CN113195670A - 粘着剂组合物 - Google Patents
粘着剂组合物 Download PDFInfo
- Publication number
- CN113195670A CN113195670A CN201880100281.4A CN201880100281A CN113195670A CN 113195670 A CN113195670 A CN 113195670A CN 201880100281 A CN201880100281 A CN 201880100281A CN 113195670 A CN113195670 A CN 113195670A
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- China
- Prior art keywords
- component
- adhesive
- composition
- layer
- polyol
- Prior art date
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- 150000001875 compounds Chemical class 0.000 claims abstract description 52
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- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 27
- 239000010452 phosphate Substances 0.000 claims abstract description 27
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 25
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
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- JIABEENURMZTTI-UHFFFAOYSA-N 1-isocyanato-2-[(2-isocyanatophenyl)methyl]benzene Chemical class O=C=NC1=CC=CC=C1CC1=CC=CC=C1N=C=O JIABEENURMZTTI-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/088—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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Abstract
一种聚胺酯粘着剂组合物,例如双组分聚胺酯粘着剂,其包含(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及(B)至少一种多元醇组分,包含:(Bi)至少一种聚酯多元醇化合物;和(Bii)至少一种磷酸酯多元醇化合物;以及一种用于制备上述组合物的方法。
Description
技术领域
本发明涉及一种粘着剂组合物;且更特定地说,本发明涉及一种双组分聚胺酯粘着剂组合物。
背景技术
迄今为止,已经生产出多种双组分(2K)型聚胺酯粘着剂组合物用于多种应用。如本领域所知,2K聚胺酯组合物是基于多元醇组分与聚异氰酸酯组分的反应混合物,并且长期以来作为粘着剂使用。当两种组分混合时,聚异氰酸酯与多元醇反应形成固化的聚胺酯粘着剂;并且反应可以形成与许多类型的衬底形成牢固的粘着性接合。
举例来说,以下参考文献揭示一种具有良好粘着力的2K粘着剂:美国专利第8,716,427B2号;CN104228210(A);CN107614648A;US20140242333(A1);US20150380695(A1);US20160204395(A1);以及WO 2015/168670。
尽管关于多种应用中所用的2K聚胺酯组合物的技术领域已有一些进展,但粘着剂的技术领域仍有发展空间,特定来说,展现增强的特性(例如接合强度、可塑性和耐热性)的层压粘着剂,使得粘着剂组合物能适当地用于生产层压复合膜结构,例如箔基复合结构层压制品。
举例来说,用于包装锂离子电池(LIB)的包装典型地具有箔基层压结构并且所述箔基层压结构可以是例如尼龙、箔与蒸煮流延聚丙烯(RCPP)组合(尼龙/箔/RCPP);并且所述箔基层压结构通常由尼龙/箔/RCPP层压膜通过深度拉伸成型方法制成。迄今为止,此类LIB应用中所用的已知层压粘着剂组合物无法通过深拉伸和高温接合强度测试(例如在120℃下,在尼龙与箔之间达成大于(>)每15毫米2牛顿[N/15mm]的接合强度)。因此,期望提供一种基于溶剂的2K层压粘着剂组合物,其具有良好接合强度、可塑性和耐热性;且能用于制造箔基结构层压制品,例如LIB的层压膜包装。
