JP6030560B2 - 組成物及びそれを用いた部材の仮固定方法 - Google Patents
組成物及びそれを用いた部材の仮固定方法 Download PDFInfo
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- JP6030560B2 JP6030560B2 JP2013533741A JP2013533741A JP6030560B2 JP 6030560 B2 JP6030560 B2 JP 6030560B2 JP 2013533741 A JP2013533741 A JP 2013533741A JP 2013533741 A JP2013533741 A JP 2013533741A JP 6030560 B2 JP6030560 B2 JP 6030560B2
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- acrylate
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- 238000000034 method Methods 0.000 title claims description 40
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- 239000000853 adhesive Substances 0.000 claims description 141
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- 239000003795 chemical substances by application Substances 0.000 claims description 59
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- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical class C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 3
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- 230000001771 impaired effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- SGGOJYZMTYGPCH-UHFFFAOYSA-L manganese(2+);naphthalene-2-carboxylate Chemical compound [Mn+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 SGGOJYZMTYGPCH-UHFFFAOYSA-L 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- GYVGXEWAOAAJEU-UHFFFAOYSA-N n,n,4-trimethylaniline Chemical compound CN(C)C1=CC=C(C)C=C1 GYVGXEWAOAAJEU-UHFFFAOYSA-N 0.000 description 1
- HKJNHYJTVPWVGV-UHFFFAOYSA-N n,n-diethyl-4-methylaniline Chemical compound CCN(CC)C1=CC=C(C)C=C1 HKJNHYJTVPWVGV-UHFFFAOYSA-N 0.000 description 1
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 description 1
- DQMWMUMCNOJLSI-UHFFFAOYSA-N n-carbamothioylbenzamide Chemical compound NC(=S)NC(=O)C1=CC=CC=C1 DQMWMUMCNOJLSI-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- REEZZSHJLXOIHL-UHFFFAOYSA-N octanoyl chloride Chemical compound CCCCCCCC(Cl)=O REEZZSHJLXOIHL-UHFFFAOYSA-N 0.000 description 1
- 239000011242 organic-inorganic particle Substances 0.000 description 1
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 1
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- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- PWGIEBRSWMQVCO-UHFFFAOYSA-N phosphono prop-2-enoate Chemical compound OP(O)(=O)OC(=O)C=C PWGIEBRSWMQVCO-UHFFFAOYSA-N 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
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- 229920001155 polypropylene Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
