JP5719194B2 - 再剥離用水分散型アクリル系粘着剤組成物及び粘着シート - Google Patents
再剥離用水分散型アクリル系粘着剤組成物及び粘着シート Download PDFInfo
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- JP5719194B2 JP5719194B2 JP2011040691A JP2011040691A JP5719194B2 JP 5719194 B2 JP5719194 B2 JP 5719194B2 JP 2011040691 A JP2011040691 A JP 2011040691A JP 2011040691 A JP2011040691 A JP 2011040691A JP 5719194 B2 JP5719194 B2 JP 5719194B2
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- 239000003999 initiator Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 125000000555 isopropenyl group Chemical group [H]\C([H])=C(\*)C([H])([H])[H] 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- SJPFBRJHYRBAGV-UHFFFAOYSA-N n-[[3-[[bis(oxiran-2-ylmethyl)amino]methyl]phenyl]methyl]-1-(oxiran-2-yl)-n-(oxiran-2-ylmethyl)methanamine Chemical compound C1OC1CN(CC=1C=C(CN(CC2OC2)CC2OC2)C=CC=1)CC1CO1 SJPFBRJHYRBAGV-UHFFFAOYSA-N 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- HRRDCWDFRIJIQZ-UHFFFAOYSA-N naphthalene-1,8-dicarboxylic acid Chemical compound C1=CC(C(O)=O)=C2C(C(=O)O)=CC=CC2=C1 HRRDCWDFRIJIQZ-UHFFFAOYSA-N 0.000 description 1
- GNHGCDCAOUNOCA-UHFFFAOYSA-N naphthalene-2,6-dicarbohydrazide Chemical compound C1=C(C(=O)NN)C=CC2=CC(C(=O)NN)=CC=C21 GNHGCDCAOUNOCA-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- MDYPDLBFDATSCF-UHFFFAOYSA-N nonyl prop-2-enoate Chemical compound CCCCCCCCCOC(=O)C=C MDYPDLBFDATSCF-UHFFFAOYSA-N 0.000 description 1
- 229940065472 octyl acrylate Drugs 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- REJKHFKLPFJGAQ-UHFFFAOYSA-N oxiran-2-ylmethanethiol Chemical compound SCC1CO1 REJKHFKLPFJGAQ-UHFFFAOYSA-N 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical group 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- AXLMPTNTPOWPLT-UHFFFAOYSA-N prop-2-enyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OCC=C AXLMPTNTPOWPLT-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- 230000009993 protective function Effects 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000007717 redox polymerization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical group 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- ZJKOMXZUJBYOOK-UHFFFAOYSA-M tetraphenylazanium;hydroxide Chemical compound [OH-].C1=CC=CC=C1[N+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 ZJKOMXZUJBYOOK-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000000326 ultraviolet stabilizing agent Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/08—Homopolymers or copolymers of acrylic acid esters
