CN101372607A - Emulsion pressure-sensitive adhesive for soft PVC electric adhesive tape and preparation thereof - Google Patents
Emulsion pressure-sensitive adhesive for soft PVC electric adhesive tape and preparation thereof Download PDFInfo
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- CN101372607A CN101372607A CNA2007101656501A CN200710165650A CN101372607A CN 101372607 A CN101372607 A CN 101372607A CN A2007101656501 A CNA2007101656501 A CN A2007101656501A CN 200710165650 A CN200710165650 A CN 200710165650A CN 101372607 A CN101372607 A CN 101372607A
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Abstract
The invention relates to emulsion pressure-sensitive adhesive which has better plasticizer transport resistance and is applied to the manufacturing of soft polyvinyl chloride (SPVC) electric gluing belt. The emulsion pressure-sensitive adhesive is made by co-mixing specially synthesized acrylate copolymer emulsion and other resin emulsion and/or rubber latex. Special soft monomers and special functional monomers are adopted in the acrylate copolymer emulsion synthesis formulation. And a Core-Shell emulsion copolymerization method is adopted in the acrylate copolymer emulsion synthesis technology.
Description
Technical field the present invention relates to a kind of emulsion pressure-sensitive adhesive and manufacture method thereof.Specifically, the present invention relates to a kind ofly have plasticizer-resistant migration performance preferably, thereby be applicable to and be coated on the emulsion pressure-sensitive adhesive and the manufacture method thereof of making electric adhesive tape on the flexible PVC film substrate that contains a large amount of softening agent.
Technical background is that the electric pressure-sensitive adhesive tape of base material has advantages such as good mechanical property (especially snappiness and stretchiness), flame retardant properties, electrical insulation capability, heat-resistant deforming performance and processed and applied performance with flexible PVC (SPVC) film, thereby the insulation that is widely used in various electric elements and electric wire in fields such as automobile, machinofacture, instrument and household electrical appliances coats and ties up.Flexible PVC (SPVC) electric adhesive tape is a class bigger in the Pressuresensitive Tape goods.
At present, industrial SPVC adhesive tape product is all coated drying on the flexible PVC film substrate, rolling and is divided with solvent-borne type rubber pressure sensitive adhesive and cuts into.The organic solvent (being generally toluene) that contains a large amount of (about 70%) in the used rubber pressure sensitive adhesive.These organic solvents evaporate into and not only cause the wasting of resources in the air in process of production, more can cause the serious environmental pollution, and the organic solvent of denier can be difficult to remain in the glue-line of sealing tape product with avoiding, pollutes environment for use thereby also can slowly release in the sealing tape use.Therefore, industrial extremely stand-byly a kind ofly do not have or seldom have the pressure sensitive adhesive of environmental pollution to replace the serious solvent-borne type rubber pressure sensitive adhesive of environmental pollution to make the SPVC electric adhesive tape.
Emulsion pressure-sensitive, especially the acrylic ester emulsion pressure sensitive adhesive is generally use in the industry of pressure sensitive adhesive goods a kind of with the pressure-sensitive adhesive of water as medium, essentially no environmental pollution, uses in a large number in some important pressure sensitive adhesive goods fields such as packing sealing tape, pressure sensitive adhesive label.
Contain a large amount of simple plasticizers in the flexible PVC film substrate, as dioctyl phthalate (DOP) (DOP), dibutyl phthalate (DBP) and TRI N BUTYL PHOSPHATE (TBP) etc.In sealing tape product stock and use, these monomerics in the base material can move to pressure-sensitive adhesive layer gradually, and at the interface of base material and glue-line and the inside of glue-line assemble, the performance that may make sealing tape especially 180 ° of stripping strengths obviously descends, even can produce serious quality problems such as " coming unstuck " and can't use at all.Pressure sensitive adhesive is referred to as the plasticizer-resistant migration performance of pressure sensitive adhesive by industry to the sensitivity of softening agent diffusive migration in the base material.The pressure sensitive adhesive that is used to make the SPVC electric adhesive tape must have plasticizer-resistant migration performance preferably, and promptly migration of plasticizer can not cause that the performance of sealing tape produces very big deterioration.
