CN117715999A - 粘接剂、层叠体、层叠体的制造方法、包装材料 - Google Patents
粘接剂、层叠体、层叠体的制造方法、包装材料 Download PDFInfo
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- CN117715999A CN117715999A CN202280052121.3A CN202280052121A CN117715999A CN 117715999 A CN117715999 A CN 117715999A CN 202280052121 A CN202280052121 A CN 202280052121A CN 117715999 A CN117715999 A CN 117715999A
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- polyol
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- 238000004448 titration Methods 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
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- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 description 1
- 239000001069 triethyl citrate Substances 0.000 description 1
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
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- CAPOZRICGSDRLP-UHFFFAOYSA-N tris(2,3-dimethylphenyl) phosphate Chemical compound CC1=CC=CC(OP(=O)(OC=2C(=C(C)C=CC=2)C)OC=2C(=C(C)C=CC=2)C)=C1C CAPOZRICGSDRLP-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- HQUQLFOMPYWACS-UHFFFAOYSA-N tris(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCCl HQUQLFOMPYWACS-UHFFFAOYSA-N 0.000 description 1
- LIPMRGQQBZJCTM-UHFFFAOYSA-N tris(2-propan-2-ylphenyl) phosphate Chemical compound CC(C)C1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C(C)C)OC1=CC=CC=C1C(C)C LIPMRGQQBZJCTM-UHFFFAOYSA-N 0.000 description 1
- WDRCVXGINNJWPH-UHFFFAOYSA-N tris(6-methylheptyl) benzene-1,2,4-tricarboxylate Chemical compound CC(C)CCCCCOC(=O)C1=CC=C(C(=O)OCCCCCC(C)C)C(C(=O)OCCCCCC(C)C)=C1 WDRCVXGINNJWPH-UHFFFAOYSA-N 0.000 description 1
- YPDXSCXISVYHOB-UHFFFAOYSA-N tris(7-methyloctyl) benzene-1,2,4-tricarboxylate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCC(C)C)C(C(=O)OCCCCCCC(C)C)=C1 YPDXSCXISVYHOB-UHFFFAOYSA-N 0.000 description 1
- FJFYFBRNDHRTHL-UHFFFAOYSA-N tris(8-methylnonyl) benzene-1,2,4-tricarboxylate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC(C)C)C(C(=O)OCCCCCCCC(C)C)=C1 FJFYFBRNDHRTHL-UHFFFAOYSA-N 0.000 description 1
- SMYKBXMWXCZOLU-UHFFFAOYSA-N tris-decyl benzene-1,2,4-tricarboxylate Chemical compound CCCCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCCCC)C(C(=O)OCCCCCCCCCC)=C1 SMYKBXMWXCZOLU-UHFFFAOYSA-N 0.000 description 1
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- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- VNTDZUDTQCZFKN-UHFFFAOYSA-L zinc 2,2-dimethyloctanoate Chemical compound [Zn++].CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O VNTDZUDTQCZFKN-UHFFFAOYSA-L 0.000 description 1
- LFOXXKXKYHIANI-UHFFFAOYSA-L zinc;7,7-dimethyloctanoate Chemical class [Zn+2].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O LFOXXKXKYHIANI-UHFFFAOYSA-L 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
本发明提供与金属箔、金属蒸镀层的密合性优异的2液固化型粘接剂、使用该粘接剂而得到的层叠体、包装材料。一种粘接剂,其包含多异氰酸酯组合物(X)和多元醇组合物(Y),多异氰酸酯组合物(X)包含多异氰酸酯化合物(A),多元醇组合物(Y)包含多元醇(B)和化合物(C),上述化合物(C)为选自二羟甲基丙酸、二羟甲基丁酸中的至少一种。
Description
技术领域
