CN102399501B - Re-stripping type adhesive piece - Google Patents
Re-stripping type adhesive piece Download PDFInfo
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- CN102399501B CN102399501B CN201110196597.8A CN201110196597A CN102399501B CN 102399501 B CN102399501 B CN 102399501B CN 201110196597 A CN201110196597 A CN 201110196597A CN 102399501 B CN102399501 B CN 102399501B
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Abstract
The invention provides a re-stripping type adhesive sheet which can be easily detached and removed in a regenerating process and easily peeled by a hand and applied for attaching a label. The re-stripping type adhesive sheet which is formed by pressing stripping sheets, an adhesive layer and a surface substrate layer in a layered way is characterized in that the adhesive layer is formed by water dispersion adhesive compounds having aqueous latex and cross-linking agents. The aqueous latex comprises an acrylic acid series copolymer and adhesive granting agents. The monomer components forming the acrylic acid series copolymer include 2-ethylhexyl acrylate, acrylonitrite and unsaturated vinyl monomer having carboxyl. The contents of the 2-ethylhexyl acrylate and the acrylonitrite respectively occupy more than 90 weight% and 0.5-5 weigh% of the monomer constitution. The gel rate of the adhesive layer is 40-80 weight%.
Description
Technical field
The present invention relates to the releasable adhesive sheet of the adhesive label on the surface that can be used for pasting such as polyethylene terephthalate bottle (being sometimes designated as PET bottle below) etc., more particularly, in particular to when recycling PET bottle, the adhesive label releasable adhesive sheet of overburden operation easily can be carried out.
Background technology
Releasable adhesive sheet or adhesion label, have can by paste adherend label after certain hour easily from the function that adherend is peeled off, can be used for as the Management label in many price tag, the commodity logistics progress such as food, groceries of such as price transformation or index tab, waited by printing and record essential information, in the purposes can peeled off when the object of communicating information etc. no longer needs etc. (such as patent documentation 1,2).
In patent documentation 1 and 2, be used in the acrylic acid polymer with carboxyl the tackiness agent having coordinated adhesion imparting agent and many glycidyl compound.
On the other hand, as the adhesive label with described such adhesive label different field, the adhesive label of known various beverage bottle.
As the container of tap water, refreshment drink, fruit juice, tea, black tea, pure mellow wine, liquor etc., widely use PET bottle.For this PET bottle, in recent years, from the viewpoint of environment protection, the requirement of recycling significantly improves.PET bottle nearly all being pasted the adhesive label being used for display of commodity name or content etc., when recycling PET bottle, needing to peel off removing by the regeneration process of this adhesive label in manipulation of regeneration equipment (hot-water cure etc.).In addition, in order to effectively carry out manipulation of regeneration, wishing before waste PET bottle, by each family, adhesive label being peeled off.Therefore, described adhesive label requires to have to the adhibit quality of PET bottle and the good characteristic of paste operation, require to have until before the content of PET bottle consumed simultaneously, with bottle good adhesion paste and be not easy to peel off, but the contrary characteristic can peeled off simply again after content has been consumed.
In addition, adhesive label being adhered to after on empty bottle, when filling content, washing in bottle with water or weakly alkaline washings etc. before filling content.In this washing process, need adhesive label not peel off, and keep the state of stickup.
As the tackiness agent of such adhesive label, in the last few years, in sanitary viewpoint, do not use the purpose of the water dispersible tackiness agent of solvent strong, carry out various research.
Such as in patent documentation 3, disclose the label that adhesive sheet that the tackiness agent that is made up of the polymer layer with alkali-solubility formed is used as bottle class, but need to improve in the balance of tackiness and releasable.
In addition, in patent documentation 4, disclose a kind of label, it is characterized in that, this label contains emulsion type adhesive and the linking agent of alkali-soluble acrylic, relative to the emulsion type adhesive of alkali-soluble acrylic described in 100 weight parts, adds the linking agent of 1-3 weight part.But, peeled off by hand, label releasable or hot water separability insufficient.
Further, in patent documentation 5, propose by use using ethyl acrylate as main monomer component and and used the acrylic copolymer of nitrogenous vinyl monomer as adhesion resin, achieve the suitable tackiness of tackiness agent and good releasable, but need to design the tackiness agent that just can obtain the balance with water tolerance, tackiness and releasable to collocation composition further.
[at first technical literature]
[patent documentation]
[patent documentation 1] Unexamined Patent 8-183935 publication
[patent documentation 2] Unexamined Patent 8-225774 publication
[patent documentation 3] Unexamined Patent 7-82537 publication
[patent documentation 4] JP 2003-098969 publication
[patent documentation 5] JP 2008-239872 publication
Summary of the invention
The present invention carries out based on such situation, the object of the present invention is to provide adhesive label releasable adhesive sheet, by this adhesive label releasable adhesive sheet process adhesive label to the adhibit quality of bottle and paste operation good, after adhesive label is pasted simultaneously, until before the content of bottle consumed, be difficult to peel off from bottle, and after the content of bottle has been consumed, simply removing can be peeled off in regeneration process in manipulation of regeneration equipment, further, can easily peel off with hand.
To achieve these goals, the present inventor is through repeatedly furtheing investigate, found that: by stripping film, adhering agent layer, in the releasable adhesive sheet of the structure of surface substrate lamination, containing water-based emulsion and linking agent in described adhering agent layer, described water-based emulsion contains acrylic copolymer and adhesion imparting agent, the monomer component forming described acrylic copolymer comprises the combination of specific kind and content, and use the gel fraction of adhering agent layer at the water dispersible adhesion agent composition of specified range, thus, can solve the problem, thus complete the present invention.
