JP2014019801A - Double-sided adhesive tape for fixing abrasive member - Google Patents
Double-sided adhesive tape for fixing abrasive member Download PDFInfo
- Publication number
- JP2014019801A JP2014019801A JP2012160267A JP2012160267A JP2014019801A JP 2014019801 A JP2014019801 A JP 2014019801A JP 2012160267 A JP2012160267 A JP 2012160267A JP 2012160267 A JP2012160267 A JP 2012160267A JP 2014019801 A JP2014019801 A JP 2014019801A
- Authority
- JP
- Japan
- Prior art keywords
- sensitive adhesive
- pressure
- parts
- resin
- adhesive layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002390 adhesive tape Substances 0.000 title abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 99
- 239000011347 resin Substances 0.000 claims abstract description 99
- 238000005498 polishing Methods 0.000 claims abstract description 96
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 66
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 66
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 30
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 30
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003208 petroleum Substances 0.000 claims abstract description 24
- 239000012790 adhesive layer Substances 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 229920003023 plastic Polymers 0.000 claims abstract description 13
- 239000004033 plastic Substances 0.000 claims abstract description 13
- 125000003118 aryl group Chemical group 0.000 claims abstract description 9
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 174
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- 239000000178 monomer Substances 0.000 claims description 56
- 150000002148 esters Chemical group 0.000 claims description 29
- 230000009477 glass transition Effects 0.000 claims description 19
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- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 57
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- 125000004185 ester group Chemical group 0.000 abstract 1
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- 239000000243 solution Substances 0.000 description 45
- -1 2-ethylhexyl Chemical group 0.000 description 41
- 239000000853 adhesive Substances 0.000 description 38
- 230000001070 adhesive effect Effects 0.000 description 38
- 238000000034 method Methods 0.000 description 29
- 229920000139 polyethylene terephthalate Polymers 0.000 description 25
- 239000005020 polyethylene terephthalate Substances 0.000 description 25
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- 239000000203 mixture Substances 0.000 description 15
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 13
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- 229920002803 thermoplastic polyurethane Polymers 0.000 description 11
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- 125000005442 diisocyanate group Chemical group 0.000 description 9
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 9
- 239000004342 Benzoyl peroxide Substances 0.000 description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 description 8
- 239000012948 isocyanate Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000013522 chelant Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000002585 base Substances 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 150000002513 isocyanates Chemical class 0.000 description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- WWUCYCYSEUEANO-UHFFFAOYSA-N 2-(aziridin-1-yl)acetamide Chemical compound NC(=O)CN1CC1 WWUCYCYSEUEANO-UHFFFAOYSA-N 0.000 description 3
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
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- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- 239000007864 aqueous solution Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
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- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 2
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
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Images
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本発明は、研磨品の製造に使用する両面粘着テープに関する。 The present invention relates to a double-sided pressure-sensitive adhesive tape used for manufacturing an abrasive product.
従来、自動車、光学機器、半導体等の分野では様々な部品、部材の表面研磨が行われている。例えば、液晶ディスプレイ用ガラス、ハードディスク用基板、光学レンズ、シリコンウェハや集積回路等の被研磨体は、研磨装置に両面粘着テープを用いて取り付けられた硬質樹脂シートや軟質樹脂シート、研磨布等の研磨パッドと研磨液により室温から約８０℃雰囲気下で研磨されるのが一般的である。
さらに、軟質ウレタン発泡体シートに代表される軟質樹脂シート等の研磨用吸着パッドと称される研磨用樹脂シートを、被研磨体の保持および固定に用いることで、被研磨体を安定的に研磨できる。
Conventionally, surface polishing of various parts and members has been performed in the fields of automobiles, optical devices, semiconductors, and the like. For example, objects to be polished such as glass for liquid crystal displays, substrates for hard disks, optical lenses, silicon wafers and integrated circuits are hard resin sheets, soft resin sheets, polishing cloths, etc. attached to the polishing apparatus using double-sided adhesive tape. In general, polishing is performed in an atmosphere of about 80 ° C. from room temperature with a polishing pad and a polishing liquid.
In addition, a polishing resin sheet called a polishing adsorption pad such as a soft resin sheet represented by a soft urethane foam sheet is used for holding and fixing the object to be polished, thereby stably polishing the object to be polished. it can.
研磨用樹脂シートは被研磨体表面を可能な限り平坦に研磨することが重要であるため、それ自体の平坦性が高いことが必要である。そのため研磨用樹脂シート表面をバフと称される工法等で研削することで平坦化し、例えば軟質ウレタン発泡シートを研磨した場合は、研磨面に発泡セル開放面が形成される。 Since it is important for the polishing resin sheet to polish the surface of the object to be polished as flat as possible, the polishing resin sheet needs to have high flatness. Therefore, the surface of the polishing resin sheet is flattened by grinding with a method called a buff or the like. For example, when a soft urethane foam sheet is polished, a foam cell open surface is formed on the polishing surface.
一般的に、研磨部材のうち研磨用部材は、研磨用樹脂シートと両面粘着テープから構成されている。また、研磨部材のうち被研磨体固定部材は、研磨用吸着パッドと両面粘着テープから構成されている。
両者の両面粘着テープとも両面粘着テープの一方の粘着剤層が、シートまたはパッドを固定し、他方の粘着剤層が研磨装置と固定する。
Generally, the polishing member among the polishing members is composed of a polishing resin sheet and a double-sided adhesive tape. Moreover, the to-be-polished member fixing member among the polishing members is composed of a polishing suction pad and a double-sided adhesive tape.
In both double-sided pressure-sensitive adhesive tapes, one pressure-sensitive adhesive layer of the double-sided pressure-sensitive adhesive tape fixes the sheet or pad, and the other pressure-sensitive adhesive layer fixes the polishing apparatus.
図１により両面粘着テープの使用方法を説明する。まず、両面粘着テープ２Aは、研磨装置の上定盤１Ａと研磨用吸着パッド３を接着する。そして被研磨体５は、その外周をテンプレート４で保持された状態で研磨用吸着パッド３と密着する。次に、両面粘着テープ２Ｂは、研磨装置の下定盤１Ｂと研磨パッド６を接着する。
The usage method of a double-sided adhesive tape is demonstrated with FIG. First, the double-sided pressure-sensitive
研磨工程に使用する研磨液は、被研磨体の種類によるが、ｐＨが約１〜１２の懸濁水溶液を使用するのが一般的である。このような環境の中、研磨部材を固定する両面粘着テープは、研磨工程の開始と同時に研磨液に曝されながら、時には摩擦熱による加熱にも曝されながら使用される。
このような過酷な条件下では、研磨時に研磨部材から両面粘着テープが剥離する問題や、両面粘着テープの粘着剤層が芯材の基材から剥離する問題が生じる場合があった。
The polishing liquid used in the polishing step depends on the type of the object to be polished, but it is common to use a suspended aqueous solution having a pH of about 1 to 12. Under such circumstances, the double-sided pressure-sensitive adhesive tape that fixes the polishing member is used while being exposed to the polishing liquid simultaneously with the start of the polishing process, and sometimes also being exposed to heating by frictional heat.
Under such severe conditions, there may be a problem that the double-sided pressure-sensitive adhesive tape peels off from the polishing member during polishing and a problem that the pressure-sensitive adhesive layer of the double-sided pressure-sensitive adhesive tape peels off from the base material of the core material.
また、被研磨体の生産性を向上するため、研磨部材を長時間連続使用する場合が増加している。従来、研磨部材を固定する両面粘着テープを短時間使用する場合は研磨部材や研磨装置との密着性に問題が生じなかった。しかし、長期間連続使用すると、研磨時の摩擦熱や研磨液の作用によりにより研磨部材や研磨装置との密着性が低下し、両面粘着シートが、研磨部材または研磨装置から剥離することで研磨工程が中断する問題があった。そのため、両面粘着テープは、特に研磨部材との貼付直後の密着性向上を目的として様々な工夫がなされてきた。 Moreover, in order to improve the productivity of a to-be-polished body, the case where a polishing member is continuously used for a long time is increasing. Conventionally, when the double-sided pressure-sensitive adhesive tape for fixing the polishing member is used for a short time, there is no problem in the adhesion with the polishing member or the polishing apparatus. However, if used continuously for a long period of time, the adhesion between the polishing member and the polishing apparatus decreases due to the frictional heat during polishing and the action of the polishing liquid, and the double-sided PSA sheet is peeled off from the polishing member or the polishing apparatus. There was a problem that interrupted. For this reason, the double-sided pressure-sensitive adhesive tape has been devised in various ways for the purpose of improving the adhesion immediately after being attached to the polishing member.
特許文献１では、アクリル系重合体に、軟化点１００〜１７０℃の重合ロジンエステルを配合した粘着テープが開示されている。
また、特許文献２では、（メタ）アクリル酸ブチルを９０重量％以上含有するモノマー混合物を共重合して得られた（メタ）アクリル酸アルキルエステル系共重合体にキシレン樹脂を配合した粘着テープが開示されている。 Moreover, in patent document 2, the adhesive tape which mix | blended xylene resin with the (meth) acrylic-acid alkylester type-copolymer obtained by copolymerizing the monomer mixture containing 90 weight% or more of (meth) butyl acrylate is provided. It is disclosed.
しかし、従来の両面粘着テープは、粘着付与樹脂に重合ロジンエステルのみ使用し、かつその芯材には不織布を使用しているため、長時間研磨したときに研磨液により両面粘着テープが劣化し、さらに粘着テープの密着性が不足する問題があった。また、従来の両面粘着テープは、キシレン樹脂やテルペンフェノール樹脂を配合しているため柔軟性が低下することにより研磨用樹脂シートとの密着性が不足する問題があった。 However, the conventional double-sided pressure-sensitive adhesive tape uses only polymerized rosin ester as the tackifier resin and uses a non-woven fabric as its core material, so the double-sided pressure-sensitive adhesive tape deteriorates due to the polishing liquid when polished for a long time, Furthermore, there was a problem that the adhesiveness of the adhesive tape was insufficient. Moreover, since the conventional double-sided pressure-sensitive adhesive tape contains a xylene resin or a terpene phenol resin, there is a problem that the adhesiveness with the polishing resin sheet is insufficient due to a decrease in flexibility.
本発明は、研磨部材や基材に対する密着性が良好であるため長時間研磨工程を行っても研磨時の摩擦熱や研磨液で劣化せずに密着性を維持できる研磨部材固定用両面粘着テープの提供を目的とする。 The present invention provides a double-sided pressure-sensitive adhesive tape for fixing an abrasive member, which has good adhesion to an abrasive member and a substrate, and can maintain adhesion without being deteriorated by frictional heat or polishing liquid during polishing even after a long polishing step. The purpose is to provide.
本発明は、粘着剤層（１）と、プラスチック基材（２）と、粘着剤層（３）とを備えた研磨部材固定用両面粘着テープであって、
粘着剤層（１）は、アクリル系樹脂（イ）とロジンエステル骨格を有する粘着付与樹脂（ｘ）および芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）とを含有する粘着剤（Ａ）から形成され、
粘着剤（Ａ）は、アクリル系樹脂（イ）１００重量部に対して、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との合計量１５〜３５重量部を含み、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との重量比が（ｘ）／（ｙ）＝３／２〜９／２であり、
アクリル系樹脂（イ）は、そのガラス転移温度が−７０℃以上０℃以下で、その重量平均分子量が４０万〜７０万であり、かつアクリル酸ブチル８５〜９７重量％とアクリル酸ブチル以外のモノマー３〜１５重量％を重合してなることを構成とする研磨部材固定用両面粘着テープである。
The present invention is a double-sided pressure-sensitive adhesive tape for fixing an abrasive member comprising an adhesive layer (1), a plastic substrate (2), and an adhesive layer (3),
The pressure-sensitive adhesive layer (1) comprises a pressure-sensitive adhesive (A) containing an acrylic resin (I), a tackifying resin (x) having a rosin ester skeleton, and a tackifying resin (y) having an aromatic petroleum-based skeleton. )
The pressure-sensitive adhesive (A) includes a total amount of 15 to 35 parts by weight of the tackifier resin (x) and the tackifier resin (y) with respect to 100 parts by weight of the acrylic resin (b), and the tackifier resin (x ) And the tackifier resin (y) are (x) / (y) = 3/2 to 9/2,
The acrylic resin (A) has a glass transition temperature of −70 ° C. or more and 0 ° C. or less, a weight average molecular weight of 400,000 to 700,000, and 85 to 97% by weight of butyl acrylate and butyl acrylate. It is a double-sided pressure-sensitive adhesive tape for fixing an abrasive member comprising polymerizing 3 to 15% by weight of a monomer.