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- 239000000523 sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 238000012719 thermal polymerization Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000004992 toluidines Chemical class 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Chemical class 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
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- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
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- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/003—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2009/00—Layered products
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- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
(1)部材同士の接着に使用する組成物の硬化体を水に浸漬して接着した部材同士を水に浸漬し取り外す仮固定用の組成物であり、かつ、(A)多官能(メタ)アクリレート、(B)単官能(メタ)アクリレート、(C)有機過酸化物、(D)分解促進剤、(E)光重合開始剤及び(G)粒状物質を含有する組成物を二剤に分け、第一剤が少なくとも(C)を含有し、第二剤が少なくとも(D)を含有する二剤型の組成物。
(2)更に、(F)有機系熱膨張性粒子を含有する(1)に記載の組成物。
(3)硬化体のガラス転移温度が0〜45℃である(1)または(2)に記載の組成物。
(4)(1)〜(3)の何れかに記載の組成物において、下記1〜4を満たす、組成物:
1.(E)が、ベンジルジメチルケタール、オキシ−フェニル−アセチックアシッド2−[2−オキソ−2−フェニル−アセトキシ−エトキシ]−エチルエステル及びオキシ−フェニル−アセチックアシッド2−[2−ヒドロキシ−エトキシ]−エチルエステルからなる群のうちの1種又は2種以上であること;
2.(G)が架橋ポリ(メタ)アクリル酸メチル粒子、架橋ポリスチレン粒子及び架橋ポリ(メタ)アクリル酸メチルポリスチレン共重合体粒子からなる群のうちの1種又は2種以上であること;
3.(A)多官能(メタ)アクリレートが、多官能(メタ)アクリレートオリゴマー/ポリマー、及び/又は、多官能(メタ)アクリレートモノマーを含有すること;
4.(B)単官能(メタ)アクリレートが、フェノールエチレンオキサイド2モル変性(メタ)アクリレート、2−(1,2−シクロヘキサンジカルボキシイミド)エチル(メタ)アクリレート及び2−ヒドロキシ−3−フェノキシプロピル(メタ)アクリレートからなる群のうちの1種又は2種以上を含有すること。
(5)重合禁止剤を含有する(1)〜(4)の何れかに記載の組成物。
(6)硬化性樹脂である(1)〜(5)の何れかに記載の組成物。
(7)光硬化性である(1)〜(6)の何れかに記載の組成物。
(8)常温硬化性である(1)〜(7)の何れかに記載の組成物。
(9)光硬化性かつ常温硬化性である(1)〜(8)の何れかに記載の組成物。
(10)(1)〜(9)の何れかに記載の組成物を含有する接着剤組成物。
(11)光線透過率が0.1%未満の部位と光線透過率が50%以上の部位を併せ持つ部材同士の接着に使用する(10)に記載の接着剤組成物。
(12)光線透過率が0.1%未満の部材同士の接着に使用する(10)に記載の接着剤組成物。
(13)(10)に記載の接着剤組成物を用いて部材同士を接着し固定してなる構造体。
(14)可視光線又は紫外線を(10)に記載の接着剤組成物に照射して部材同士を接着して仮固定し、該仮固定された部材を加工後、可視光線又は紫外線を該接着剤組成物に照射し、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
(15)可視光線又は紫外線を(10)に記載の接着剤組成物に照射して部材同士を接着した後、放置して仮固定し、該仮固定された部材を加工後、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
(16)(10)に記載の接着剤組成物を放置して部材同士を接着、仮固定し、該仮固定された部材を加工後、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
(17)接着剤組成物が第一剤と第二剤を予め混合して得られたものである(14)〜(16)の何れかに記載の部材の仮固定方法。
(18)2〜100枚の部材を接着し積層させて積層接着体を作製した後、該積層接着体を水に浸漬して接着剤組成物の硬化体を積層接着体から取り外す(14)〜(17)の何れかに記載の部材の仮固定方法。
(19)(14)〜(18)の何れかに記載の部材が、光線透過率が0.1%未満の部位と該透過率が50%以上の部位を併せ持つ部材である部材の仮固定方法。
(20)(14)〜(18)の何れかに記載の部材が、光線透過率が0.1%未満の部材である部材の仮固定方法。
流速:1.0ml/min
設定温度:40℃カラム構成:東ソー社製「TSK guardcolumn MP(×L)」6.0mmID×4.0cm1本、および東ソー社製「TSK−GELMULTIPOREHXL−M」7.8mmID×30.0cm(理論段数16,000段)2本、計3本(全体として理論段数32,000段)、
サンプル注入量:100μl(試料液濃度1mg/ml)