That is, the invention provides:
(1) a kind of releasable adhesive sheet, it is characterized in that, by stripping film, adhering agent layer, in the releasable adhesive sheet of surface substrate lamination, described adhering agent layer is formed by the water dispersible adhesion agent composition containing water-based emulsion and linking agent, described water-based emulsion contains acrylic copolymer and adhesion imparting agent, the monomer component forming described acrylic copolymer comprises ethyl acrylate, vinyl cyanide and there is the unsaturated vinyl monomer of carboxyl, the content of described ethyl acrylate is more than the 90 quality % in described monomer component, the content of described vinyl cyanide is 0.5-5 quality %, the gel fraction of described adhering agent layer is 40-80 quality %,
(2) releasable adhesive sheet according to above-mentioned (1), wherein, described gel fraction is 40-60 quality %;
(3) according to (1) or the releasable adhesive sheet described in (2), wherein, the content of described ethyl acrylate is more than 96 quality %;
(4) content according to (1) or the releasable adhesive sheet described in (2), wherein, with the unsaturated vinyl monomer of carboxyl is 0.1-5 quality %;
(5) according to (1) or the releasable adhesive sheet described in (2), wherein, the content of described vinyl cyanide is 0.5-3 quality %;
(6) according to (1) or the releasable adhesive sheet described in (2), wherein, the softening temperature of described adhesion imparting agent is 80-160 DEG C;
(7) according to (1) or the releasable adhesive sheet described in (2), wherein, described linking agent be selected from molecule there is two or more glycidyl many glycidyl compound, have in molecule Liang Yi have in the carbodiimide based compound of plural carbodiimide-based in oxazolinyl oxazoline based compound, molecule more than one;
(8) according to (1) or the releasable adhesive sheet described in (2), wherein, described releasable adhesive sheet is for pasting the label of polyethylene terephthalate bottle;
(9) releasable adhesive sheet according to claim 8, wherein, paste after on polyethylene terephthalate bottle, described adhering agent layer floods within latter 30 minutes in the hot water of 80 DEG C to be peeled off from this polyethylene terephthalate bottle.
According to the present invention, by the releasable adhesive sheet using adhering agent layer to be formed by exfoliated water-based adhesion agent composition again, described exfoliated water-based adhesion agent composition again contains water-based emulsion and linking agent, described water-based emulsion contains acrylic copolymer and adhesion imparting agent, the ethyl acrylate as main component is contained as the monomer component forming described acrylic copolymer, vinyl cyanide, and there is the unsaturated vinyl monomer of carboxyl, thus can be provided in the manipulation of regeneration operation in manipulation of regeneration equipment and can peel off removing simply, and with the adhesive label releasable adhesive sheet that hand can easily be peeled off.
Embodiment
Below the present invention is described in detail.
Releasable adhesive sheet in the present invention, by the washing procedure of PET bottle, by PET bottle dipping in the hot water, can remove from PET bottle.As the substrate sheets of supporter, there is no particular limitation, in order to the adhesion label utilizing the proportion official post in the hot water of PET bottle and adhesive label to peel off easily is separated, suitably can use the base material of proportion less than 1, such as, suitably can use the stationery of free sheet, crepe paper, wet-strong paper etc., there is the synthetic paper in cavity inside, polypropylene fibre film, polyethylene film, polyethylene foamed film, also suitably can use extension film or non-extension film.
Wherein, from the view point of having good printing, rigidity, cost, labeling adaptability etc. as label substrate, the polyolefins synthetic resin film formed by polyvinyl resin or acrylic resin etc., the synthetic paper etc. prepared by this polyolefin resin suitably can be used.
As the synthetic resin film of substrate sheets, can not extend, also can extend to vertical or horizontal single shaft direction or the biaxially oriented of waiting.
The thickness of substrate sheets has no particular limits, and is generally the scope of 10-200 μm, from the aspect of processing ease, is preferably 25-150 μm.
Substrate sheets can be painted, also can be water white.In addition, can also carry out on the surface of substrate sheets or the inside printing or lettering etc.
Therefore, heat sensitive recording layer can also be set in substrate sheets; Can the lettering receiving layer of hot transfer printing, ink-jet, laser lettering etc.; Printing enhancement layer etc.
In addition, in order to improve the adhesivity (キ ー イ Application グ power between the reverse side (adhering agent layer forming surface) of substrate sheets and adhering agent layer), can also prime treatment or corona treatment be carried out.
In order to form the adhering agent layer of releasable adhesive sheet of the present invention, adhesion agent composition contains water-based emulsion and linking agent, described water-based emulsion contains acrylic copolymer and adhesion imparting agent, contains ethyl acrylate, vinyl cyanide as the monomer component forming described acrylic copolymer and has the unsaturated vinyl monomer of carboxyl.
In the present invention, the content of vinyl cyanide, by 0.5-5 quality %, is preferably 0.5-4 quality %, adjusts, can realize effect of the present invention in the scope being more preferably 0.5-3 quality %.By making the content of vinyl cyanide more than above-mentioned lower limit, when forming the adhering agent layer of sticking tablet, the cohesive force of adhering agent layer becomes good.Thus, when peeling off adhesive sheet from adherend, the pasty substance of tackiness agent can be suppressed to remain or peel off bad, therefore preferably.In addition, by below the above-mentioned upper limit, do not damage initial tack of adhesive (タ ッ Network) or cohesiveness, good cohesiveness can be kept.
As the unsaturated vinyl monomer with carboxyl, vinylformic acid, methacrylic acid, toxilic acid, methylene-succinic acid etc. can be used.Wherein, from the balance easily obtaining tackiness and releasable, hold facile viewpoint and set out, preferably use vinylformic acid, methacrylic acid.