上記構成の本発明によれば、両面粘着テープの粘着剤層の少なくとも一方が、ロジンエステル骨格を有する粘着付与樹脂（ｘ）および芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）とを含有する粘着剤（Ａ）から形成され、かつ、粘着剤（Ａ）は、アクリル系樹脂（イ）１００重量部に対して、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との合計量１５〜３５重量部を含み、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との重量比が（ｘ）／（ｙ）＝３／２〜９／２であることにより、接着面積が非常に少ない研磨用樹脂シートの発泡セル開放面に対して良好な粘着力を実現できたことで高い密着性が得られた。この高い密着性により長期間にわたり研磨液に曝された場合でも両面粘着テープの劣化を最小限に抑制できたことで、当該両面粘着テープを使用した研磨用樹脂シートを研磨工程に使用すると被研磨体の生産性を向上することができた。 According to the present invention having the above configuration, at least one of the pressure-sensitive adhesive layers of the double-sided pressure-sensitive adhesive tape comprises a tackifier resin (x) having a rosin ester skeleton and a tackifier resin (y) having an aromatic petroleum resin skeleton. It is formed from the pressure-sensitive adhesive (A) contained, and the pressure-sensitive adhesive (A) is a total amount of the tackifying resin (x) and the tackifying resin (y) with respect to 100 parts by weight of the acrylic resin (A). Including 15 to 35 parts by weight, and the weight ratio of the tackifying resin (x) and the tackifying resin (y) is (x) / (y) = 3/2 to 9/2 High adhesiveness was obtained by realizing a good adhesive force with respect to the open surface of the foamed cell of the polishing resin sheet. Due to this high adhesion, deterioration of the double-sided pressure-sensitive adhesive tape can be minimized even when exposed to the polishing liquid for a long period of time, and if a polishing resin sheet using the double-sided pressure-sensitive adhesive tape is used in the polishing process, it will be polished. We were able to improve body productivity.
本発明により、研磨部材や基材に対する密着性が良好であるため長時間研磨工程を行っても研磨時の摩擦熱や研磨液で劣化せずに密着性を維持できる研磨部材固定用両面粘着テープを提供できた。 The double-sided pressure-sensitive adhesive tape for fixing a polishing member that can maintain the adhesion without being deteriorated by frictional heat or polishing liquid even during a long-time polishing step because of good adhesion to the polishing member and the substrate according to the present invention. Was able to provide.
本発明の研磨部材固定用両面粘着テープは、少なくとも粘着剤層（１）と、プラスチック基材（２）とを備えたものである。また、他の粘着剤層である粘着剤層（３）は、粘着剤層（１）を使用しても良いが、粘着剤層（１）以外の一般的な粘着剤層を使用しても良い。 The double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention comprises at least an adhesive layer (1) and a plastic substrate (2). Moreover, although the adhesive layer (3) which is another adhesive layer may use an adhesive layer (1), even if it uses general adhesive layers other than an adhesive layer (1). good.
この粘着剤層（１）は、アクリル系樹脂（イ）と、ロジンエステル骨格を有する粘着付与樹脂および芳香族系石油系樹脂骨格を有する粘着付与樹脂とを含有する粘着剤（Ａ）から形成することが好ましい。粘着剤（Ａ）を使用することで研磨液に対する耐性、および密着性が優れる粘着剤層（１）が得られる。 This pressure-sensitive adhesive layer (1) is formed from a pressure-sensitive adhesive (A) containing an acrylic resin (I), a tackifier resin having a rosin ester skeleton, and a tackifier resin having an aromatic petroleum resin skeleton. It is preferable. By using the pressure-sensitive adhesive (A), a pressure-sensitive adhesive layer (1) having excellent resistance to the polishing liquid and excellent adhesion can be obtained.
アクリル系樹脂（イ）は、ラジカル重合性不飽和モノマーを、重合開始剤を用いて従来公知の重合法、例えば溶液重合法、塊状重合法、乳化重合法等によって重合することにより得ることができる。
ラジカル重合性不飽和モノマーとしては、（メタ）アクリル酸アルキルエステル、カルボキシル基含有モノマー、および前記以外のモノマーが好ましい。
The acrylic resin (A) can be obtained by polymerizing a radical polymerizable unsaturated monomer by a conventionally known polymerization method such as a solution polymerization method, a bulk polymerization method, an emulsion polymerization method, etc. using a polymerization initiator. .
As the radical polymerizable unsaturated monomer, a (meth) acrylic acid alkyl ester, a carboxyl group-containing monomer, and monomers other than those mentioned above are preferable.
（メタ）アクリル酸アルキルエステルは、アルキル基の炭素数が１〜１４の(メタ)アクリル酸アルキルエステルが好ましい。かかる（メタ）アクリル酸アルキルエステルとしては、例えば（メタ）アクリル酸メチル、（メタ）アクリル酸エチル、（メタ）アクリル酸プロピル、（メタ）アクリル酸ｉｓｏ−プロピル、（メタ）アクリル酸ブチル、（メタ）アクリル酸ｉｓｏ−ブチル、（メタ）アクリル酸ヘキシル、（メタ）アクリル酸オクチル、（メタ）アクリル酸２−エチルヘキシル、（メタ）アクリル酸デシル、（メタ）アクリル酸ドデシル等の直鎖または分岐脂肪族アルコールのアクリル酸エステル及び対応するメタクリル酸エステル等が挙げられる。これらの中でも（メタ）アクリル酸アルキルエステルは、アルキル基の炭素数１〜１０が好ましく、炭素数１〜８がより好ましい。具体的には、アクリル酸ブチルが特に好ましい。（メタ）アクリル酸アルキルエステルは、単独または２種以上使用できる。 The (meth) acrylic acid alkyl ester is preferably a (meth) acrylic acid alkyl ester having 1 to 14 carbon atoms in the alkyl group. Examples of the (meth) acrylic acid alkyl ester include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, iso-propyl (meth) acrylate, butyl (meth) acrylate, ( Linear or branched such as iso-butyl (meth) acrylate, hexyl (meth) acrylate, octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, decyl (meth) acrylate, dodecyl (meth) acrylate Examples include aliphatic alcohol acrylic acid esters and corresponding methacrylic acid esters. Among these, the (meth) acrylic acid alkyl ester preferably has 1 to 10 carbon atoms and more preferably 1 to 8 carbon atoms in the alkyl group. Specifically, butyl acrylate is particularly preferable. The (meth) acrylic acid alkyl ester can be used alone or in combination of two or more.
（メタ）アクリル酸アルキルエステルは、ラジカル重合性不飽和モノマーの合計１００重量％中７０〜９９．９重量％使用することが好ましく、８５〜９７重量％がより好ましい。そして、アクリル酸ブチルは、ラジカル重合性不飽和モノマーの合計１００重量％中、８５〜９７重量％を使用することが好ましい。 The (meth) acrylic acid alkyl ester is preferably used in an amount of 70 to 99.9% by weight, more preferably 85 to 97% by weight, based on a total of 100% by weight of the radical polymerizable unsaturated monomer. And it is preferable to use 85 to 97 weight% of butyl acrylate in the total 100 weight% of a radically polymerizable unsaturated monomer.
カルボキシル基含有モノマーは、例えばアクリル酸、メタクリル酸、無水マレイン酸、マレイン酸、イタコン酸、クロトン酸等が挙げられる。これらの中でもアクリル酸が好ましい。カルボキシル基含有モノマーは、単独または２種以上使用できる。
カルボキシル基含有モノマーは、ラジカル重合性不飽和モノマーの合計１００重量％中０．１〜１０重量％使用することが好ましく、０．２〜５重量％がより好ましく、１〜４重量％がさらに好ましい。カルボキシル基含有モノマーを０．１〜１０重量％使用することで良好な密着性を実現するための粘着力が得やすくなる。
Examples of the carboxyl group-containing monomer include acrylic acid, methacrylic acid, maleic anhydride, maleic acid, itaconic acid, and crotonic acid. Among these, acrylic acid is preferable. The carboxyl group-containing monomer can be used alone or in combination of two or more.
The carboxyl group-containing monomer is preferably used in an amount of 0.1 to 10% by weight, more preferably 0.2 to 5% by weight, even more preferably 1 to 4% by weight, based on a total of 100% by weight of the radical polymerizable unsaturated monomer. . By using 0.1 to 10% by weight of the carboxyl group-containing monomer, it becomes easy to obtain an adhesive force for realizing good adhesion.
（メタ）アクリル酸アルキルエステルおよびカルボキシル基含有モノマー以外のモノマーは、必要に応じて使用することができる。具体的には、例えば（メタ）アクリル酸２−ヒドロキシエチル、（メタ）アクリル酸２−ヒドロキシプロピル、（メタ）アクリル酸２−ヒドロキシブチル、ポリエチレングリコール（メタ）アクリレート等のアルコール性水酸基含有モノマー、
グリシジルアクリレート、グリシジルメタクリレート等のエポキシ基含有モノマー、 Ｎ−ヒドロキシアルキル（メタ）アクリルアミド、Ｎ―アルコキシアルキル（メタ）アクリルアミド、メチロール化アクリルアミド、Ｎ−（１，１−ジメチル−３オキソブチル）アクリルアミド、ダイアセトンアクリルアミド等の（メタ）アクリルアミドモノマー、
燐酸基含有ビニルモノマーや酢酸ビニル、スチレン、ブタジエン等のビニルモノマー、
アセトアセトキシエチルメタクリレート、アルコキシシリル基含有モノマー等が挙げられる。（メタ）アクリル酸アルキルエステルおよびカルボキシル基含有モノマー以外のモノマーは、必要に応じて単独または２種以上使用できる。
これらのモノマーは、ラジカル重合性不飽和モノマーの合計１００重量％中、０〜１０重量％使用することができる。
Monomers other than the (meth) acrylic acid alkyl ester and the carboxyl group-containing monomer can be used as necessary. Specifically, for example, an alcoholic hydroxyl group-containing monomer such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, polyethylene glycol (meth) acrylate,
Epoxy group-containing monomers such as glycidyl acrylate and glycidyl methacrylate, N-hydroxyalkyl (meth) acrylamide, N-alkoxyalkyl (meth) acrylamide, methylolated acrylamide, N- (1,1-dimethyl-3oxobutyl) acrylamide, diacetone (Meth) acrylamide monomers such as acrylamide,
Phosphoric acid group-containing vinyl monomers and vinyl monomers such as vinyl acetate, styrene and butadiene,
Examples include acetoacetoxyethyl methacrylate and alkoxysilyl group-containing monomers. Monomers other than the (meth) acrylic acid alkyl ester and the carboxyl group-containing monomer can be used alone or in combination of two or more as required.
These monomers can be used in an amount of 0 to 10% by weight in a total of 100% by weight of the radical polymerizable unsaturated monomer.
本発明の研磨部材固定用両面粘着テープが所望の密着性を得るためには、その粘着力を高めることが好ましい。そのため、極性基を有するモノマーを使用することが好ましい。具体的には、カルボキシル基含有モノマーに加えて水酸基含有モノマーを使用することが好ましい。 In order for the double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention to obtain desired adhesion, it is preferable to increase its adhesive strength. Therefore, it is preferable to use a monomer having a polar group. Specifically, it is preferable to use a hydroxyl group-containing monomer in addition to the carboxyl group-containing monomer.
アクリル系樹脂（イ）は、種々の重合開始剤を用い、その量、重合温度等の重合諸条件を適宜調整することにより得ることができる。重合開始剤は、過酸化物やアゾ系化合物を使用することが一般的である。
過酸化物は、例えばケトンパーオキサイド類、パーオキシケタール類、ハイドロパーオキサイド類、ジアルキルパーオキサイド類、ジアシルパーオキサイド類、パーオキシジカーボネート類、パーオキシエステル類等が好ましい。
The acrylic resin (A) can be obtained by using various polymerization initiators and appropriately adjusting the polymerization conditions such as the amount and polymerization temperature. As the polymerization initiator, a peroxide or an azo compound is generally used.
As the peroxide, for example, ketone peroxides, peroxyketals, hydroperoxides, dialkyl peroxides, diacyl peroxides, peroxydicarbonates, peroxyesters and the like are preferable.
ケトンパーオキサイド類としては、例えばメチルエチルケトンパーオキシド、シクロヘキサノンパーオキシド、アセチルアセトンパーオキシド等が挙げられる。 Examples of ketone peroxides include methyl ethyl ketone peroxide, cyclohexanone peroxide, and acetylacetone peroxide.
パーオキシケタール類としては、例えば１，１−ジ（ｔ−ヘキシルパーオキシ）−３，３，５−トリメチルシクロヘキサン、１，１−ジ（ｔ−ヘキシルパーオキシ）シクロヘキサン、１，１−ジ（ｔ−ブチルパーオキシ）−２−メチルシクロヘキサン、１，１−ジ（ｔ−ブチルパーオキシ）シクロヘキサン、２，２−ジ（ｔ−ブチルパーオキシ）ブタン等が挙げられる。 Examples of peroxyketals include 1,1-di (t-hexylperoxy) -3,3,5-trimethylcyclohexane, 1,1-di (t-hexylperoxy) cyclohexane, 1,1-di ( t-Butylperoxy) -2-methylcyclohexane, 1,1-di (t-butylperoxy) cyclohexane, 2,2-di (t-butylperoxy) butane and the like.