发明内容
一般来说,本发明涉及新颖的基于溶剂的层压粘着剂组合物。在一个实施例中,本发明的粘着剂是基于溶剂的双组分层压粘着剂组合物(即,两部分***),其包含:(1)作为异氰酸酯封端的化合物部分(NCO-组分)的第一部分,及(2)作为羟基封端的多元醇(OH-组分)的第二部分。本发明的新颖粘着剂组合物是基于(1)聚酯多元醇与(2)磷酸酯多元醇的新颖多元醇混合物(即,2K粘着剂组合物的第二部分)。磷酸酯多元醇组分作为助粘剂提供于本发明的2K粘着剂组合物中。
在一个较佳实施例中,本发明涉及一种聚胺酯层压粘着剂组合物,例如2K聚胺酯粘着剂,其包含:(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及(B)至少一种多元醇组分,包含:(Bi)至少一种具有高分子量(例如>8,000克/摩尔[g/mol])的聚酯多元醇化合物;和(Bii)至少一种磷酸酯多元醇化合物。在以上实施例中,组分(A)、组分(B)或组分(A)与(B)均能够任选地包含至少一种溶剂化合物。
在另一实施例中,本发明包含一种用于制备上述聚胺酯层压粘着剂组合物的方法。
本发明的基于溶剂的2K层压粘着剂组合物有利地使得适用于制造多种制品的箔基层压结构(例如尼龙/箔/RCPP)的特性增强,例如接合强度、耐热性和可塑性。举例来说,尽管本发明的2K粘着剂可以用于多种应用,但本发明粘着剂可以特别适用于LIB应用。
另外,本发明的粘着剂组合物可以根据深度拉伸应用设计,所述深度拉伸应用需要使用高数值分子量(Mn)的聚酯多元醇,例如Mn>8,000g/mol的聚酯多元醇。
另外,本领域中通常已知当粘着剂组合物中的磷酸酯含量过高时,观察到所述组合物在深度拉伸应用中的性能较差。然而,本发明粘着剂组合物中的磷酸酯使用量是以适当的预定量使用,从而避免组合物的性能较差。
使用本发明粘着剂组合物的其它益处/优点包含例如:(1)最终层压粘着剂中不需要加入金属化合物;(2)最终粘着剂组合物中不需要加入丙烯酸类多元醇;(3)聚酯多元醇中所用的脂肪族羧酸和/或芳香族羧酸的含量无限制;(4)不需要使用环氧基封端的聚酯;以及(5)异氰酸酯封端的化合物中所用的脂肪族异氰酸酯和/或芳香族异氰酸酯的含量无限制。
附图说明
图1是示意性说明,其展示LIB包装层压膜的典型五层结构,大体如元件符号10所示,从其外侧,其包含外层侧树脂膜层(11)、外层侧粘着剂层(14)、金属箔层(12)、内层侧粘着剂层(15),以及由热密封层或其类似物构成的内表面层(13)。
具体实施方式
在一个通用实施例中,本发明包含双组分(2K)粘着剂组合物;且更特定地说,本发明包含2K PU粘着剂,包含(A)至少一种含有异氰酸酯基的组分;及(B)至少一种多元醇组分(或含有羟基的组分)。作为本发明的一个说明,当组分(A)与组分(B)混合时,(B):(A)之比率(即,OH/NCO干重指数)在一个实施例中可以是1至20;在另一个实施例中可以是2至15;且在再另一个实施例中可以是5至12。
含有异氰酸酯基团的组分(组分(A))可以是一或多种化合物的混合物或掺混物,包含例如至少一种含有异氰酸酯基的化合物,例如一或多种聚异氰酸酯化合物。含有异氰酸酯基的组分(组分(A))也可包含至少一溶剂化合物(例如如下文所述的乙酸乙酯)作为任选地存在的组分。
适用于本发明粘着剂调配物中的含有异氰酸酯基团的化合物可以包含例如芳香族异氰酸酯、脂肪族异氰酸酯或其混合物。适用于本发明的芳香族异氰酸酯的实施例包含例如亚甲基二苯基二异氰酸酯(“MDI”)的异构体,例如4,4-MDI、2,4-MDI及2,2'-MDI;经修饰的MDI,例如碳化二亚胺修饰的MDI或脲基甲酸酯修饰的MDI;甲苯二异氰酸酯(“TDI”)的异构体,例如2,4-TDI及2,6-TDI;萘二异氰酸酯(“NDI”)的异构体,例如1,5-NDI;以及其组合。
适用于本发明的含有脂肪族异氰酸酯基团的化合物的实施例包含例如六亚甲基二异氰酸酯(“HDI”)的异构体;异佛尔酮二异氰酸酯(“IPDI”)的异构体;二甲苯二异氰酸酯(“XDI”)的异构体;氢化亚甲基二苯基二异氰酸酯(“H12MDI”)的异构体;及其组合。
在一个优选实施例中,适用于本发明的含有异氰酸酯基的化合物可以选自由以下组成的群组:例如异氰酸酯单体、聚异氰酸酯、异氰酸酯预聚物,以及其中两种或更多种的混合物。
适用于粘着剂调配物中的例示性异氰酸酯单体可以包含芳香族二异氰酸酯,例如MDI异构体、TDI异构体;或脂肪族异氰酸酯,例如HDI、IPDI以及其混合物。
适用于粘着剂调配物的例示性聚异氰酸酯化合物可包含例如聚异氰酸酯加合物或三聚物。举例来说,聚异氰酸酯化合物可包含(但不限于)TDI-三羟甲基丙烷加合物(TDI-TMP加合物)及IPDI-三聚物。聚异氰酸酯化合物可以具有大于或等于(≥)2.8且小于或等于(≤)5的平均NCO官能度(f)(即,2.8≤f≤5)。