From the view point of Cross-linked starting point can be made to be dispersed in the inside and outside of emulsion particle, preferably also with vinylformic acid and methacrylic acid.
The content with the unsaturated vinyl monomer of carboxyl is preferably 0.1-5 quality %, is more preferably 0.5-2 quality %.By being more than 0.1 quality %, cohesive force and mechanical stability can be improved; By being below 5 quality %, the permanent stability of the releasable adhesive sheet before label can be made to process are good, and the balance of releasable and cohesive force becomes good.
Be form more than the 90 quality % in the monomer component of described acrylic copolymer by making the content of ethyl acrylate, can give paste in PET bottle through after a period of time with hand peel off peel off again time moist feeling, prevent the pollution of adherend.From the view point of can obtaining the low multipolymer of Tg and the performance of the balance of clinging power and releasable can being obtained, the content of ethyl acrylate is preferably more than 96 quality %, be more preferably more than 97 quality %, more preferably more than 98 quality %.
In addition, in order to control the various characteristics of adhering agent layer, suitably monomer component other than the above can also be used.As other monomer component, except ethyl acrylate, preferably use (methyl) alkyl acrylate with the alkyl of carbonatoms 1-12.Such as, can illustrate out: the monomer component of (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) n-butyl acrylate, (methyl) isobutyl acrylate, (methyl) tert-butyl acrylate, (methyl) n-octyl, (methyl) Isooctyl acrylate monomer, (methyl) vinylformic acid ester in the different ninth of the ten Heavenly Stems, (methyl) cyclohexyl acrylate, methacrylic acid-2-ethylhexyl etc., they one or more can be used.Wherein, preferred monomer component is (methyl) n-butyl acrylate, (methyl) isobutyl acrylate, (methyl) tert-butyl acrylate, (methyl) Isooctyl acrylate monomer, (methyl) n-octyl, particularly preferably n-butyl acrylate.The content of described monomer component is preferably the 0-9.5 quality % in the monomer component forming acrylic copolymer.By within the scope of this, do not damage releasable, can be pasted onto in PET bottle good adhesion.
Further, except above-mentioned monomer, in order to improve the cohesive force of adhering agent layer, can use in the polyfunctionality monomer being selected from (gathering) ethylene glycol bisthioglycolate (methyl) acrylate, methylene-bisacrylamide, 1,6-hexylene glycol two (methyl) acrylate, trimethylolpropane tris (methyl) CALCIUM ACRYLATE, Vinylstyrene etc. more than one.The content of these polyfunctionality monomers, relative to described whole monomer 100 mass parts, about can adding 0-2 mass parts.When this consumption is more than 2 mass parts, adhesivity and the releasable of effects on surface base material can be reduced.
Use above-mentioned monomer component, during the acrylic copolymer utilizing emulsion polymerization method to prepare in the adhering agent layer of releasable adhesive sheet of the present invention, as spendable polymerization starter, can 2 be enumerated, 2 '-azo two (2-methyl-propyl amidine) dihydrochloride (2, 2 '-ア ゾ PVC ス (2-メ チ Le プ ロ ピ オ Application ア ミ ジ Application), 2, 2 '-azo diisobutyl amidine dihydrochloride (2, 2'-ア ゾ PVC ス (2-ア ミ ジ ノ プ ロ パ Application) ジ ヒ De ロ Network ロ ラ イ De) etc. azo, Potassium Persulphate, the persulfuric acid hydrochlorate of ammonium persulphate etc., benzoyl peroxide, tertbutyl peroxide, the superoxide of hydrogen peroxide etc.Or the redox initiator be combined to form of the combination of persulphate and sodium bisulfite or superoxide and sodium ascorbate can be used.Usually at these polymerization starters of each stage interpolation specified amount of emulsion polymerization, polyreaction can be carried out.
When being prepared the water-based emulsion of the acrylic copolymer in the adhering agent layer of releasable adhesive sheet of the present invention by emulsion polymerization method, in order to ensure polymerization stability, negatively charged ion system or positively charged ion system emulsifying agent can be used in right amount.As negatively charged ion system emulsifying agent, sodium lauryl sulphate, ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate, pareth sulfate, Alkylphenyl polyoxyethylene ether sufate salts etc. can be enumerated particularly.As positively charged ion system emulsifying agent, Voranol EP 2001, polyoxyethylene alkylphenol ether etc. can be enumerated.In addition, the free-radical polymerised reactive emulsifier introducing propenyl, acryl etc. can also be used.These emulsifying agents can be used alone and also can be used together.
As the condition of emulsion polymerization, there is no particular limitation, directly can be suitable for the condition be suitable in common emulsion polymerization.Usually, with rare gas element to after replacing in reactor, under reflux, stir while start to heat up, and be warming up to the temperature range of about 40-100 DEG C, heat up after starting and carry out polymerization 1-8 hours.
The adhesion agent composition of releasable adhesive sheet of the present invention contains adhesion imparting agent as required composition.
As the adhesion imparting agent used, can to illustrate out the rosin series resin of rosin (ロ ジ Application), rosin phenolic resin and ester cpds thereof, hydrogenated wood rosin glycerol ester (water adds ロ ジ Application エ ス テ Le) etc., the terpenic series resin of terpene oligomers, terpene phenol resin, aromatic modified terpine resin etc., C5 through-stone oleo-resinous, the adhesion imparting agent of C9 through-stone oleo-resinous etc.Wherein, being preferably softening temperature is the adhesion imparting agent of 80-160 DEG C, or it is two or more to can be used together in these adhesion imparting agents.