ハイドロパーオキサイド類としては、例えばｐ−メンタンハイドロパーオキサイド、ジイソプロピルベンゼンハイドロパーオキサイド、１，１，３，３−テトラメチルブチルハイドロパーオキサイド、ｔ−ブチルハイドロパーオキサイド等が挙げられる。 Examples of hydroperoxides include p-menthane hydroperoxide, diisopropylbenzene hydroperoxide, 1,1,3,3-tetramethylbutyl hydroperoxide, t-butyl hydroperoxide, and the like.
ジアルキルパーオキサイド類としては、例えばα，α’−ジ（ｔ−ブチルパーオキシ）ジイソプロピルベンゼン、ジクミルパーオキシド、ｔ−ブチルクミルパーオキシド、ジ−ｔ−ブチルパーオキシド、ジ−ｔ−ヘキシルパーオキシド等を挙げることができる。 Examples of the dialkyl peroxides include α, α′-di (t-butylperoxy) diisopropylbenzene, dicumyl peroxide, t-butylcumyl peroxide, di-t-butyl peroxide, and di-t-hexyl peroxide. An oxide etc. can be mentioned.
ジアシルパーオキサイド類としては、例えばジイソブチルパーオキシド、ジ（３，５，５，−トリメチルヘキサノイル）パーオキシド、ジラウロイルパーオキシド、ベンゾイルパーオキシド等を挙げることができる。 Examples of diacyl peroxides include diisobutyl peroxide, di (3,5,5-trimethylhexanoyl) peroxide, dilauroyl peroxide, and benzoyl peroxide.
パーオキシジカーボネート類としては、例えばジイソプロピルパーオキシジカーボネート、ジ−ｎ−プロピルパーオキシジカーボネート、ビス（４−ｔ−ブチルシクロヘキシル）パーオキシジカーボネート等を挙げることができる。 Examples of peroxydicarbonates include diisopropyl peroxydicarbonate, di-n-propyl peroxydicarbonate, bis (4-t-butylcyclohexyl) peroxydicarbonate, and the like.
パーオキシエステル類としては、例えばｔ−ヘキシルパーオキシピバレート、ｔ−ブチルパーオキシピバレート、ｔ−ヘキシルパーオキシ−２−エチルヘキサノエート、ｔ−ブチルパーオキシ−２−エチルヘキサノエート、ｔ−ブチルパーオキシラウレート、ｔ−ブチルパーオキシ−３，５，５−トリメチルヘキサノエート等を挙げることができる。 Examples of peroxyesters include t-hexyl peroxypivalate, t-butyl peroxypivalate, t-hexyl peroxy-2-ethylhexanoate, t-butylperoxy-2-ethylhexanoate, Examples thereof include t-butyl peroxylaurate and t-butyl peroxy-3,5,5-trimethylhexanoate.
本発明において用いられるアゾ系化合物としては、例えば２，２’−アゾビスイソブチロニトリル、２，２’−アゾビス(２−メチルブチロニトリル)、１，１’−アゾビス（シクロヘキサン１−カルボニトリル）、２，２’−アゾビス（２，４−ジメチルバレロニトリル）、２，２’−アゾビス（２，４−ジメチル−４−メトキシバレロニトリル）、ジメチル２，２’−アゾビス（２−メチルプロピオネート）、４，４’−アゾビス（４−シアノバレリック酸）、２，２’−アゾビス（２−ヒドロキシメチルプロピオニトリル）、２，２’−アゾビス［２−（２−イミダゾリン−２−イル）プロパン］等を挙げることができる。これらの中でも反応性、重合安定性を考慮すると、２，２’−アゾビスイソブチロニトリルが好ましい。 Examples of the azo compound used in the present invention include 2,2′-azobisisobutyronitrile, 2,2′-azobis (2-methylbutyronitrile), 1,1′-azobis (cyclohexane 1-carbohydrate). Nitrile), 2,2′-azobis (2,4-dimethylvaleronitrile), 2,2′-azobis (2,4-dimethyl-4-methoxyvaleronitrile), dimethyl 2,2′-azobis (2-methyl) Propionate), 4,4'-azobis (4-cyanovaleric acid), 2,2'-azobis (2-hydroxymethylpropionitrile), 2,2'-azobis [2- (2-imidazoline- 2-yl) propane] and the like. Among these, 2,2'-azobisisobutyronitrile is preferable in consideration of reactivity and polymerization stability.
アクリル系樹脂（イ）は、そのガラス転移温度が−７０℃以上０℃以下であることが好ましく、−７０℃以上−１０℃以下がより好ましく、−６０℃以上−３０℃以下がより好ましい。ガラス転移温度が−７０℃以上０℃以下の範囲内にあることで密着性が得やすくなる。
なお、アクリル系樹脂（イ）のガラス転移温度は、それを構成するラジカル重合性不飽和モノマーの組成比と、それぞれのモノマーからなるホモポリマーのガラス転移温度を基に、公知の方法（ＦＯＸの数式（１）により算出することができる。
数式（１）：
１／Ｔｇ＝［（Ｗ１／Ｔｇ１）＋（Ｗ２／Ｔｇ２）＋・・・＋（Ｗｎ／Ｔｇｎ）］／１００
（ここで温度は絶対温度である）
Ｗｎ：単量体ｎの重量％
Ｔｇｎ：単量体ｎからなるホモポリマーのガラス転移温度
The acrylic resin (A) preferably has a glass transition temperature of −70 ° C. or higher and 0 ° C. or lower, more preferably −70 ° C. or higher and −10 ° C. or lower, and more preferably −60 ° C. or higher and −30 ° C. or lower. Adhesiveness is easily obtained when the glass transition temperature is in the range of −70 ° C. or more and 0 ° C. or less.
The glass transition temperature of the acrylic resin (A) is determined by a known method (FOX) based on the composition ratio of the radical polymerizable unsaturated monomer constituting the acrylic resin (a) and the glass transition temperature of the homopolymer composed of each monomer. It can be calculated by Equation (1).
Formula (1):
1 / Tg = [(W1 / Tg1) + (W2 / Tg2) +... + (Wn / Tgn)] / 100
(Where temperature is absolute)
Wn:% by weight of monomer n
Tgn: Glass transition temperature of homopolymer composed of monomer n
アクリル系樹脂（イ）は、その重量平均分子量が４０万〜７０万であることが好ましく、４５万〜６５万がより好ましい。 重量平均分子量が４０万〜７０万の範囲内にあることで、粘着剤の凝集力を適切にし易くなるため所望の密着性を得やすくなる。なお、重量平均分子量はゲルパーミエーションクロマトグラフィー（ＧＰＣ）による、標準のポリスチレン換算の値である。 The acrylic resin (I) preferably has a weight average molecular weight of 400,000 to 700,000, more preferably 450,000 to 650,000. When the weight average molecular weight is in the range of 400,000 to 700,000, the cohesive force of the pressure-sensitive adhesive is easily made appropriate, so that desired adhesion can be easily obtained. The weight average molecular weight is a standard polystyrene equivalent value determined by gel permeation chromatography (GPC).
粘着剤（Ａ）には、アクリル系樹脂（イ）に加えて、ロジンエステル骨格を有する粘着付与樹脂（ｘ）および芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）を配合することが好ましい。 In addition to the acrylic resin (A), the pressure-sensitive adhesive (A) may include a tackifier resin (x) having a rosin ester skeleton and a tackifier resin (y) having an aromatic petroleum resin skeleton. preferable.
ロジンエステル骨格を有する粘着付与樹脂（ｘ）としては、例えばロジンエステル樹脂、水添ロジンエステル樹脂、不均化ロジンエステル樹脂、および重合ロジンエステル樹脂が好ましい。ロジンエステル骨格を有する粘着付与樹脂（ｘ）の軟化点は、１００℃〜１４０℃が好ましく、１１０℃〜１３０℃がより好ましい。軟化点が１００℃〜１４０℃にあることで粘着力がより向上し研磨液に耐えうる密着性が得やすくなる。さらに研磨時に摩擦熱が発生しても粘着剤層が軟化しにくくいため凝集力をより維持しやすくなる。 As the tackifier resin (x) having a rosin ester skeleton, for example, a rosin ester resin, a hydrogenated rosin ester resin, a disproportionated rosin ester resin, and a polymerized rosin ester resin are preferable. The softening point of the tackifier resin (x) having a rosin ester skeleton is preferably 100 ° C to 140 ° C, more preferably 110 ° C to 130 ° C. When the softening point is in the range of 100 ° C. to 140 ° C., the adhesive force is further improved, and the adhesiveness that can withstand the polishing liquid is easily obtained. Furthermore, even if frictional heat is generated during polishing, the pressure-sensitive adhesive layer is not easily softened, so that the cohesive force is more easily maintained.
芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）としては、例えばスチレンオリゴマー、α−メチルスチレン／スチレン共重合体等が好ましい。芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）の軟化点は、８０℃〜１３０℃が好ましく、９０℃〜１２０℃がより好ましい。軟化点が８０℃〜１３０℃にあることで粘着力がより向上し研磨液に耐えうる密着性が得やすくなる。さらに研磨時に摩擦熱が発生しても粘着剤層が軟化しにくくいため凝集力をより維持しやすくなる。 As the tackifier resin (y) having an aromatic petroleum resin skeleton, for example, a styrene oligomer, an α-methylstyrene / styrene copolymer, and the like are preferable. The softening point of the tackifier resin (y) having an aromatic petroleum resin skeleton is preferably 80 ° C to 130 ° C, more preferably 90 ° C to 120 ° C. When the softening point is in the range of 80 ° C. to 130 ° C., the adhesive force is further improved, and the adhesiveness that can withstand the polishing liquid is easily obtained. Furthermore, even if frictional heat is generated during polishing, the pressure-sensitive adhesive layer is not easily softened, so that the cohesive force is more easily maintained.
また、粘着剤（Ａ）は、アクリル系樹脂（イ）１００重量部に対して、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との合計量１５〜３５重量部を含むことが好ましい。合計１５〜３５重量部配合することで凝集力と粘着力のバランスがとりやすくなるため所望の密着性が得やすくなる。
さらに粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との割合は、重量比で（ｘ）／（ｙ）＝３／２〜９／２が好ましく、４／２〜８／２がより好ましく、４／２〜６／２がさらに好ましい。重量比が（ｘ）／（ｙ）＝３／２〜９／２の範囲にあることで凝集力と粘着力のバランスがとりやすくなるため所望の密着性が得やすくなる。
Moreover, it is preferable that an adhesive (A) contains 15-35 weight part of total amounts of tackifying resin (x) and tackifying resin (y) with respect to 100 weight part of acrylic resin (ii). By blending 15 to 35 parts by weight in total, it becomes easy to balance the cohesive force and the adhesive force, so that desired adhesion can be easily obtained.
Furthermore, the ratio of the tackifying resin (x) and the tackifying resin (y) is preferably (x) / (y) = 3/2 to 9/2, more preferably 4/2 to 8/2 in weight ratio. 4/2 to 6/2 is more preferable. When the weight ratio is in the range of (x) / (y) = 3/2 to 9/2, it becomes easy to balance the cohesive force and the adhesive force, so that desired adhesion can be easily obtained.
粘着剤（Ａ）は、硬化剤を配合することで粘着剤が硬化し、粘着剤層に凝集力を付与できる。硬化剤は、例えば、金属キレート系硬化剤、エポキシ系硬化剤、イソシアネート系硬化剤、アジリジン系硬化剤、エポキシ系硬化剤やイソシアネート系硬化剤等が好ましい。これらの硬化剤はアクリル樹脂の官能基に応じて適宜組み合わせることができる。
カルボキシル基と反応し得る硬化剤としては、金属キレート系硬化剤、エポキシ系硬化剤、イソシアネート系硬化剤、アジリジン系硬化剤等が挙げられる。
The pressure-sensitive adhesive (A) can harden the pressure-sensitive adhesive by adding a curing agent, and can impart cohesive force to the pressure-sensitive adhesive layer. The curing agent is preferably, for example, a metal chelate curing agent, an epoxy curing agent, an isocyanate curing agent, an aziridine curing agent, an epoxy curing agent or an isocyanate curing agent. These curing agents can be appropriately combined depending on the functional group of the acrylic resin.
Examples of the curing agent that can react with a carboxyl group include a metal chelate curing agent, an epoxy curing agent, an isocyanate curing agent, and an aziridine curing agent.