送液圧力:39kg/cm2
検出器:RI検出器
(F)有機系熱膨張性粒子としては、(A)〜(E)に溶解しない有機系熱膨張性粒子が好ましい。(F)有機系熱膨張性粒子としては、マイクロカプセル内に、有機材料(ポリマー)により有機溶剤が封入された熱膨張性のマイクロカプセルを使用することができる。例えば、外殻の有機材料が加熱により軟化するとともに内殻の溶剤がガス化し、体積が5〜250倍に膨張する粒子である。例えば、内殻の溶剤としては、イソブタン、ペンタン、石油エーテル、ヘキサン、オクタン、イソオクタン等の有機溶剤が挙げられ、それらの有機溶剤を、外殻である塩化ビニリデン、アクリロニトリル、アクリル酸エステル、メタクリル酸エステル等からなる熱可塑性樹脂で包み込んだ熱膨張性マイクロカプセルを好ましく使用できる。
(接着剤組成物の作製)
表1の使用材料を用いた。表2の組成で各使用材料を混合して、第一剤と第二剤からなる二剤型仮固定用接着剤組成物を調製した(二剤を二液ということもある)。得られた接着剤組成物を使用して、以下に示す評価方法にてガラス転移温度測定、引張せん断接着強さ測定、接着・剥離試験(A)〜(F)、積層接着・剥離試験を行った。結果を表3〜5に示す。表2の組成物名には、表1に示す略号を用いた。積算光量は紫外線積算照度計(アイグラフィック社製:EYE UVMETER UVPF−A1(365nm受光器使用))により測定した。
UV硬化による接着剤硬化体のガラス転移温度(表の「2液+UV」):第一剤と第二剤を等量混合した接着剤組成物を、1mm厚のシリコンシートを型枠とし、PETフィルムに挟み込んだ。接着剤組成物を、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量2000mJ/cm2の条件にて光を上面から照射、硬化させた後、更に下面から365nmの波長の積算光量2000mJ/cm2の条件にて光を下面から照射、硬化させ、厚さ1mmの接着剤組成物の硬化体を作製した。作製した硬化体をカッターにて長さ50mm×幅5mmに切断し、ガラス転移温度測定用硬化体とした。得られた硬化体をセイコー電子産業社製、動的粘弾性測定装置「DMS210」により、窒素雰囲気中にて前記硬化体に1Hzの引張方向の応力及び歪みを加え、昇温速度毎分2℃の割合で昇温しながらtanδを測定し、該tanδのピークトップの温度をUV照射による接着剤硬化体のガラス転移温度とした。
接着基材である青板硝子A(長さ150mm×幅150mm×厚さ1.7mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)を貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量2000mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体が完全に接着していることを確認した後、接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ2回照射し、合計4000mJ/cm2の光を照射した(剥離用UV照射)。その後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。剥離時間は、温水に浸漬してから、部材が剥離するまでの時間をいう。
接着基材である青板硝子A(長さ150mm×幅150mm×厚さ1.7mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)を貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量2000mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体を23℃で24時間養生して硬化させ、完全に接着していることを確認した後、接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ8回照射し、合計16000mJ/cm2の光を照射した(剥離用UV照射)。その後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
接着基材である青板硝子A(長さ150mm×幅150mm×厚さ1.7mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)を貼り合わせ、23℃で24時間養生して硬化させ、完全に接着していることを確認した後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
接着基材である青板硝子A(長さ150mm×幅150mm×厚さ1.7mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)を貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量2000mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体を23℃で24時間養生して硬化させ、完全に接着していることを確認した。その後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