Mixing number is different according to the monomer used, and relative to total amount 100 mass parts of the monomer component of formation acrylic copolymer, usually adds 0.1-20 mass parts, preferably adds 1-15 mass parts.By adding more than adhesion imparting agent 0.1 mass parts, as the effect of essence, good clinging power, substrate adherence can be obtained.By adding below 20 mass parts, can prevent the apparent Tg of adhering agent layer from uprising, preventing the reduction of clinging power, substrate adherence.
Adhesion imparting agent can add by the adhesion imparting agent as emulsion-type in the water-based emulsion of acrylic copolymer after emulsion polymerization sometimes, also can add before emulsion polymerization or in emulsion polymerization process.Consider with in the adhering situation of surface substrate, preferably when emulsion polymerization and monomer component coexist.With monomer component coexist carry out emulsion polymerization time, easily cause to adhesion imparting agent chain tra nsfer, exist adhering agent layer gel fraction reduce possibility, in the present invention, by containing linking agent as required composition, make gel fraction be the scope of 40-80 quality %, can target effect be obtained.Gel fraction described in the present invention obtains gel fraction by the measuring method in embodiment described later.
In the present invention, by the consumption of the linking agent of interpolation after increase and decrease polymerization, gel fraction can being adjusted to the scope of 40-80 quality %, also can be used together by the usage chain transfer agent when being polymerized the method for the adjustment gel fraction that the polymerization degree adjusts.As chain-transfer agent, known chain-transfer agent can be used, as lauryl mercaptan, glycidyl mercaptan, Thiovanic acid (acid of メ Le カ プ ト jealous woman), 2 mercapto ethanol, Thiovanic acid (acid of チ オ グ リ コ ー Le), thioglycollic acid-2-ethyl hexyl ester, 2,3-dimercapto-1-propyl alcohol.
As adhering agent layer, when gel fraction is less than 40 quality %, due to oozing out of adhering agent layer, adhesive label cut out and the secondary processing type of perforation etc. is deteriorated, in addition, during more than 80 quality %, can not get sufficient clinging power.The preferable range of gel fraction is 40-60 quality %.
The median size of the water-based emulsion particle of the acrylic copolymer in releasable adhesive sheet of the present invention is 80-500nm, is preferably 150-400nm.
When median size is in above-mentioned scope, the physical property balance of gained adhering agent layer can be obtained, i.e. clinging power and releasable, and then the adhering agent layer that the balance of mechanical stability is good.
By making median size be more than 80nm, stable emulsion ion can be obtained, preventing the many with quantitative change of tensio-active agent.By making median size be below 400nm, the adhesivity to substrate sheets can be obtained, prevent the reduction of the water tolerance of gained adhering agent layer.
Oxidant layer is given in the adhesion of releasable adhesive sheet of the present invention, containing linking agent as required composition.
As linking agent, be mainly the linking agent carrying out with the carboxyl from the unsaturated vinyl monomer in acrylic copolymer being cross-linked, from to the adhesivity of substrate sheets or releasable, to paste after adherend the rising of clinging power in time less, aspect that stain resistance is good, mainly can use epoxy compound, oxazoline based compound, carbodiimide based compound.And, these linking agents can be used alone, also can be two or more and use, also can also use ethylenimine based compound as required, polymeric polyisocyanate, trimeric cyanamide based compound, metal complex based compound, amine compound, other linking agent such as the hydrazine derivative of adipic dihydrazide, sebacic dihydrazide etc.
These linking agents are relative to adding with the ratio of 0.4-1 equivalent as carboxyl 1 equivalent contained in the acrylic copolymer of principal resinous ingredients in water dispersible adhesion agent composition.By making addition be more than 0.4 equivalent, the too low effect that can not get essence of gel fraction can be prevented, prevent substrate adherence, cohesive force to be deteriorated.By for below 1 equivalent, can prevent gel fraction from becoming too high and make linking agent to adherend or substrate interface infiltration, preventing the reduction of adherend contamination or substrate adherence, prevent caustic solubility from reducing.
As epoxy compound, as long as have the compound of two or more epoxy group(ing) or glycidyl in molecule, such as, can enumerate biphenol A Epicholorohydrin type epoxy resin, sorbitol polyglycidylether (ソ Le ビ ト ー Le Port リ グ リ シ ジ ル エ ー テ Le) (" the デ ナ コ ー Le EX-611 " of such as Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-612 ", " デ ナ コ ー Le EX-614 ", " デ ナ コ ー Le EX-614B ", " デ ナ コ ー Le EX-622 " etc.), polyglycerol polyglycidyl ether (Port リ グ リ セ ロ ー Le Port リ グ リ シ ジ ル エ ー テ Le) (" the デ ナ コ ー Le EX-512 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-521 " etc.), tetramethylolmethane polyglycidyl ether (ペ Application タ エ リ ス リ ト ー Le Port リ グ リ シ ジ ル エ ー テ Le) " the デ ナ コ ー Le EX-411 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), Glycerol dimer polyglycidyl ether (ジ グ リ セ ロ ー Le Port リ グ リ シ ジ ル エ ー テ Le) " the デ ナ コ ー Le EX-421 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), glycerol polyglycidylether (" the デ ナ コ ー Le EX-313 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-314 " etc.), TriMethylolPropane(TMP) polyglycidyl ether (ト リ メ チ ロ ー Le プ ロ パ Application Port リ グ リ シ ジ ル エ ー テ Le) " the デ ナ コ ー Le EX-321 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), neopentylglycol diglycidyl ether " the デ ナ コ ー Le EX-211 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), 1,6-hexanediol diglycidyl ether " the デ ナ コ ー Le EX-212 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), ethylene glycol diglycidylether (" the デ ナ コ ー Le EX-810 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-811 " etc.), diethylene glycol diglycidyl glyceryl ether (" the デ ナ コ ー Le EX-850 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-851 " etc.), polyethyleneglycol diglycidylether (" the デ ナ コ ー Le EX-821 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-830 ", " デ ナ コ ー Le EX-832 ", " デ ナ コ ー Le EX-841 ", " デ ナ コ ー Le EX-861 " etc.), propylene glycol diglycidylether " the デ ナ コ ー Le EX-911 " of Na ガ セ ケ system テ ッ Network ス society (such as, etc.), polypropylene glycol diglycidyl ether (" the デ ナ コ ー Le EX-941 " of such as, Na ガ セ ケ system テ ッ Network ス society, " デ ナ コ ー Le EX-920 ", " デ ナ コ ー Le EX-931 " etc.), diglycidylaniline, N, N, N ', N '-four glycidyl group O-phthalic amine, 1,3-pair (N, N '-diglycidyl amino methyl) hexanaphthene etc.