公知のアジリジン系硬化剤としては、１分子中に少なくともアジリジニル基を２個以上有する化合物であり、例えば、トリ１−アジリジニルホスフィンオキサイド、Ｎ，Ｎ’−ヘキサメチレン−１，６−ビス（１−アジリジンカルボキシアマイド）、Ｎ，Ｎ’−ジフェニルエタン−４，４’−ビス（１−アジリジンカルボキシアマイド）、トリメチロールプロパン−トリβ−アジリジニルプロピオネート、Ｎ，Ｎ’−トルエン−２，４−ビス（アジリジンカルボキシアマイド）、ビスイソフタロイル−１−（２−メチルアジリジン）ホスフィン、トリメチロールプロパン−トリβ−（２−メチルアジリジン）プロピオネート等が挙げられる。 Known aziridine-based curing agents are compounds having at least two aziridinyl groups in one molecule, such as tri-1-aziridinylphosphine oxide, N, N′-hexamethylene-1,6-bis ( 1-aziridinecarboxyamide), N, N′-diphenylethane-4,4′-bis (1-aziridinecarboxyamide), trimethylolpropane-triβ-aziridinylpropionate, N, N′-toluene- Examples include 2,4-bis (aziridinecarboxyamide), bisisophthaloyl-1- (2-methylaziridine) phosphine, trimethylolpropane-tri β- (2-methylaziridine) propionate, and the like.
公知のエポキシ系硬化剤としては、エポキシ基を分子内に複数個有する化合物であればよく、特に限定されるものではない。具体的には、例えば、エチレングリコールジグリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、１，６−ヘキサンジオールジグリシジルエーテル、ビスフェノールＡ・エピクロロヒドリン型エポキシ樹脂、Ｎ，Ｎ，Ｎ’Ｎ’−テトラグリシジル−ｍ−キシレンジアミン、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、Ｎ，Ｎ−ジグリシジルアニリン、Ｎ，Ｎ−ジグリシジルトルイジン等が挙げられる。 The known epoxy curing agent is not particularly limited as long as it is a compound having a plurality of epoxy groups in the molecule. Specifically, for example, ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, bisphenol A / epichlorohydrin type epoxy resin, N, N, N′N′-tetra Examples thereof include glycidyl-m-xylenediamine, 1,3-bis (N, N-diglycidylaminomethyl) cyclohexane, N, N-diglycidylaniline, N, N-diglycidyltoluidine and the like.
公知の金属キレート系硬化剤としては、チタンキレート硬化剤、アルミキレート硬化剤、ジルコニウムキレート硬化剤等が挙げられる。これらの中でもアルミキレート硬化剤が好ましい Examples of known metal chelate curing agents include titanium chelate curing agents, aluminum chelate curing agents, and zirconium chelate curing agents. Among these, an aluminum chelate curing agent is preferable.
カルボキシル基と反応し得る硬化剤は、アクリル系樹脂（イ）１００重量部に対して、０．０１〜１０重量部を使用することが好ましく、０．２５〜５重量部がより好ましい。０．０１重量部未満だと、粘着剤層としての凝集力が得にくく、１０重量部を超えると、被着体に対する密着性が不足する恐れがある。 The curing agent capable of reacting with a carboxyl group is preferably used in an amount of 0.01 to 10 parts by weight, more preferably 0.25 to 5 parts by weight with respect to 100 parts by weight of the acrylic resin (ii). If the amount is less than 0.01 part by weight, the cohesive force as the pressure-sensitive adhesive layer is difficult to obtain, and if it exceeds 10 parts by weight, the adhesion to the adherend may be insufficient.
公知のイソシアネート系硬化剤としては、公知のジイソシアネート化合物、公知のジイソシアネート化合物を３官能ポリオール成分で変性したいわゆるアダクト体、ジイソシアネート化合物が水と反応したビュレット体、ジイソシアネート化合物３分子から形成されるイソシアヌレート環を有する３量体（イソシアヌレート体）を使用することができる。これらは３官能のイシシアネート基を有するのが一般的である。 Known isocyanate curing agents include known diisocyanate compounds, so-called adducts obtained by modifying known diisocyanate compounds with trifunctional polyol components, burettes obtained by reacting diisocyanate compounds with water, and isocyanurates formed from three diisocyanate compounds. A trimer having a ring (isocyanurate) can be used. These generally have a trifunctional isocyanate group.
公知のジイソシアネート化合物としては、芳香族ジイソシアネート、脂肪族ジイソシアネート、芳香脂肪族ジイソシアネート、脂環族ジイソシアネート等が挙げられる。 Known diisocyanate compounds include aromatic diisocyanates, aliphatic diisocyanates, araliphatic diisocyanates, alicyclic diisocyanates, and the like.
芳香族ジイソシアネートとしては、１，３−フェニレンジイソシアネート、４，４’−ジフェニルジイソシアネート、１，４−フェニレンジイソシアネート、４，４’−ジフェニルメタンジイソシアネート、２，４−トリレンジイソシアネート、２，６−トリレンジイソシアネート、４，４’−トルイジンジイソシアネート、ジアニシジンジイソシアネート、４，４’−ジフェニルエーテルジイソシアネート等を挙げることができる。 As aromatic diisocyanates, 1,3-phenylene diisocyanate, 4,4'-diphenyl diisocyanate, 1,4-phenylene diisocyanate, 4,4'-diphenylmethane diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate Examples thereof include isocyanate, 4,4′-toluidine diisocyanate, dianisidine diisocyanate, and 4,4′-diphenyl ether diisocyanate.
脂肪族ジイソシアネートとしては、トリメチレンジイソシアネート、テトラメチレンジイソシアネート、ヘキサメチレンジイソシアネート、ペンタメチレンジイソシアネート、１，２−プロピレンジイソシアネート、２，３−ブチレンジイソシアネート、１，３−ブチレンジイソシアネート、ドデカメチレンジイソシアネート、２，４，４−トリメチルヘキサメチレンジイソシアネート等を挙げることができる。 Aliphatic diisocyanates include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1,2-propylene diisocyanate, 2,3-butylene diisocyanate, 1,3-butylene diisocyanate, dodecamethylene diisocyanate, 2,4 , 4-trimethylhexamethylene diisocyanate and the like.
芳香脂肪族ジイソシアネートとしては、ω，ω’−ジイソシアネート−１，３−ジメチルベンゼン、ω，ω’−ジイソシアネート−１，４−ジメチルベンゼン、ω，ω’−ジイソシアネート−１，４−ジエチルベンゼン、１，４−テトラメチルキシリレンジイソシアネート、１，３−テトラメチルキシリレンジイソシアネート等を挙げることができる。 Examples of the araliphatic diisocyanate include ω, ω′-diisocyanate-1,3-dimethylbenzene, ω, ω′-diisocyanate-1,4-dimethylbenzene, ω, ω′-diisocyanate-1,4-diethylbenzene, 1, Examples include 4-tetramethylxylylene diisocyanate and 1,3-tetramethylxylylene diisocyanate.
脂環族ジイソシアネートとしては、３−イソシアネートメチル−３，５，５−トリメチルシクロヘキシルイソシアネート、１，３−シクロペンタンジイソシアネート、１，３−シクロヘキサンジイソシアネート、１，４−シクロヘキサンジイソシアネート、メチル−２，４−シクロヘキサンジイソシアネート、メチル−２，６−シクロヘキサンジイソシアネート、４，４’−メチレンビス（シクロヘキシルイソシアネート）、１，４−ビス（イソシアネートメチル）シクロヘキサン、１，４−ビス（イソシアネートメチル）シクロヘキサン等を挙げることができる。 Examples of alicyclic diisocyanates include 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate, 1,3-cyclopentane diisocyanate, 1,3-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, methyl-2,4- Examples include cyclohexane diisocyanate, methyl-2,6-cyclohexane diisocyanate, 4,4′-methylenebis (cyclohexyl isocyanate), 1,4-bis (isocyanate methyl) cyclohexane, 1,4-bis (isocyanate methyl) cyclohexane, and the like. .
本発明に用いられるジイソシアネート化合物としては、２，４−トリレンジイソシアネート、ヘキサメチレンジイソシアネート、３−イソシアネートメチル−３，５，５−トリメチルシクロヘキシルイソシアネート（別名：イソホロンジイソシアネート）が好ましい。 As the diisocyanate compound used in the present invention, 2,4-tolylene diisocyanate, hexamethylene diisocyanate, and 3-isocyanate methyl-3,5,5-trimethylcyclohexyl isocyanate (also known as isophorone diisocyanate) are preferable.
また、これらのジイソシアネート化合物のアダクト体、ビュレット体、イソシアヌレート体も好適に使用することができる。 In addition, adducts, burettes and isocyanurates of these diisocyanate compounds can also be suitably used.
水酸基と反応し得る硬化剤としては、エポキシ系硬化剤やイソシアネート系硬化剤等が好ましい。
水酸基と反応し得る硬化剤は、アクリル系樹脂（イ）１００重量部に対して、０．０１〜１０重量部を使用することが好ましく、０．０５〜５重量部がより好ましい。
これらの硬化剤は、単独または２種以上使用することができる。
As the curing agent capable of reacting with a hydroxyl group, an epoxy curing agent, an isocyanate curing agent, or the like is preferable.
The curing agent capable of reacting with a hydroxyl group is preferably used in an amount of 0.01 to 10 parts by weight, more preferably 0.05 to 5 parts by weight with respect to 100 parts by weight of the acrylic resin (ii).
These curing agents can be used alone or in combination of two or more.
粘着剤（Ａ）には、各種の添加剤等を配合することができる。具体的には、シランカップリング剤、界面活性剤、消泡剤、中和剤、可塑剤、着色剤、フィラー、撥水剤等の添加剤が挙げられる。 Various additives etc. can be mix | blended with an adhesive (A). Specific examples include additives such as silane coupling agents, surfactants, antifoaming agents, neutralizing agents, plasticizers, colorants, fillers, and water repellents.
粘着剤層（１）は、粘着剤（Ａ）を塗工し、乾燥することで形成できる。具体的には、粘着剤を剥離ライナー上に塗工し、乾燥することで粘着剤層を形成した後、当該粘着剤層とプラスチック基材（２）とを貼り合わせ、粘着剤層をシート基材上に転写する方法が挙げられる（転写法ともいう）。
またはプラスチック基材（２）に直接粘着剤を塗工し、乾燥することで粘着剤層を形成した後、剥離ライナーを貼り合わせる方法が挙げられる。また、粘着剤層は、必要に応じてエージングすることで凝集力をより向上することができる。
The pressure-sensitive adhesive layer (1) can be formed by applying the pressure-sensitive adhesive (A) and drying it. Specifically, after the pressure-sensitive adhesive is coated on a release liner and dried to form a pressure-sensitive adhesive layer, the pressure-sensitive adhesive layer and the plastic base material (2) are bonded together, and the pressure-sensitive adhesive layer is attached to the sheet base. There is a method of transferring onto a material (also referred to as transfer method).
Alternatively, a method in which a pressure-sensitive adhesive is directly applied to the plastic substrate (2) and dried to form a pressure-sensitive adhesive layer, and then a release liner is pasted together. Moreover, the pressure-sensitive adhesive layer can further improve the cohesive force by aging as necessary.
粘着剤を塗工する方法としては特に制限されるものではなく、コンマコーター、ブレードコーター、グラビアコーター等のロールコーター、スロットダイコーター、リップコーター、カーテンコーター等の従来公知のコーティング装置によることができる。
粘着剤層（１）の厚さは、１５〜２００μｍが好ましく、２０〜１５０μｍがより好ましく、３０〜１００μｍがさらに好ましい。
The method of applying the adhesive is not particularly limited, and can be performed by a conventionally known coating apparatus such as a roll coater such as a comma coater, a blade coater, or a gravure coater, a slot die coater, a lip coater, or a curtain coater. .
15-200 micrometers is preferable, as for the thickness of an adhesive layer (1), 20-150 micrometers is more preferable, and 30-100 micrometers is further more preferable.
本発明の研磨部材固定用両面粘着テープは、研磨部材を研磨装置に固定するために使用することが好ましい。
研磨部材は、被研磨体を研磨するための研磨パッド、および被研磨体を吸着、保持する研磨用吸着パッドを含む。この研磨パッドには被研磨体の種類や１次研磨、仕上げ研磨等の研磨段階で種々の素材が使用されているが、研磨液の作用に耐えうる特性および研磨砥粒を保持する観点からウレタン樹脂発泡体が広く使用されている。そして荒く研磨する１次研磨には硬質ウレタン樹脂発泡体シートが使用され、鏡面に研磨する仕上げ研磨には軟質ウレタン樹脂発泡体シートを使用するのが一般的である。この研磨パッドは、被研磨体を平坦に研磨するためにパッド表面を平坦に加工しているが、パッド表面を切削等により平坦化処理するのが一般的である。図２は、平坦化処理前の研磨パッド（ウレタン樹脂発泡体）の１例の模式的断面図である。また、図３は、平坦化処理後の研磨パッド（ウレタン樹脂発泡体）の１例の模式的断面図である。
The double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention is preferably used for fixing the abrasive member to a polishing apparatus.