But the plasticizer-resistant migration performance of at present industrial ACRYLIC EMULSION pressure sensitive adhesive commonly used is more far short of what is expected than solvent-borne type rubber pressure sensitive adhesive, can't be used for making the SPVC electric adhesive tape.Here it is why present industrial manufacturing SPVC electric adhesive tape also nearly all can only the with serious pollution solvent-borne type rubber of environment for use pressure-sensitive adhesive reason.
Summary of the invention the invention provides a kind of new emulsion pressure-sensitive adhesive and manufacture method thereof.This emulsion pressure-sensitive has plasticizer-resistant migration performance preferably, is applicable to make various flexible PVCs (SPVC) electric adhesive tape.That is to say, this new emulsion pressure-sensitive is coated the SPVC electric adhesive tape of making on the SPVC film substrate, in storage and use or behind 60～80 ℃ high bake, though the softening agent that base material has taken place is to the glue-line diffusive migration, but the performance that can't cause sealing tape produces very big deterioration, thereby sealing tape still can keep good performance, satisfies its service requirements fully.That is to say that the invention provides a kind of is the emulsion pressure-sensitive of medium, basic non-environmental-pollution with water, can replace at present industrial generally use but the serious solvent-borne type rubber pressure sensitive adhesive of environmental pollution is used to make the SPVC electric adhesive tape.
This new emulsion pressure-sensitive adhesive that the present invention relates to also as present industrial general acrylic ester emulsion pressure sensitive adhesive, is that medium carries out letex polymerization and makes with water by acrylate soft monomer, function monomer and other vinyl monomer.But because the present invention (1) has also adopted special soft monomer and special function monomer in the monomer prescription of letex polymerization; (2) special polymerization processs such as nuclear-shell (Core-Shell) polymerization in emulsion polymerization technique, have also been adopted; (3) after making acrylate copolymer emulsion, also adopt with the method for other resin emulsion and/or rubber latex co-blended and carry out technical measures such as modification, so the emulsion pressure-sensitive adhesive that the present invention makes has not only reached the traditional performance index of SPVC electric adhesive tape with pressure sensitive adhesive, also has plasticizer-resistant migration performance preferably.The SPVC electric adhesive tape goods that make with these emulsion pressure-sensitives store and use in or after 60～80 ℃ are toasted slaking, though softening agent has taken place from the diffusive migration of SPVC base material to interface and pressure-sensitive adhesive layer, the performance that also can not cause sealing tape especially 180 ° of stripping strengths changes a lot, serious quality problems such as " coming unstuck " more can not occur, can satisfy the service requirements of sealing tape fully.
The present invention is in the monomer prescription of letex polymerization, except present acrylic ester emulsion pressure sensitive adhesive butyl acrylate (BA) commonly used, Isooctyl acrylate monomer soft monomers such as (2-EHA), vinylformic acid n-octyl (n-OA), dibutyl maleate (DBM), dioctyl maleate (DOM) and vinylformic acid norborneol ester special soft monomers such as (IBOA) have also been adopted, amount ranges is 1-50 (wt.) % of monomer total amount, and the optimum amount scope is 10-30 (wt.) % of monomer total amount.In the monomer prescription except vinylformic acid (AA) commonly used, Hydroxyethyl acrylate (HEA), Propylene glycol monoacrylate (HPA), methacrylic acid function monomers such as (MAA), also adopted Methacrylamide (AM), N-n-methylolacrylamide (N-MAM), N-butoxy acrylamide (N-BAM), β-CEA (
, n=0～3) etc. the specific function monomer, amount ranges is 0～5 (wt.) % of monomer total amount, the optimum amount scope is 0.5～3.0 (wt.) % of monomer total amount.