Zuo Wei oxazoline based compound, the carbon location can enumerating 2 has the multipolymer etc. of the substituent addition polymerization 2-oxazoline (such as 2-ethyl propylene base-2-oxazoline) with unsaturated C-C and other unsaturated monomer, as commercially available product, " エ Port Network ロ ス WS-500 ", " エ Port Network ロ ス WS-700 ", " the エ Port Network ロ ス K-2010E ", " エ Port Network ロ ス K-2020E ", " エ Port Network ロ ス K-2030E " etc. of Japanese catalyst society can be enumerated.
As carbodiimide based compound, such as, as long as the compound at least containing two or more carbodiimide-based, can enumerate " カ Le ボ ジ ラ イ ト V-02 ", " カ Le ボ ジ ラ イ ト V-02-L2 ", " the カ Le ボ ジ ラ イ ト V-04 ", " カ Le ボ ジ ラ イ ト V-06 ", " カ Le ボ ジ ラ イ ト E-01 ", " カ Le ボ ジ ラ イ ト E-02 ", " カ Le ボ ジ ラ イ ト E-04 " etc. of Nisshinbo society.
In addition, in adhering agent layer in releasable adhesive sheet of the present invention, as required, suitably can contain plasticizer (such as liquid polybutene, mineral oil, lanolin, liquid polyisoprene, liquid polyacrylate, dioctyl phthalate (DOP), glycerine, thanomin etc.), sanitas, rust-preventive agent, freeze melt stability agent, pigment, tinting material, weighting agent (zinc oxide, titanium white, calcium carbonate, clay etc.), metal-powder, defoamer, tackifier, tensio-active agent, antioxidant, UV light absorber etc.
Above-mentioned additive is many to be added in water-based emulsion after polymerisation, also can add before emulsion polymerization or in emulsion polymerization process.
The solids component of aqueous dispersion type adhesion agent composition of the present invention (containing acrylic copolymer and the adhesion water-based emulsion of imparting agent and linking agent) is 30-65 quality %, is preferably 40-55 quality %.
In addition, the viscosity of aqueous dispersion type adhesion agent composition is 50-12000mPas (BM type viscometer, 25 DEG C), is preferably 100-10000mPas.
Preferably pH is the scope of 6-9 further.When the solids component of aqueous dispersion type adhesion agent composition, viscosity and pH are in above-mentioned scope, from the aspect of drying property, coating and operability preferably.
As the preparation method of releasable adhesive sheet of the present invention, have no particular limits.Such as mixed cross-linker etc. (when not adding adhesion imparting agent during the emulsion polymerization of acrylic copolymer in above-mentioned water-based emulsion, the also adhesion imparting agent of mixed emulsion type), add as required and the tackifier of polypropylene acid etc., be formulated in the tackiness agent of the water dispersible adhesion agent composition formation at 25 DEG C, viscosity being adjusted to about 5000-10000mPas.
Then, can adopt and tackiness agent is applied to stripping film, and after dry formation adhering agent layer, by the print-on coating method that adhering agent layer and substrate sheets are fitted.Further, also can adopt and first tackiness agent is coated directly onto substrate sheets surface, and after dry formation adhering agent layer, by the direct coating method that adhering agent layer and stripping film are fitted.
As stripping film, there is no particular limitation, as support base material, such as, can enumerate paper, synthetic paper, synthetic resin film etc.
As paper, the paper base material of free sheet, glassine paper, enamelled paper etc. can be enumerated, the paper base material that the laminated paper of the thermoplastic resin of laminated polyethylene, polypropylene etc. is such on these paper base materials, and with the paper base material etc. after the sealing pores such as fiber, starch, polyvinyl alcohol, styrene-acrylic resin on free sheet, glassine paper, enamelled paper etc.; As plastic synthetic resin film, such as can enumerate the polyolefin resin of polyvinyl resin, acrylic resin etc., the film of the vibrin formation of polybutylene terephthalate resin, pet resin etc., and these synthetic resin film are implemented to the film of easy binder-treatment of Corona discharge Treatment etc., preferably they are implemented to the film of lift-off processing.
As stripping treatment agent, the rubber series elastomerics of such as silicone resin, polyolefin-based resins (stripping film for beyond polyolefin resin), isoprene resin, butadiene-based resin etc., Synolac, fluoro-resin can be used, containing known treatment agents such as chain alkyl resins.
The thickness of the layer of stripping treatment agent is preferably 0.05-2.0 μm, is more preferably 0.1-1.5 μm.
The thickness of the support base material of stripping film has no particular limits, and is generally 30-200 μm.