The polishing member includes a polishing pad for polishing the object to be polished, and a polishing suction pad for adsorbing and holding the object to be polished. Various materials are used for this polishing pad in the polishing stage such as the type of the object to be polished, primary polishing, and final polishing. From the viewpoint of maintaining the characteristics that can withstand the action of the polishing liquid and the abrasive grains. Resin foam is widely used. A hard urethane resin foam sheet is generally used for the primary polishing for rough polishing, and a soft urethane resin foam sheet is generally used for the final polishing for mirror polishing. In this polishing pad, the pad surface is processed to be flat in order to polish the object to be polished flat, but the pad surface is generally flattened by cutting or the like. FIG. 2 is a schematic cross-sectional view of an example of a polishing pad (urethane resin foam) before the planarization treatment. FIG. 3 is a schematic cross-sectional view of an example of the polishing pad (urethane resin foam) after the planarization treatment.
また研磨用吸着パッドは、上述した仕上げ研磨用の軟質ウレタン樹脂発泡体を使用する場合があるが、この場合は図４のようにテンプレート４と呼ばれる被研磨体外周を型取ったエポキシ樹脂等の部材を使用して被研磨体の横ずれを防止することが一般的である。さらに図５のようにテンプレートを使用せず軟質ウレタン樹脂発泡体シートのスキン層（非切削面）で被研磨体を保持して使用することがある。前記の平坦化処理を行った軟質ウレタン樹脂発泡シートの発泡セル開放面と両面粘着テープを貼り合わせる場合は、両者の接触面積は、他方のスキン層と比較して数％程度であるため両面粘着テープの密着性が不足することが多かった。 The polishing suction pad may use the above-described soft urethane resin foam for finish polishing. In this case, as shown in FIG. It is common to use a member to prevent lateral displacement of the object to be polished. Furthermore, as shown in FIG. 5, the object to be polished may be held and used by the skin layer (non-cutting surface) of the soft urethane resin foam sheet without using a template. In the case where the foamed cell open surface of the soft urethane resin foam sheet subjected to the flattening treatment is bonded to the double-sided adhesive tape, the contact area between the two is about several percent compared to the other skin layer, so that the double-sided adhesive is used. In many cases, the adhesiveness of the tape was insufficient.
本発明の研磨部材固定用両面粘着テープの第一の特徴は、研磨部材、例えば接触面積が少ない軟質ポリウレタンの発泡セル開放面との密着性が優れることである。また第二の特徴は、両面粘着テープを使用して研磨部材を研磨装置の定盤に固定して、研磨工程を行ったときに、例えば、強酸性溶液、強塩基性溶液、または過酸化水素を含有する研磨液に曝されても粘着剤層の密着性が優れているため両面粘着テープが研磨部材から剥離せず、また両面粘着テープ自体が粘着剤層と基材に分離しないことである。 The first feature of the double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention is that it has excellent adhesion to an abrasive member, for example, a foamed cell open surface of soft polyurethane having a small contact area. The second feature is that when a polishing member is fixed to a surface plate of a polishing apparatus using a double-sided adhesive tape and a polishing process is performed, for example, a strongly acidic solution, a strongly basic solution, or hydrogen peroxide The double-sided pressure-sensitive adhesive tape does not peel from the polishing member because the adhesive layer has excellent adhesiveness even when exposed to a polishing liquid containing, and the double-sided pressure-sensitive adhesive tape itself does not separate into the pressure-sensitive adhesive layer and the substrate. .
本発明の研磨部材固定用両面粘着テープは、粘着剤層（１）と、プラスチック基材（２）と、粘着剤層（３）とを備えている。粘着剤層（１）が研磨部材とプラスチック基材（２）と接する側に使用し、粘着剤層（３）はプラスチック基材（２）と定盤に接する側に使用することが好ましい。 The double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention comprises a pressure-sensitive adhesive layer (1), a plastic substrate (2), and a pressure-sensitive adhesive layer (3). The pressure-sensitive adhesive layer (1) is preferably used on the side in contact with the polishing member and the plastic substrate (2), and the pressure-sensitive adhesive layer (3) is preferably used on the side in contact with the plastic substrate (2) and the surface plate.
粘着剤層（３）は、粘着剤層（１）に使用した粘着剤（Ａ）を使用しても良いが、粘着剤層（１）以外の粘着剤層を使用しても良い。粘着剤層（１）以外の粘着剤層を使用する場合は、アクリル系樹脂、ウレタン系樹脂、シリコン系樹脂、ゴム系樹脂、およびポリエステル系樹脂等を適宜選択できる。 As the pressure-sensitive adhesive layer (3), the pressure-sensitive adhesive (A) used for the pressure-sensitive adhesive layer (1) may be used, but a pressure-sensitive adhesive layer other than the pressure-sensitive adhesive layer (1) may be used. When an adhesive layer other than the adhesive layer (1) is used, an acrylic resin, a urethane resin, a silicon resin, a rubber resin, a polyester resin, and the like can be appropriately selected.
粘着剤層（３）の厚さは、１５〜１５０μｍが好ましく、２０〜１００μｍがより好ましく、２５〜８０μｍさらに好ましい。厚さが１５〜１５０μｍにあることで凝集力と粘着力のバランスを取りやすくなるため、所望の密着性が得やすくなる。粘着剤層（３）は、粘着剤層（１）と同様の方法により形成できる。 The thickness of the pressure-sensitive adhesive layer (3) is preferably 15 to 150 μm, more preferably 20 to 100 μm, and further preferably 25 to 80 μm. Since it becomes easy to balance cohesion force and adhesive force when the thickness is 15 to 150 μm, it is easy to obtain desired adhesion. The pressure-sensitive adhesive layer (3) can be formed by the same method as the pressure-sensitive adhesive layer (1).
プラスチック基材（２）は、シート状、またはフィルム状であり、その表面は平滑なものが好ましい。各種基材は単独でも用いることもできるし、複数のものを積層してなる多層状態にあるものも用いることができる。 The plastic substrate (2) is in the form of a sheet or film, and the surface thereof is preferably smooth. Various base materials can be used alone or in a multi-layered state in which a plurality of base materials are laminated.
プラスチック基材（２）は、例えばポリビニルアルコール、トリアセチルセルロース、ポリプロピレン、ポリエチレン、ポリシクロオレフィン、エチレン−酢酸ビニル共重合体などのポリオレフィン系樹脂；
ポリエチレンテレフタレート、ポリブチレンテレフタレートなどのポリエステル系樹脂；
ポリカーボネート系樹脂、ポリノルボルネン系樹脂、ポリアリレート系樹脂、アクリル系樹脂、ポリフェニレンサルファイド樹脂、ポリスチレン樹脂、ビニル系樹脂、ポリアミド系樹脂、ポリイミド系樹脂、エポキシ系樹脂などが挙げられる。
プラスチック基材（２）は、単一の樹脂、複数の樹脂の積層体、複数の樹脂を混合した樹脂等を使用できる。
The plastic substrate (2) is, for example, a polyolefin resin such as polyvinyl alcohol, triacetyl cellulose, polypropylene, polyethylene, polycycloolefin, ethylene-vinyl acetate copolymer;
Polyester resins such as polyethylene terephthalate and polybutylene terephthalate;
Examples thereof include polycarbonate resins, polynorbornene resins, polyarylate resins, acrylic resins, polyphenylene sulfide resins, polystyrene resins, vinyl resins, polyamide resins, polyimide resins, and epoxy resins.
As the plastic substrate (2), a single resin, a laminate of a plurality of resins, a resin in which a plurality of resins are mixed, or the like can be used.
本発明の研磨部材固定用両面粘着テープを保存するときや市場を流通するときには、粘着剤層に剥離ライナーを貼り付けることでその表面を保護することが一般的である。 When the double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention is stored or distributed in the market, it is common to protect the surface by attaching a release liner to the pressure-sensitive adhesive layer.
本発明の研磨部材固定用両面粘着テープは、あらゆる被研磨体の研磨に使用できるが、表面を精密に研磨する用途に使用することが好ましい。例えば、液晶ディスプレイ用ガラス、ハードディスク用基板、光学レンズ、シリコンウェハや集積回路等が挙げられる。 Although the double-sided pressure-sensitive adhesive tape for fixing an abrasive member of the present invention can be used for polishing any object to be polished, it is preferably used for the purpose of precisely polishing the surface. Examples thereof include glass for liquid crystal display, a substrate for hard disk, an optical lens, a silicon wafer, an integrated circuit, and the like.
以下に、本発明の具体的な実施例を比較例と併せて説明するが、本発明は、下記実施例に限定されない。また、下記実施例および比較例中、「部」は「重量部」を示し、「％」は「重量％」を示す。 Specific examples of the present invention will be described below together with comparative examples, but the present invention is not limited to the following examples. In the following examples and comparative examples, “part” represents “part by weight” and “%” represents “% by weight”.
また、実施例で使用するモノマー等のホモポリマーのガラス転移温度値を各々下記に示した。
アクリル酸：１０６℃、メタクリル酸：１８６℃、アクリル酸メチル８℃、：アクリル酸エチル：−２２℃、アクリル酸ブチル：−５２℃、アクリル酸２−エチルヘキシル：−７０℃、アクリル酸イソプロピル：−５℃、メタクリル酸メチル：１０５℃、メタクリル酸エチル：６５℃、メタクリル酸イソプロピル：８１℃、メタクリル酸ｎブチル：２０℃、メタクリル酸イソブチル：６７℃、メタクリル酸ｎヘキシル：−５℃、酢酸ビニル：２９℃、アクリル酸２−ヒドロキシエチル：−１５℃、メタクリル酸２−ヒドロキシルエチル：５５℃。
The glass transition temperature values of homopolymers such as monomers used in the examples are shown below.
Acrylic acid: 106 ° C, methacrylic acid: 186 ° C,
（実施例１）
加熱装置、撹拌機、還流冷却装置、温度計、窒素導入管および滴下槽を備えた重合用容器を用意し、アクリル酸ブチル：７．７部、アクリル酸エチル：０．１部、アクリル酸：０．２部、アクリル酸２−ヒドロキシエチル：０．０２部、オクチルチオグリコレート：０．００５部、さらに酢酸エチル：２７部、ベンゾイルパーオキサイドを適量仕込んだ。また、滴下槽にラジカル重合性不飽和モノマーとしてアクリル酸ブチル：３１部、アクリル酸エチル：０．３部、アクリル酸：０．７部、アクリル酸２−ヒドロキシエチル：０．１部、オクチルチオグリコレート：０．０２２部、さらに酢酸エチル:9.5部を仕込み混合した。別途、滴下用開始剤槽にベンゾイルパーオキサイドを適量仕込んだ。
重合用容器内の空気を窒素ガスで置換した後、攪拌しながら窒素雰囲気下、還流温度下で滴下槽と滴下用開始剤槽から滴下を開始した。滴下終了後、さらに攪拌しながらサンプリングを行い重合率が８０％に達したところで、ベンゾイルパーオキサイドを適量添加して反応を５時間継続した。
次いで、酢酸エチル適量を加えつつ、液温が室温になるまで重合用容器を冷却して、アクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．６重量％、共重合体の重量平均分子量は５２０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５０℃である。
Example 1
A polymerization vessel equipped with a heating device, a stirrer, a reflux cooling device, a thermometer, a nitrogen introducing tube and a dropping tank was prepared, butyl acrylate: 7.7 parts, ethyl acrylate: 0.1 parts, acrylic acid: 0.2 parts, 2-hydroxyethyl acrylate: 0.02 parts, octylthioglycolate: 0.005 parts, further ethyl acetate: 27 parts, and appropriate amounts of benzoyl peroxide were charged. In addition, butyl acrylate: 31 parts, ethyl acrylate: 0.3 parts, acrylic acid: 0.7 parts, 2-hydroxyethyl acrylate: 0.1 parts, octylthio as radical polymerizable unsaturated monomer in the dropping tank Glycolate: 0.022 part, and ethyl acetate: 9.5 part were charged and mixed. Separately, an appropriate amount of benzoyl peroxide was charged into the initiator tank for dropping.
After the air in the polymerization vessel was replaced with nitrogen gas, dropping was started from a dropping tank and a dropping initiator tank under a nitrogen atmosphere and a reflux temperature while stirring. After completion of the dropping, sampling was performed while stirring, and when the polymerization rate reached 80%, an appropriate amount of benzoyl peroxide was added and the reaction was continued for 5 hours.
Next, while adding an appropriate amount of ethyl acetate, the polymerization vessel was cooled until the liquid temperature reached room temperature, to obtain an acrylic resin solution. This resin solution was colorless and transparent, had a nonvolatile content of 38.6% by weight, and the copolymer had a weight average molecular weight of 520,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -50 degreeC.
得られたアクリル樹脂溶液１００部に対して酸価：１０ｍｇＫＯＨ／ｇ、軟化点１２０℃の重合ロジンエステルであるペンセルＣ（荒川化学社製）を７．５部、軟化点９５℃の石油樹脂日石ネオポリマーＬ９０（新日本石油社製）を２．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に２５μｍの粘着剤層（１）として形成した。また他方の面に得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。形成された粘着剤層の外観（透明性）を目視にて観察した。結果は表1に示した。
Petroleum resin having an acid value of 10 mg KOH / g and a polymerized rosin ester of 120 ° C., which is a polymerized rosin ester (Arakawa Chemical Co., Ltd.) 7.5 parts, and a softening point of 95 ° C. 2.8 parts of stone neopolymer L90 (manufactured by Nippon Oil Corporation), 15 parts of ethyl acetate, and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive. .