接着基材である青板硝子(長さ80mm×幅80mm×厚さ1.1mm)上に、黒色インクを上記青板硝子の中央に塗工し、長さ80mm×幅18mm×厚さ10μmのUV不透過部3と青板硝子表面4を有する黒色インク塗工ガラス11を2枚作製した(図2、2枚の黒色インク塗工ガラスを11A、11Bということもある)。350〜450nmの光線透過率を、UV不透過部又はUV透過部に対して1nm毎に測定し、その平均値を、UV不透過部又はUV透過部の350〜450nmの波長における光線透過率とした。その際には、空気をブランクとして採用した。該測定を行った結果、UV不透過部の350〜450nmの波長における光線透過率は0.0%、UV透過部の350〜450nmの波長における光線透過率は91%であった。黒色インク塗工ガラス11は、18mmの加飾印刷部を有する接着基材であり、接着・剥離試験(E)の青板硝子A(長さ80mm×幅80mm×厚さ1.1mm)、青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)が該当する。18mmの加飾印刷部を有する青板硝子Aに、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、18mmの加飾印刷部を有する青板硝子B(長さ80mm×幅80mm×厚さ1.1mm)を、黒色インク塗工部が重なるように貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量50mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体を23℃で4時間養生して硬化させ、完全に接着していることを確認した後、接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ8回照射し、合計16000mJ/cm2の光を照射した(剥離用UV照射)。その後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
18mmの加飾印刷部を有する青板硝子A(黒色インク塗工ガラス11、長さ80mm×幅80mm×厚さ1.1mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、18mmの加飾印刷部を有する青板硝子B(黒色インク塗工ガラス11、長さ80mm×幅80mm×厚さ1.1mm)を、黒色インク塗工部が重なるように貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量50mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体を23℃で24時間養生して硬化させ、完全に接着していることを確認した後、接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ8回照射し、合計16000mJ/cm2の光を照射した(剥離用UV照射)。その後、得られた試験体を、温水(90℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
18mmの加飾印刷部を有する青板硝子A(黒色インク塗工ガラス11、長さ80mm×幅80mm×厚さ1.1mm)上に、第一剤と第二剤を等量混合した接着剤組成物を2.5g塗布し、18mmの加飾印刷部を有する青板硝子B(黒色インク塗工ガラス11、長さ80mm×幅80mm×厚さ1.1mm)を、黒色インク塗工部が重なるように貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量50mJ/cm2の条件にて青板硝子B上面から光を照射、硬化させ、青板硝子同士を接着した(固定用UV照射)。得られた接着試験体を23℃で24時間養生して硬化させ、完全に接着していることを確認した後、接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ8回照射し、合計16000mJ/cm2の光を照射した(剥離用UV照射)。その後、得られた試験体を、温水(80℃)に浸漬し、青板硝子同士が剥離する時間を測定し、又剥離後のフィルムの状態も確認した。
1.板ガラス積層体の作製
接着基材である板ガラス(長さ530mm×幅420mm×厚さ0.7mm)上に、黒色インクを上記青板硝子の端から180mmの位置及び360mmの位置に塗工し、長さ530mm×幅35mm×厚さ10μmのUV不透過部5を2カ所と青板硝子表面6を有する黒色インク塗工ガラス12を12枚作製した(図3)。UV不透過部5の幅の中央が、上記青板硝子の端から180mmの位置及び360mmの位置になるように塗工した。第一剤と第二剤を等量混合した接着剤組成物を介して黒色インク塗工ガラス12を12枚貼り合わせ、板ガラスの積層体を作製した。具体的には、1枚目の黒色インク塗工ガラス12上に上記接着剤組成物4gを接着基材全面に塗布した後、1枚目の黒色インク塗工ガラス12の上に、2枚目の黒色インク塗工ガラス12を、黒色インク塗工部が重なるようにして貼り合わせた。1枚目の黒色インク塗工ガラス12の下面側からUV照射し、上記接着剤組成物を硬化させた。ベルトコンベア式メタルハライドランプを使用し、365nmの波長のUV照射量は50mJ/cm2とした(固定用UV照射)。固定用UV照射後に、養生時間を採用することなく、直ちにこの手順を繰り返すことで、12枚の板ガラスからなる板ガラス積層体を作製した。350〜450nmの波長における光線透過率は、分光光度計(型式UV−2550(島津製作所社製))を用いて測定した。350〜450nmの光線透過率を、UV不透過部又はUV透過部に対して1nm毎に測定し、その平均値を、UV不透過部又はUV透過部の350〜450nmの波長における光線透過率とした。その際には、空気をブランクとして採用した。該測定を行った結果、UV不透過部の350nm〜450nmの波長における光線透過率は0.0%、UV透過部の350〜450nmの波長における光線透過率は91%であった。
次に、板ガラスの積層体を受け台に固定した後、円板カッターによって所定の切断線に沿って厚み方向に切断し、分割された板ガラスの積層体を作製した。このとき、各板ガラスは、横100mm×縦50mm×厚み0.7mmに分割された。
次に、受け台に分割された板ガラス積層体を固定し、受け台上の板ガラス積層体に回転砥石を用いて研削することで外形を加工した。
表6に示す種類の原材料を表6に示す組成で使用したこと以外は実施例1と同様にして接着剤組成物を作製した。得られた接着剤組成物について、実施例1と同様にガラス転移温度、引張せん断接着強さを測定した。結果を表7に示す。