本发明涉及粘接剂、使用该粘接剂而得到的层叠体、层叠体的制造方法、包装材料。
背景技术
各种包装材料、标签等中使用的层叠体通过各种多种多样的塑料膜、金属箔、纸等基材的层压而被赋予设计性、功能性、保存性、便利性、耐输送性等。将该层叠体成形为袋状而成的包装材料被用作食品、医药品、洗剂等的包装材料。
以往,对于包装材料中使用的层叠体而言,主流是通过将溶解于挥发性有机溶剂中的粘接剂(有时称为溶剂型层压粘接剂)涂敷于基材、在通过烘箱的过程中使有机溶剂挥发、并贴合其他基材的干式层压方式而得到的层叠体,但近年来,从降低环境负荷和改善作业环境的观点出发,不含有挥发性有机溶剂的反应型2液型的层压粘接剂(以下称为无溶剂型粘接剂)的需求也不断提高(专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开2014-159548号公报
发明内容
发明要解决的课题
无溶剂型粘接剂具有无干燥工序且无溶剂的排出、节能且运行成本低、在将塑料膜彼此贴合后的层叠体、将塑料膜与金属箔、金属蒸镀层贴合后的层叠体中没有溶剂残留的担心等许多优点。另一方面,无溶剂型粘接剂中使用的成分为了达到在加热至40℃~100℃左右时能够涂敷的粘度而需要将分子量设计得低,与金属箔、金属蒸镀层的密合性不充分。
本发明是鉴于这样的情况而完成的,其目的在于提供即使在分子量低的情况下与金属箔、金属蒸镀层的密合性也优异的2液固化型粘接剂、使用该粘接剂而得到的层叠体、包装材料。
用于解决课题的手段
本发明涉及以下的2液固化型粘接剂,其特征在于,包含多异氰酸酯组合物(X)和多元醇组合物(Y),多异氰酸酯组合物(X)包含多异氰酸酯化合物(A),多元醇组合物(Y)包含多元醇(B)和化合物(C),所述化合物(C)为选自二羟甲基丙酸、二羟甲基丁酸中的至少一种。
发明效果
根据本发明,能够提供即使在分子量低的情况下与金属箔、金属蒸镀层的密合性也优异的2液固化型粘接剂。
具体实施方式
<<粘接剂>>
本发明的粘接剂为包含多异氰酸酯组合物(X)和多元醇组合物(Y)的2液固化型。以下,对本发明的粘接剂进行详细说明。
<多异氰酸酯组合物(X)>
(多异氰酸酯化合物(A))
多异氰酸酯组合物(X)包含具有多个异氰酸酯基的多异氰酸酯化合物(A)。作为多异氰酸酯化合物(A),没有特别限定,可举出芳香族二异氰酸酯、芳香脂肪族二异氰酸酯、脂肪族二异氰酸酯、脂环族二异氰酸酯、以及这些二异氰酸酯的缩二脲体、脲酸酯体、加合物、脲基甲酸酯体、碳二亚胺改性体、脲二酮改性体、使这些多异氰酸酯与多元醇进行反应而得的氨基甲酸酯预聚物等,它们可以单独使用或组合多种而使用。
作为芳香族二异氰酸酯,例如可举出2,2’-二苯基甲烷二异氰酸酯、2,4’-二苯基甲烷二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、多亚甲基多苯基多异氰酸酯(也称为聚合MDI或粗MDI)、1,3-苯二异氰酸酯、4,4’-二苯基二异氰酸酯、1,4-苯二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4’-甲苯胺二异氰酸酯、2,4,6-三异氰酸酯甲苯、1,3,5-三异氰酸酯苯、邻联茴香胺二异氰酸酯、4,4’-二苯基醚二异氰酸酯、4,4’,4”-三苯基甲烷三异氰酸酯等,但不限定于这些。
芳香脂肪族二异氰酸酯是指在分子中具有1个以上芳香环的脂肪族异氰酸酯,可举出间或对苯二亚甲基二异氰酸酯(别名:XDI)、α,α,α’,α’-四甲基苯二亚甲基二异氰酸酯(别名:TMXDI)等,但不限定于这些。
作为脂肪族二异氰酸酯,可举出三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯(别名:HDI)、五亚甲基二异氰酸酯、1,2-亚丙基二异氰酸酯、2,3-亚丁基二异氰酸酯、1,3-亚丁基二异氰酸酯、十二亚甲基二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯等,但不限定于这些。
作为脂环族二异氰酸酯,可举出3-异氰酸酯甲基-3,5,5-三甲基环己基异氰酸酯、异佛尔酮二异氰酸酯(别名:IPDI)、1,3-环戊烷二异氰酸酯、1,3-环己烷二异氰酸酯、1,4-环己烷二异氰酸酯、甲基-2,4-环己烷二异氰酸酯、甲基-2,6-环己烷二异氰酸酯、4,4’-亚甲基双(环己基异氰酸酯)、1,4-双(异氰酸酯甲基)环己烷等,但不限定于这些。
关于氨基甲酸酯预聚物的合成中使用的多元醇,例如可举出乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、3-甲基-1,5-戊二醇、1,6-己二醇、新戊二醇、甲基戊二醇、二甲基丁二醇、丁基乙基丙二醇、1,4-环己二醇、1,4-环己烷二甲醇等亚烷基二醇;
双酚A、双酚F、氢化双酚A、氢化双酚F等双酚;
二聚体二醇;
双羟基乙氧基苯;
二乙二醇、三乙二醇、其他聚乙二醇、聚丙二醇、聚丁二醇等聚亚烷基二醇;
将聚亚烷基二醇进一步用芳香族或脂肪族多异氰酸酯进行高分子量化而得的含氨基甲酸酯键的聚醚多元醇;
使上述亚烷基二醇或聚亚烷基二醇与草酸、丙二酸、琥珀酸、戊二酸、己二酸、富马酸、马来酸、辛二酸、壬二酸、癸二酸、十一烷二酸、十二烷二酸、十三烷二酸等碳原子数为2~13的范围的脂肪族二羧酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、偏苯三酸、均苯四酸等芳香族多元羧酸中的至少一种进行反应而得到的聚酯多元醇;
作为通过丙内酯、丁内酯、ε-己内酯、σ-戊内酯、β-甲基-σ-戊内酯等环状酯化合物的开环聚合反应而得到的聚酯与二醇、甘油、三羟甲基丙烷、季戊四醇等多价醇的反应物的聚酯多元醇等。
从成为即使在40℃左右的较低温度的加热下涂敷性也优异的粘接剂的方面出发,作为多异氰酸酯化合物(A),优选包含氨基甲酸酯预聚物(A1),该氨基甲酸酯预聚物(A1)是至少包含4,4’-二苯基甲烷二异氰酸酯的多异氰酸酯(a1-1)与多元醇(a1-2)的反应产物。
(氨基甲酸酯预聚物(A1))
多异氰酸酯(a1-1)包含4,4’-二苯基甲烷二异氰酸酯,但也可以包含其他多异氰酸酯化合物。作为能够与4,4’-二苯基甲烷二异氰酸酯并用的多异氰酸酯化合物,没有特别限制,可以使用作为多异氰酸酯化合物(A)而例示的物质中的一种或将它们中的两种以上组合使用。4,4’-二苯基甲烷二异氰酸酯在多异氰酸酯(a1-1)中所占的配合量优选为40~99质量%,优选为75~90质量%。
作为多元醇(a1-2),可以使用与多异氰酸酯化合物(A)的说明中例示的多元醇相同的物质。优选使用聚亚烷基二醇和聚酯多元醇中的至少一种。聚亚烷基二醇、聚酯多元醇的数均分子量优选为200~6,000。需要说明的是,在本申请中,重均分子量(Mw)、数均分子量(Mn)是利用下述条件的凝胶渗透色谱(GPC)而测定的值。
测定装置:东曹株式会社制HLC-8320GPC
