CN106103627B - 热敏性粘合剂 - Google Patents
热敏性粘合剂 Download PDFInfo
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- CN106103627B CN106103627B CN201580014210.9A CN201580014210A CN106103627B CN 106103627 B CN106103627 B CN 106103627B CN 201580014210 A CN201580014210 A CN 201580014210A CN 106103627 B CN106103627 B CN 106103627B
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- Prior art keywords
- methyl
- acrylate
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- thermal
- alkyl
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- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims abstract description 44
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 38
- 229920000642 polymer Polymers 0.000 claims abstract description 38
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
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- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 5
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- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical compound C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 claims description 2
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- 125000002947 alkylene group Chemical group 0.000 claims 1
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
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- 125000002511 behenyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 7
- 239000007767 bonding agent Substances 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- 125000001118 alkylidene group Chemical group 0.000 description 3
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
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- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- UXUDJAVFUJMRFG-UHFFFAOYSA-N COC(C=C)=O.[C] Chemical compound COC(C=C)=O.[C] UXUDJAVFUJMRFG-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
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- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
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- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
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- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J143/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Adhesives based on derivatives of such polymers
- C09J143/04—Homopolymers or copolymers of monomers containing silicon
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L83/04—Polysiloxanes
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- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
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- C09J7/255—Polyesters
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- H—ELECTRICITY
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- H01G4/00—Fixed capacitors; Processes of their manufacture
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- H01—ELECTRIC ELEMENTS
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- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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Abstract
本发明的热敏性粘合剂含有通过使至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯聚合所得的侧链结晶性聚合物,在低于上述侧链结晶性聚合物的熔点的温度下粘合力降低。上述侧链结晶性聚合物包含进一步使反应性聚硅氧烷化合物聚合所得的共聚物,上述至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯和上述反应性聚硅氧烷化合物的比率以重量比计为至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯:反应性聚硅氧烷化合物=91∶9~99∶1。
Description
技术领域
本发明是可通过热来可逆地控制粘合力的热敏性粘合剂。
背景技术
热敏性粘合剂是可通过热来可逆地控制其粘合力的热敏性粘合剂。更具体地,热敏性粘合剂若冷却至低于含有的作为主成分的侧链结晶性聚合物的熔点的温度时,由于侧链结晶性聚合物发生结晶化而使粘合力降低。
热敏性粘合剂的一种使用形态即热敏性粘合带用于制造叠层陶瓷电容器等陶瓷构件(例如参照专利文献1)。在陶瓷构件的制造中,热敏性粘合带使用于构件的临时固定用途。希望如此的用途所使用的热敏性粘合带在将暂时贴合的粘合带进行再剥离的方面为粘合性与剥离性的均衡性优异的热敏性粘合带。
另一方面,本案申请人率先开发出一种通过将反应性聚硅氧烷化合物与侧链结晶性聚合物共聚而发挥优异的剥离性的专利文献2所述的热敏性粘合带。反应性聚硅氧烷化合物因为价格较高,故希望使共聚的比率越少越好。另外,若反应性聚硅氧烷化合物的比率变多,则热敏性粘合带的粘合性与剥离性的均衡性有变得不稳定的隐患。
现有技术文献