Owing in the monomer prescription of letex polymerization, adopted above-mentioned special soft monomer and special function monomer, make softening agent commonly used such as the glue-line of the emulsion pressure-sensitive that the present invention makes and dioctyl phthalate (DOP) (DOP) that consistency preferably be arranged, can absorb and contain most of softening agent that diffusive migration is come from the SPVC base material, softening agent can not gathered on the interface of base material and glue-line in a large number, and glue-line can not make its performance that bigger decline be arranged because of having absorbed more softening agent yet.
The present invention except using semi-continuous polymerzation technology commonly used in present acrylic ester emulsion pressure sensitive adhesive synthesis technique, has also adopted special emulsion polymerisation process such as nuclear-shell (Core-Shell) emulsion copolymerization in emulsion polymerization technique.This is the emulsion polymerisation process that carries out in a kind of branch two stages; In reactor, a part of monomer mixture (prescription A) is carried out letex polymerization earlier, make the less polymer emulsion of latex particle (being called " nuclear " emulsion), again all the other monomer mixtures (prescription B) are added reactor and carry out the letex polymerization of subordinate phase, form one deck " shell " emulsion polymer in " nuclear " emulsion particle outside, thus the special emulsion polymer that makes emulsion particle and have " nuclear-shell " structure.Because prescription A and prescription B difference are bigger, therefore " nuclear " strata compound that makes and " shell " strata compound have on performance than big difference, and for example the stratum nucleare polymkeric substance firmly and the shell polymkeric substance is softer or opposite or the like.Facts have proved that the emulsion pressure-sensitive that this emulsion particle has " nuclear-shell " structure has better plasticizer-resistant migration performance than the emulsion pressure-sensitive of traditional even structure.
In order further to improve plasticizer-resistant migration performance and other performance of emulsion pressure-sensitive, the present invention makes after the acrylate copolymer emulsion with above-mentioned monomer prescription and emulsion polymerization technique, also use the blend with it of other resin emulsion and/or rubber latex, make final required emulsion pressure-sensitive.Other resin emulsion that can be used for blend has: polyvinyl acetate emulsion, polystyrene emulsion, vinyl acetate-ethylene copolymerization emulsions, ethyl propenoate-ethylene copolymerization emulsions etc., its amount ranges is 5～40 (wt.) % of acrylate copolymer emulsion, and the optimum amount scope is 10～30 (wt.) % of acrylate copolymer emulsion.The rubber latex that can be used for blend has: styrene butadiene rubber latex, natural rubber latex, paracril latex, chloroprene rubber latex etc., its amount ranges is 0～30 (wt.) % of acrylate copolymer emulsion, and the optimum amount scope is 5～20 (wt.) % of acrylate copolymer emulsion.
As seen, the manufacture method of emulsion pressure-sensitive of the present invention comprises: (a) with the method acrylic acid synthesizing ester copolymer emulsion of nuclear-shell emulsion copolymerization and (b) above-mentioned copolymer emulsion and other resin emulsion and/or rubber latex co-blended are mixed with two concrete steps such as emulsion pressure-sensitive.
Narration specific embodiments more of the present invention below the specific implementation method, but the present invention is not limited to these embodiment.
Embodiment 1 acrylate copolymer emulsion synthetic 1. with total monomer prescription [Isooctyl acrylate monomer (2-EHA) 20g, butyl acrylate (BA) 50g, dibutyl maleate (DBM) 60g, methyl methacrylate (MMA) 50g, Hydroxyethyl acrylate (HEA) 7.5g, vinylformic acid (AA) 4.5g, N hydroxymethyl acrylamide (N-MAM) 8.0g] be divided into A, B two components are mixed respectively and make pre-emulsion.Wherein, the composition of component A is: BA 50g, MMA 50g, HEA4.5g, AA 2.8g, N-MAM 8.0g; The composition of B component is: 2-HEA 20g, DBM 60g, HEA 3.0g, AA 1.7g.