As the coating process of tackiness agent, have no particular limits, known coating process can be used, such as, can enumerate the method for apparatus for coating utilizing knife coater, roll coater, knife over roll coating machine, gravure coater, electronic gravure coating machine (バ リ オ グ ラ PVC ア コ ー タ ー), air knife coaters, excellent coating machine, die coater (ダ イ コ ー タ ー), curtain coater etc.
The thickness of adhering agent layer has no particular limits, and is generally 10-50 μm, is preferably 12-30 μm.Further, releasable adhesive sheet of the present invention can be the sheet of plane, also can for being rolled into the shape of roll.
The releasable adhesive sheet of the present invention of preparation as described above, is characterized in that, pasting after on PET bottle, in the manipulation of regeneration operation in manipulation of regeneration equipment, when being immersed in the hot water of 80 DEG C, adhering agent layer was peeled off from this PET bottle within 30 minutes.
Releasable adhesive sheet of the present invention, in above-mentioned operation, can peel off removing simply from PET bottle, and, easily can peel off with hand, therefore particularly preferably be used as PET bottle stickup label.
Embodiment
The present invention will be described in more detail below by way of embodiments and comparative examples, but the present invention is not limited in them.In addition, in following embodiment and comparative example, part or % all represent mass parts or quality %.
Embodiment 1
As monomer component, add ethyl acrylate (being designated as 2EHA below) 98.4 parts, 0.2 part, vinylformic acid (being designated as AA below), methacrylic acid (being designated as MAA below) 0.4 part, vinyl cyanide (being designated as AN below) 1.0 parts, add the polyethenoxy ether sodium sulfovinate salt (tensio-active agent of Kao Corp, trade name: ラ テ system Le E-118B) 0.5 part, the polyxyethylated alkyl ether sulfate ammonium salt (tensio-active agent of the first industrial pharmaceutical society, trade name: ア Network ア ロ Application KH-05) 0.1 part, Voranol EP 2001 (the tensio-active agent of Hua Wangshe, trade name: エ マ Le ゲ Application 103) 1 part, the adhesion imparting agent of hydrogenated wood rosin glycerol ester (イ ー ス ト マ Application ケ ミ カ Le society, trade(brand)name: フ ォ ー ラ Le 105) 2.0 parts, aromatic modified terpine resin (the adhesion imparting agent of ヤ ス Ha ラ ケ ミ カ Le society, trade(brand)name: YS レ ジ Application TO-125) 0.5 part and ion exchanged water 80 mass parts, put into stirrer, reflux exchanger, thermometer, in the reaction vessel of nitrogen ingress pipe and dropping funnel, at room temperature stir, prepare the emulsification of the mixture of monomer component in advance.
In addition, ion exchanged water 28 mass parts is added in the reaction unit with stirrer, reflux exchanger, thermometer, nitrogen ingress pipe and dropping funnel, enclose nitrogen temperature until interior temperature to 80 DEG C, keep this temperature, add ammonium persulfate aqueous solution 0.5 mass parts of 10 quality % simultaneously.Then, the emulsification of the mixture of the monomer component prepared in advance is transferred in dropping funnel, spends and carry out dropping liquid in 4 hours.
Walk abreast therewith, drip 5 quality % ammonium persulfate aqueous solution 4 mass parts, the temperature of 80 DEG C will be maintained in reaction vessel, carry out emulsion polymerization.After dropping terminates, at 80 DEG C aging 4 hours, obtain the water-based emulsion (1) containing acrylic copolymer and adhesion imparting agent.
Then, be cooled to room temperature, add water with after the ammonia neutralization of 25%, to obtain solids component be 50 quality %, pH be 8.0 water-based emulsion (2).Then, add polyoxyethylene 0.5 part (ラ イ オ Application ア Network ゾ society system, trade name: エ ソ ミ Application C/25) as plasticizer, obtain water-based emulsion (3).
Then, in this water-based emulsion (3) 100 mass parts, polyacrylic tackifier (ロ ー system ア Application ド ハ ー ス society system is added, ASE-60), make viscosity thickening at 25 DEG C to 8000mPas.
Further, measure by relative to acrylic copolymer 100 mass parts in above-mentioned water-based emulsion (3), add the viscosity of the tackiness agent of the aqueous dispersion type adhesion agent composition formation that linking agent (glycerol polyglycidylether of Na ガ セ ケ system テ ッ Network ス society, trade name: デ ナ コ ー Le EX-313 (effective constituent more than 99%)) 0.9 mass parts obtains.
Use knife over roll coating machine, in stripping film (リ ンテック society system, the glassine paper after lift-off processing is carried out with silicone resin, trade name: SP-8K ア オ) stripper treated side on, this tackiness agent is coated with in the mode that dried coating thickness is 15 μm, at 90 DEG C, drying 2 minutes, forms adhering agent layer.
Then, with one side, there is surface substrate synthetic paper (the ユ ポ コ ー ポ レ ー シ ョ Application system of printing receiving layer, trade name: ユ Port SGS80) do not have printing receiving layer face laminating, at 23 DEG C, under the atmosphere of relative humidity 50%, place 7 days, prepare releasable adhesive sheet thus.
In addition, substitute above-mentioned synthetic paper, with stripping film (リ ンテック society system, the polyester film of lift-off processing has been carried out with silicone resin, trade name: SP-PET3811) lift-off processing face laminating, at 23 DEG C, under the atmosphere of relative humidity 50%, place and prepare adhesive sheet in 7 days, use this adhesive sheet to measure gel fraction.
This releasable adhesive sheet is fitted in respectively on SUS plate, polyester sheet, measures clinging power, then, this releasable adhesive sheet is processed into adhesive label, measure water tolerance and releasable.