表8に示す種類の原材料を表8に示す組成で使用したこと以外は実施例1と同様にして接着剤組成物を作製した。得られた接着剤組成物について、実施例1と同様にガラス転移温度、引張せん断接着強さ、接着・剥離試験(F)、積層接着・加工・剥離試験を実施した。結果を表9に示す。
表10に示す実施例や比較例の接着剤組成物を用いて長さ80mm×幅80mm×厚さ1mmの青板硝子Aと長さ150mm×幅150mm×厚さ2mmの青板硝子Bを、第一剤と第二剤を等量混合した接着剤組成物を用いて貼り合わせ、ベルトコンベア式メタルハライドランプを使用し、365nmの波長の積算光量2000mJ/cm2の条件にて青板硝子A上面から光を照射、硬化させ、青板硝子同士を接着した。この接着試験体の青板ガラスA部分のみをダイシング装置を使用して10mm角に切断し、切断接着試験体を得た。実施例の場合、切断中に青板ガラスAの脱落は発生せず、良好な加工性を示した。その後、切断接着試験体にベルトコンベア式メタルハライドランプを使用し、365nmの波長の光を接着剤組成物に2000mJ/cm2ずつ5回照射し、合計10000mJ/cm2の光を照射した(剥離用UV照射)。その後、切断接着試験体を90℃の温水に浸漬し、青板硝子A及び青板硝子Bを剥離させ、切断試験片を得た。剥離した切断試験片を無作為に10個取り出し、その切断試験片の裏面(接着剤組成物で仮固定した面)の各片を、光学顕微鏡を用いて観察し、ガラスが欠けている箇所の最大幅を測定し、その平均値と標準偏差を求めた。結果を表10に示す。
本発明の組成物は、その組成故に常温硬化性を有し、常温で硬化し、その硬化体は切削水等に影響されずに、高い接着強度を発現できる。
2 板ガラス表面
3、5 UV不透過部
4、6 青板ガラス表面
10 携帯電話の表示画面
11、12 黒色インク塗工ガラス
Claims (20)
- 部材同士の接着に使用する組成物の硬化体を水に浸漬して接着した部材同士を取り外す仮固定用の組成物であり、かつ、(A)多官能(メタ)アクリレート、(B)単官能(メタ)アクリレート、(C)有機過酸化物、(D)有機過酸化物の分解促進剤、(E)光重合開始剤及び(G)粒状物質を含有する組成物を二剤に分け、第一剤が少なくとも(C)を含有し、第二剤が少なくとも(D)を含有する二剤型の組成物。
- 更に、(F)有機系熱膨張性粒子を含有する請求項1に記載の組成物。
- 硬化体のガラス転移温度が0〜45℃である請求項1または2に記載の組成物。
- 請求項1〜3の何れか1項に記載の組成物において、下記(1)〜(4)を満たす、組成物:
(1)(E)が、ベンジルジメチルケタール、オキシ−フェニル−アセチックアシッド2−[2−オキソ−2−フェニル−アセトキシ−エトキシ]−エチルエステル及びオキシ−フェニル−アセチックアシッド2−[2−ヒドロキシ−エトキシ]−エチルエステルからなる群のうちの1種又は2種以上であること;
(2)(G)が架橋ポリ(メタ)アクリル酸メチル粒子、架橋ポリスチレン粒子及び架橋ポリ(メタ)アクリル酸メチルポリスチレン共重合体粒子からなる群のうちの1種又は2種以上であること;
(3)(A)多官能(メタ)アクリレートが、多官能(メタ)アクリレートオリゴマー/ポリマー、及び/又は、多官能(メタ)アクリレートモノマーを含有すること;
(4)(B)単官能(メタ)アクリレートが、フェノールエチレンオキサイド2モル変性(メタ)アクリレート、2−(1,2−シクロヘキサンジカルボキシイミド)エチル(メタ)アクリレート及び2−ヒドロキシ−3−フェノキシプロピル(メタ)アクリレートからなる群のうちの1種又は2種以上を含有すること。 - 重合禁止剤を含有する請求項1〜4の何れか1項に記載の組成物。
- 硬化性樹脂である請求項1〜5の何れか1項に記載の組成物。
- 光硬化性である請求項1〜6の何れか1項に記載の組成物。
- 常温硬化性である請求項1〜7の何れか1項に記載の組成物。
- 光硬化性かつ常温硬化性である請求項1〜8の何れか1項に記載の組成物。
- 請求項1〜9の何れか1項に記載の組成物を含有する接着剤組成物。
- 光線透過率が0.1%未満の部位と光線透過率が50%以上の部位を併せ持つ部材同士の接着に使用する請求項10に記載の接着剤組成物。
- 光線透過率が0.1%未満の部材同士の接着に使用する請求項10に記載の接着剤組成物。
- 請求項10に記載の接着剤組成物を用いて部材同士を接着し固定してなる構造体。
- 可視光線又は紫外線を請求項10に記載の接着剤組成物に照射して部材同士を接着して仮固定し、該仮固定された部材を加工後、可視光線又は紫外線を該接着剤組成物に照射し、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
- 可視光線又は紫外線を請求項10に記載の接着剤組成物に照射して部材同士を接着した後、放置して仮固定し、該仮固定された部材を加工後、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
- 請求項10に記載の接着剤組成物を放置して部材同士を接着、仮固定し、該仮固定された部材を加工後、該接着剤組成物の硬化体を水に浸漬して該接着剤組成物の硬化体を部材から取り外す部材の仮固定方法。
- 接着剤組成物が第一剤と第二剤を予め混合して得られたものである請求項14〜16の何れか1項に記載の部材の仮固定方法。
- 2〜100枚の部材を接着し積層させて積層接着体を作製した後、該積層接着体を水に浸漬して接着剤組成物の硬化体を積層接着体から取り外す請求項14〜17の何れか1項に記載の部材の仮固定方法。
- 請求項14〜18の何れか1項に記載の部材が、光線透過率が0.1%未満の部位と該透過率が50%以上の部位を併せ持つ部材である部材の仮固定方法。
- 請求項14〜18の何れか1項に記載の部材が、光線透過率が0.1%未満の部材である部材の仮固定方法。
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