acetate, discharging after stirring, obtain solvent-type acrylic ester pressure-sensitive composition A.
2. the preparation method of solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterized in that: described (methyl) acrylate containing two double bonds is one or more in Ethylene glycol dimethacrylate, TEGDMA, dimethacrylate TEG ester, 1,6 hexanediol diacrylate, allyl methacrylate(AMA).
3. the preparation method of solvent-type acrylic ester pressure-sensitive according to claim 1, is characterized in that: described composition B is the aziridine system linking agent of three-functionality-degree.
4. a compound method for the solvent-type acrylic ester pressure-sensitive described in claim 1 or 2, is characterized in that: comprise the steps:
(1) take quality be the composition A of 100 parts in joining in glue bucket, start stirring;
(2) the composition B taking respective quality on request, in container, adds the ethyl acetate of 4 times of composition B quality, stirs;
(3) the composition B diluted slowly is added in composition A, continue stirring 15 minutes.
5. the application of a solvent-type acrylic ester pressure-sensitive according to claim 1 in ASA section bar surface protective film.
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| CN201210312005.9A CN103205226B (en) | 2012-08-29 | 2012-08-29 | Solvent type acrylate pressure-sensitive adhesive, and preparation method and application thereof |
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|---|---|---|---|
| CN201210312005.9A CN103205226B (en) | 2012-08-29 | 2012-08-29 | Solvent type acrylate pressure-sensitive adhesive, and preparation method and application thereof |
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| CN103205226A CN103205226A (en) | 2013-07-17 |
| CN103205226B true CN103205226B (en) | 2014-12-24 |
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| CN105946304A (en) * | 2016-06-17 | 2016-09-21 | 东莞市纳利光学材料有限公司 | Fully-laminated tempered glass protective film and preparation method thereof |
| CN106117416B (en) * | 2016-07-15 | 2017-11-28 | 上海英诺威新材料科技有限公司 | The preparation method of acrylate adhesive and its application in low viscous diaphragm |
| CN107201200A (en) * | 2017-06-23 | 2017-09-26 | 无锡海特新材料研究院有限公司 | A kind of low peel strength diaphragms of low VOC are with without vaporific residual acrylic acid ester pressure-sensitive, its preparation method and its application |
| CN107502214A (en) * | 2017-09-01 | 2017-12-22 | 泾县麦蓝网络技术服务有限公司 | A kind of gas permeability automobile black film and preparation method thereof |
| CN108384491A (en) * | 2018-03-16 | 2018-08-10 | 华南理工大学 | A kind of heat-resistant pressure-sensitive adhesives, heat-resistant pressure-sensitive adhesives band and preparation method thereof |
| CN108659749A (en) * | 2018-06-22 | 2018-10-16 | 西安航天三沃化学有限公司 | A kind of solvent-type acrylic pressure sensitive adhesive and preparation method thereof |
| CN112175543A (en) * | 2020-09-30 | 2021-01-05 | 广东安利华新材料科技有限公司 | Pressure-sensitive adhesive tape applied to connection of aluminum foil coiled materials in lithium battery production and preparation method of pressure-sensitive adhesive tape |
| CN114921199A (en) * | 2022-06-07 | 2022-08-19 | 东莞市胜昊新材料科技有限公司 | Solvent type high-stripping-force high-temperature-resistant high-humidity-resistant glue and preparation method thereof |
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| CN102127183A (en) * | 2010-01-20 | 2011-07-20 | 3M创新有限公司 | Crosslinkable acrylate adhesive polymer composite |
| CN102220098A (en) * | 2011-04-13 | 2011-10-19 | 高建宾 | Anti-ultraviolet laminating adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7652103B2 (en) * | 2008-02-14 | 2010-01-26 | 3M Innovative Properties Company | Acrylic pressure-sensitive adhesives with aziridine crosslinking agents |
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|---|---|---|---|---|
| CN102127183A (en) * | 2010-01-20 | 2011-07-20 | 3M创新有限公司 | Crosslinkable acrylate adhesive polymer composite |
| CN102260472A (en) * | 2010-12-14 | 2011-11-30 | 上海凯鑫森产业投资控股有限公司 | High-strength repeelable pressure-sensitive adhesive for window film and preparation method thereof |
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