2. in three mouthfuls of round-bottomed flasks of 1000ml, add deionized water 160g, buffer reagent sodium bicarbonate 2.6g, emulsifying agent Co-436 (product of a kind of Rhodia Inc.) 0.78g, the post-heating that stirs heats up.Treat that temperature rises to the aqueous solution that adds initiator ammonium persulfate 0.40g after 78 ℃.Holding temperature at the uniform velocity adds the emulsion copolymerization that the monomeric pre-emulsion of component A carries out the fs at 82-84 ℃ then, 1.5h add, continue after adding to maintain and at the uniform velocity add the monomeric pre-emulsion of B component in this temperature range, carry out the emulsion copolymerization of subordinate phase, 2.5h adds.
3. maintain 83-85 ℃ and continue stirring reaction 1.0h.The cooled and filtered discharging promptly obtains can be used for the acrylate copolymer emulsion of the emulsion pressure-sensitive of further preparation cost invention.
The normal temperature that is formulated in of emulsion pressure-sensitive constantly stirs down, commercially available polyvinyl acetate emulsion 45g joined in the above-mentioned synthetic acrylate copolymer emulsion of 300g mix with it, regulate pH value with ammoniacal liquor again and be 7-8, the emulsion pressure-sensitive that gets final product requiredly, its solids content is 53%.
Performance test is coated the emulsion pressure-sensitive of gained and is made the electric pressure-sensitive adhesive tape rouleau that drying adhesive layer thickness is 20um on the thick flexible PVC of 0.15mm (SPVC) film substrate.The various performances of sealing tape are tested in slaking after 8 hours in 70 ℃ of environment: 180 ° of stripping strengths of pressing CNS GB/T2792-1998 test tape; Press the initial cohesiveness of CNS GB/T4852-1984 test tape; Press the low speed uncoiling intensity of CNS GB/T 4850-1984 test tape; Hold the viscosity energy by CNS GB/T4851-1998 test tape.With the ratio of corresponding numerical value before 180 ° of peel strength value of sealing tape behind 70 ℃ of slaking 8h and the slaking, be defined as the plasticizer-resistant migration performance of the used pressure sensitive adhesive of this sealing tape, with percentage ratio (%) expression.Make the test result of the above-mentioned performance of SPVC electric adhesive tape goods with the emulsion pressure-sensitive of embodiment 1 gained and list in table 1.
The composition of embodiment 2 monomer prescription: component A is: BA 30g, and VAc 69g, HEA 6.0g, AA 4.0g, the composition of B component is: 2-HEA 123g, DOM 60g, HEA 3.0g, AA 0.5g, Cops-1 4.5g.Other resin emulsion of blend is commercially available ethene-vinyl acetate (EVA) copolymer emulsion 45g, and the rubber latex of blend is natural rubber latex 30g.All the other are all with embodiment 1.Make the Pressuresensitive Tape rouleau and test its performance with embodiment 1 identical method, the results are shown in table 1.
The composition of embodiment 3 monomer prescription: component A is BA 50g, MMA 50g, HEA 4.5g, AA 2.8g, N-MAM4.5g; The composition of B component is 2-HEA 121g, DOM 60g, HEA 3.5g, MMA 1.5g, Cops-1 3.2g.Other resin emulsion of blend be commercially available ethene-vinyl acetate (EVA) copolymer emulsion 75g. all the other all with embodiment 1.Make pressure-sensitive adhesive tape rouleau and test performance with embodiment 1 identical method, the results are shown in table 1.
Comparative example 1 monomer prescription is identical with total prescription of embodiment 1, but and without separating into A, B two portions.Do not adopt the method for nuclear-shell polymerization (polymerization of two stages) during letex polymerization and only adopt general semi-continuous polymerzation technology in the present acrylic ester emulsion pressure sensitive adhesive synthesis technique.All the other are all with embodiment 1.Make SPVC adhesive tape rouleau and test performance with embodiment 1 identical method, the result also is listed as in the table 1.