适用于粘着剂调配物的例示性异氰酸酯预聚物可以包含例如至少一种预聚物-多元醇-增链剂化合物结构,例如MDI(亚甲基二苯基二异氰酸酯)封端的预聚物,所述预聚物基于以EO(环氧乙烷)和/或PO(环氧丙烷)为主的二醇或三醇。
以调配物中的组分的总干重计,2K粘着剂调配物中的异氰酸酯化合物含量的范围在一个实施例中通常可以是1重量%(wt%)至30wt%;在另一个实施例中可以是2wt%至25wt%;且在再另一个实施例中可以是4wt%至15wt%。含有异氰酸酯基团的组分(组分(A))的含固量可以是例如30wt%至100wt%。
多元醇组分(组分(B))可以是一或多种化合物的溶液、混合物或掺混物,包含例如:(Bi)至少一种聚酯多元醇化合物(例如分子量>8,000g/mol的聚酯多元醇);和(Bii)至少一种磷酸酯多元醇化合物。
适用于本发明的粘着剂调配物中的聚酯多元醇化合物(组分(Bi))可以包含例如由多羧酸与多元醇衍生的聚酯多元醇。在一个实施例中,适用于多元醇组分(B)的聚酯多元醇化合物可选自例如具有至少8,000g/mol数目平均分子量的聚酯多元醇。另外,合适的聚酯多元醇可以具有≥1.8至≤3的OH官能度(f)(即,1.8≤f≤3)以及小于(<)15mg KOH/g的OH数。如本文所用,“OH数”由等效于一克多元醇中的羟基含量的氢氧化钾毫克数表征。
在另一实施例中,适用于粘着剂调配物的聚酯多元醇化合物可以包含例如二醇和任选地存在的多元醇(例如三醇、四醇)以及其混合物与二羧酸以及其混合物的缩聚物。在另一个实施例中,聚酯多元醇化合物也可衍生自二羧酸、其相应酸酐,或低碳醇的相应酯类。
适用于本发明的二醇可以包含(但不限于)乙二醇;丁二醇;二乙二醇;1,2-丙二醇;1,3-丙二醇;1,3-丁二醇;1,4-丁二醇;1,6-己二醇;2-甲基-1,3-丙二醇;新戊二醇;以及其混合物。在一个实施例中,为获得OH官能度>2的聚酯多元醇,粘着剂组合物中可以任选地包含OH官能度为3或>3的多元醇(例如三羟甲基丙烷、丙三醇、赤藻糖醇或季戊四醇)。
适用于本发明的二羧酸可以包含(但不限于)脂肪族酸、芳香族酸以及其组合。适合芳香族酸的实例包含邻苯二甲酸、间苯二甲酸、对苯二甲酸及其混合物。适合脂肪族酸的实例包含环己烷二甲酸、己二酸、壬二酸、癸二酸、戊二酸、顺丁烯二酸、反丁烯二酸、衣康酸、丙二酸、辛二酸、2-甲基丁二酸、3,3-二乙基戊二酸、2,2-二甲基丁二酸、偏苯三甲酸以及其混合物。也可使用此类酸的酸酐。另外,单羧酸(例如苯甲酸及己烷甲酸)在本发明的组合物中应减至最少或排除。在一个优选实施例中,本发明中可以使用饱和脂肪族或饱和芳香族酸,例如壬二酸、癸二酸、己二酸、对苯二甲酸、间苯二甲酸以及其混合物。
聚酯多元醇化合物(组分(Bi))可以具有-25℃至40℃范围内的玻璃转移温度(Tg)。-25℃与40℃之间的所有个别范围一及子范围包含于本发明的范围中;举例来说,聚酯多元醇化合物在一个实施例中可以具有-15℃至5℃范围内的Tg且在另一个实施例中可以具有-20℃至10℃范围内的Tg。
以调配物中的组分的总干重计,双组分粘着剂调配物中的聚酯多元醇化合物(组分(Bi))含量范围在一个实施例中通常可以是70wt%至95wt%;在另一个实施例中可以是75wt%至90wt%;且在再另一个实施例中可以是80wt%至90wt%。
一般来说,聚酯多元醇化合物的分子量(Mn)在一个实施例中可以是>8,000g/mol,在另一个实施例中可以是>10,000g/mol,在再另一个实施例中可以是>12,000g/mol,且在又另一个实施例中可以是>20,000g/mol。另外,聚酯多元醇化合物的Mn在一个实施例中可以是>8,000g/mol至200,000g/mol,在另一实施例中可以是10,000g/mol至150,000g/mol,且在再另一个实施例中可以是20,000g/mol至100,000g/mol。
或者,可以基于聚酯多元醇化合物的羟基值来选择聚酯多元醇化合物,所述羟基值在一个实施例中可以是<15mg KOH/g,在另一个实施例中可以是<10mg KOH/g,且在再另一个实施例中可以是<5mg KOH/g。
在一个通用实施例中,磷酸酯多元醇化合物(组分(Bii))可以包含例如如下结构(I)或结构(II)的化合物:
其中在上述结构(I)及结构(II)中,R'可选自任何有机基团。除结构(I)及(II)中所示的侧基之外,R'可以或可以不具有一或多个其它侧接-OH基团,且R'可以或可以不具有一或多个其它侧接-P(=O)(OH)2。在另一个实施例中,磷酸酯多元醇可通过磷酸型酸与多元醇反应而获得。举例来说,合适的磷酸型酸包含(但不限于)正磷酸、可以通过消去水使正磷酸缩合而制得之一系列化合物中的任何成员,例如焦磷酸、三聚磷酸及聚磷酸,以及其混合物。举例来说,合适的多元醇包含(但不限于)二醇、三醇、聚醚多元醇、聚酯多元醇以及其混合物。