专利文献
专利文献1:日本特开平9-251923号公报
专利文献2:日本专利第5231775号公报
发明内容
发明想要解决的课题
本发明的课题是提供一种可降低成本,且粘合性和剥离性的均衡性优异的热敏性粘合剂。
用以解决课题的手段
本发明的热敏性粘合剂含有通过使至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯聚合所得的侧链结晶性聚合物,在低于上述侧链结晶性聚合物的熔点的温度下粘合力降低,上述侧链结晶性聚合物包含通过进一步聚合反应性聚硅氧烷化合物所得的共聚物,上述至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯和上述反应性聚硅氧烷化合物的比率以重量比计为:至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯∶反应性聚硅氧烷化合物=91∶9~99∶1。
发明的效果
若依据本发明,具有可降低成本,且粘合性和剥离性的均衡性优异的效果。
具体实施方式
<热敏性粘合剂/热敏性粘合片/热敏性粘合带>
以下,详细说明本发明的一个实施方式的热敏性粘合剂。本实施方式的热敏性粘合剂含有侧链结晶性聚合物。侧链结晶性聚合物是具有熔点的聚合物。所谓熔点是通过某种平衡过程,起初被整合成有秩序排列的聚合体的特定部分变成无秩序状态的温度,是指利用差示扫描量热计(DSC)以10℃/分钟的测定条件测定所得的值。
侧链结晶性聚合物在上述的低于熔点的温度下发生结晶化,且在熔点以上的温度发生相转移而显示流动性。即,侧链结晶性聚合物具有与温度变化相应地可逆地引起结晶状态与流动状态的热敏性。而且,本实施方式的热敏性粘合剂依侧链结晶性聚合物在低于熔点的温度进行结晶化时粘合力降低的比例含有侧链结晶性聚合物。也就是说,本实施方式的热敏性粘合剂含有侧链结晶性聚合物作为主成分,实质上由侧链结晶性聚合物构成,故从构件剥离热敏性粘合剂时,若使热敏性粘合剂冷却至低于侧链结晶性聚合物的熔点的温度,则由于侧链结晶性聚合物发生结晶化而使粘合力降低。另外,若使热敏性粘合剂加热至侧链结晶性聚合物的熔点以上的温度,则侧链结晶性聚合物显示流动性而恢复粘合力,故可重复使用。
熔点以30℃以上为较优,以40至65℃为更优,以50至60℃为最优。熔点可通过调整侧链结晶性聚合物的组成等而控制成所希望的值。本实施方式的侧链结晶性聚合物包含:通过使具有至少碳数16以上的直链状烷基的(甲基)丙烯酸酯、和反应性聚硅氧烷化合物聚合所得的共聚物。
具有碳数16以上的直链状烷基的(甲基)丙烯酸酯其碳数16以上的直链状烷基发挥侧链结晶性聚合物中的侧链结晶性部位的作用。即,侧链结晶性聚合物是在侧链具有碳数16以上的直链状烷基的梳形的聚合物,此侧链通过分子间力等而整合成有秩序的排列由此进行结晶化。如此的具有碳数16以上的直链状烷基的(甲基)丙烯酸酯可列举例如:(甲基)丙烯酸鲸蜡酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸二十烷基酯、(甲基)丙烯酸二十二烷基酯等具有碳数16至22的线状烷基的(甲基)丙烯酸酯,它们可以使用1种或混合使用2种以上。所例示的这些(甲基)丙烯酸酯之中,以(甲基)丙烯酸二十二烷基酯为较优。另外,(甲基)丙烯酸酯意指丙烯酸酯或甲基丙烯酸酯。
反应性聚硅氧烷化合物意指具有显示反应性的官能基,且在主链具有硅氧烷键的聚硅氧烷化合物。反应性聚硅氧烷化合物在室温(23℃)可为蜡状,但在高效聚合的方面,在室温显示流动性的油状、即聚硅氧油为较优。
另外,上述的官能基可列举例如:乙烯基、烯丙基、(甲基)丙烯酸基、(甲基)丙烯酰基、(甲基)丙烯酰氧基等烯属不饱和双键;环氧基(包含缩水甘油基和环氧环烷基)、巯基、甲醇基、羧基、硅烷醇基、酚基、氨基、羟基等。
所例示的官能基可导入主链所具有的侧链,也可导入主链的两末端或单末端。即,反应性聚硅氧烷化合物根据所导入的官能基的键合位置,可列举例如:所谓侧链型、两末端型、单末端型和侧链两末端型这4种,尤其,在可得到优异的粘合性与剥离性的方面,以单末端型、即单末端反应性聚硅氧烷化合物为较优。推断其理由是因为若使用单末端型进行聚合,则可使聚硅氧烷成分呈梳形接枝于聚合体的主链,由此,无损粘合性,且侧链结晶性聚合物进行结晶化时高效表现出基于聚硅氧烷化合物的脱模性。
单末端反应性聚硅氧烷化合物的具体例可列举例如:下述通式(I)所示的改性聚二甲基硅氧烷化合物。此化合物与上述具有碳数16以上的直链状烷基的(甲基)丙烯酸酯的相容性优异,故可高效得到共聚物。