柱:东曹株式会社制TSKgel 4000HXL、TSKgel 3000HXL、TSKgel 2000HXL、TSKgel1000HXL
检测器:RI(差示折射计)
数据处理:东曹株式会社制MultiStation GPC-8020modelII
测定条件:柱温 40℃
溶剂 四氢呋喃
流速 0.35ml/分钟
标准:单分散聚苯乙烯
试样:将以树脂固体成分换算计为0.2质量%的四氢呋喃溶液用微型过滤器过滤而得的物质(100μl)
氨基甲酸酯预聚物(A1)优选是在多异氰酸酯(a1-1)所具有的异氰酸酯基与多元醇(a1-2)所具有的羟基的当量比[NCO]/[OH]为1.5~5.0的范围内进行反应而得到的。另外,氨基甲酸酯预聚物(A1)的基于滴定法(使用二正丁胺)的异氰酸酯含有率优选为5~20质量%。由此,能够制成涂敷适应性优异的粘接剂。
(其他异氰酸酯化合物(A2))
多异氰酸酯组合物(X)可以包含氨基甲酸酯预聚物(A1)以外的异氰酸酯化合物(A2)。作为异氰酸酯化合物(A2),可以适当使用作为多异氰酸酯化合物(A)而例示的物质。优选碳二亚胺改性二异氰酸酯、多亚甲基多苯基多异氰酸酯(也称为聚合MDI或粗MDI)。
在多异氰酸酯组合物(X)包含异氰酸酯化合物(A2)的情况下,关于其配合比例,与氨基甲酸酯预聚物(A1)的质量比、氨基甲酸酯预聚物(A1)/异氰酸酯化合物(A2)优选为50/50~99/1,更优选为70/30~97/3。
<多元醇组合物(Y)>
(多元醇(B))
作为本发明中使用的多元醇(B),没有特别限定,可举出乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、3-甲基-1,5-戊二醇、1,6-己二醇、新戊二醇、甲基戊二醇、二甲基丁二醇、丁基乙基丙二醇、二乙二醇、三乙二醇、四乙二醇、二丙二醇、三丙二醇、双羟基乙氧基苯、1,4-环己二醇、1,4-环己烷二甲醇、三乙二醇等二醇;
甘油、三羟甲基丙烷、季戊四醇、聚丙二醇的三醇体等3官能或4官能的脂肪族醇;
双酚A、双酚F、氢化双酚A、氢化双酚F等双酚;
二聚体二醇;
在上述二醇、3官能或4官能的脂肪族醇等聚合引发剂的存在下将环氧乙烷、环氧丙烷、环氧丁烷、氧化苯乙烯、表氯醇、四氢呋喃、环己烯等环氧烷进行加成聚合而得的聚醚多元醇;
作为通过丙内酯、丁内酯、ε-己内酯、σ-戊内酯、β-甲基-σ-戊内酯等环状酯化合物的开环聚合反应而得到的聚酯与上述二醇、甘油、三羟甲基丙烷、季戊四醇等多价醇的反应物的聚酯多元醇(1);
使上述二醇、二聚体二醇或上述双酚等2官能型多元醇与多元羧酸进行反应而得到的聚酯多元醇(2);
使上述3官能或4官能的脂肪族醇与多元羧酸进行反应而得到的聚酯多元醇(3);
使上述二醇、二聚体二醇或上述双酚等2官能型多元醇、上述3官能或4官能的脂肪族醇、以及多元羧酸进行反应而得到的聚酯多元醇(4);
作为二羟甲基丙酸、蓖麻油脂肪酸等羟基酸的聚合物的聚酯多元醇(5);
使上述聚醚多元醇与多元羧酸进行反应而得到的聚醚聚酯多元醇;
使上述聚醚多元醇、选自上述二醇、二聚体二醇、双酚等2官能型多元醇、3官能或4官能的脂肪族醇中的至少一种、以及多元羧酸进行反应而得到的聚醚聚酯多元醇;
蓖麻油、脱水蓖麻油、作为蓖麻油的氢化物的氢化蓖麻油、蓖麻油的环氧烷5~50摩尔加成物等植物油多元醇;
作为上述多元醇中的至少一种与多异氰酸酯化合物的反应产物的聚氨酯多元醇、聚醚聚氨酯多元醇、聚酯聚氨酯多元醇、聚醚聚酯多元醇等,可以使用1种或组合使用2种以上。
在此,作为多元羧酸,可举出琥珀酸、己二酸、壬二酸、癸二酸、十二烷二甲酸、马来酸酐、富马酸、1,3-环戊烷二甲酸、1,4-环己烷二甲酸等脂肪族二羧酸;邻苯二甲酸、间苯二甲酸、对苯二甲酸、1,4-萘二甲酸、2,5-萘二甲酸、2,6-萘二甲酸、萘二甲酸、联苯二甲酸、1,2-双(苯氧基)乙烷-p,p’-二甲酸等芳香族二羧酸;以及这些脂肪族或二羧酸的酸酐或酯形成性衍生物;对羟基苯甲酸、对(2-羟基乙氧基)苯甲酸和这些二羟基羧酸的酯形成性衍生物、二聚酸等多元酸类。
作为多异氰酸酯化合物,可以使用与作为多异氰酸酯化合物(A)而例示的多异氰酸酯化合物相同的物质。
(聚醚醇(B1)、植物油多元醇(B2))
从成为即使在40℃左右的较低温度的加热下涂敷性也优异的粘接剂的方面出发,多元醇(B)优选包含聚醚多元醇(B1)或植物油多元醇(B2)中的至少一种。从涂敷适应性的观点出发,多元醇(B)中的聚醚多元醇(B1)或植物油多元醇(B2)的配合量优选为20质量%以上,更优选为30质量%。也可以为100质量%,更优选为80质量%以下。
从层压强度的观点出发,多元醇(B)优选包含数均分子量为130以上且3000以下的聚醚二醇(B1-1)。通过使用聚醚二醇(B1-1),能够使粘接层具有适度的柔软性,层压强度变得良好。在多元醇(B)包含聚醚多元醇(B1-1)的情况下,在多元醇(B)中的配合量优选为10质量%以上且50质量%以下。
从热封强度的观点出发,优选包含3官能以上的聚醚多元醇(B1-2)。由此,在粘接剂的固化涂膜中导入交联结构,热封强度提高。聚醚多元醇(B1-2)的数均分子量可以适当调整,作为一例,为450以上且1000以下。在多元醇(B)包含聚醚多元醇(B1-2)的情况下,在多元醇(B)中的配合量优选为10质量%以上且30质量%以下。
(聚酯多元醇(B3))
在本发明中,多元醇(B)优选包含聚酯多元醇(B3)。由此,能够提高与尼龙膜等硬质膜的粘接性。
作为聚酯多元醇(B3),可以适当使用上述例示的聚酯多元醇,但从能够成为即使在40℃左右的较低温度的加热下涂敷性也优异的粘接剂、并且与聚醚多元醇(B 1)、植物油多元醇(B2)的相容性优异的方面出发,优选使用包含脂肪族多元醇和脂肪多元羧酸的组合物的反应产物。聚酯多元醇(B3)的合成中使用的多元醇中,脂肪族多元醇的配合量优选为80质量%以上,优选为90质量%以上,优选为95质量%以上。全部量可以为脂肪族多元醇。聚酯多元醇(B3)的合成中使用的多元羧酸中,脂肪族多元羧酸的配合量优选为80质量%以上,优选为90质量%以上,优选为95质量%以上。多元羧酸的全部量可以为脂肪族多元羧酸。
从与硬质膜的密合性和密封强度的平衡的观点出发,多元醇(B)中的聚酯多元醇(B3)的配合量优选为5质量%以上且50质量%以下,更优选为20质量%以上且30质量%以下。
(化合物(C))
本发明中使用的化合物(C)为选自2,2-二羟甲基乙酸、2,2-二羟甲基丙酸、2,2-二羟甲基丁酸、2,2-二羟甲基戊酸中的至少一种,优选包含2,2-二羟甲基丙酸、2,2-二羟甲基丁酸中的至少一种,更优选包含2,2-二羟甲基丙酸。通过多元醇组合物(Y)包含化合物(C),由此能够制成对金属基材的密合性、适用期优异的粘接剂。
从与金属箔、金属蒸镀层的密合性的观点出发,化合物(C)在多元醇组合物(Y)中所占的配合量优选为0.1质量%以上,更优选为0.5质量%以上。如果粘接层的柔软性降低,则容易引起与基材的界面附近处的表层剥离,在应用于柔软的基材时存在粘接性降低的倾向,因此,化合物(C)在多元醇组合物(Y)中所占的配合量优选为10质量%以下,更优选为2.5质量%以下。