在另一个实施例中,适用于粘着剂调配物中的磷酸酯多元醇化合物可以包含例如聚磷酸与多元醇的反应产物,其中多元醇选自聚醚多元醇、聚酯多元醇,以及两种或更多种多元醇的组合。在一个优选实施例中,适用于本发明的磷酸酯多元醇化合物可选自例如聚酯多元醇与百分之115(%)聚磷酸的反应产物。
以调配物中的组分的总干重计,双组分粘着剂调配物中的磷酸酯多元醇化合物(组分(Bii))含量的范围在一个实施例中通常可以是0.1wt%至7wt%;在另一个实施例中可以是0.5wt%至5wt%;且在再另一个实施例中是1wt%至4wt%。
多元醇组分(组分(B))可以进一步含有溶剂;且在一个优选实施例中,多元醇成分中的每一者可溶于组分(B)所用的溶剂中。举例来说,以基于溶剂重量的重量计,多元醇成分中的每一者在一个实施例中可以10wt%或更大,在另一个实施例中以50wt%或更大且在再另一个实施例中以100wt%或更大的量溶解。在一个优选实施例中,溶剂可选自烃溶剂、极性非质子性溶剂、极性质子性溶剂以及其混合物。在另一个优选实施例中,溶剂可以是极性非质子溶剂。在再另一个优选实施例中,溶剂可选自乙酸乙酯、丙酮、甲基乙基酮以及其混合物。当组分(B)中使用溶剂时,以基于组分B总重量的重量计,溶剂的量在一个实施例中可以是10wt%或更大,在另一个实施例中是20wt%或更大且在再另一个实施例中是40wt%或更大。当组分(B)中使用溶剂时,以基于组分B总重量的重量计,溶剂的量在一个实施例中可以是90%或更小,且在另一实施例中可以是80%或更小。
尽管本发明涉及双组分***,但本发明的粘着剂调配物可用多种任选地存在的添加剂调配以能够发挥特定功能,同时维持本发明粘着剂产品的极佳益处/特性。可以将聚胺酯粘着剂中任选地存在的组分(组分(C))添加至含有异氰酸酯基的第一组分(A)中;或可以将聚胺酯粘着剂中任选地存在的组分添加至第二多元醇组分(B)中。举例来说,在一个实施例中,可将任选地存在的溶剂化合物添加至本发明的粘着剂调配物的组分(A)中;且在另一个实施例中,可将任选地存在的溶剂化合物添加至本发明的粘着剂调配物的组分(B)中。在再另一个实施例中,可以将任选地存在的相同或不同溶剂化合物添加至粘着剂调配物组分(A)与组分(B)中。
使用时,任选地存在的溶剂化合物可包含例如乙酸乙酯、丁酮、丙酮、甲基苯以及其它胺基甲酸酯级有机溶剂,其能溶解:组分(A)、聚酯、环氧树脂、硅烷、磷酸酯以及其任何混合物。在另一个实施例中,在组分(A)与(B)已混合在一起之后,可以将如上文所述的相同溶剂添加至组合物中。
在其它实施例中,适用于调配物中的任选地存在的化合物或添加剂可以包含例如其它溶剂;助粘剂,例如硅烷、环氧树脂和酚类树脂;增链剂,例如甘油、三羟甲基丙烷、二乙二醇、丙二醇和2-甲基-1,3-丙二醇;以及催化剂,例如潜在锡催化剂,例如二辛基硫醇锡;基于非锡的金属有机催化剂,例如新癸酸铋(III);或热敏性胺催化剂,DBU(1,8-二氮杂双环-[5.4.0]十一碳-7-烯);填充剂,例如二氧化硅;以及其混合物。
当用于2K粘着剂调配物中时,以调配物中的组分的总重量计,任选地存在的添加剂(组分(C))的含量范围在一个实施例中通常可以是0wt%至20wt%;在另一个实施例中可以是0.01wt%至10wt%;且在再另一个实施例中可以是1wt%至5wt%。
在一个宽泛实施例中,用于制备本发明的粘着剂调配物的方法包含混合、掺合或掺混:(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;和上述任选地存在的所需化合物中的任一种,例如溶剂化合物;以及(B)至少一种多元醇组分,包含:(Bi)至少一种聚酯多元醇化合物;(Bii)至少一种磷酸酯多元醇化合物;及上述任选地存在的所需化合物中的任一种,例如溶剂化合物。需要时,可以将一或多种其它任选地存在的组分添加至粘着剂调配物中。举例来说,组分(A)与(B)可以上文所论述的期望浓度混合在一起,混合时的温度在一个实施例中为20℃至25℃;且在另一实施例中为15℃至35℃。组分混合次序并非关键且可以将两种或更多种组分混合在一起,随后添加其余组分。粘着剂调配物组分可以通过任何已知混合方法和设备混合在一起。
一般来说,两种组分(A)与(B)可彼此分开制备;且所述组分可各自储存于单独容器中。聚胺酯粘着剂调配物中的其它组分和任选地存在的添加剂可作为第一组分(A)或第二组分(B)的一部分存在。适用于储存各组分的容器可以是例如圆筒、带盖桶、袋、桶、罐、筒或管。施加粘着剂组合物之前,两种组分(A)与(B)分别存储且仅在施加期间或施加之前彼此混合。
通过本发明方法产生的本发明粘着剂调配物相较于常规粘着剂调配物具有若干有利特性和益处。举例来说,粘着剂调配物展现的一些特性可以包含增强的接合强度、可塑性和耐热性;在制造箔基结构层压制品(例如用于生产LIB包装的层压膜)的方法中有益的特性。