[式中,R1表示烷基。R2表示基团:CH2=CHCOOR3-或CH2=C(CH3)COOR3-(式中,R3表示亚烷基。)。n表示5~200的整数。]
通式I)中,R1表示的烷基可列举例如:甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、戊基、异戊基、新戊基、己基等碳数1~6的直链或支链的烷基。R3表示的亚烷基可列举例如:亚甲基、亚乙基、三亚甲基、甲基亚乙基、亚丙基、四亚甲基、五亚甲基、六亚甲基等碳数1~6的直链或支链的亚烷基等。
通式(I)所示的改性聚二甲基硅氧烷化合物的具体例可列举例如:下述通式(II)所示的化合物等。
[式中,R1、n与上文相同。]
改性聚二甲基硅氧烷化合物可使用市售品,具体例可列举例如:均为信越化学工业株式会社制的单末端反应性聚硅氧油“X-22-2475”、“X-24-8201”、“X-22-2426”、“KF-2012”等。
另一方面,包含上述的具有碳数16以上的直链状烷基的(甲基)丙烯酸酯与反应性聚硅氧烷化合物的共聚物的本实施方式的侧链结晶性聚合物中,可进一步聚合例如具有碳数1~8的烷基的(甲基)丙烯酸酯、极性单体等。
具有碳数1~8的烷基的(甲基)丙烯酸酯可列举例如:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸己酯等,它们可以使用1种或混合使用2种以上。所例示的这些(甲基)丙烯酸酯之中,以(甲基)丙烯酸甲酯为较优。
极性单体可列举例如:丙烯酸、甲基丙烯酸、巴豆酸、伊康酸、马来酸、富马酸等含有羧基的乙烯不饱和单体;(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸2-羟基己酯等具有羟基的乙烯不饱和单体等,它们可以使用1种或混合使用2种以上。所例示的这些极性单体之中以丙烯酸为较优。
此处,本实施方式中,至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯和反应性聚硅氧烷化合物的比率以重量比计为:至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯∶反应性聚硅氧烷化合物=91∶9~99∶1,优选为95∶5~99∶1,更优选为96∶4~99∶1。如此的比率中价格较高的反应性聚硅氧烷化合物的比例少,因此,若依本实施方式,可降低成本。另外,若采用上述的比率,则可抑制因反应性聚硅氧烷化合物的比率变多使热敏性粘合剂的粘合性与剥离性的均衡性不稳定,并且可得到由聚硅氧烷化合物所产生的脱模性,故即使粘合力设计得较高,剥离时也可充分降低粘合力,结果可发挥优异的粘合性和剥离性。
上述的具有至少碳数16以上的直链状烷基的(甲基)丙烯酸酯,在仅使具有碳数16以上的直链状烷基的(甲基)丙烯酸酯与反应性聚硅氧烷化合物聚合时,意指具有碳数16以上的直链状烷基的(甲基)丙烯酸酯,在进一步聚合上述的具有碳数1~8的烷基的(甲基)丙烯酸酯、极性单体等时,意指进一步含有具有碳数1~8的烷基的(甲基)丙烯酸酯、极性单体等。
进一步聚合具有碳数1~8的烷基的(甲基)丙烯酸酯和极性单体时的比率以重量比计,优选为具有碳数16以上的直链状烷基的(甲基)丙烯酸酯∶具有碳数1~8的烷基的(甲基)丙烯酸酯∶极性单体∶反应性聚硅氧烷化合物=44~46∶39~51∶4~6∶1~9,更优选为44~46∶43~51∶4~6∶1~5,最优选为44~46∶44~51∶4~6∶1~4。
聚合方法是并无特别限定,可采用例如溶液聚合法、本体聚合法、悬浮聚合法、乳液聚合法等。采用溶液聚合法时,将上述的单体混合于溶剂中,以40~90℃左右搅拌2~10小时左右即可。
构成侧链结晶性聚合物的共聚物的重均分子量优选为25万~100万,更优选为50万~70万。重均分子量是将共聚物通过凝胶渗透色谱(GPC)测定所得的测定值以聚苯乙烯换算的值。
本实施方式中,优选80℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度为0.1N/25mm以上,以0.2N/25mm以上更优。由此,即使在高温环境下也可固定构件。80℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度是依据JIS Z0237测定所得到的值。