(多胺(D))
多元醇组合物(Y)优选包含具有多个氨基的多胺(D)。在本说明书中,氨基是指NH2基或NHR基(R为可以具有官能团的烷基或芳基)。通过多元醇组合物包含多胺(D),另外在贴合阻隔性的基材的情况下也能够得到外观良好的层叠体。
向基材涂敷时卷入到粘接剂中的微细的气泡如果保持原样,则人的眼睛看不到,因此不会成为外观不良,但在熟化工序中逐渐凝聚而成为可看到的尺寸的情况下成为外观不良。另外,在粘接层中存在能够看到的尺寸的气泡的情况下,基材与粘接层的接触面积减少与气泡对应的量,粘接强度有可能会降低。通过多元醇组合物(Y)包含多胺(D),多异氰酸酯组合物(X)与多元醇组合物(Y)的反应迅速进行,因而气泡的凝聚受到妨碍,因此认为能够抑制层压强度的降低、层叠体中的气泡所引起的外观不良的发生。
作为多胺(D),可以没有特别限制地使用公知的多胺,可举出甲二胺、乙二胺、异佛尔酮二胺、3,9-二丙胺-2,4,8,10-四氧杂螺十一烷、赖氨酸、苯二胺、2,2,4-三甲基六亚甲基二胺、甲苯二胺、肼、哌嗪、六亚甲基二胺、丙二胺、二环己基甲烷-4,4-二胺、2-羟基乙基乙二胺、二-2-羟基乙基乙二胺、二-2-羟基乙基丙二胺、2-羟基丙基乙二胺或二-2-羟基丙基乙二胺、聚(丙二醇)二胺、聚(丙二醇)三胺、聚(丙二醇)四胺、1,2-二氨基丙烷、1,3-二氨基丙烷、
1,4-二氨基丁烷、1,5-二氨基戊烷、1,6-二氨基己烷、1,7-二氨基庚烷、1,8-二氨基辛烷、1,9-二氨基壬烷、1,10-二氨基癸烷等、苄胺、二亚乙基三胺、二亚丙基三胺、三亚乙基四胺、三亚丙基四胺、四亚乙基五胺、四亚丙基五胺、五亚乙基六胺、九亚乙基十胺、三甲基六亚甲基二胺等、四(氨基甲基)甲烷、四(2-氨基乙基氨基甲基)甲烷、1,3-双(2’-氨基乙基氨基)丙烷、三亚乙基-双(三亚甲基)六胺、双(3-氨基乙基)胺、双六亚甲基三胺等、1,4-环己二胺、4,4’-亚甲基双环己胺、4,4’-异亚丙基双环己胺、降冰片烷二胺、
双(氨基甲基)环己烷、二氨基二环己基甲烷、异佛尔酮二胺、薄荷烯二胺(日文原文:メンセンジアミン)等、双(氨基烷基)苯、双(氨基烷基)萘、双(氰基乙基)二亚乙基三胺、邻苯二甲胺、间苯二甲胺、对苯二甲胺、苯二胺、萘二胺、二氨基二苯基甲烷、二氨基二乙基苯基甲烷、2,2-双(4-氨基苯基)丙烷、4,4’-二氨基二苯基醚、4,4’-二氨基二苯甲酮、4,4’-二氨基二苯基醚、4,4’-二氨基二苯基砜、2,2’-二甲基-4,4’-二氨基二苯基甲烷、2,4’-二氨基联苯、2,3’-二甲基-4,4’-二氨基联苯、3,3’-二甲氧基-4,4’-二氨基联苯、双(氨基甲基)萘、双(氨基乙基)萘等、N-甲基哌嗪、吗啉、1,4-双-(8-氨基丙基)-哌嗪、哌嗪-1,4-二氮杂环庚烷、1-(2’-氨基乙基哌嗪)、1-[2’-(2”-氨基乙基氨基)乙基]哌嗪、三环癸烷二胺、作为上述各种多胺与上述各种异氰酸酯成分的反应产物的聚脲胺等具有多个氨基的胺化合物(D1)、
单乙醇胺、单异丙醇胺、单丁醇胺、N-甲基乙醇胺、N-乙基乙醇胺、N-甲基丙醇胺、二乙醇胺、二异丙醇胺等伯烷醇胺或仲烷醇胺(D2)、
乙胺、辛胺、月桂胺、肉豆蔻胺、硬脂胺、油胺、二乙胺、二丁胺、二硬脂胺等伯胺或仲胺(D3)等。
从对金属基材的密合性、层叠体的外观、适用期的平衡的观点出发,关于多胺(D)的配合量,优选以多元醇组合物(Y)的胺值成为20~70mgKOH/g、更优选成为25~50mgKOH/g的方式进行配合。
需要说明的是,本说明书中的胺值是指相对于中和试样1g所需的HCl量而成为当量的KOH的毫克数,没有特别限制,可以使用公知的方法算出。在已知胺化合物(C)的化学结构、进而根据需要的平均分子量等的情况下,可以根据(每1分子的氨基的数量/平均分子量)×56.1×1000来算出。在胺化合物的化学结构、平均分子量等不明确的情况下,可以按照公知的胺值测定方法、例如JISK7237-1995进行测定。
(氨基甲酸酯化催化剂(E))
本发明的粘接剂可以根据需要而通过使用催化剂来促进固化反应。作为催化剂,只要促进多异氰酸酯组合物(X)与多元醇组合物(Y)的氨基甲酸酯化反应就没有特别限制,例示有金属系催化剂(E1)、脂肪族环状酰胺化合物(E2)等。
作为金属系催化剂(E1),可举出金属络合物系、无机金属系、有机金属系的催化剂。作为金属络合物系的催化剂,例示有选自Fe(铁)、Mn(锰)、Cu(铜)、Zr(锆)、Th(钍)、Ti(钛)、Al(铝)、Co(钴)中的金属的乙酰丙酮盐、例如乙酰丙酮铁、乙酰丙酮锰、乙酰丙酮铜、乙酰丙酮氧化锆等。从毒性和催化活性的方面出发,优选乙酰丙酮铁(Fe(acac)3)或乙酰丙酮锰(Mn(acac)2)。
作为无机金属系的催化剂,可举出选自Sn、Fe、Mn、Cu、Zr、Th、Ti、Al、Co等中的物质。
作为有机金属系催化剂,可举出辛酸锌、新癸酸锌、环烷酸锌等有机锌化合物、二乙酸亚锡、二辛酸亚锡、二油酸亚锡、二月桂酸亚锡、二乙酸二丁基锡、二月桂酸二丁基锡、二月桂酸二辛基锡、二丁基氧化锡、二丁基二氯化锡等有机锡化合物、辛酸镍、环烷酸镍等有机镍化合物、辛酸钴、环烷酸钴等有机钴化合物、辛酸铋、新癸酸铋、环烷酸铋等有机铋化合物、四异丙基氧钛酸酯(日文原文:テトライソプロピルオキシチタネート)、二丁基二氯化钛、钛酸四丁酯、丁氧基三氯化钛、将脂肪族二酮、芳香族二酮、碳原子数2~10的醇中的至少1种作为配体的钛螯合物等钛系化合物等。
脂肪族环状酰胺化合物(E2)例如可举出δ-戊内酰胺、ε-己内酰胺、ω-庚内酰胺、η-辛内酰胺、β-丙内酰胺等。这些之中,ε-己内酰胺更有效地促进固化。
这些催化剂(E)可以单独使用或组合使用2种以上。通过使用金属系催化剂(E1),能够制成密封强度优异的粘接剂。通过使用脂肪族环状酰胺化合物(E2),能够制成初始凝聚力优异、对金属基材的密合性、不易产生由气泡引起的外观不良的粘接剂。还优选将金属系催化剂(E1)与脂肪族环状酰胺化合物(E2)组合使用。
相对于多异氰酸酯组合物(X)和多元醇组合物(Y)的固体成分总量100质量份,催化剂(E1)的配合量优选设为0.001~3质量份,更优选设为0.01~2质量份。相对于多异氰酸酯组合物(X)和多元醇组合物(Y)的固体成分总量100质量份,催化剂(E2)的配合量优选设为0.001~3质量份,更优选设为0.01~2质量份。
(颜料)
本发明的粘接剂可以根据需要包含颜料。作为所使用的颜料,没有特别限制,可举出涂料原料便览1970年度版(日本涂料工业会编)中记载的体质颜料、白颜料、黑颜料、灰色颜料、红色颜料、茶色颜料、绿色颜料、蓝颜料、金属粉颜料、发光颜料、珍珠色颜料等有机颜料、无机颜料、以及塑料颜料等。
作为体质颜料,例如可举出沉降性硫酸钡、白色颜料(日文原文:ご粉)、沉降碳酸钙、碳酸氢钙、寒水石、氧化铝白、二氧化硅、含水微粉二氧化硅(白碳)、超微粉无水二氧化硅(AEROSIL)、硅砂(二氧化硅砂)、滑石、沉降性碳酸镁、膨润土、粘土、高岭土、黄土等。