Embodiment 2
Except 2-EHA and AN being changed to except the amount shown in table 1, similarly carry out according to such as embodiment 1.Result is as shown in table 1.
Embodiment 3
Except the content of AA and MAA being pressed change shown in table 1, carry out similarly to Example 1, make releasable adhesive sheet.Result is as shown in table 1.
Embodiment 4
The carbodiimide (trade name: カ Le ボ ジ ラ イ ト V-04) 1.0 parts made except using Nisshinbo (strain), as except linking agent, carries out similarly to Example 1, makes releasable adhesive sheet.Result is as shown in table 1.
Embodiment 5
Except using containing having propenyl main chain oxazolinyl water-soluble polymers (Japanese catalyst society system, trade name: エ Port Network ロ ス WS-700, solids component 25%) 2.0 parts as beyond linking agent, carry out similarly to Example 1, make releasable adhesive sheet.Result is as shown in table 1.
Comparative example 1,2
Except making the amount of AN be 0.4 part, or not using, 2-EHA being changed to beyond the amount shown in table 1, carrying out similarly to Example 1, the releasable adhesive sheet of comparison.Result is as shown in table 1.
Comparative example 3
Except using 8.0 parts of AN, 2-EHA being changed to beyond the amount shown in table 1, carrying out similarly to Example 1, the releasable adhesive sheet of comparison.Result is as shown in table 1.
Comparative example 4,5
Except not using デ ナ コ ー Le EX-313, or beyond using 0.3 part, carry out similarly to Example 1, the releasable adhesive sheet of comparison.Result is as shown in table 1.
Comparative example 6
Except using 3.0 parts of デ ナ コ ー Le EX-313, carry out similarly to Example 1, comparison releasable adhesive sheet.Result is as shown in table 1.
Comparative example 7
Except not adding フ ォ ー ラ Le 105 and YS レ ジ Application TO-125, similarly carry out according to embodiment 1, prepare the releasable adhesive sheet compared.Result is as shown in table 1.
Comparative example 8
Using except 2-EHA and n-butyl acrylate except pressing the amount shown in table 1, carrying out similarly to Example 1, making releasable adhesive sheet.Result is as shown in table 1.
Reference example 1,2
Except using relative to commercially available alkali soluble type label tackiness agent, (East Asia synthesis society does not contain AN tackiness agent, trade name: RP-275, solids component 52-54%, viscosity 8000-18000mPas/25 DEG C, pH 6.5-7.5) 100 mass parts, add linking agent (the polyglycerol polyglycidyl ether of Na ガ セ ケ system テ ッ Network ス society respectively, trade name: デ ナ コ ー Le EX-521 (effective constituent more than 99%)) beyond 1.0 parts or 3.0 parts of tackiness agents obtained, carry out similarly to Example 1, make referential releasable adhesive sheet.Result is as shown in table 1.
The each physical property measured at embodiment and comparative example and the evaluation of performance are carried out according to following.
The mensuration > of each physics value of <
(1) viscosity
According to JISK-6833, under the environment of 25 DEG C, adopt BM type viscometer (Tokyo gauge society system), use No.4 rotor, measure the viscosity (unit: mPas) of adhesion agent composition with 12 revs/min.
(2) gel fraction
Adhering agent layer is about the SUS screen cloth that 500mg wraps in #300, flood in tetrahydrofuran (THF) after 72 hours, take out together with SUS screen cloth, at 120 DEG C after dry 3 hours, by with dipping before mass ratio calculate the gel fraction (unit: quality %) of adhering agent layer.
The testing of characteristic > of < releasable adhesive sheet and adhesive label
(1) clinging power
Releasable adhesive sheet is cut into width 25mm, be pasted onto SUS plate, polyester sheet (PET plate) respectively, back pressure is carried out once with the roller that quality is 2kg (19.6N), after relative humidity places 24 hours 50% time, with peeling rate 300mm/ minute, measured value when peel angle 180 ° is peeled off, unit is N/25mm.
(2) water tolerance
Releasable adhesive sheet is made the adhesive label of wide 25mm × 50mm, this adhesive label is pasted PET bottle, when impregnated of in the water of 23 DEG C 72 hours, the stripping of visual observations label.
Zero: without peeling off
×: there is stripping
(3) releasable
[hand separability]
The adhesive label identical with being used for water tolerance test is pasted PET bottle, 40 DEG C, place one week under the condition of relative humidity 80% after, peel off with hand and confirm releasable.
Zero: releasable is good, remain without pasty substance
×: can not peel off again, have pasty substance to remain
[hot water separability]
The adhesive label identical with being used for water tolerance test is pasted PET bottle, and when flooding 30 minutes in 80 DEG C of hot water, whether visual observations label is peeled off naturally
Zero: label is peeled off completely.
△ a: part for label is peeled off.
×: label is completely unstripped.
[use starting material]
Monomer component in table 1 and the numeric representation of linking agent are relative to the amount of the effective constituent of total amount 100 mass parts of monomer component.The raw-material abbreviation grade used is as shown in following.