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- C09J2301/00—Additional features of adhesives in the form of films or foils
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/308—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive tape or sheet losing adhesive strength when being stretched, e.g. stretch adhesive
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2852—Adhesive compositions
- Y10T428/2878—Adhesive compositions including addition polymer from unsaturated monomer
- Y10T428/2891—Adhesive compositions including addition polymer from unsaturated monomer including addition polymer from alpha-beta unsaturated carboxylic acid [e.g., acrylic acid, methacrylic acid, etc.] Or derivative thereof
Landscapes
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
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- Adhesive Tapes (AREA)
Description
本発明の粘着剤組成物におけるアクリルエマルション系重合体(A)は、(メタ)アクリル酸アルキルエステル及びカルボキシル基含有不飽和単量体を必須の原料モノマー(原料モノマー成分)として構成された重合体である。即ち、アクリルエマルション系重合体(A)は、(メタ)アクリル酸アルキルエステル及びカルボキシル基含有不飽和単量体を必須成分とするモノマー混合物より得られる重合体である。アクリルエマルション系重合体(A)は単独で、又は2種以上を組み合わせて使用することができる。なお、本発明では、「(メタ)アクリル」とは「アクリル」及び/又は「メタクリル」(「アクリル」及び「メタクリル」のうち、いずれか一方又は両方)のことをいう。
(溶剤不溶分の測定方法)
アクリルエマルション系重合体(A):約0.1gを採取し、平均孔径0.2μmの多孔質テトラフルオロエチレンシート(商品名「NTF1122」、日東電工(株)製)に包んだ後、凧糸で縛り、その際の重量を測定し、該重量を浸漬前重量とする。なお、該浸漬前重量は、アクリルエマルション系重合体(A)(上記で採取したもの)と、テトラフルオロエチレンシートと、凧糸の総重量である。また、テトラフルオロエチレンシートと凧糸の合計重量も測定しておき、該重量を包袋重量とする。
次に、上記のアクリルエマルション系重合体(A)をテトラフルオロエチレンシートで包み凧糸により縛ったもの(「サンプル」と称する)を、酢酸エチルで満たした50ml容器に入れ、23℃にて7日間静置する。その後、容器からサンプル(酢酸エチル処理後)を取り出して、アルミニウム製カップに移し、130℃で2時間、乾燥機中で乾燥して酢酸エチルを除去した後、重量を測定し、該重量を浸漬後重量とする。
そして、下記の式から溶剤不溶分を算出する。
溶剤不溶分(重量%)=(a−b)/(c−b)×100 (1)
(式(1)において、aは浸漬後重量であり、bは包袋重量であり、cは浸漬前重量である。)
本発明の粘着剤組成物における非水溶性架橋剤(B)は、非水溶性の化合物であり、分子中(1分子中)にカルボキシル基と反応しうる官能基を2個以上(例えば、2〜6個)有する化合物である。1分子中のカルボキシル基と反応しうる官能基の個数は、特に限定されないが、3〜5個が好ましい。1分子中のカルボキシル基と反応しうる官能基の個数が多くなるほど、粘着剤組成物が密に架橋する(即ち、粘着剤層を形成するポリマーの架橋構造が密になる)。このため、粘着剤層形成後の粘着剤層のぬれ広がりを防ぐことが可能となる。また、粘着剤層を形成するポリマーが拘束されるため、粘着剤層中の官能基(カルボキシル基)が被着体面に偏析して、粘着剤層と被着体との粘着力が経時で上昇することを防ぐことが可能となる。一方、1分子中のカルボキシル基と反応しうる官能基の個数が6個を超えて多すぎる場合には、ゲル化物が生じる場合がある。
(水に対する溶解度の測定方法)
同重量の水(25℃)と架橋剤を、攪拌機を用いて回転数300rpm、10分の条件で混合し、遠心分離により水相と油相に分ける。次いで、水相を採取し120℃で1時間乾燥して、乾燥減量から水相中の不揮発分(水100重量部に対する不揮発成分の重量部)を求める。
非水溶性架橋剤(B)の有するカルボキシル基と反応しうる官能基のモル数 = [非水溶性架橋剤(B)の配合量(添加量)]/[官能基当量] = 4/110
例えば、非水溶性架橋剤(B)として、エポキシ当量が110(g/eq)のエポキシ系架橋剤を4g添加(配合)する場合、エポキシ系架橋剤の有するエポキシ基のモル数は、例えば、以下のように算出できる。
エポキシ系架橋剤の有するエポキシ基のモル数 = [エポキシ系架橋剤の配合量(添加量)]/[エポキシ当量] = 4/110