另外,本实施方式中,优选23℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度为0.1N/25mm,以0.05N/25mm以下为更优。由此,可从构件顺利地剥离。23℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度是在80℃的环境温度下贴合于聚对苯二甲酸乙二酯膜后,使环境温度从80℃冷却至23℃,依据JIS Z0237测定180°剥离强度所得的值。
上述的本实施方式的热敏性粘合剂例如能够以无基材的片状的形态进行使用。使用热敏性粘合剂制成热敏性粘合片时,其厚度以5~100μm为较优,以10~50μm更优。
另外,本实施方式的热敏性粘合剂也能够以带状的形态使用。使用热敏性粘合剂制成热敏性粘合带时,只要使包含热敏性粘合剂的粘合剂层层叠于膜状的基材的单面或双面即可。所谓膜状是指,并非仅限定于膜状,只要无损及本实施方式的效果就也包含膜状乃至片状的概念。
基材的构成材料可列举例如:聚乙烯、聚对苯二甲酸乙二酯、聚丙烯、聚酯、聚酰胺、聚酰亚胺、聚碳酸酯、乙烯乙酸乙烯酯共聚物、乙烯丙烯酸乙酯共聚物、乙烯聚丙烯共聚物、聚氯乙烯等合成树脂。
基材可为单层体或多层体中的任一者,其厚度一般为5~500μm左右。在提高对于粘合剂层的密合性的方面,可对基材施予例如电晕处理、等离子体处理、喷砂处理、化学蚀刻处理、底漆处理等表面处理。
为了在基材的单面或双面设置粘合剂层,只要将在热敏性粘合剂中加入有溶剂的涂布液通过涂布机等涂布于基材的单面或双面并使之干燥即可。涂布机可列举例如:刮刀涂布机、辊涂机、压延涂布机、逗号涂布机、凹版涂布机、棒涂机等。
粘合剂层的厚度以5~60μm为较优,以10~60μm为更优,以10~50μm为最优。单面的粘合剂层的厚度和另一面的粘合剂层的厚度可相同也可相异。
另外,本实施方式中,只要单面的粘合剂层包含热敏性粘合剂,就对另一面的粘合剂层没有特别限定。使另一面的粘合剂层例如由包含热敏性粘合剂的粘合剂层构成时,其组成可与单面的粘合剂层的组成相同,也可相异。
另外,也可使另一面的粘合剂层由例如包含压敏性粘接剂的粘合剂层构成。压敏性粘接剂是具有粘合性的聚合物,可列举例如:天然橡胶粘接剂、合成橡胶粘接剂、苯乙烯/丁二烯乳胶基粘接剂、丙烯酸系粘接剂等。
优选在上述的热敏性粘合片和热敏性粘合带的表面层叠脱模膜。可列举例如在包含聚对苯二甲酸乙二酯等的膜的表面涂布硅酮等脱模剂后作为脱模膜。另外,上述的热敏性粘合剂、热敏性粘合片和热敏性粘合带中可添加例如交联剂、增粘剂、增塑剂、抗老化剂、紫外线吸收剂等各种添加剂。
<陶瓷构件的制造方法/叠层陶瓷电容器的制造方法>
接着,描述本发明的一个实施方式的陶瓷构件的制造方法和叠层陶瓷电容器的制造方法。本实施方式的陶瓷构件的制造方法使用上述的热敏性粘合带,并且具备以下的(i)~(iv)的工序。本实施方式的叠层陶瓷电容器的制造方法进一步具备以下的(v)的工序。
(i)将热敏性粘合带贴合于陶瓷生坯片层叠体。
(ii)经由热敏性粘合带将陶瓷生坯片层叠体固定于基座上。
(iii)切断陶瓷生坯片层叠体而形成多个生坯切片。
(iv)使热敏性粘合带为低于侧链结晶性聚合物的熔点的温度而使粘合剂层的粘合力降低,从热敏性粘合带取出上述多个生坯切片。
(v)对所得的生坯切片进行烧制而得到陶瓷切片,在陶瓷切片的端面形成外部电极而得到叠层陶瓷电容器。
上述的(i)至(v)的工序中,(i)和(ii)的工序是所谓的层叠工序,(iii)的工序是所谓的裁切工序,(iv)的工序是所谓的分离工序。若依本实施方式,因使用发挥优异的粘合性和剥离性的上述热敏性粘合带,故可切实地进行(i)至(v)的工序,结果,可高良品率地得到陶瓷构件和叠层陶瓷电容器。
另外,(i)的工序中的陶瓷生坯片层叠体可如下得到:用刮刀使陶瓷粉末的浆液薄薄地扩展而形成陶瓷生坯片,在此陶瓷生坯片的表面印刷多个电极后,使多个陶瓷生坯片层叠成一体而得到。
(ii)的工序中在基座上的固定方法无特别限定,可列举例如:在热敏性粘合带的基材和基座之间夹着特定的粘合剂或粘接剂而进行固定的方法;采用具备吸附机构等固定单元的基座的方法等。另外,热敏性粘合带的构成为在基材膜的双面设有粘合剂层的双面带时,也可经由与贴合陶瓷生坯片层叠体的单面粘合剂层相反的另一面的粘合剂层而固定于基座上。
(iii)的工序中的切断可为利用切割刀的冲切,也可为利用旋转刀的切断。