The obtained pressure-sensitive adhesive was formed as a 25-μm pressure-sensitive adhesive layer (1) on one surface of a 25-μm thick polyethylene terephthalate film by a transfer method. A pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed from the pressure-sensitive adhesive obtained on the other surface by a transfer method to obtain a double-sided pressure-sensitive adhesive tape. The appearance (transparency) of the formed pressure-sensitive adhesive layer was visually observed. The results are shown in Table 1.
なお、不揮発分、および重量平均分子量は以下の方法に従って求めた。 The nonvolatile content and the weight average molecular weight were determined according to the following methods.
＜不揮発分の測定＞
各反応溶液約１ｇを金属容器に秤量し、１５０℃オーブンにて２０分間乾燥して、残分を秤量して残率計算をし、不揮発分濃度（不揮発分）とした。
<Measurement of non-volatile content>
About 1 g of each reaction solution was weighed in a metal container, dried in an oven at 150 ° C. for 20 minutes, the residue was weighed, and the remaining rate was calculated to obtain a nonvolatile content concentration (nonvolatile content).
＜重量平均分子量の測定＞
東ソー社製ＧＰＣ（ゲルパーミエーションクロマトグラフィー；ＨＰＣ−８０２０ 測定カラム；東ソー社社製 ＴＳＫｇｅｌＧＭＨ）を用いた。ＧＰＣは溶媒（ＴＨＦ；テトラヒドロフラン）に溶解した物質をその分子サイズの差によって分離定量する液体クロマトグラフィーであり、重量平均分子量の決定はポリスチレン換算で行った。
<Measurement of weight average molecular weight>
Tosoh GPC (gel permeation chromatography; HPC-8020 measuring column; TSKgelGMH, Tosoh Corporation) was used. GPC is liquid chromatography in which a substance dissolved in a solvent (THF; tetrahydrofuran) is separated and quantified by the difference in molecular size, and the weight average molecular weight was determined in terms of polystyrene.
＜評価用試料作製＞
得られた両面粘着テープの粘着剤層（３）に厚さ２５μｍのポリエチレンテレフタレートフィルムを貼り付けた。それを幅２５ｍｍ、長さ２００ｍｍに裁断し、粘着剤層（１）と軟質ウレタン発泡シート（密度：０．３２ｇ／ｃｍ３、Ａ硬度（ｓｈｏｒｅ−Ａ）：２４）の発泡セル開放面側に、２．０ｋｇｆの圧着ロールを用い、速度：３００ｍｍ／分で１往復して圧着した。圧着後、２３℃雰囲気下で２４時間放置して試料とした。
<Evaluation sample preparation>
A 25 μm thick polyethylene terephthalate film was attached to the pressure-sensitive adhesive layer (3) of the obtained double-sided pressure-sensitive adhesive tape. It is cut into a width of 25 mm and a length of 200 mm, on the foam cell open surface side of the pressure-sensitive adhesive layer (1) and the flexible urethane foam sheet (density: 0.32 g /
＜粘着力評価＞
得られた試料を２３℃雰囲気下で引張試験機を用いて、１８０度方向へ剥離速度３００ｍｍ／分で引き剥がすことで粘着力を測定した。
<Adhesive strength evaluation>
The obtained sample was peeled off in a 180 ° direction at a peeling speed of 300 mm / min using a tensile tester in an atmosphere of 23 ° C. to measure the adhesive force.
＜薬品浸漬後評価＞
得られた試料をｐＨ１１の４０℃の水酸化カリウム水溶液に１６８時間浸漬した。１６８時間経過後、４０℃の温水で洗浄して、すぐに４０℃雰囲気下で引張試験機を用いて、１８０度方向へ剥離速度３００ｍｍ／分で引き剥がすことで粘着力を測定した。
また、薬液をｐＨ１．５の硫酸水溶液に変えた以外は水酸化カリウム水溶液と同様に行い粘着力を測定した。
<Evaluation after chemical immersion>
The obtained sample was immersed in a 40 ° C. aqueous potassium hydroxide solution having a pH of 11 for 168 hours. After 168 hours had passed, the film was washed with 40 ° C. warm water, and immediately peeled off in the direction of 180 ° at a peeling rate of 300 mm / min using a tensile tester in a 40 ° C. atmosphere.
Further, the adhesive strength was measured in the same manner as the aqueous potassium hydroxide solution except that the chemical solution was changed to a sulfuric acid aqueous solution of pH 1.5.
＜保持力評価＞
得られた試料の粘着剤層（１）を、ＪＩＳＺ０２３７に準拠した表面を有するステンレス板（ＳＵＳ３０４ 横３０ｍｍ・縦１２０ｍｍ）に対してＪＩＳＺ０２３７に準拠した方法で、２．０ｋｇｆの圧着ロールを用い、速度：３００ｍｍ／分で１往復して圧着した。圧着後、１００℃雰囲気下で２０分間放置した以外はＪＩＳＺ０２３７に準拠し、ずれ距離を記録した。
<Retention force evaluation>
The pressure-sensitive adhesive layer (1) of the obtained sample is a method in accordance with JISZ0237 with respect to a stainless steel plate (SUS304 width 30 mm, length 120 mm) having a surface in conformity with JISZ0237, using a 2.0 kgf pressure roll. : Reciprocated once at 300 mm / min. The displacement distance was recorded in accordance with JISZ0237 except that it was left in a 100 ° C. atmosphere for 20 minutes after crimping.
＜総合評価＞
粘着力評価、薬品浸漬後評価、保持力評価の結果から、以下のような区分に評価した。
◎：より良好に使用可能
粘着力＝２４Ｎ／２５ｍｍ以上 薬品浸漬後評価＝２４Ｎ／２５ｍｍ以上
保持力＝０．６ｍｍ以下
○：良好に使用可能
粘着力＝２０Ｎ／２５ｍｍ以上 薬品浸漬後評価＝２０Ｎ／２５ｍｍ以上
保持力＝１ｍｍ以下
△：使用可能
粘着力＝２０Ｎ／２５ｍｍ以上 薬品浸漬後評価＝２０Ｎ／２５ｍｍ以上
保持力＝２ｍｍ以下
×：使用不可
粘着力＝２０Ｎ／２５ｍｍ未満、または薬品浸漬後評価＝２０Ｎ／２５ｍｍ未満
<Comprehensive evaluation>
Based on the results of evaluation of adhesive strength, evaluation after chemical immersion, and evaluation of holding power, evaluation was made in the following categories.
◎: Can be used better Adhesive strength = 24 N / 25 mm or more Evaluation after chemical immersion = 24 N / 25 mm or more Holding power = 0.6 mm or less Good: Usable well Adhesive strength = 20 N / 25 mm or more Evaluation after chemical immersion = 20 N / 25 mm or more Holding force = 1 mm or less Δ: Usable adhesive strength = 20 N / 25 mm or more Evaluation after chemical immersion = 20 N / 25 mm or more Holding force = 2 mm or less ×: Unusable Adhesive strength = less than 20 N / 25 mm or evaluation after chemical immersion = Less than 20N / 25mm
（実施例２）
重合用容器に仕込んだ原料をアクリル酸ブチル：７．６部、アクリル酸エチル：０．３部、アクリル酸：０．２部、アクリル酸２−ヒドロキシエチル：０．０２部、オクチルチオグリコレート：０．００５部、酢酸エチル：２７部、ベンゾイルパーオキサイド適量に変更した。また、滴下槽に仕込んだ原料をアクリル酸ブチル：３０部、アクリル酸エチル：１．２部、アクリル酸：０．７部、アクリル酸２−ヒドロキシエチル：０．１部、オクチルチオグリコレート：０．０２２部、酢酸エチル：９．５部に変更した以外は、実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．９重量％、共重合体の重量平均分子量は５５０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−４８℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合することで粘着剤を得た。得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Example 2)
The raw materials charged in the polymerization vessel were butyl acrylate: 7.6 parts, ethyl acrylate: 0.3 parts, acrylic acid: 0.2 parts, 2-hydroxyethyl acrylate: 0.02 parts, octyl thioglycolate : 0.005 part, ethyl acetate: 27 parts, benzoyl peroxide was changed to an appropriate amount. The raw materials charged in the dropping tank were butyl acrylate: 30 parts, ethyl acrylate: 1.2 parts, acrylic acid: 0.7 parts, 2-hydroxyethyl acrylate: 0.1 parts, octyl thioglycolate: An acrylic resin solution was obtained by synthesizing in the same manner as in Example 1 except that 0.022 parts and ethyl acetate were changed to 9.5 parts. This resin solution was colorless and transparent, had a non-volatile content of 38.9% by weight, and the copolymer had a weight average molecular weight of 550,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -48 degreeC.
An adhesive was obtained by blending the obtained acrylic resin solution in the same manner as in Example 1. By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 35 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
（実施例３）
重合用容器に仕込んだ原料をアクリル酸ブチル：７．０部、アクリル酸エチル：０．８部、アクリル酸：０．２部、アクリル酸２−ヒドロキシエチル：０．０２部、オクチルチオグリコレート：０．００５部、酢酸エチル：２７部、ベンゾイルパーオキサイド適量に変更した。また、滴下槽に仕込んだ原料をアクリル酸ブチル：２８部、アクリル酸エチル：３．０部、アクリル酸：０．７部、アクリル酸２−ヒドロキシエチル：０．１部、オクチルチオグリコレート：０．０２２部、酢酸エチル：９．５部に変更した以外は、実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３９．２重量％、共重合体の重量平均分子量は６００，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−４７℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合することで粘着剤を得た。得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ４０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Example 3)
Raw materials charged in the polymerization vessel were butyl acrylate: 7.0 parts, ethyl acrylate: 0.8 parts, acrylic acid: 0.2 parts, 2-hydroxyethyl acrylate: 0.02 parts, octyl thioglycolate : 0.005 part, ethyl acetate: 27 parts, benzoyl peroxide was changed to an appropriate amount. The raw materials charged in the dropping tank were butyl acrylate: 28 parts, ethyl acrylate: 3.0 parts, acrylic acid: 0.7 parts, 2-hydroxyethyl acrylate: 0.1 parts, octyl thioglycolate: An acrylic resin solution was obtained by synthesizing in the same manner as in Example 1 except that 0.022 parts and ethyl acetate were changed to 9.5 parts. This resin solution was colorless and transparent, had a non-volatile content of 39.2% by weight, and the copolymer had a weight average molecular weight of 600,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radically polymerizable unsaturated monomer for Numerical formula (1) is -47 degreeC.
An adhesive was obtained by blending the obtained acrylic resin solution in the same manner as in Example 1. By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 40 μm is formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm is formed on the other side. The formed double-sided adhesive tape was obtained.
（実施例４）
滴下槽のモノマーのうちオクチルチオグリコレートを０．０１１部に変更し、重合用容器のモノマーのうちオクチルチオグリコレートを０．００２５部に変更した以外は実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．２重量％、共重合体の重量平均分子量は６４０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５０℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合して粘着剤を得、さらに実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ６０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
Example 4
Synthesis is performed in the same manner as in Example 1 except that octyl thioglycolate is changed to 0.011 part of the monomer in the dropping tank and octyl thioglycolate is changed to 0.0025 part of the monomer for the polymerization vessel. The acrylic resin solution was obtained. This resin solution was colorless and transparent, had a non-volatile content of 38.2% by weight, and the copolymer had a weight average molecular weight of 640,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -50 degreeC.
The obtained acrylic resin solution was blended in the same manner as in Example 1 to obtain a pressure-sensitive adhesive, and further coated in the same manner as in Example 1, so that a pressure-sensitive adhesive layer (60 μm thick) was formed on one side of a 25 μm-thick polyethylene terephthalate film. 1) A double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer (3) having a thickness of 30 μm formed on the other side was obtained.
（実施例５）
実施例４で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を８．５部と、石油樹脂Ｌ９０（新日本石油社製）を１．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１と同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ６０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Example 5)
8.5 parts of Pencel C (manufactured by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 1.8 parts of petroleum resin L90 (manufactured by Nippon Oil Co., Ltd.) with respect to 100 parts of the acrylic resin solution obtained in Example 4 Then, 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 60 μm on one side of a polyethylene terephthalate film having a thickness of 25 μm and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm on the other side. Thus, a double-sided pressure-sensitive adhesive tape on which was formed was obtained.
（実施例６）
滴下槽のモノマーのうちオクチルチオグリコレートを０．０３３部に変更し、重合用容器のモノマーのうちオクチルチオグリコレートを０．００７５部に変更した以外は実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３９．０重量％、共重合体の重量平均分子量は４００，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５０℃である。
得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を６．５部と、石油樹脂Ｌ９０（新日本石油社製）を３．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ６０μｍ粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Example 6)
Synthesis is performed in the same manner as in Example 1 except that octyl thioglycolate is changed to 0.033 part of the monomer in the dropping tank and octyl thioglycolate is changed to 0.0075 part of the monomer for the polymerization vessel. The acrylic resin solution was obtained. This resin solution was colorless and transparent, had a nonvolatile content of 39.0% by weight, and the copolymer had a weight average molecular weight of 400,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -50 degreeC.