本発明の粘着剤組成物におけるカルボン酸含有アクリル系重合体(C)は、(メタ)アクリル酸(アクリル酸及びメタクリル酸のうち、いずれか一方又は両方)を必須の原料モノマーとして構成された重合体である。
本発明の再剥離用水分散型アクリル系粘着剤組成物は、上述の通り、アクリルエマルション系重合体(A)、非水溶性架橋剤(B)、及びカルボン酸含有アクリル系重合体(C)を必須の成分として含有している。さらに、必要に応じて、非水溶性架橋剤(B)以外の架橋剤(「その他の架橋剤」と称する場合がある)、その他の添加剤を含有していてもよい。
(アクリルエマルション系重合体(A)の調製)
容器に、水90重量部、表1に示した配合量の原料モノマー、及び乳化剤を配合した後、ホモミキサーにより攪拌混合し、モノマーエマルションを調製した。
次いで、冷却管、窒素導入管、温度計および攪拌機を備えた反応容器に、水50重量部、重合開始剤(過硫酸アンモニウム)0.01重量部、及び、上記で調製したモノマーエマルションのうち10重量%にあたる量を添加し、攪拌しながら、75℃で1時間乳化重合した。その後、さらに重合開始剤(過硫酸アンモニウム)0.05重量部を添加し、次いで、攪拌しながら、残りのモノマーエマルションの全て(90重量%にあたる量)を3時間かけて添加して、その後、75℃で3時間反応させた。次いで、これを30℃に冷却して、濃度10重量%のアンモニア水を加えてpH8に調整して、アクリルエマルション系重合体(A)の水分散液(アクリルエマルション系重合体(A)の濃度:42重量%)を調製した。
上記で得られたアクリルエマルション系重合体(A)の水分散液(42重量%)238重量部(アクリルエマルション系重合体100重量部)に対して、非水溶性架橋剤であるエポキシ系架橋剤[三菱ガス化学(株)製、商品名「テトラッド−C」、1,3−ビス(N,N−ジグリシジルアミノメチル)シクロヘキサン、エポキシ当量:110、官能基数:4]3重量部、及びカルボン酸含有アクリル系重合体(C)を含む増粘剤[サンノプコ(株)製、商品名「SNシックナー630」、有効成分:30重量%]を水で希釈し有効成分を5重量%とした水溶液20重量部を加え、攪拌機を用いて、23℃、300rpm、10分の攪拌条件で攪拌混合し、再剥離用水分散型アクリル系粘着剤組成物を調製した。
なお、表1の「[カルボキシル基と反応しうる官能基のモル数]/[カルボキシル基のモル数]」の欄には、アクリルエマルション系重合体(A)の原料モノマーとして用いられる全てのカルボキシル基含有不飽和単量体のカルボキシル基の総モル数に対する、全ての非水溶性架橋剤のカルボキシル基と反応しうる官能基の総モル数の割合を示した。
さらに、上記で得られた再剥離用水分散型アクリル系粘着剤組成物を、PETフィルム(三菱樹脂(株)製、商品名「T100N38」、厚さ:38μm)のコロナ処理面上に、テスター産業(株)製アプリケーターを用いて、乾燥後の厚さが15μmとなるように塗布した。その後、熱風循環式オーブンを用いて120℃で2分間乾燥させ、さらにその後、50℃で3日間養生(エージング)して粘着シートを得た。
表1に示すように、カルボン酸含有アクリル系重合体(C)を含む増粘剤の種類を変更し、実施例1と同様にして、再剥離用水分散型アクリル系粘着剤組成物および粘着シートを得た。
表1に示すように、カルボン酸含有アクリル系重合体(C)を含む増粘剤(カルボン酸含有アクリル系重合体(C)を含む増粘剤の水溶液)を添加しないこと以外は実施例1と同様にして、再剥離用水分散型アクリル系粘着剤組成物および粘着シートを得た。
表1に示すように、カルボン酸含有アクリル系重合体(C)を含む増粘剤の水溶液の代わりに、ウレタン会合系増粘剤[(株)ADEKA製、商品名「アデカノール UH−550」、有効成分30重量%]を水で希釈し有効成分を5重量%とした水溶液を用いたこと以外は実施例1と同様にして、再剥離用水分散型アクリル系粘着剤組成物および粘着シートを得た。
表1に示すように、カルボン酸含有アクリル系重合体(C)を含む増粘剤を用いずに、また、非水溶性架橋剤を用いずに水溶性架橋剤のみを用いたこと以外は実施例1と同様にして、再剥離用水分散型アクリル系粘着剤組成物および粘着シートを得た。
実施例および比較例で得られた粘着シートについて、下記の測定方法又は評価方法により評価を行った。なお、粘着剤層(架橋後)の溶剤不溶分は、前述の測定方法で測定した。
評価結果を表1に示した。
(初期粘着力)
実施例および比較例で得られた粘着シート(サンプルサイズ:25mm幅×100mm長さ)を、貼り合わせ機(テスター産業(株)製、小型貼り合せ機)を用いて、0.25MPa、0.3m/分の条件で、偏光板(材質:トリアセチルセルロース(TAC)、表面の算術平均粗さRaがMD方向で約21nm、TD方向で約31nm、MD方向とTD方向の平均で約26nmである)に貼り合わせた。
上記の粘着シートと偏光板の貼り合わせサンプルを用い、23℃、50%RHの環境下、20分間放置後に、下記の条件に従って180°剥離試験を行い、粘着シートの偏光板に対する粘着力(N/25mm)を測定し、「初期粘着力」とした。
(40℃1週間貼付保存後粘着力)
実施例および比較例で得られた粘着シート(サンプルサイズ:25mm幅×100mm長さ)を、貼り合わせ機(テスター産業(株)製、小型貼り合せ機)を用いて、0.25MPa、0.3m/分の条件で、偏光板(材質:トリアセチルセルロース(TAC)、表面の算術平均粗さRaがMD方向で約21nm、TD方向で約31nm、MD方向とTD方向の平均で約26nmである)に貼り合わせた。
上記の粘着シートと偏光板の貼り合わせサンプルを用い、40℃の環境に1週間保存した後、23℃、50%RHの環境下に2時間放置し、その後、下記の条件に従って180°剥離試験を行い、粘着シートの偏光板に対する粘着力(N/25mm)を測定し、「40℃1週間貼付保存後粘着力」とした。