除了上述叠层陶瓷电容器以外,本实施方式的陶瓷构件的制造方法还可适用于例如陶瓷电感器、陶瓷变阻器等其它陶瓷构件。
以下,举出合成例和实施例详细说明本发明,但本发明并非仅限定于以下的合成例和实施例。另外,以下的说明中“份”意指重量份。
(合成例1)
依日油公司制的丙烯酸二十二烷基酯45份、日本触媒公司制的丙烯酸甲酯49份、丙烯酸5份、改性聚二甲基硅氧烷化合物1份、和作为聚合引发剂的日油公司制的“PerbutylND”0.2份的比率分别加入乙酸乙酯230份中并混合,以55℃搅拌4小时,使这些单体聚合。所得的共聚物的重均分子量为58万,熔点为56℃。另外,所使用的改性聚二甲基硅氧烷化合物如下述。
改性聚二甲基硅氧烷化合物:上述的通式(II)所示的信越化学工业株式会社制的单末端反应性聚硅氧油“KF-2012”
(合成例2)
除使丙烯酸二十二烷基酯为45份、丙烯酸甲酯为46份、丙烯酸为5份、改性聚二甲基硅氧烷化合物为4份以外,其余与合成例1同样地进行,使这些单体聚合。所得的共聚物的重均分子量为63万、熔点为55℃。
(合成例3)
除使丙烯酸二十二烷基酯为45份、丙烯酸甲酯为45份、丙烯酸为5份、改性聚二甲基硅氧烷化合物为5份以外,其余与合成例1同样地进行,使这些单体聚合。所得的共聚物的重均分子量为60万、熔点为55℃。
(合成例4)
除使丙烯酸二十二烷基酯为45份、丙烯酸甲酯为41份、丙烯酸为5份、改性聚二甲基硅氧烷化合物为9份以外,其余与合成例1同样地进行,使这些单体聚合。所得的共聚物的重均分子量为64万、熔点为56℃。
(比较合成例1)
除使丙烯酸二十二烷基酯为45份、丙烯酸甲酯为50份、丙烯酸为5份,且不添加改性聚二甲基硅氧烷化合物以外,其余与合成例1同样地进行,使这些单体聚合。所得的共聚物的重均分子量为62万、熔点为56℃。
(比较合成例2)
除使丙烯酸二十二烷基酯为45份、丙烯酸甲酯为40份、丙烯酸为5份,改性聚二甲基硅氧烷化合物为10份以外,其余与合成例1同样地进行,使这些单体聚合。所得的共聚物的重均分子量为66万、熔点为56℃。
将合成例1~4和比较合成例1~2的共聚物表示于表1。另外,重均分子量如下得到:用GPC对共聚物进行测定,对所得的测定值进行聚苯乙烯换算,由此得到。熔点是用DSC以10℃/分钟的测定条件对共聚物进行测定而得到的。
[表1]
1)C22A:丙烯酸二十二烷基酯、C1A:丙烯酸甲酯、AA:丙烯酸
KF-2012:改性聚二甲基硅氧烷化合物
[实施例1~4和比较例1~2]
<热敏性粘合带的制作>
首先,将合成例1~4和比较合成例1~2中得到的各共聚物利用乙酸乙酯调整至固体成分为30重量%,得到涂布液。其次,将涂布液涂布于厚度100μm的由聚对苯二甲酸乙二酯构成的膜状的基材的单面并干燥,得到形成有厚度10μm的粘合剂层的热敏性粘合带。
<评价>
对于所得的热敏性粘合带,评价180°剥离强度。将评价方法表示如下,并且其结果表示于表2。
(180°剥离强度)
对于所得的热敏性粘合带,依据JIS Z0237对80℃和23℃的各环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度进行测定。具体而言,在以下的条件下将热敏性粘合带贴合于聚对苯二甲酸乙二酯膜后,使用负载器(load cell)以300mm/分钟的速度进行180°剥离。
[80℃]
在80℃的环境温度下将热敏性粘合带贴合于聚对苯二甲酸乙二酯膜并静置20分钟后,进行180°剥离。
[23℃]
在80℃的环境温度下将热敏性粘合带贴合于聚对苯二甲酸乙二酯膜,在此环境温度下静置20分钟后,将环境温度降至23℃,在此环境温度下静置20分钟后,进行180°剥离。
另外,聚对苯二甲酸乙二酯膜使用厚度25μm的未经处理的聚对苯二甲酸乙二酯膜。另外,热敏性粘合带对聚对苯二甲酸乙二酯膜的贴合通过使2kg的滚筒在热敏性粘合带上往返5次来进行。
[表2]
从表2明显可知,实施例1~4中,在80℃和23℃的各环境温度下的180°剥离强度显示良好的结果。
Claims (14)
1.一种热敏性粘合剂,其只含有侧链结晶性聚合物或由侧链结晶性聚合物与添加剂组成,其在低于所述侧链结晶性聚合物的熔点的温度下粘合力降低,
所述侧链结晶性聚合物通过使至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯聚合所得,
所述侧链结晶性聚合物包含通过进一步聚合反应性聚硅氧烷化合物所得的共聚物,