作为有机颜料的具体例,可举出联苯胺黄、汉莎黄、色淀红4R等各种不溶性偶氮颜料;色淀红C、胭脂红6B、枣红10等可溶性偶氮颜料;酞菁蓝、酞菁绿等各种(铜)酞菁系颜料;罗丹明色淀、甲基紫色淀等各种碱性染色色淀;喹啉色淀、坚牢天蓝等各种媒染染料系颜料;蒽醌系颜料、硫靛系颜料、紫环酮系颜料等各种还原染料系颜料;Cinquasia Red B等各种喹吖啶酮系颜料;二噁嗪紫等各种二噁嗪系颜料;固美透等各种缩合偶氮颜料;苯胺黑等。
作为无机颜料,可举出铬黄、铬酸锌、钼橙等之类的各种铬酸盐;普鲁士蓝等各种亚铁氰化合物;氧化钛、锌白、棕黄、氧化铁、铁丹、氧化铬绿、氧化锆等各种金属氧化物;镉黄、镉红、硫化汞等各种硫化物或硒化物;硫酸钡、硫酸铅等各种硫酸盐;硅酸钙、群青等各种硅酸盐;碳酸钙、碳酸镁等各种碳酸盐;钴紫、锰紫等各种磷酸盐;铝粉、金粉、银粉、铜粉、青铜粉、黄铜粉等各种金属粉末颜料;这些金属的薄片颜料、云母/薄片颜料;被覆有金属氧化物的形态的云母/薄片颜料、云母状氧化铁颜料等金属颜料、珠光颜料;石墨、炭黑等。
作为塑料颜料,例如可举出DIC株式会社制“GRANDOLL PP-1000”、“PP-2000S”等。
关于使用的颜料,根据目的适当选择即可,例如从耐久性、耐候性、设计性优异的方面出发,作为白色颜料,优选使用氧化钛、锌白等无机氧化物,作为黑色颜料,优选使用炭黑。
关于颜料的配合量,作为一例,相对于多异氰酸酯组合物(X)和多元醇组合物(Y)的固体成分总量100质量份而言为1~400质量份,为了使粘接性、抗粘连性更加良好,更优选设为10~300质量份。
(粘接促进剂)
本发明的粘接剂可以包含粘接促进剂。作为粘接促进剂,可举出硅烷偶联剂、钛酸酯系偶联剂、铝系偶联剂等偶联剂、环氧树脂等。
作为硅烷偶联剂,可举出γ-氨基丙基三乙氧基硅烷、γ-氨基丙基三甲氧基硅烷、N-β(氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-β(氨基乙基)-γ-氨基丙基三甲基二甲氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷等氨基硅烷;β-(3,4-环氧环己基)乙基三甲氧基硅烷、γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三乙氧基硅烷等环氧硅烷;乙烯基三(β-甲氧基乙氧基)硅烷、乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷等乙烯基硅烷;六甲基二硅氮烷、γ-巯基丙基三甲氧基硅烷等。
作为钛酸酯系偶联剂,例如可举出四异丙氧基钛、四正丁氧基钛、钛酸丁酯二聚物、钛酸四硬脂酯、乙酰丙酮钛、乳酸钛、四辛二醇钛酸酯、乳酸钛、四硬脂氧基钛等。
作为铝系偶联剂,例如可举出乙酰烷氧基二异丙醇铝等。
作为环氧树脂,可举出通常市售的Epi-Bis型、线性酚醛型、β-甲基环氧氯丙烷(日文原文:β-メチルエピクロ)型、环状环氧乙烷型、缩水甘油醚型、缩水甘油酯型、聚二醇醚型、二醇醚型、环氧化脂肪酸酯型、多元羧酸酯型、氨基缩水甘油基型、间苯二酚型等各种环氧树脂、三缩水甘油基三(2-羟基乙基)异氰脲酸酯、新戊二醇二缩水甘油醚、1,6-己二醇二缩水甘油醚、烯丙基缩水甘油醚、2-乙基己基缩水甘油醚、苯基缩水甘油醚、苯酚缩水甘油醚、对叔丁基苯基缩水甘油醚、己二酸二缩水甘油酯、邻苯二甲酸二缩水甘油酯、甲基丙烯酸缩水甘油酯、丁基缩水甘油醚等化合物等。
(其他添加剂)
本发明的粘接剂除了上述成分以外还可以包含流平剂、胶体状二氧化硅、氧化铝溶胶等无机微粒、聚甲基丙烯酸甲酯系的有机微粒、消泡剂、防流挂剂、湿润分散剂、粘性调节剂、紫外线吸收剂、金属钝化剂、过氧化物分解剂、阻燃剂、增强剂、增塑剂、润滑剂、防锈剂、荧光性增白剂、无机系热射线吸收剂、防火剂、抗静电剂、脱水剂、公知惯用的热塑性弹性体、增粘剂、磷酸化合物、三聚氰胺树脂、反应性弹性体等。这些添加剂的配合量在不损害本发明的粘接剂的期望的范围内适当调整。
作为增塑剂,例如可举出苯二甲酸系增塑剂、脂肪酸系增塑剂、芳香族多元羧酸系增塑剂、磷酸系增塑剂、多元醇系增塑剂、环氧系增塑剂、聚酯系增塑剂、碳酸酯系增塑剂等。
作为苯二甲酸系增塑剂,例如可举出邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二异丁酯、邻苯二甲酸二己酯、邻苯二甲酸二庚酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯、邻苯二甲酸二壬酯、邻苯二甲酸二异壬酯、邻苯二甲酸二癸酯、邻苯二甲酸二异癸酯、邻苯二甲酸二(十三烷基)酯、邻苯二甲酸二(十一烷基)酯、邻苯二甲酸二月桂酯、邻苯二甲酸二硬脂酯、邻苯二甲酸二苯酯、邻苯二甲酸二苄酯、邻苯二甲酸丁基苄酯、邻苯二甲酸二环己酯、邻苯二甲酸辛基癸酯、间苯二甲酸二甲酯、间苯二甲酸二(2-乙基己基)酯、间苯二甲酸二异辛酯等苯二甲酸酯系增塑剂,例如四氢邻苯二甲酸二(2-乙基己基)酯、四氢邻苯二甲酸二正辛酯、四氢邻苯二甲酸二异癸酯等四氢苯二甲酸酯系增塑剂。
作为脂肪酸系增塑剂,例如可举出己二酸二正丁酯、己二酸二(2-乙基己基)酯、己二酸二异癸酯、己二酸二异壬酯、己二酸二(C6-C10烷基)酯、己二酸二(丁基二乙二醇酯)(日文原文:ジブチルジグリコールアジペート)等己二酸系增塑剂、例如壬二酸二正己酯、壬二酸二(2-乙基己基)酯、壬二酸二异辛酯等壬二酸系增塑剂、例如癸二酸二正丁酯、癸二酸二(2-乙基己基)酯、癸二酸二异壬酯等癸二酸系增塑剂、例如马来酸二甲酯、马来酸二乙酯、马来酸二正丁酯、马来酸二(2-乙基己基)酯等马来酸系增塑剂、例如富马酸二正丁酯、富马酸二(2-乙基己基)酯等富马酸系增塑剂、例如衣康酸单甲酯、衣康酸单丁酯、衣康酸二甲酯、衣康酸二乙酯、衣康酸二丁酯、衣康酸二(2-乙基己基)酯等衣康酸系增塑剂、例如硬脂酸正丁酯、甘油单硬脂酸酯、二乙二醇二硬脂酸酯等硬脂酸系增塑剂、例如油酸丁酯、甘油单油酸酯、二乙二醇单油酸酯等油酸系增塑剂、例如柠檬酸三乙酯、柠檬酸三正丁酯、乙酰柠檬酸三乙酯、乙酰柠檬酸三丁酯、乙酰柠檬酸三(2-乙基己基)酯等柠檬酸系增塑剂、例如乙酰蓖麻油酸甲酯、乙酰蓖麻油酸丁酯、甘油单蓖麻油酸酯、二乙二醇单蓖麻油酸酯等蓖麻油酸系增塑剂、以及二乙二醇单月桂酸酯、二乙二醇二壬酸酯、季戊四醇脂肪酸酯等其他脂肪酸系增塑剂等。
作为芳香族多元羧酸系增塑剂,例如可举出偏苯三酸三正己酯、偏苯三酸三(2-乙基己基)酯、偏苯三酸三正辛酯、偏苯三酸三异辛酯、偏苯三酸三异壬酯、偏苯三酸三癸酯、偏苯三酸三异癸酯等偏苯三酸系增塑剂、例如均苯四酸四(2-乙基己基)酯、均苯四酸四正辛酯等均苯四酸系增塑剂等。
作为磷酸系增塑剂,例如可举出磷酸三乙酯、磷酸三丁酯、磷酸三(2-乙基己基)酯、磷酸三(丁氧基乙基)酯、磷酸三苯酯、磷酸辛基二苯酯、磷酸甲苯基二苯酯、磷酸甲苯基苯酯、磷酸三(甲苯基)酯、磷酸三(二甲苯基)酯、磷酸三(氯乙基)酯、磷酸三(氯丙基)酯、磷酸三(二氯丙基)酯、磷酸三(异丙基苯基)酯等。