Comparative example 2 usefulness and embodiment 1 identical method acrylic acid synthesizing ester copolymer emulsion, but no longer adopt any other resin emulsion and rubber latex co-blended with it, but, make the identical Pressuresensitive Tape rouleau of specification with directly coating the SPVC film substrate behind the ammoniacal liquor adjusting pH value as emulsion pressure-sensitive.With the identical method test performance of embodiment 1, the result also lists in table 1.
Comparative example 3 is applied to the SPVC film substrate with the commercially available present industrial acrylic ester emulsion pressure sensitive adhesive that generally is used to make BOPP (Biaxially oriented polypropylene film (BOPP)) packing sealing tape, make pressure-sensitive adhesive tape rouleau with embodiment 1 same size, and test performance, the result also tabulates in 1.
The performance data of the various emulsion pressure-sensitives of table 1
From the performance data of table 1 as can be seen: embodiment 1 compares with comparative example 1, and in the acrylate copolymer emulsion building-up process, if adopt the synthetic process of nuclear-shell polymerization, the plasticizer-resistant migration performance of gained emulsion pressure-sensitive increases; Embodiment 1 compares with comparative example 2, adopts the method with other resin emulsion and/or rubber latex blend, can significantly improve the plasticizer-resistant migration performance of acrylic ester emulsion pressure sensitive adhesive; At the industrial acrylic ester emulsion pressure sensitive adhesive of making BOPP packing sealing tape that is common to, its plasticizer-resistant migration performance extreme difference is seen comparative example 3 at present.Therefore, have only the method for the present invention of employing, could synthesize and make the emulsion pressure-sensitive adhesive that the plasticizer-resistant migration performance is better, be applicable to manufacturing SPVC electric adhesive tape.
Claims (5)
1. one kind has better plasticizer-resistant migration performance thereby is applicable to the emulsion pressure-sensitive adhesive and the manufacture method thereof of making flexible PVC (SPVC) electric adhesive tape, it is characterized in that:
(a) make by a kind of special synthetic acrylate copolymer emulsion and other resin emulsion and/or rubber latex blend;
(b) some special soft monomer and special function monomer in the synthesizing formula of this acrylate copolymer emulsion, have been adopted;
(c) in the synthesis technique of this acrylate copolymer emulsion, also adopted the method for nuclear-shell emulsion polymerization.
2. other resin emulsion as claimed in claim 1 has: polyvinyl acetate emulsion, polystyrene emulsion, vinyl acetate between to for plastic ethylene copolymerization emulsions, ethyl propenoate-ethylene copolymerization emulsions etc., amount ranges is 5～40 (wt.) % of acrylate copolymer emulsion, and the optimum amount scope is 10～30 (wt.) % of acrylate copolymer emulsion.
3. rubber latex as claimed in claim 1 has: styrene butadiene rubber latex, natural rubber latex, paracril latex, chloroprene rubber latex etc., amount ranges is 0～30 (wt.) % of acrylate copolymer emulsion, and the optimum amount scope is 5～20 (wt.) % of acrylate copolymer emulsion.
4. special soft monomer as claimed in claim 1 has: vinylformic acid n-octyl, dibutyl maleate, dioctyl maleate, vinylformic acid norborneol ester etc., amount ranges is 1～50 (wt.) % of monomer total amount, and the optimum amount scope is 10～30 (wt.) % of monomer total amount.
5. specific function monomer as claimed in claim 1 has: Methacrylamide, N hydroxymethyl acrylamide, N-butoxy acrylamide, β-CEA etc., amount ranges is 0～5 (wt.) % of monomer total amount, and the optimum amount scope is 0.5～3.0 (wt.) % of monomer total amount.