举例来说,在120℃下,尼龙层与铝箔层之间通过粘着剂调配物所展现的接合强度通常可以是1N/15mm或更大,原因在于接合强度越高,则粘着剂调配物的键结性能越佳。举例来说,粘着剂的接合强度在一个实施例中可以是≥1N/15mm,在另一个实施例中可以是≥1.5N/15mm,且在另一个实施例中可以是≥2.5N/15mm。粘着剂接合强度的其它优选实施例可以包含如下范围:在一个实施例中是1N/15mm至8N/15mm;在另一个实施例中是2.5N/15mm至8N/15mm;在再另一个实施例中是1.5N/15mm至5.5N/15mm;且在又另一个实施例中是1N/15mm至5N/15mm。粘着剂接合强度可通过下文实例的测试方法中所述的通用程序量测。
在另一个实施例中,可塑性是本发明的粘着剂所展现的有益特性。粘着剂的可塑性可根据此类深度拉伸方法的深度拉伸设定的深度量测。且,粘着剂的可塑性通常可以是1毫米(mm)或更大,原因在于深度拉伸的深度越高,则粘着剂调配物的可塑性能越佳。举例来说,粘着剂的可塑性在一个实施例中可以是≥1mm,在另一实施例中是≥3mm,且在另一实施例中是≥4mm。粘着剂可塑性的其它优选实施例可以包含1mm至15mm、在另一个实施例中3mm至8mm且在再另一个实施例中4mm至6mm的深度拉伸设定的深度范围。粘着剂的可塑性可通过下文实例的测试方法中所述的通用程序量测。
在再另一个实施例中,本发明的粘着剂调配物的耐热性是调配物的另一种有益特性。粘着剂耐热性可依据由粘着剂制得的层压结构、通过或未通过老化测试来测定,所述老化测试选自本领域中已知的常规老化测试。典型地,对层压结构进行历时特定小时数的老化测试;且接着根据分层、穿隧的任何迹象或任何类型的结构失效,可目视观察到由粘着剂制得的层压结构通过或未通过测试。通常,老化测试可以进行例如期望的时间段,如可以通过下文实例的测试方法中所述的程序所量测。通常,粘着剂组合物应在85℃和85%湿度下经过>60小时(hr)的老化时间。
通常,使用本发明粘着剂将两个衬底接合可以工业规模进行以生产大量的层压产品。有利的是,两种组分(A)及(B)分开填充并且储存在圆筒或带盖桶中,直至所述组分即用为止。如前所述,在施加粘着剂组合物之前,两种组分分开储存;且仅在粘着剂施加期间或施加之前,将两种组分彼此混合。在施加期间,借助于进料泵迫使所述组分从储存容器中排出,且在混合设备之直通管线中计量,例如工业生产中常用于2K粘着剂的那些管线。
两种组分(A)与(B)的混合可以通过静态混合器或借助于动态混合器进行。当混合组分(A)与(B)时,应注意确保将两种组分尽可能均匀地混合。如果两种组分的混合不良,则相对于有利混合比将产生局部偏差,此可能与使用粘着剂制得的所得产品的机械特性恶化有关。
可以通过常规方法,例如使用辊涂机、刮刀或挤出设备及方法,将粘着剂施加至至少一个衬底的表面上。粘着剂组合物可以一定的水平(每平方米的干燥组合物克数)施加,在一个实施例中为1或更大且在另一个实施例中为2或更大。粘着剂组合物可以一定水平(每平方米的干燥组合物克数)施加,在一个实施例中为10或更小且在另一个实施例中为7或更小。
本发明的另一实施例涉及一种使至少一个第一衬底与至少一个第二衬底接合的方法,包含以下步骤:(a)混合如上文所述的两种组分(A)与(B)以形成聚胺酯粘着剂,(b)将步骤(a)的聚胺酯粘着剂施加至至少一个待接合的衬底表面上且蒸发溶剂(若存在),(c)用聚胺酯粘着剂使待接合的第一与第二衬底接触(或连接)在一起,及(d)使聚胺酯粘着剂固化。举例来说,可以加热粘着剂以使粘着剂完全固化;且在一个通用实施例中,可以在25℃至80℃的温度下加热粘着剂。
在上述方法中,具有异氰酸酯基的第一组分(A)(NCO-组分)与具有羟基的第二组分(B)(OH-组分)接触形成聚胺酯粘着剂后,通过化学反应开始固化。通常,组分(B)中存在的羟基与组分(A)中存在的异氰酸酯基反应。作为上述反应的结果,聚胺酯粘着剂固化形成固体材料,继而使两个衬底接合在一起。该固化过程也称为交联。
两个衬底可以由相同或不同的材料组成。可以在上述方法中使用的合适衬底可以包含例如织造和非织造织物、金属箔、聚合物及金属涂覆的聚合物。膜任选地具有用墨水印有影像的表面;并且墨水可与粘着剂组合物接触。在一些实施例中,膜是聚合物膜和金属箔。在一个优选实施例中,尼龙膜与铝箔的组合可以用作待接合在一起的两个衬底。
本发明的2K聚胺酯粘着剂可以用于例如以下应用中:用于制造LIB包装的LIB应用;以及其它各种包装应用,例如食品包装应用,例如罐或容器、包装袋、包装托盘等。
在一个优选实施例中,可以根据本发明制造LIB包装膜材料。举例来说,参看图1,展示一种大体由元件符号10指示的层压膜结构,其包含三个衬底膜层11、12和13,所述三个层通过第一外层侧粘着剂14和第二内层侧粘着剂15接合在一起。在第一步骤中,可通过使用根据本发明的外层侧聚胺酯粘着剂14使外层侧树脂膜层11与金属箔层12层压于彼此上以形成第一中间层压物。接着,在第二步骤中,可通过使用内层侧粘着剂15使内表面层13层压于中间层压物的金属箔层12表面上。