作为多元醇系增塑剂,例如可举出二乙二醇二苯甲酸酯、二丙二醇二苯甲酸酯、三乙二醇二苯甲酸酯、三乙二醇二(2-乙基丁酸酯)、三乙二醇二(2-乙基己酸酯)、亚甲基双硫代乙醇酸二丁酯等二醇系增塑剂、例如甘油单乙酸酯、甘油三乙酸酯、甘油三丁酸酯等甘油系增塑剂等。
作为环氧系增塑剂,例如可举出环氧化大豆油、环氧硬脂酸丁酯、环氧六氢邻苯二甲酸二(2-乙基己基)酯、环氧六氢邻苯二甲酸二异癸酯、环氧甘油三酯、环氧化油酸辛酯、环氧化油酸癸酯等。
作为聚酯系增塑剂,例如可举出己二酸系聚酯、癸二酸系聚酯、苯二甲酸系聚酯等。
作为碳酸酯系增塑剂,可举出碳酸亚丙酯、碳酸亚乙酯等。
另外,作为增塑剂,除此以外,还可举出部分氢化三联苯、粘接性增塑剂、以及邻苯二甲酸二烯丙酯、丙烯酸系单体、低聚物等聚合性增塑剂等。这些增塑剂可以单独使用或并用2种以上。
<<层叠体的制造方法>>
本发明的层叠体可以通过公知的方法得到。例如可通过具有2液混合工序的方法、具有2液分别涂敷工序的方法而得到,在上述2液混合工序中,将多异氰酸酯组合物(X)和多元醇组合物(Y)预先混合后涂布于第一基材,接着在涂布面层叠第二基材,使粘接剂层固化而得到层叠体,在上述2液分别涂敷工序中,将多异氰酸酯组合物(X)和多元醇组合物(Y)分别涂布于第一基材和第二基材后,使各自的涂布面接触并压接,从而使第一基材与第二基材层叠,使粘接剂层固化而得到层叠体。
作为2液分别涂敷的另一方式,也优选在一个基材上涂布多异氰酸酯组合物(X)与具有活性氢基的化合物的混合物,在另一个基材上涂敷多元醇组合物(Y)后,使各自的涂布面接触并压接,由此使这些基材层叠,使粘接剂层固化。作为与多异氰酸酯组合物(X)混合的具有活性氢基的化合物,可以使用作为多元醇(B)、化合物(C)而例示的物质。
特别是,从更容易确保多元醇组合物(Y)在基材上润湿扩展为止的时间的方面出发,本发明的粘接剂优选用于具有分别涂敷工序的方法。在将多异氰酸酯组合物(X)和多元醇组合物(Y)分别涂敷于不同的基材后、直至使它们接触为止的期间,多异氰酸酯组合物(X)、多元醇组合物(Y)能够充分地在基材上润湿扩展。
作为本发明的层叠体的制造方法的优选的方式,可举出以下方法:在具有铝蒸镀层的基材的铝蒸镀层上涂敷多元醇组合物(Y),在另一个基材上涂敷多异氰酸酯组合物(X),使多异氰酸酯组合物(X)与多元醇组合物(Y)接触并压接。无溶剂型粘接剂与铝蒸镀层的密合性大多较差,但通过使用本发明的粘接剂并采用上述方法,能够使粘接层与铝蒸镀层的密合性良好。
作为本发明的层叠体的制造方法的另一优选方式,可举出以下方法:在具有印刷层的基材的印刷层上涂敷多异氰酸酯组合物(X),在另一个基材上涂敷多元醇组合物(Y),使多异氰酸酯组合物(X)与多元醇组合物(Y)接触并压接。如果使用无溶剂型粘接剂将印刷层与其他基材贴合,则存在粘接剂使印刷层溶解等而产生外观不良的情况。通过采用上述方法,能够抑制层叠体的外观不良。
在通过具有2液混合工序的方法来制造本发明的层叠体的情况下,关于粘接剂(多异氰酸酯组合物(X)与多元醇组合物(Y)的混合物)的涂布量,作为一例,为0.5~5.0g/m2。在通过具有2液分别涂敷工序的方法来制造本发明的层叠体的情况下,多异氰酸酯组合物(X)和多元醇组合物(Y)的涂布量分别优选以0.3~3.0g/m2、更优选以0.3~2.0g/m2左右的方式使用。
压接方法优选为一边通过2个辊(层压辊)之间一边利用辊间的压力进行贴合的方法,层压辊的温度优选为室温~80℃左右,压力优选为0.05~0.5MPa左右。
无论是哪种方法,在使用本发明的2液固化型粘接剂的情况下,在层压后,在常温(20~25℃)或加热下、更具体而言在15~35℃的温度下,用12~72小时使粘接剂固化,表现出实用物性。
<<层叠体>>
本发明的层叠体是通过上述方法将多个基材贴合而得到的。另外,也可以在本发明的层叠体上进一步贴合其他基材。此时使用的粘接剂可以为上述粘接剂,也可以为通用的2液固化型粘接剂。另外,在通过本发明的方法得到的层叠体上进一步贴合其他基材的情况下,可以使用干式层压法或无溶剂层压法,也可以使用分别涂敷方法。
作为具体的层叠体的构成,可举出:
(1)基材1/粘接层1/密封膜
(2)基材1/粘接层1/金属蒸镀未拉伸膜
(3)基材1/粘接层1/金属蒸镀拉伸膜
(4)透明蒸镀拉伸膜/粘接层1/密封膜
(5)基材1/粘接层1/基材2/粘接层2/密封膜
(6)基材1/粘接层1/金属蒸镀拉伸膜/粘接层2/密封膜
(7)基材1/粘接层1/透明蒸镀拉伸膜/粘接层2/密封膜
(8)基材1/粘接层1/金属层/粘接层2/密封膜
(9)基材1/粘接层1/基材2/粘接层2/金属层/粘接层3/密封膜
(10)基材1/粘接层1/金属层/粘接层2/基材2/粘接层3/密封膜等,但不限于此。
作为构成(1)中使用的基材1,可举出OPP膜、PET膜、尼龙膜、纸等。另外,作为基材1,也可以使用实施了以提高气体阻隔性、设置后述的印刷层时的油墨接受性等为目的的涂布而得的基材。作为实施了涂布而得的基材膜1的市售品,可举出K-OPP膜、K-PET膜等。粘接层1为本发明的粘接剂的固化涂膜。作为密封膜,可举出CPP膜、LLDPE膜等。可以在基材1的粘接层1侧的面(在使用实施了涂布而得的材料作为基材膜1的情况下,为涂布层的粘接层1侧的面)或与粘接层1相反侧的面设置印刷层。印刷层是利用凹版油墨、柔版油墨、胶版油墨、孔版油墨、喷墨油墨等各种印刷油墨、并通过以往用于对聚合物膜、纸进行印刷的通常的印刷方法而形成的。
作为构成(2)、(3)中使用的基材1,可举出OPP膜、PET膜、纸等。粘接层1为本发明的粘接剂的固化涂膜。作为金属蒸镀未拉伸膜,可以使用对CPP膜实施了铝等的金属蒸镀而得的VM-CPP膜,作为金属蒸镀拉伸膜,可以使用对OPP膜实施了铝等的金属蒸镀而得的VM-OPP膜。也可以与构成(1)同样地在基材1的任意面设置印刷层。
作为构成(4)中使用的透明蒸镀拉伸膜,可举出对OPP膜、PET膜、尼龙膜等实施了二氧化硅、氧化铝蒸镀而得的膜。也可以使用以二氧化硅、氧化铝的无机蒸镀层的保护等为目的而在蒸镀层上实施了涂布而得的膜。粘接层1是本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以在透明蒸镀拉伸膜的粘接层1侧的面(当使用在无机蒸镀层上实施了涂布而得的材料时,为涂布层的粘接层1侧的面)设置印刷层。印刷层的形成方法与构成(1)相同。
作为构成(5)中使用的基材1,可举出PET膜、纸等。作为基材2,可举出尼龙膜等。粘接层1、粘接层2中的至少一者为本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以与构成(1)同样地在基材1的任意面设置印刷层。