所述至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯和所述反应性聚硅氧烷化合物的比率以重量比计为至少具有碳数16以上的直链状烷基的(甲基)丙烯酸酯:反应性聚硅氧烷化合物=96:4~99:1,
所述添加剂选自交联剂、增粘剂、增塑剂、抗老化剂、紫外线吸收剂中的至少一种,
80℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度为0.2N/25mm以上,
23℃的环境温度下对于聚对苯二甲酸乙二酯膜的180°剥离强度为0.05N/25mm以下。
2.如权利要求1所述的热敏性粘合剂,其中,所述侧链结晶性聚合物包含通过进一步聚合具有碳数1~8的烷基的(甲基)丙烯酸酯和极性单体所得的共聚物,
所述具有碳数16以上的直链状烷基的(甲基)丙烯酸酯、所述具有碳数1~8的烷基的(甲基)丙烯酸酯、所述极性单体和所述反应性聚硅氧烷化合物的比率以重量比计为:具有碳数16以上的直链状烷基的(甲基)丙烯酸酯:具有碳数1~8的烷基的(甲基)丙烯酸酯:极性单体:反应性聚硅氧烷化合物=44~46:44~51:4~6:1~4。
3.如权利要求1或2所述的热敏性粘合剂,其中,所述熔点为50~60℃。
4.如权利要求1或2所述的热敏性粘合剂,其中,所述共聚物的重均分子量为50万~70万。
5.如权利要求1或2所述的热敏性粘合剂,其中,所述反应性聚硅氧烷化合物为下述通式(I)所示的改性聚二甲基硅氧烷化合物,
式中,R1表示烷基,R2表示基团:CH2=CHCOOR3-或CH2=C(CH3)COOR3-,式中R3表示亚烷基,n表示5~200的整数。
6.如权利要求1或2所述的热敏性粘合剂,其中,所述反应性聚硅氧烷化合物为下述通式(II)所示的改性聚二甲基硅氧烷化合物,
式中,R1表示烷基,n表示5~200的整数。
7.如权利要求1或2所述的热敏性粘合剂,其中,所述具有碳数16以上的直链状烷基的(甲基)丙烯酸酯为(甲基)丙烯酸二十二烷基酯。
8.如权利要求2所述的热敏性粘合剂,其中,所述具有碳数1~8的烷基的(甲基)丙烯酸酯为(甲基)丙烯酸甲酯,
所述极性单体为丙烯酸。
9.如权利要求1或2所述的热敏性粘合剂,其用于制造陶瓷构件。
10.如权利要求9所述的热敏性粘合剂,所述陶瓷构件为叠层陶瓷电容器。
11.一种热敏性粘合片,其包含权利要求1~10中任一项所述的热敏性粘合剂。
12.一种热敏性粘合带,其是使包含权利要求1~10中任一项所述的热敏性粘合剂的粘合剂层层叠于膜状的基材单面或双面而成的。
13.一种陶瓷构件的制造方法,其具备如下工序:
将权利要求12所述的热敏性粘合带贴合于陶瓷生坯片层叠体的工序;
利用所述热敏性粘合带将所述陶瓷生坯片层叠体固定于基座上的工序;
切断所述陶瓷生坯片层叠体而形成多个生坯切片的工序;
使所述热敏性粘合带为低于所述侧链结晶性聚合物的熔点的温度而使所述粘合剂层的粘合力降低,从所述热敏性粘合带取出所述多个生坯切片的工序。
14.一种叠层陶瓷电容器的制造方法,其是如下得到的叠层陶瓷电容器:
对由权利要求13所述的陶瓷构件的制造方法得到的生坯切片进行烧制而得到陶瓷切片,在所述陶瓷切片的端面形成外部电极而得到叠层陶瓷电容器。
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KR102428192B1 (ko) * | 2019-07-03 | 2022-08-02 | 주식회사 엘지화학 | 점착 필름, 이의 제조 방법 및 이를 포함하는 플라스틱 유기 발광 디스플레이 |
CN110655883B (zh) * | 2019-09-24 | 2021-07-13 | 南京清尚新材料科技有限公司 | 一种冷关型粘合剂及其制备方法和一种粘合带的制备方法 |
KR102409532B1 (ko) * | 2019-10-22 | 2022-06-15 | 주식회사 엘지화학 | 점착제 조성물, 이를 포함하는 점착 필름, 점착 필름을 포함하는 백플레이트 필름 및 점착 필름을 포함하는 플라스틱 유기 발광 디스플레이 |
KR102481004B1 (ko) * | 2021-02-22 | 2022-12-23 | 주식회사 켐코 | 내한성 및 내열성이 우수한 점착제 조성물 및 이를 이용한 점착테이프 |
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