To 100 parts of the resulting acrylic resin solution, 6.5 parts of Pencel C (Arakawa Chemical Co., Ltd.), a polymerized rosin ester, 3.8 parts of petroleum resin L90 (Shin Nippon Oil Co., Ltd.), ethyl acetate: 15 parts, Tolylene diisocyanate trimethylolpropane adduct: 0.7 parts as a curing agent was added and mixed to obtain a pressure-sensitive adhesive.
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a 60 μm-thick pressure-sensitive adhesive layer (1) is formed on one side of a 25 μm-thick polyethylene terephthalate film, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm is formed on the other side. A double-sided adhesive tape was obtained.
（実施例７）
滴下槽のモノマーのうちオクチルチオグリコレートを０．０１１部に変更し、重合用容器のモノマーのうちオクチルチオグリコレートを０．００２５部に変更した以外は実施例２と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．９重量％、共重合体の重量平均分子量は７００，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−４８℃である。
得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を６．５部と、石油樹脂Ｌ９０（新日本石油社製）を３．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ４５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Example 7)
Synthesis is performed in the same manner as in Example 2 except that octyl thioglycolate is changed to 0.011 part of the monomer in the dropping tank and octyl thioglycolate is changed to 0.0025 part of the monomer for the polymerization vessel. The acrylic resin solution was obtained. This resin solution was colorless and transparent, had a non-volatile content of 38.9% by weight, and the copolymer had a weight average molecular weight of 700,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -48 degreeC.
To 100 parts of the resulting acrylic resin solution, 6.5 parts of Pencel C (Arakawa Chemical Co., Ltd.), a polymerized rosin ester, 3.8 parts of petroleum resin L90 (Shin Nippon Oil Co., Ltd.), ethyl acetate: 15 parts, Tolylene diisocyanate trimethylolpropane adduct: 0.7 parts as a curing agent was added and mixed to obtain a pressure-sensitive adhesive.
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 45 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
（実施例８）
滴下槽のモノマーのうちオクチルチオグリコレートを０．０３３部に変更し、重合用容器のモノマーのうちオクチルチオグリコレートを０．００７５部に変更した以外は実施例２と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．９重量％、共重合体の重量平均分子量は４５０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−４８℃である。
得られたアクリル樹脂溶液１００部に対して酸価：１０ｍｇＫＯＨ／ｇ、軟化点１１５℃の重合ロジンエステルであるＳ１１５（荒川化学社製）を７．５部、軟化点９８℃の石油樹脂ペトコールＬＸ（東ソー社製）を２．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に４５μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ３１５６Ｄを主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 8)
The synthesis is performed in the same manner as in Example 2 except that octyl thioglycolate is changed to 0.033 part of the monomer in the dropping tank and octyl thioglycolate is changed to 0.0075 part of the monomer for the polymerization vessel. The acrylic resin solution was obtained. This resin solution was colorless and transparent, had a non-volatile content of 38.9% by weight, and the copolymer had a weight average molecular weight of 450,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -48 degreeC.
Petroleum LX petroleum resin having an acid value of 10 mg KOH / g and a polymerized rosin ester S115 (manufactured by Arakawa Chemical Co., Ltd.) having a softening point of 115 ° C. and a softening point of 98 ° C. with respect to 100 parts of the resulting acrylic resin solution. 2.8 parts (manufactured by Tosoh Corporation), 15 parts of ethyl acetate, and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
The obtained pressure-sensitive adhesive was formed as a 45 μm pressure-sensitive adhesive layer (1) on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. On the other side, BPS3156D manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct body: 0.7 part is added and mixed as a curing agent, and the resulting adhesive is transferred to the adhesive layer having a thickness of 30 μm. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例９）
実施例８で得られたアクリル樹脂溶液１００部に対して、重合ロジンエステルであるＳ１１５（荒川化学社製）を８．５部と、石油樹脂ペトコールＬＸ（東ソー社製）を１．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に４５μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ３１５６Ｄを主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
Example 9
For 100 parts of the acrylic resin solution obtained in Example 8, 8.5 parts of S115 (manufactured by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 1.8 parts of petroleum resin Petol LX (manufactured by Tosoh Corporation), 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
The obtained pressure-sensitive adhesive was formed as a 45 μm pressure-sensitive adhesive layer (1) on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. On the other side, BPS3156D manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct body: 0.7 part is added and mixed as a curing agent, and the resulting adhesive is transferred to the adhesive layer having a thickness of 30 μm. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例１０）
実施例１で得られたアクリル樹脂溶液１００部に対して酸価：１４ｍｇＫＯＨ／ｇ、軟化点１２３℃の重合ロジンエステルであるハリタックＰＣＪ（ハリマ化成社製）を７．５部、軟化点９８℃の石油樹脂ペトコール１００Ｔ（東ソー社製）を２．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に４０μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ１１０９を主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：１．６８部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 10)
7.5 parts of a Haritac PCJ (Harima Kasei Co., Ltd.) which is a polymerized rosin ester having an acid value of 14 mg KOH / g and a softening point of 123 ° C. with respect to 100 parts of the acrylic resin solution obtained in Example 1, a softening point of 98 ° C. 2.8 parts of petroleum resin Petol 100T (manufactured by Tosoh Corporation), 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
The obtained pressure-sensitive adhesive was formed as a pressure-sensitive adhesive layer (1) having a thickness of 40 μm on one surface of a polyethylene terephthalate film having a thickness of 25 μm by a transfer method. Also, on the other side, BPS1109 manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct: 1.68 parts are added and mixed as a curing agent, and the resulting pressure-sensitive adhesive is a pressure-sensitive adhesive layer having a thickness of 30 μm by a transfer method. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例１１）
実施例１０で得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に１００μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ１１０９を主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：１．６８部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 11)
The pressure-sensitive adhesive obtained in Example 10 was formed as a 100 μm pressure-sensitive adhesive layer (1) on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. Also, on the other side, BPS1109 manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct: 1.68 parts are added and mixed as a curing agent, and the resulting pressure-sensitive adhesive is a pressure-sensitive adhesive layer having a thickness of 30 μm by a transfer method. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例１２）
実施例３で得られたアクリル樹脂溶液１００部に対して酸価：１４ｍｇＫＯＨ／ｇ、軟化点１２３℃の重合ロジンエステルであるハリタックＰＣＪ（ハリマ化成社製）を７．５部、軟化点９８℃の石油樹脂ペトコール１００Ｔ（東ソー社製）を２．８部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に８０μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ１１０９を主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：１．６８部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 12)
7.5 parts of a Haritac PCJ (Harima Kasei Co., Ltd.), which is a polymerized rosin ester having an acid value of 14 mg KOH / g and a softening point of 123 ° C., relative to 100 parts of the acrylic resin solution obtained in Example 3, a softening point of 98 ° C. 2.8 parts of petroleum resin Petol 100T (manufactured by Tosoh Corporation), 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
The obtained adhesive was formed as an adhesive layer (1) having a thickness of 80 μm on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. Also, on the other side, BPS1109 manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct: 1.68 parts are added and mixed as a curing agent, and the resulting pressure-sensitive adhesive is a pressure-sensitive adhesive layer having a thickness of 30 μm by a transfer method. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例１３）
実施例２で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルを１０．０部、石油樹脂を３．５部配合した以外を実施例１と同様に配合することで粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に３５μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ１１０９を主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：１．６８部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 13)
A pressure-sensitive adhesive was obtained by blending in the same manner as in Example 1 except that 10.0 parts of polymerized rosin ester and 3.5 parts of petroleum resin were blended with 100 parts of the acrylic resin solution obtained in Example 2. .
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 35 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
The obtained pressure-sensitive adhesive was formed as a 35 μm pressure-sensitive adhesive layer (1) on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. Also, on the other side, BPS1109 manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct: 1.68 parts are added and mixed as a curing agent, and the resulting pressure-sensitive adhesive is a pressure-sensitive adhesive layer having a thickness of 30 μm by a transfer method. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（実施例１４）
実施例２で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルを４．４部、石油樹脂を１．５部配合した以外を実施例１と同様に配合することで粘着剤を得た。
得られた粘着剤を転写法で厚み２５μｍのポリエチレンテレフタレートフィルムの一方の面に３５μｍの粘着剤層（１）として形成した。また他方の面にトーヨーケム社製ＢＰＳ１１０９を主剤とし、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：１．６８部を添加及び混合し、得られた粘着剤を転写法で厚み３０μｍの粘着剤層（３）を形成し、両面粘着テープを得た。
(Example 14)
An adhesive was obtained by blending in the same manner as in Example 1 except that 4.4 parts of polymerized rosin ester and 1.5 parts of petroleum resin were blended with 100 parts of the acrylic resin solution obtained in Example 2. .
The obtained pressure-sensitive adhesive was formed as a 35 μm pressure-sensitive adhesive layer (1) on one surface of a 25 μm-thick polyethylene terephthalate film by a transfer method. Also, on the other side, BPS1109 manufactured by Toyochem Co., Ltd. is used as the main agent, and tolylene diisocyanate trimethylolpropane adduct: 1.68 parts are added and mixed as a curing agent, and the resulting pressure-sensitive adhesive is a pressure-sensitive adhesive layer having a thickness of 30 μm by a transfer method. (3) was formed to obtain a double-sided pressure-sensitive adhesive tape.
（比較例１）
滴下槽および重合用容器にオクチルチオグリコレートを仕込まない以外は、実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．９重量％、共重合体の重量平均分子量は８００，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５０℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合して粘着剤を得、さらに実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３０μｍ、の粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 1)
An acrylic resin solution was obtained by synthesizing in the same manner as in Example 1 except that octylthioglycolate was not charged into the dropping tank and the polymerization vessel. This resin solution was colorless and transparent, had a non-volatile content of 38.9% by weight, and the copolymer had a weight average molecular weight of 800,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -50 degreeC.
The obtained acrylic resin solution was blended in the same manner as in Example 1 to obtain a pressure-sensitive adhesive, and further coated in the same manner as in Example 1, so that a pressure-sensitive adhesive layer having a thickness of 30 μm was formed on one side of a 25 μm-thick polyethylene terephthalate film. (1) A double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer (3) having a thickness of 30 μm formed on the other side was obtained.
（比較例２）
滴下槽のモノマーのうちオクチルチオグリコレートを０．０４４部に変更し、重合用容器のモノマーのうちオクチルチオグリコレートを０．０１に変更した以外は実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．７重量％、共重合体の重量平均分子量は３００，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５０℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合して粘着剤を得、さらに実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ４５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
得られたアクリル樹脂溶液を実施例１と配合して粘着剤を得、さらに実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３０μｍ、の粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 2)
By synthesizing in the same manner as in Example 1 except that octyl thioglycolate was changed to 0.044 parts of the monomer in the dropping tank and octyl thioglycolate was changed to 0.01 among the monomers in the polymerization vessel. An acrylic resin solution was obtained. This resin solution was colorless and transparent, had a nonvolatile content of 38.7% by weight, and the copolymer had a weight average molecular weight of 300,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -50 degreeC.
The obtained acrylic resin solution was blended in the same manner as in Example 1 to obtain a pressure-sensitive adhesive, and further coated in the same manner as in Example 1, so that a 45 μm-thick pressure-sensitive adhesive layer ( 1) A double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer (3) having a thickness of 30 μm formed on the other side was obtained.
The obtained acrylic resin solution was blended with Example 1 to obtain a pressure-sensitive adhesive, and further coated in the same manner as in Example 1, whereby a pressure-sensitive adhesive layer (1 μm in thickness of 30 μm on one side of a 25 μm-thick polyethylene terephthalate film). ), And a double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer (3) having a thickness of 30 μm formed on the other side.
（比較例３）
重合用容器に仕込んだ原料をアクリル酸ブチル：７．８部、アクリル酸エチル：０．０５部、アクリル酸：０．１部、アクリル酸２−ヒドロキシエチル：０．０２部、オクチルチオグリコレート：０．００５部、酢酸エチル：２７部、ベンゾイルパーオキサイド適量に変更した。また、滴下槽に仕込んだ原料をアクリル酸ブチル：３２部、アクリル酸エチル：０．１５部、アクリル酸：０．３５部、アクリル酸２−ヒドロキシエチル：０．１部、オクチルチオグリコレート：０．０２２部、酢酸エチル：９．５部に変更した以外は、実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．６重量％、共重合体の重量平均分子量は４９０，０００でであった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５１℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合することで粘着剤を得た。得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 3)
Raw materials charged in the polymerization vessel were butyl acrylate: 7.8 parts, ethyl acrylate: 0.05 parts, acrylic acid: 0.1 parts, 2-hydroxyethyl acrylate: 0.02 parts, octyl thioglycolate : 0.005 part, ethyl acetate: 27 parts, benzoyl peroxide was changed to an appropriate amount. The raw materials charged in the dropping tank were butyl acrylate: 32 parts, ethyl acrylate: 0.15 parts, acrylic acid: 0.35 parts, 2-hydroxyethyl acrylate: 0.1 parts, octylthioglycolate: An acrylic resin solution was obtained by synthesizing in the same manner as in Example 1 except that 0.022 parts and ethyl acetate were changed to 9.5 parts. This resin solution was colorless and transparent, had a non-volatile content of 38.6% by weight, and the copolymer had a weight average molecular weight of 490,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -51 degreeC.