作为构成(6)的基材1,可举出与构成(2)、(3)同样的基材。作为金属蒸镀拉伸膜,可举出对OPP膜、PET膜实施了铝等的金属蒸镀而得的VM-OPP膜、VM-PET膜。粘接层1、粘接层2中的至少一者为本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以与构成(1)同样地在基材1的任意面设置印刷层。
作为构成(7)的基材1,可举出PET膜、纸等。作为透明蒸镀拉伸膜,可举出与构成(4)同样的透明蒸镀拉伸膜。粘接层1、2中的至少一者为本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以与构成(1)同样地在基材1的任意面设置印刷层。
作为构成(8)的基材1,可举出PET膜、纸等。作为金属层,可举出铝箔等。粘接层1、2中的至少一者为本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以与构成(1)同样地在基材1的任意面设置印刷层。
作为构成(9)、(10)的基材1,可举出PET膜、纸等。作为基材2,可举出尼龙膜等。作为金属层,可举出铝箔等。粘接层1、2、3中的至少一层为本发明的粘接剂的固化涂膜。密封膜可举出与构成(1)同样的密封膜。可以与构成(1)同样地在基材1的任意面设置印刷层。
<<包装材料>>
本发明的包装材料是将本发明的层叠体成型为袋状而成的。作为制袋方法,可举出以下方法:将本发明的层叠体折弯或重叠而使其内层的面(密封膜的面)对置,对于其周边端部,根据例如侧面密封型、两侧密封型、三侧密封型、四侧密封型、信封贴合密封型、合掌贴合密封型、带褶密封型、平底密封型、方底密封型、角撑型、其它热封型等形式进行热封。本发明的包装材料可以根据内容物、使用环境、使用形式而采取各种形式。也可以是自立性包装材料(自立袋)等。作为热封的方法,可以通过棒密封、旋转辊密封、带密封、脉冲密封、高频密封、超声波密封等公知的方法来进行。可以设置易开封处理、再封性手段。
本发明的包装材料主要可以作为填充食品、洗剂、药剂的包装材料在工业上使用。关于具体的用途,作为洗剂、药剂,可举出洗涤用液体洗剂、厨房用液体洗剂、洗浴用液体洗剂、洗浴用液体皂、液体洗发水、液体护发素、医药用片剂等。另外,也可以用于包装上述容器的2次包装材料。
实施例
以下,列举具体的合成例、实施例来更详细地说明本发明,但本发明并不限定于这些实施例。需要说明的是,在以下的例子中,只要没有特别说明,则“份”和“%”分别表示“质量份”和“质量%”。
<多异氰酸酯组合物(X)的制备>
(多异氰酸酯组合物(X-1))
在具备搅拌机、温度计、氮气导入管的烧瓶中,将4,4-二苯基甲烷二异氰酸酯(以下,简记为“MDI”)40.2份和六亚甲基二异氰酸酯脲酸酯体(以下,简记为“HDI脲酸酯”)10.0份投入到反应容器内,在氮气下进行搅拌,加热至60℃。进一步混合数均分子量1000的2官能的聚丙二醇(以下,简记为“PPG”。)37.9份和2,2,4-三甲基-1,3-戊二醇2.0份并将其分数次地滴加至该烧瓶中,在80℃搅拌5~6小时,进行氨基甲酸酯化反应,由此得到了多异氰酸酯。将所得到的多异氰酸酯与碳二亚胺改性异氰酸酯10.0份进行混合,得到了多异氰酸酯组合物(X-1)。
<多元醇组合物(Y)的制备>
按照表1~3所示的配方制备多元醇组合物(Y-1)~(Y-13)、(Y’-1)~(Y’-3)。表中的化合物如下所述。
多元醇(B1-1-1):ACTCOL D-1000(三井化学公司制,数均分子量1000,2官能的聚亚丙基多元醇)
多元醇(B1-1-2):ACTCOL T-1000(三井化学公司制,数均分子量1000,3官能的聚亚丙基多元醇)
多元醇(B1-1-3):ACTCOL D-400(三井化学公司制,数均分子量400,2官能的聚亚丙基多元醇)
多元醇(B1):D-4000(三井化学公司制,数均分子量4000,2官能的聚亚丙基多元醇)
多元醇(B1-2):SANNIX HD-402(三洋化成工业公司制,数均分子量600,4官能的聚亚丙基多元醇)
多元醇(B2):蓖麻油
多元醇(B3):KURARAY POLYOL F-510(由三羟甲基丙烷、3-甲基-1,5-戊二醇、己二酸形成的重均分子量500的聚酯三醇)
化合物(C-1):二羟甲基丙酸
化合物(C-2):二羟甲基丁酸
多胺(D1):JEFFAMINE T-403(Huntsman公司制,聚氧亚丙基三胺,Mw=400,胺值=355mgKOH/g)
多胺(D2):单乙醇胺
多胺(D3):二乙胺
催化剂(E1-1):BiCAT8(Shepherd公司制,新癸酸铋与新癸酸锌的混合物)
催化剂(E1-2):二月桂酸二丁基锡
催化剂(E2):ε-己内酰胺
KBM-403:Shin-Etsu Silicone制,3-环氧丙氧基丙基三甲氧基硅烷
KBE-903:Shin-Etsu Silicone制,3-氨基丙基三乙氧基硅烷
流平剂:SURFYNOL 420(EVONIK公司制,乙炔系二醇的聚醚化物)
[表1]
Y-1 | Y-2 | Y-3 | Y-4 | Y-5 | |
多元醇(B1-1-1) | 40.00 | ||||
多元醇(B1-1-2) | 13.66 | ||||
多元醇(B1-1-3) | 40.00 | 40.00 | 40.00 | ||
多元醇(B1) | 40.00 | ||||
多元醇(B1-2) | 10.00 | 10.00 | |||
多元醇(B2) | 44.40 | 44.40 | 44.40 | 33.20 | |
多元醇(B3) | 25.00 | ||||
化合物(C-1) | 0.90 | 0.90 | 0.90 | 0.90 | 0.90 |
化合物(C-2) | |||||
多胺(D1) | 7.80 | 7.80 | 7.80 | 14.00 | 9.00 |
多胺(D2) | |||||
多胺(D3) | |||||
催化剂(E1-1) | 1.00 | 1.00 | 1.00 | 1.00 | 0.50 |
催化剂(E1-2) | |||||
催化剂(E2) | 0.94 | 0.94 | 0.94 | 0.90 | 0.94 |
KBM-403 | |||||
KBE-903 | |||||
流平剂 | 5.00 | 5.00 | 5.00 | ||
胺值(mgKOH/g) | 27.8 | 27.8 | 27.8 | 50.0 | 32.1 |
[表2]
Y-6 | Y-7 | Y-8 | Y-9 | Y-10 | Y-11 | |
多元醇(B1-1-1) | ||||||
多元醇(B1-1-2) | 13.66 | 14.66 | 11.56 | 18.66 | 18.66 | 14.86 |
多元醇(B1-1-3) | 40.00 | 40.00 | 40.00 | 40.00 | 40.00 | 40.00 |
多元醇(B1) | ||||||
多元醇(B1-2) | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 |
多元醇(B2) | ||||||