2EHA: ethyl acrylate
N-BA: n-butyl acrylate
AA: vinylformic acid
MAA: methacrylic acid
AN: vinyl cyanide
The glycerol polyglycidylether (trade name: デ ナ コ ー Le EX-313 (effective constituent more than 99%)) of EX-313: Na ガ セ ケ system テ ッ Network ス society
V-04: the carbodiimide (trade name: カ Le ボ ジ ラ イ ト V-04 (active constituent content 40%)) that Nisshinbo (strain) is made
WS-700: Japanese catalyst society system contains and has propenyl main chain oxazolinyl water-soluble polymers (trade name: エ Port Network ロ ス WS-700, solids component 25%)
The polyglycerol polyglycidyl ether (trade name: デ ナ コ ー Le EX-521 (effective constituent more than 99%)) of EX-521: Na ガ セ ケ system テ ッ Network ス society
Industrial applicibility
Releasable adhesive sheet of the present invention, particularly as the bottle of various beverage, the adhesive label more specifically as PET bottle is useful.Adhering agent layer for releasable adhesive sheet of the present invention is alkali-soluble, therefore, easily can carry out the overburden operation of necessary adhesive label when recycling PET bottle, exceedingly useful in this field.
Claims (9)
1. a releasable adhesive sheet, it is characterized in that, by stripping film, adhering agent layer, in the releasable adhesive sheet of surface substrate lamination, described adhering agent layer is formed by the water dispersible adhesion agent composition containing water-based emulsion and linking agent, described water-based emulsion contains acrylic copolymer and adhesion imparting agent, relative to total amount 100 mass parts of the monomer component of the described acrylic copolymer of formation, described adhesion imparting agent is 0.1-20 mass parts, the monomer component forming described acrylic copolymer comprises ethyl acrylate, vinyl cyanide and there is the unsaturated vinyl monomer of carboxyl, the content of described ethyl acrylate is more than the 90 quality % in the total amount 100 quality % of described monomer component, the content of described vinyl cyanide is 0.5-5 quality %, the gel fraction of described adhering agent layer is 40-80 quality %, wherein, described linking agent is the linking agent carrying out with the carboxyl from the unsaturated vinyl monomer in described acrylic copolymer being cross-linked, and relative to described carboxyl 1 equivalent, the consumption of described linking agent is the ratio of 0.4-1 equivalent, the measuring method of the gel fraction of described adhering agent layer is: SUS screen cloth adhering agent layer 500mg being wrapped in #300, flood in tetrahydrofuran (THF) after 72 hours, take out together with SUS screen cloth, at 120 DEG C after dry 3 hours, by with dipping before mass ratio calculate the gel fraction of described adhering agent layer.
2. releasable adhesive sheet according to claim 1, wherein, described gel fraction is 40-60 quality %.
3. releasable adhesive sheet according to claim 1 and 2, wherein, the content of described ethyl acrylate is more than 96 quality %.
4. releasable adhesive sheet according to claim 1 and 2, wherein, described in there is the unsaturated vinyl monomer of carboxyl content be 0.1-5 quality %.
5. releasable adhesive sheet according to claim 1 and 2, wherein, the content of described vinyl cyanide is 0.5-3 quality %.
6. releasable adhesive sheet according to claim 1 and 2, wherein, the softening temperature of described adhesion imparting agent is 80-160 DEG C.
7. releasable adhesive sheet according to claim 1 and 2, wherein, described linking agent be selected from molecule there is two or more glycidyl many glycidyl compound, have in molecule Liang Yi have in the carbodiimide based compound of plural carbodiimide-based in oxazolinyl oxazoline based compound, molecule more than one.
8. releasable adhesive sheet according to claim 1 and 2, wherein, described releasable adhesive sheet is for pasting the label of polyethylene terephthalate bottle.
9. releasable adhesive sheet according to claim 8, wherein, pastes after on polyethylene terephthalate bottle, and described adhering agent layer floods within latter 30 minutes in the hot water of 80 DEG C to be peeled off from this polyethylene terephthalate bottle.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2010208576A JP5638891B2 (en) | 2010-09-16 | 2010-09-16 | Removable adhesive sheet |
| JP2010-208576 | 2010-09-16 |
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| JP6027856B2 (en) * | 2012-11-12 | 2016-11-16 | リンテック株式会社 | Water-dispersed pressure-sensitive adhesive composition, method for producing releasable pressure-sensitive adhesive sheet, and re-peelable pressure-sensitive adhesive sheet |
| KR101991974B1 (en) * | 2013-04-02 | 2019-06-21 | 동우 화인켐 주식회사 | Adhesive composition |
| JP6510891B2 (en) * | 2015-06-01 | 2019-05-08 | マクセルホールディングス株式会社 | Adhesive tape |
| BR112020003187A2 (en) * | 2017-08-16 | 2020-09-15 | Dow Global Technologies Llc | pressure sensitive adhesive compositions and methods for making the same |
| JP7205144B2 (en) * | 2018-09-28 | 2023-01-17 | 三菱ケミカル株式会社 | Adhesive composition, and adhesive and adhesive sheet using the same |
| JP2020132207A (en) * | 2019-02-18 | 2020-08-31 | リンテック株式会社 | Bag shaped package with adhesive sheet |
| CN110791209B (en) * | 2019-09-26 | 2023-08-29 | 江苏晶华新材料科技有限公司 | Easily-removed high-peel-force adhesive tape and preparation method thereof |
| CN111662675B (en) * | 2020-06-19 | 2021-10-22 | 西北工业大学深圳研究院 | Mural and colored drawing cultural relic reinforcing agent with self-healing function and preparation method thereof |
| WO2024122596A1 (en) * | 2022-12-06 | 2024-06-13 | 株式会社レゾナック | Pressure-sensitive adhesive agent composition, pressure-sensitive adhesive tape, adhesion method, and set |
| JP7385796B1 (en) | 2023-01-19 | 2023-11-24 | 東洋インキＳｃホールディングス株式会社 | Adhesive composition for decorative sheet, decorative sheet, decorative structure and manufacturing method thereof |
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| JP5638891B2 (en) | 2014-12-10 |
| JP2012062416A (en) | 2012-03-29 |
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