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| CN103045133A (en) * | 2012-12-26 | 2013-04-17 | 青岛文创科技有限公司 | Preparation method of terpene resin-containing acrylate pressure-sensitive adhesive |
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| JP2017114958A (en) * | 2015-12-22 | 2017-06-29 | 株式会社大阪ソーダ | Acrylic rubber and rubber crosslinked article thereof |
| CN107696727A (en) * | 2017-09-19 | 2018-02-16 | 南京金陵金箔集团股份有限公司 | A kind of production technology for being packed for 3D stereo metal texture bracing wires |
| WO2018165827A1 (en) * | 2017-03-13 | 2018-09-20 | Dow Global Technologies Llc | Water-based pressure sensitive adhesive compositions and methods of making same |
| CN109705753A (en) * | 2018-11-30 | 2019-05-03 | 万洲胶粘制品(江苏)有限公司 | A kind of flexible PVC electrical adhesive tape and its processing method |
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| CN112126389A (en) * | 2020-09-28 | 2020-12-25 | 杭州英创新材料有限公司 | Plasticizer migration resistant aqueous pressure-sensitive adhesive and preparation method thereof |
| CN112724323A (en) * | 2020-12-22 | 2021-04-30 | 安徽明讯新材料科技股份有限公司 | Core-crosslinked core-shell acrylate pressure-sensitive adhesive emulsion and preparation method thereof |
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| KR100418310B1 (en) * | 1995-02-16 | 2005-05-31 | 미네소타 마이닝 앤드 매뉴팩춰링 캄파니 | Articles containing pressure sensitive adhesives with improved adhesion to plasticized polyvinyl chloride |
| DE10259618A1 (en) * | 2002-12-18 | 2004-07-08 | Tesa Ag | Adhesive tape for protecting, labeling, isolating and wrapping |
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| JP2017114958A (en) * | 2015-12-22 | 2017-06-29 | 株式会社大阪ソーダ | Acrylic rubber and rubber crosslinked article thereof |
| EP3916064A1 (en) | 2016-02-03 | 2021-12-01 | Hebei Yongle Tape Co., Ltd. | Uv-crosslinked hot-melt pressure-sensitive adhesive used for polyvinyl-chloride insulated adhesive tape |
| CN106118524A (en) * | 2016-06-24 | 2016-11-16 | 合肥得润电子器件有限公司 | The micropore radiating insulating binder that a kind of waterproof mildew-resistant strengthens |
| CN110582548A (en) * | 2017-03-13 | 2019-12-17 | 陶氏环球技术有限责任公司 | Water-based pressure-sensitive adhesive composition and method for producing the same |
| WO2018165827A1 (en) * | 2017-03-13 | 2018-09-20 | Dow Global Technologies Llc | Water-based pressure sensitive adhesive compositions and methods of making same |
| CN107696727A (en) * | 2017-09-19 | 2018-02-16 | 南京金陵金箔集团股份有限公司 | A kind of production technology for being packed for 3D stereo metal texture bracing wires |
| CN109705753A (en) * | 2018-11-30 | 2019-05-03 | 万洲胶粘制品(江苏)有限公司 | A kind of flexible PVC electrical adhesive tape and its processing method |
| CN109762486A (en) * | 2018-11-30 | 2019-05-17 | 万洲胶粘制品(江苏)有限公司 | A kind of pressure-sensitive adhesive making flexible PVC electrical adhesive tape and its processing method |
| CN112126389A (en) * | 2020-09-28 | 2020-12-25 | 杭州英创新材料有限公司 | Plasticizer migration resistant aqueous pressure-sensitive adhesive and preparation method thereof |
| CN112724323A (en) * | 2020-12-22 | 2021-04-30 | 安徽明讯新材料科技股份有限公司 | Core-crosslinked core-shell acrylate pressure-sensitive adhesive emulsion and preparation method thereof |
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Effective date of registration: 20170327 Address after: 072750 Baoding City, Zhuozhou Province Development Zone Industrial Park, Yan Yi Road, No. 9, No. Patentee after: Hebei Yongle adhesive tape Co., Ltd. Address before: 072750 Zhuozhou Yongle Road, Hebei, No. 88 Patentee before: Hebei Huaxia Enterprise Co., Ltd. |
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