多元醇(B3) | 25.00 | 25.00 | 25.00 | 25.00 | 25.00 | 25.00 |
化合物(C-1) | 0.10 | 3.00 | 0.90 | 0.90 | 0.90 | |
化合物(C-2) | 0.90 | |||||
多胺(D1) | 9.00 | 9.00 | 9.00 | 9.00 | ||
多胺(D2) | 4.00 | |||||
多胺(D3) | 4.00 | |||||
催化剂(E1-1) | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | |
催化剂(E1-2) | 0.20 | |||||
催化剂(E2) | 0.94 | 0.94 | 0.94 | 0.94 | 0.94 | |
KBM-403 | ||||||
KBE-903 | ||||||
流平剂 | ||||||
胺值(mgKOH/g) | 32.1 | 32.1 | 32.1 | 21.8 | 0.0 | 32.1 |
[表3]
Y-12 | Y-13 | Y′-1 | Y′-2 | Y′-3 | |
多元醇(B1-1-1) | |||||
多元醇(B1-1-2) | 14.06 | 13.46 | 15.06 | 23.00 | |
多元醇(B1-1-3) | 40.00 | 40.00 | 40.00 | 40.00 | 40.00 |
多元醇(B1) | |||||
多元醇(B1-2) | 10.00 | 10.00 | 10.00 | 10.00 | |
多元醇(B2) | 45.30 | ||||
多元醇(B3) | 25.00 | 25.00 | 25.00 | 25.00 | |
化合物(C-1) | 0.90 | 0.50 | |||
化合物(C-2) | |||||
多胺(D1) | 9.00 | 9.00 | 7.80 | 9.00 | |
多胺(D2) | |||||
多胺(D3) | |||||
催化剂(E1-1) | 1.00 | 0.50 | 1.00 | 0.50 | |
催化剂(E1-2) | |||||
催化剂(E2) | 0.94 | 0.94 | 0.94 | 0.94 | |
KBM-403 | 0.40 | 0.40 | |||
KBE-903 | 0.20 | 0.20 | |||
流平剂 | 5.00 | ||||
胺值(mgKOH/g) | 32.1 | 32.1 | 27.8 | 32.1 | 0.0 |
<评价>
(层压强度OPP/VMCPP)
将加热后的多异氰酸酯组合物(X)涂布于OPP膜(东洋纺公司制,P2161),将加热后的多元醇组合物(Y)涂布于VMCPP膜(TORAY ADVANCED FILM公司制,2703),将OPP膜和VMCPP膜用夹持辊(50℃)进行压接,在25℃熟化24小时,得到了OPP/粘接层/VMCPP的层叠体1。多异氰酸酯组合物(X)、多元醇组合物(Y)的涂布量(g/m2)如表4、5所示。
将层叠体1切成长度300mm、宽度15mm,使用Instron公司制拉伸试验机,在25℃的环境下,以剥离速度300mm/分钟的剥离速度进行拉伸,以15mm宽度测定OPP/VMCPP间的T型剥离强度。将该试验进行5次,求出其平均值,按照以下的基准进行评价,将结果汇总于表4、5。
5:1.5N/15mm以上
4:1.0N/15mm以上且小于1.5N/15mm
3:0.5N/15mm以上且小于1.0N/15mm
2:0.2N/15mm以上且小于0.5N/15mm
1:小于0.2N/15mm
(层压强度OPP/CPP)
将加热后的多异氰酸酯组合物(X)涂布于OPP膜(东洋纺公司制,P2161),将加热后的多元醇组合物(Y)涂布于CPP膜(东洋纺公司制,P1128),将OPP膜和CPP膜用夹持辊(50℃)进行压接,得到了OPP/粘接层/CPP的层叠体2。多异氰酸酯组合物(X)、多元醇组合物(Y)的涂布量(g/m2)如表4、5所示。与层叠体1同样地测定层压强度并进行评价,将结果汇总于表4、5。
(加工外观)
对电晕处理PET膜(厚度12μm)使用多异氰酸酯组合物(X),对VMCPP膜(厚度25μm)使用多元醇组合物(Y),以100、150、200、250m/min的加工速度将它们各自贴合。多异氰酸酯组合物(X)、多元醇组合物(Y)的涂布量(g/m2)如表4、5所示。在25℃熟化24小时后,确认层叠体中有无残留的气泡,调查未残留气泡的加工速度范围。按照以下的5等级评价进行评价,将结果汇总于表4、5。
5:在100~250m/min无气泡残留
4:在100~200m/min无气泡残留
3:在100~150m/min无气泡残留
2:在100m/min无气泡残留
1:在100m/min有气泡残留
[表4]
[表5]
/>
Claims (11)
1.一种2液固化型粘接剂,其特征在于,包含多异氰酸酯组合物(X)和多元醇组合物(Y),
所述多异氰酸酯组合物(X)包含多异氰酸酯化合物(A),
所述多元醇组合物(Y)包含多元醇(B)和化合物(C),所述化合物(C)为选自2,2-二羟甲基乙酸、2,2-二羟甲基丙酸、2,2-二羟甲基丁酸、2,2-二羟甲基戊酸中的至少一种。
2.根据权利要求1所述的2液固化型粘接剂,其中,所述多元醇组合物(Y)包含多胺(D)。
3.根据权利要求1或2所述的2液固化型粘接剂,其中,所述多元醇(B)包含聚醚多元醇(B 1)或植物油多元醇(B2)中的至少一种。
4.根据权利要求1~3中任一项所述的2液固化型粘接剂,其中,所述多元醇(B)包含数均分子量为130以上且3000以下的聚醚二醇(B 1-1)。
5.根据权利要求1~4中任一项所述的2液固化型粘接剂,其中,所述多元醇(B)包含3官能以上的聚醚多元醇(B 1-2)。
6.根据权利要求1~5中任一项所述的2液固化型粘接剂,其中,所述多元醇(B)包含聚酯多元醇(B3)。
7.根据权利要求6所述的2液固化型粘接剂,其中,所述聚酯多元醇(B3)为包含多元羧酸和多价醇的组合物的反应产物,脂肪族多元羧酸在所述多元羧酸中所占的配合量为80质量%以上,脂肪族多价醇在所述多价醇中所占的配合量为80质量%以上。
8.根据权利要求1~7中任一项所述的2液固化型粘接剂,其中,所述多元醇组合物(Y)包含氨基甲酸酯化催化剂(E)。
9.一种层叠体,其特征在于,包含第1基材、第2基材、以及将所述第1基材与所述第2基材贴合的粘接层,所述粘接层为权利要求1~8中任一项所述的粘接剂的固化涂膜。
10.一种层叠体的制造方法,其包括:
在第1基材上涂布多异氰酸酯组合物(X)的工序;
在第2基材上涂布多元醇组合物(Y)的工序;以及
将所述第1基材和所述第2基材以所述多异氰酸酯组合物(X)与所述多元醇组合物(Y)接触的方式贴合的工序。
11.一种包装材料,其包含权利要求9所述的层叠体。
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