上記の180°剥離試験は、引張試験機を用いて、23℃、50%RHの環境下、引張速度0.3m/分で行った。
初期粘着力と40℃1週間貼付保存後粘着力の差[(40℃1週間貼付保存後粘着力)−(初期粘着力)]が、0.10N/25mm以下であれば、粘着力上昇防止性に優れていると判断できる。
実施例および比較例で得られた粘着シート(サンプルサイズ:25mm幅×100mm長さ)を、貼り合わせ機(テスター産業(株)製、小型貼り合せ機)を用いて、0.25MPa、0.3m/分の条件で、偏光板(日東電工(株)製、商品名「SEG1425DUHC」、70mm幅×120mm長さ)上に貼り合わせた。
上記粘着シートを貼り合わせた偏光板を、粘着シートを貼り合わせたまま80℃で4時間放置した後、粘着シートを剥離した。その後、粘着シートを剥離した偏光板を加湿環境下(23℃、90%RH)で12時間放置し、偏光板表面を目視にて観察して、以下の基準で低汚染性を評価した。
低汚染性良好(○) : 粘着シートを貼付した部分と貼付していない部分で変化が見られない。
低汚染性不良(×) : 粘着シートを貼付した部分に白化が見られた。
実施例および比較例で得られた粘着シートの粘着剤層表面の状態を、目視で観察した。縦10cm×横10cmの観察範囲内の欠点(凹み及び気泡)の個数を測定し、以下の基準で外観を評価した。
欠点個数が0〜100個 : 外観が良好である(○)。
欠点個数が101個以上 : 外観が悪い(×)。
実施例および比較例で得られた再剥離用水分散型アクリル系粘着剤組成物を、表面をシリコーン処理したPETフィルム(三菱樹脂(株)製、商品名「MRF38」)のシリコーン処理面上に、乾燥後の厚さが50μmとなるようにコーティングして、その後、熱風循環式オーブンを用いて120℃で2分間乾燥させて、50℃で3日間養生を行い、粘着剤層を得た。
次いで、上記粘着剤層を丸めて円柱状の粘着剤層サンプル(長さ50mm、断面積(底面積)1mm2)を作製した。
引張試験機を用いて、測定の初期長(チャック間隔)が10mmとなるようにチャックを設定し、引張速度50mm/分の条件で引張試験を行い、上記粘着剤層サンプルの破断点の伸び(破断点伸度)を測定した。
なお、破断点の伸び(破断点伸度)は、引張試験において試験片(粘着剤層サンプル)が破断したときの伸びを表し、下記の式で計算される。
「破断点の伸び(破断点伸度)」(%) = (「破断時の試験片の長さ(破断時のチャック間隔)」−「初期長(10mm)」)÷「初期長(10mm)」×100
[原料モノマー]
2EHA : 2−エチルヘキシルアクリレート
MMA : メチルメタクリレート
AA : アクリル酸
[乳化剤]
HS−1025 : 第一工業製薬(株)製、商品名「アクアロンHS−1025」(反応性ノニオンアニオン系乳化剤)
[架橋剤]
TETRAD−C : 三菱ガス化学(株)製、商品名「TETRAD−C(テトラッド−C)」(1,3−ビス(N,N−ジグリシジルアミノメチル)シクロヘキサン、エポキシ当量:110、官能基数:4)
デナコールEX−512 : ナガセケムテックス(株)製、商品名「デナコール EX−512」(Polyglycerol Polyglycidyl Ether、エポキシ当量:168、官能基数:約4)
[カルボン酸含有アクリル系重合体(C)を含む増粘剤]
SNシックナー630 : サンノプコ(株)製、商品名「SNシックナー630」(有効成分:30重量%、カルボン酸含有アクリル系重合体(C)を構成する原料モノマー全量中のアクリル酸及びメタクリル酸の合計量(以下、単に「アクリル酸及びメタクリル酸の合計量」と称する場合がある):21重量%以上)
SNシックナー634 : サンノプコ(株)製、商品名「SNシックナー634」(有効成分:30重量%、アクリル酸及びメタクリル酸の合計量:21重量%以上)
SNシックナー640 : サンノプコ(株)製、商品名「SNシックナー640」(有効成分:30重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
アロンA−7070 : 東亞合成(株)製、商品名「アロンA−7070」(有効成分:20重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
アロンA−7075 : 東亞合成(株)製、商品名「アロンA−7075」(有効成分:20重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
アロンB−300K : 東亞合成(株)製、商品名「アロンB−300K」(有効成分:45重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
アロンB−500 : 東亞合成(株)製、商品名「アロンB−500」(有効成分:35重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
プライマル ASE−60 : ローム・アンド・ハース社製、商品名「プライマルASE−60」(有効成分:28重量%、アクリル酸及びメタクリル酸の合計量:41重量%以上)
[ウレタン会合系増粘剤]
アデカノールUH−550 : (株)ADEKA製、商品名「アデカノール UH−550」(有効成分30重量%)
一方、カルボン酸含有アクリル系重合体(C)を含有しない場合(比較例1、2)には粘着剤層にハジキ欠点が生じ、外観が不良であった。また、非水溶性架橋剤を用いない場合(比較例3)には、貼り付け保存後の粘着力(40℃1週間貼付保存後粘着力)が大きくなり、経時での粘着力上昇が大きく、また汚染も生じた。