An adhesive was obtained by blending the obtained acrylic resin solution in the same manner as in Example 1. By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 35 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
（比較例４）
重合用容器に仕込んだ原料を６．０部、アクリル酸２−エチルヘキシル：１．７部、アクリル酸：０．２部、アクリル酸２−ヒドロキシエチル：０．０２部、オクチルチオグリコレート：０．００５部、酢酸エチル：２７部、ベンゾイルパーオキサイド適量に変更した。また、滴下槽に仕込んだ原料をアクリル酸ブチル：２４．１部、アクリル酸２−エチルヘキシル：６．８部、アクリル酸：０．７部、アクリル酸２−ヒドロキシエチル：０．１部、オクチルチオグリコレート：０．０２２部、酢酸エチル：９．５部に変更した以外は、実施例１と同様に合成を行うことでアクリル樹脂溶液を得た。この樹脂溶液は、無色透明で不揮発分３８．４重量％、共重合体の重量平均分子量は４１０，０００であった。尚、上記ラジカル重合性不飽和モノマーの組成を数式（１）に代入して求めたアクリル樹脂のガラス転移温度は−５５℃である。
得られたアクリル樹脂溶液を実施例１と同様に配合することで粘着剤を得た。得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 4)
6.0 parts of raw materials charged in the polymerization vessel, 1.7 parts of 2-ethylhexyl acrylate, 0.2 parts of acrylic acid, 0.02 parts of 2-hydroxyethyl acrylate, 0.02 parts of octylthioglycolate: 0 0.005 part, ethyl acetate: 27 parts, changed to benzoyl peroxide appropriate amount. The raw materials charged in the dropping tank were butyl acrylate: 24.1 parts, 2-ethylhexyl acrylate: 6.8 parts, acrylic acid: 0.7 parts, 2-hydroxyethyl acrylate: 0.1 parts, octyl An acrylic resin solution was obtained by synthesis in the same manner as in Example 1 except that thioglycolate was changed to 0.022 parts and ethyl acetate was changed to 9.5 parts. This resin solution was colorless and transparent, had a nonvolatile content of 38.4% by weight, and the copolymer had a weight average molecular weight of 410,000. In addition, the glass transition temperature of the acrylic resin calculated | required by substituting the composition of the said radical polymerizable unsaturated monomer for Numerical formula (1) is -55 degreeC.
An adhesive was obtained by blending the obtained acrylic resin solution in the same manner as in Example 1. By applying the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 30 μm is formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm is formed on the other side. The formed double-sided adhesive tape was obtained.
（比較例５）
実施例１で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を５．３部と、石油樹脂Ｌ９０（新日本石油社製）を５．０部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 5)
For 100 parts of the acrylic resin solution obtained in Example 1, 5.3 parts of Pencel C (made by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 5.0 parts of petroleum resin L90 (made by Nippon Oil Corporation). Then, 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
By applying the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 30 μm is formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm is formed on the other side. The formed double-sided adhesive tape was obtained.
（比較例６）
実施例１で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を５．３部と、石油樹脂Ｌ９０（新日本石油社製）を５．０部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３０μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 6)
For 100 parts of the acrylic resin solution obtained in Example 1, 5.3 parts of Pencel C (made by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 5.0 parts of petroleum resin L90 (made by Nippon Oil Corporation). Then, 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
By applying the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 30 μm is formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm is formed on the other side. The formed double-sided adhesive tape was obtained.
（比較例７）
実施例２で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を１２．０部と、石油樹脂Ｌ９０（新日本石油社製）を４．２部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 7)
12.0 parts of Pencel C (made by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 4.2 parts of petroleum resin L90 (made by Shin Nippon Oil Co., Ltd.) with respect to 100 parts of the acrylic resin solution obtained in Example 2. Then, 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 35 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
（比較例８）
実施例２で得られたアクリル樹脂溶液１００部に対して重合ロジンエステルであるペンセルＣ（荒川化学社製）を３．５部と、石油樹脂Ｌ９０（新日本石油社製）を１．２部、酢酸エチル：１５部、硬化剤としてトリレンジイソシアネートトリメチロールプロパンアダクト体：０．７部を添加及び混合して粘着剤を得た。
得られた粘着剤を実施例１同様に塗工することで、厚み２５μｍのポリエチレンテレフタレートフィルムの一方に厚さ３５μｍの粘着剤層（１）、他方に厚さ３０μｍの粘着剤層（３）が形成された両面粘着テープを得た。
(Comparative Example 8)
3.5 parts of Pencel C (made by Arakawa Chemical Co., Ltd.), which is a polymerized rosin ester, and 1.2 parts of petroleum resin L90 (made by Shin Nippon Oil Co., Ltd.) with respect to 100 parts of the acrylic resin solution obtained in Example 2 Then, 15 parts of ethyl acetate and 0.7 parts of tolylene diisocyanate trimethylolpropane adduct as a curing agent were added and mixed to obtain an adhesive.
By coating the obtained pressure-sensitive adhesive in the same manner as in Example 1, a pressure-sensitive adhesive layer (1) having a thickness of 35 μm was formed on one side of a polyethylene terephthalate film having a thickness of 25 μm, and a pressure-sensitive adhesive layer (3) having a thickness of 30 μm was formed on the other side. The formed double-sided adhesive tape was obtained.
評価結果を表１〜表４に示す。 The evaluation results are shown in Tables 1 to 4.
１Ａ 上定盤
１Ｂ 下定盤
２Ａ 研磨部材固定用両面粘着テープ
２Ｂ 研磨部材固定用両面粘着テープ
３ 研磨用吸着パッド
４ テンプレート
５ 被研磨体
６ 研磨パッド
７ 粘着剤層（３）
８ プラスチック基材（２）
９ 粘着剤層（１）
１０ 軟質ウレタン樹脂発泡体
DESCRIPTION OF SYMBOLS 1A
8 Plastic base material (2)
9 Adhesive layer (1)
10 Soft urethane resin foam
Claims (3)
粘着剤層（１）は、アクリル系樹脂（イ）と、ロジンエステル骨格を有する粘着付与樹脂（ｘ）および芳香族系石油系樹脂骨格を有する粘着付与樹脂（ｙ）とを含有する粘着剤（Ａ）から形成され、
粘着剤（Ａ）は、アクリル系樹脂（イ）１００重量部に対して、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との合計量１５〜３５重量部を含み、粘着付与樹脂（ｘ）と粘着付与樹脂（ｙ）との重量比が（ｘ）／（ｙ）＝３／２〜９／２であり、
アクリル系樹脂（イ）は、そのガラス転移温度が−７０℃以上０℃以下で、その重量平均分子量が４０万〜７０万であり、かつアクリル酸ブチル８５〜９７重量％とアクリル酸ブチル以外のモノマー３〜１５重量％を共重合してなることを特徴とする研磨部材固定用両面粘着テープ。 A double-sided pressure-sensitive adhesive tape for fixing an abrasive member, comprising an adhesive layer (1), a plastic substrate (2), and an adhesive layer (3),
The pressure-sensitive adhesive layer (1) is a pressure-sensitive adhesive containing an acrylic resin (I), a tackifier resin (x) having a rosin ester skeleton, and a tackifier resin (y) having an aromatic petroleum resin skeleton ( Formed from A),
The pressure-sensitive adhesive (A) includes a total amount of 15 to 35 parts by weight of the tackifier resin (x) and the tackifier resin (y) with respect to 100 parts by weight of the acrylic resin (b), and the tackifier resin (x ) And the tackifier resin (y) are (x) / (y) = 3/2 to 9/2,
The acrylic resin (A) has a glass transition temperature of −70 ° C. or more and 0 ° C. or less, a weight average molecular weight of 400,000 to 700,000, and 85 to 97% by weight of butyl acrylate and butyl acrylate. A double-sided pressure-sensitive adhesive tape for fixing an abrasive member, comprising a copolymer of 3 to 15% by weight of a monomer.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2012160267A JP5942657B2 (en) | 2012-07-19 | 2012-07-19 | Double-sided adhesive tape for fixing abrasive members |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2012160267A JP5942657B2 (en) | 2012-07-19 | 2012-07-19 | Double-sided adhesive tape for fixing abrasive members |
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| Publication Number | Publication Date |
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| JP2014019801A true JP2014019801A (en) | 2014-02-03 |
| JP2014019801A5 JP2014019801A5 (en) | 2015-06-18 |
| JP5942657B2 JP5942657B2 (en) | 2016-06-29 |
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| JP2012160267A Active JP5942657B2 (en) | 2012-07-19 | 2012-07-19 | Double-sided adhesive tape for fixing abrasive members |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016098335A (en) * | 2014-11-25 | 2016-05-30 | 東洋インキＳｃホールディングス株式会社 | Adhesive and adhesive sheet |
| JP2017105976A (en) * | 2015-11-30 | 2017-06-15 | 日東電工株式会社 | Polishing pad fixing adhesive sheet |
| JP2020164786A (en) * | 2019-03-29 | 2020-10-08 | 住友ベークライト株式会社 | Pressure sensitive adhesive tape |
| JP2021105098A (en) * | 2019-12-26 | 2021-07-26 | 東洋インキＳｃホールディングス株式会社 | Adhesive for fixing abrasive member, and adhesive sheet |
| JP6977855B1 (en) * | 2020-12-18 | 2021-12-08 | 東洋インキＳｃホールディングス株式会社 | Double-sided adhesive sheet, polishing member, and surface plate with polishing pad |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106992112A (en) * | 2016-01-21 | 2017-07-28 | 苏州新美光纳米科技有限公司 | The polishing method of ultra thin wafer |
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| JP2002285114A (en) * | 2001-03-26 | 2002-10-03 | Sekisui Chem Co Ltd | Tape for abrasive fixing |
| JP2006249404A (en) * | 2005-02-14 | 2006-09-21 | Nitto Denko Corp | Adhesive tape and adhesive composition |
| JP2010194700A (en) * | 2009-02-27 | 2010-09-09 | Sekisui Chem Co Ltd | Adhesive double coated tape for fixing abrasive, and adhesive tape with the abrasive |
| JP2010194699A (en) * | 2009-02-27 | 2010-09-09 | Sekisui Chem Co Ltd | Adhesive double coated tape for fixing abrasive, and adhesive tape with the abrasive |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002285114A (en) * | 2001-03-26 | 2002-10-03 | Sekisui Chem Co Ltd | Tape for abrasive fixing |
| JP2006249404A (en) * | 2005-02-14 | 2006-09-21 | Nitto Denko Corp | Adhesive tape and adhesive composition |
| JP2010194700A (en) * | 2009-02-27 | 2010-09-09 | Sekisui Chem Co Ltd | Adhesive double coated tape for fixing abrasive, and adhesive tape with the abrasive |
| JP2010194699A (en) * | 2009-02-27 | 2010-09-09 | Sekisui Chem Co Ltd | Adhesive double coated tape for fixing abrasive, and adhesive tape with the abrasive |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016098335A (en) * | 2014-11-25 | 2016-05-30 | 東洋インキＳｃホールディングス株式会社 | Adhesive and adhesive sheet |
| JP2017105976A (en) * | 2015-11-30 | 2017-06-15 | 日東電工株式会社 | Polishing pad fixing adhesive sheet |
| CN107033796A (en) * | 2015-11-30 | 2017-08-11 | 日东电工株式会社 | Grinding pad fixation bonding sheet |
| JP2020164786A (en) * | 2019-03-29 | 2020-10-08 | 住友ベークライト株式会社 | Pressure sensitive adhesive tape |
| JP2021105098A (en) * | 2019-12-26 | 2021-07-26 | 東洋インキＳｃホールディングス株式会社 | Adhesive for fixing abrasive member, and adhesive sheet |
| JP7287270B2 (en) | 2019-12-26 | 2023-06-06 | 東洋インキＳｃホールディングス株式会社 | Adhesive for fixing polishing member and adhesive sheet |
| JP6977855B1 (en) * | 2020-12-18 | 2021-12-08 | 東洋インキＳｃホールディングス株式会社 | Double-sided adhesive sheet, polishing member, and surface plate with polishing pad |
| JP2022096727A (en) * | 2020-12-18 | 2022-06-30 | 東洋インキＳｃホールディングス株式会社 | Double-sided adhesive sheet, polishing member, and surface plate with polishing pad |
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| JP5942657B2 (en) | 2016-06-29 |
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