替代地,在第一步骤中,可通过使用内层侧粘着剂15使金属箔层12与内表面层13层压于彼此上以形成第一中间层压物。接着,在第二步骤中,可通过使用根据本发明的聚胺酯粘着剂14将中间层压物的金属箔层12与外层侧树脂膜层11层压于彼此上。
实例
以下实例是为了进一步说明本发明而呈现,而不应解释为限制权利要求书的范围。除非另有说明,否则所有份数和百分数均以重量计。
本发明实例(Inv.Ex.)和比较实例(Comp.Ex.)中使用的各种原料描述于表I中:
表I-原料
再次参看图1,展示LIB包装层压膜的五层结构的示意性说明,其大体上由元件符号10指示。结构10的层包含尼龙衬底层11(厚度25微米[μ]);第一粘着层14,在本文中称为“粘着剂A”;铝衬底层12(厚度40μ);第二粘着层15,在本文中称为“粘着剂B”;以及蒸煮流延聚丙烯(RCPP)衬底层13(厚度20μ)。图1中所示的衬底还描述于表II中。
表II-衬底
表II注释:实验室评估之前,首先用“粘着剂B”将铝箔层与RCPP层层压在一起(称为预层压Al/RCPP)。所有本发明实例(Inv.Ex.)和比较实例(Comp.Ex.)施加于尼龙与铝箔表面之间作为外层压层“粘着剂A”。
合成磷酸酯多元醇的通用程序
根据表III中列出的配方合成本发明实例和比较实例中所用的磷酸酯多元醇。将原料化合物PA115和Bester 648装入1,000毫升(mL)玻璃反应器中且小心地混合以形成调配物。在所有上述原料馈入之后,开始加热调配物。当调配物温度达到60℃左右时,将转速提高至每分钟50转(RPM);并且控制升温速度,并且在整个过程中监测反应。在升温过程中,PA115与Bester 648分离;并且PA115在调配物底部浓缩。同时,PA115颜色也变深。当反应温度达到约100-103℃时,反应产物变得透明且均匀。反应产物在约100-103℃下保持2小时。当调配物的羟基值达到理论值时,将反应器尽快冷却。将反应器冷却至60℃-70℃。接着,在氮气氛围下将最终产物装入密封良好的钢瓶中,以防止调配物受到污染。
表III-磷酸酯多元醇PE112配方
配方 | Bester 648 | PA 115 |
磷酸酯多元醇 | 40 | 3 |
实例中使用的NCO组分及OH组分根据表IV中所述的配方合成。实例中使用的NCO组分是催化剂F。实例中使用的OH组分是高分子量聚酯多元醇、硅烷和磷酸酯的溶液,其均溶解于表IV所述的有机溶剂中。在原料装入反应器之前,将所有原料的水分含量设定为<百万分之500(ppm)。在合成过程中搅拌原料期间,使用氮气气氛来避免水分污染。
表IV-基于双组分溶剂的粘着剂配方
实例1-7和比较实例A-J
为了制备本发明实例和比较实例,根据表V中所示的配对(作为样品名称)及混合比将异氰酸酯组分与多元醇组分混合以形成实例的粘着剂组合物。接着使用实例的粘着剂组合物形成包括尼龙膜和预层压铝(Al)箔的层压物(即,Al箔/RCPP层压物)。
表V-样品和混合比
实例 | 样品名称 | 混合比 |
比较实例A | OH-1/NCO-1 | 100/5.5 |
比较实例B | OH-2/NCO-1 | 100/5.5 |
本发明实例1 | OH-3/NCO-1 | 100/5.5 |
本发明实例2 | OH-4/NCO-1 | 100/5.5 |
本发明实例3 | OH-5/NCO-1 | 100/5.5 |
本发明实例4 | OH-6/NCO-1 | 100/5.5 |
比较实例C | OH-7/NCO-1 | 100/5.5 |
本发明实例5 | OH-8/NCO-1 | 100/5.5 |
本发明实例6 | OH-9/NCO-1 | 100/5.5 |
本发明实例7 | OH-10/NCO-1 | 100/5.5 |
比较实例D | OH-11/NCO-1 | 100/5.5 |
比较实例E | Adcote 502S/NCO-1 | 100/6.5 |
比较实例F | Adcote 811A/NCO-1 | 100/10 |
比较实例G | OH-12/NCO-1 | 100/5.5 |
比较实例H | OH-13/NCO-1 | 100/5.5 |
比较实例I | OH-14/NCO-1 | 100/5.5 |
比较实例J | OH-15/NCO-1 | 100/5.5 |
涂布和层压方法的通用程序
实例中所用的涂布和层压方法是用购自Nordmeccanica集团的Labo-Combi400层压机执行。将粘着剂施加于尼龙膜上且接着将尼龙膜/粘着剂层压至预层压Al箔/RCPP的铝箔表面上。层压机的轧辊温度保持在70℃,并且层压过程期间的涂布速度是100米/分钟(m/min)。干燥涂层重量控制在每平方米4-4.5克(g/m2)。所得层压膜接着在烘箱中固化(例如在60℃的温度下),随后测试。