このように、本発明の規定を満たさない粘着剤組成物を用いた場合には、外観特性、粘着力上昇防止性の両立はできなかった。
Claims (6)
- (メタ)アクリル酸アルキルエステル及びカルボキシル基含有不飽和単量体を必須の原料モノマーとして構成され、原料モノマー全量中の(メタ)アクリル酸アルキルエステルの含有量が70〜99.5重量%、カルボキシル基含有不飽和単量体の含有量が0.5〜10重量%であるアクリルエマルション系重合体(A)、非水溶性架橋剤(B)、並びに(メタ)アクリル酸を必須の原料モノマーとして構成され、原料モノマー全量中のアクリル酸及びメタクリル酸の合計量が11重量%以上であるカルボン酸含有アクリル系重合体(C)を含むことを特徴とする再剥離用水分散型アクリル系粘着剤組成物。
- アクリルエマルション系重合体(A)が、分子中にラジカル重合性官能基を含む反応性乳化剤を用いて重合された重合体である請求項1に記載の再剥離用水分散型アクリル系粘着剤組成物。
- アクリルエマルション系重合体(A)の原料モノマーとして用いられるカルボキシル基含有不飽和単量体のカルボキシル基1モルに対する、非水溶性架橋剤(B)のカルボキシル基と反応しうる官能基のモル数が0.3〜1.3モルである請求項1または2に記載の再剥離用水分散型アクリル系粘着剤組成物。
- 基材の少なくとも片面側に、請求項1〜3のいずれかの項に記載の再剥離用水分散型アクリル系粘着剤組成物から形成された粘着剤層を有することを特徴とする粘着シート。
- 前記粘着剤層の溶剤不溶分が90重量%以上、破断点伸度が200%以下である請求項4に記載の粘着シート。
- 光学部材用の表面保護フィルムである請求項4または5に記載の粘着シート。
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-
2011
- 2011-02-25 JP JP2011040691A patent/JP5719194B2/ja active Active
-
2012
- 2012-02-23 TW TW101106073A patent/TWI518160B/zh active
- 2012-02-24 KR KR1020120018868A patent/KR101850551B1/ko not_active Application Discontinuation
- 2012-02-24 CN CN201210044649.4A patent/CN102676094B/zh active Active
- 2012-02-24 US US13/404,823 patent/US20120219795A1/en not_active Abandoned
- 2012-02-27 EP EP12157029.5A patent/EP2492330B1/en not_active Not-in-force
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WO2019130613A1 (en) | 2017-12-28 | 2019-07-04 | Nitto Denko Corporation | Method for producing glass unit, pressure-sensitive adhesive sheet, and use of corrosion inhibitor |
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US11760066B2 (en) | 2019-06-27 | 2023-09-19 | Nitto Denko Corporation | Method for protecting Low-E glass plate, method for producing glass unit, laminate and protective sheet for Low-E glass plate |
US12017950B2 (en) | 2019-06-27 | 2024-06-25 | Nitto Denko Corporation | Low-E glass plate, protective sheet for low-E glass plate and use thereof |
WO2021215244A1 (ja) | 2020-04-22 | 2021-10-28 | 日東電工株式会社 | Low-Eガラス板の保護方法、ガラスユニットの製造方法、積層体およびLow-Eガラス板用保護シート |
Also Published As
Publication number | Publication date |
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KR20120098469A (ko) | 2012-09-05 |
JP2012177036A (ja) | 2012-09-13 |
EP2492330A2 (en) | 2012-08-29 |
CN102676094B (zh) | 2016-06-15 |
TW201239055A (en) | 2012-10-01 |
EP2492330A3 (en) | 2012-09-05 |
CN102676094A (zh) | 2012-09-19 |
TWI518160B (zh) | 2016-01-21 |
KR101850551B1 (ko) | 2018-04-19 |
EP2492330B1 (en) | 2014-07-30 |
US20120219795A1 (en) | 2012-08-30 |
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