测试方法
在120℃下,尼龙与箔层之间发生T型剥离(90°)的接合强度(手助T型剥离)
固化之后,将层压膜切成15mm宽的测试条带样品,以便在Instron 5965U5974机器中使用250毫米/分钟(mm/min)的十字头速度进行T型剥离测试。接着在120℃温热烘箱中测试三个测试条带并且记录所述三个测试条带的平均值。在测试期间,用手指轻微牵拉条带的尾部以确保条带的尾部相对于剥离方向保持90°度。接合强度测试结果以N/15mm单位量度。为了通过此接合强度测试,层压膜的接合强度应>2N/15mm。
耐老化测试
将层压物(层压膜)切成4cm x 4cm尺寸的方形测试样品;且接着对样品进行抗老化测试。使样品在恒温潮湿箱LHU-213中、在85℃和85%相对空气湿度下老化60小时。在耐老化测试期间,选择一个层压膜的六个片段用于评估。使每片层压物与环境空气充分接触。在耐老化性测试之后,评估最终层压膜的外观。为了通过耐老化测试,在薄膜中不应观察到任何气泡。并且不应检测到层压膜发生分层。
深度拉伸测试(DDT)
将固化的层压膜切成8cm x 12cm尺寸的矩形测试样品;且接着将样品定位于自动深度拉伸设备SDCK-004A的平台上进行评估。所述设备使用深度拉伸应用的特定参数操作,将空气压力调节至0.5兆帕斯卡(MPa)且使模具维持100mm/min的冲压速度。对于测试的所有层压物来说,深度拉伸成型的深度设定为5mm。深度拉伸成型后,作为外层的层压物表面的尼龙一侧形成凸形表面。层压物中使用不同粘着剂。针对任何气泡、穿隧和/或分层,目视检查层压物在深度拉伸成型之后的外观。还检查层压物中的任何衬底断裂迹象。同时,还将冲压之后的层压物在温热烘箱中加热至100℃维持1小时,且接着针对如上文所述的缺陷,再次目视检查层压物的外观。
一般来说,深度拉伸测试之后就层压物中的箔断裂来说不合格的LIB层压物包装膜不能通过对于消费者使用来说充分的品质测试;并且深度拉伸测试之后就层压物中的尼龙/箔层压复合膜分层来说不合格的LIB层压物包装膜也不能通过对于消费者使用来说充分的品质测试。
表VI:性能结果
表VI中所概述的性能结果表明,使用一定量的磷酸酯多元醇(例如0.3%至2%)能够显著地改良尼龙/箔层压物在120℃温度下的接合强度;并且能够显著地改良尼龙/箔/RCPP层压物深度拉伸的性能,包含(a)层压物深度拉伸测试和(b)通过双组分粘着剂制得的层压物的100℃老化测试之后的层压物外观。
本发明的其它示例性实施例还可包含以下:
(1)一种聚胺酯粘着剂组合物,其包含:(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及(B)至少一种多元醇组分,其中所述至少一种多元醇组分(B)包含:(Bi)分子量(Mn)>8,000g/mol的至少一种聚酯多元醇化合物;和(Bii)至少一种磷酸酯多元醇化合物。
(2)上述实施例(1)的组合物,进一步包含溶剂。
(3)上述实施例(1)的组合物,其中组分(B)对组分(A)的浓度比[B:A]以干重计是1至20。
(4)上述实施例(1)的组合物,其中所述聚胺酯粘着剂组合物:(i)在120℃下,就尼龙/箔层压物来说具有1N/15mm至8N/15mm的接合强度;(ii)在85℃和85%湿度下经历>60个小时的老化时间,且/或(iii)具有足以提供1毫米至15毫米的深度拉伸设定深度的可塑性。
(5)上述实施例(1)的组合物,其中至少一种聚酯多元醇化合物衍生自二羧酸,包括壬二酸、癸二酸、己二酸、对苯二甲酸、间苯二甲酸和其混合物。
(6)上述实施例(1)的组合物,其中至少一种磷酸酯多元醇化合物是聚磷酸与多元醇之反应产物,其中所述多元醇选自聚醚多元醇、聚酯多元醇,以及两种或更多种多元醇之组合。
(7)上述实施例(1)的组合物,其中至少一种磷酸酯多元醇化合物组分(组分(Bii))是具有以下结构(I)或结构(II)的化合物:
其中在上述结构(I)及结构(II)中,R'可选自有机基团。
(8)上述实施例(7)的组合物,其中所述R'可以是烷基部分或烷基化烷基部分。
(9)上述实施例(1)的组合物,其中至少一种磷酸酯多元醇化合物(组分(Bii))是聚酯多元醇与聚磷酸之反应产物。
(10)上述实施例(1)的组合物,进一步包含组分(C);其中(C)可以是至少一种环氧树脂、至少一种硅烷或其混合物。
(11)一种制备聚胺酯粘着剂组合物的方法,包含混合:(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及(B)至少一种多元醇组分,包含:(Bi)至少一种聚酯多元醇化合物;和(Bii)至少一种磷酸酯多元醇化合物。
(12)一种使至少一第一衬底与至少一第二衬底粘着的方法,包含:(I)使至少第一衬底的一个表面的至少一部分或至少第二衬底的一个表面的至少一部分与上述实施例(1)的粘着剂组合物接触;以及(II)将步骤(I)的经组合的第一衬底、第二衬底和粘着剂加热至足以使粘着剂组合物固化的温度。
(13)上述实施例(12)的方法,其中所述加热步骤(II)在25℃至80℃的温度下进行。
(14)一种多层复合膜结构,其通过使用上述实施例(12)的方法制得。
(15)一种包装制品,其包含上述实施例(14)的多层复合膜结构。
(16)上述实施例(15)的制品,其包含锂离子电池。
Claims (10)
1.一种聚胺酯粘着剂组合物,其包括:
(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及
(B)至少一种多元醇组分,包含:
(Bi)至少一种聚酯多元醇化合物,其具有大于8,000克/摩尔的分子量(Mn);和
(Bii)至少一种磷酸酯多元醇化合物。
2.根据权利要求1所述的组合物,其中组分(B)对组分(A)的浓度比[B:A]以干重计是1至20。
3.根据权利要求1所述的组合物,其中所述聚胺酯粘着剂组合物:(i)具有1N/15mm至8N/15mm的接合强度;(ii)在85℃及85%湿度下经历>60个小时的老化时间,且/或(iii)具有足以提供1毫米至15毫米的深度拉伸设定深度的可塑性。
5.根据权利要求1所述的组合物,其中所述至少一种磷酸酯多元醇化合物,组分(Bii),是(a)聚醚多元醇、聚酯多元醇或其混合物与(b)聚磷酸或聚磷酸和其它酸的混合物的反应产物。
6.一种制备聚胺酯粘着剂组合物的方法,其包括混合:
(A)至少一种含有异氰酸酯基的组分,包含至少一种含有异氰酸酯基的化合物;以及
(B)至少一种多元醇组分,包含:
(Bi)至少一种聚酯多元醇化合物;和
(Bii)至少一种磷酸酯多元醇化合物。
7.一种用于使至少第一衬底与至少第二衬底粘着的方法,其包括:
(I)使所述至少第一衬底的一个表面的至少一部分或所述至少第二衬底的一个表面的至少一部分与根据权利要求1所述的粘着剂组合物接触;以及
(II)将步骤(I)的经组合的所述第一衬底、第二衬底和粘着剂加热至足以使所述粘着剂组合物固化的温度。
8.根据权利要求7所述的方法,其中所述加热步骤(II)在25℃至80℃的温度下进行。
9.一种多层复合物层压膜结构,其利用根据权利要求8所述的方法制得。
10.一种用于包装锂离子电池的包装,其包括箔基层压结构,其中所述箔基层压结构包含以下各项的组合:(a)尼龙层、(b)箔层、(c)聚合物衬底层;(d)包括根据权利要求1所述的组合物的第一上部粘着剂层,其安置于所述尼龙层的一侧与所述箔层的一侧之间;以及(e)不同于根据权利要求1所述的组合物的第二下部粘着剂层,其安置于所述箔层的另一侧与所述聚合物衬底层的一侧之间。
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CN107709394A (zh) * | 2015-06-18 | 2018-02-16 | 陶氏环球技术有限责任公司 | 潜伏型两部分型聚氨基甲酸酯粘合剂 |
JP2017152349A (ja) * | 2016-02-26 | 2017-08-31 | 東洋インキScホールディングス株式会社 | 電池用包装材、電池用容器および電池 |
WO2018049672A1 (en) * | 2016-09-19 | 2018-03-22 | Dow Global Technologies Llc | Two-component solventless adhesive compositions and methods of making same |
WO2018140116A1 (en) * | 2017-01-27 | 2018-08-02 | Dow Global Technologies Llc | Two-component solventless adhesive compositions |
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TW202020091A (zh) | 2020-06-01 |
JP7404364B2 (ja) | 2023-12-25 |
JP2022519151A (ja) | 2022-03-22 |
MX2021006018A (es) | 2021-07-21 |
WO2020103072A1 (en) | 2020-05-28 |
BR112021009932A2 (pt) | 2021-08-17 |
US20240240068A1 (en) | 2024-07-18 |
AR117109A1 (es) | 2021-07-14 |
EP3884009A1 (en) | 2021-09-29 |
EP3884009A4 (en) | 2022-06-08 |
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