TWI834639B - 基於磷酸酯改質異氰酸酯之雙組分黏合劑組合物及其製造方法 - Google Patents
基於磷酸酯改質異氰酸酯之雙組分黏合劑組合物及其製造方法 Download PDFInfo
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- TWI834639B TWI834639B TW108107402A TW108107402A TWI834639B TW I834639 B TWI834639 B TW I834639B TW 108107402 A TW108107402 A TW 108107402A TW 108107402 A TW108107402 A TW 108107402A TW I834639 B TWI834639 B TW I834639B
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- Prior art keywords
- isocyanate
- component
- substrate
- adhesive composition
- polyol
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 133
- 239000000853 adhesive Substances 0.000 title claims abstract description 110
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 109
- 239000012948 isocyanate Substances 0.000 title claims abstract description 98
- 150000002513 isocyanates Chemical class 0.000 title claims abstract description 91
- -1 phosphate ester Chemical class 0.000 title claims abstract description 57
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 46
- 239000010452 phosphate Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 26
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- 150000003077 polyols Chemical class 0.000 claims abstract description 34
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
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- FPWRWTXOOZSCTB-UHFFFAOYSA-N 1-isocyanato-2-[(4-isocyanatocyclohexyl)methyl]cyclohexane Chemical compound C1CC(N=C=O)CCC1CC1C(N=C=O)CCCC1 FPWRWTXOOZSCTB-UHFFFAOYSA-N 0.000 description 1
- LFSYUSUFCBOHGU-UHFFFAOYSA-N 1-isocyanato-2-[(4-isocyanatophenyl)methyl]benzene Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=CC=C1N=C=O LFSYUSUFCBOHGU-UHFFFAOYSA-N 0.000 description 1
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
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- 239000006087 Silane Coupling Agent Substances 0.000 description 1
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
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- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- STBLQDMGPBQTMI-UHFFFAOYSA-N heptane;isocyanic acid Chemical compound N=C=O.N=C=O.CCCCCCC STBLQDMGPBQTMI-UHFFFAOYSA-N 0.000 description 1
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- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
- B32B15/12—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 paper or cardboard
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/10—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of paper or cardboard
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B32B29/00—Layered products comprising a layer of paper or cardboard
- B32B29/002—Layered products comprising a layer of paper or cardboard as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本發明之黏合劑組合物包括(A)異氰酸酯組分,其包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯與包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物。本發明之黏合劑組合物進一步包括(B)包括多元醇之異氰酸酯反應性組分多元醇組分。在一些實施例中,揭示了用於製備雙組分黏合劑調配物之方法,其包括藉由使聚異氰酸酯與包括磷酸酯多元醇的異氰酸酯反應性混合物反應來製備包括異氰酸酯封端之預聚物的異氰酸酯組分及製備包括多元醇之異氰酸酯反應性組分。所述方法進一步包括以約1.0至約5.0之化學計量比(NCO/OH)混合所述異氰酸酯組分及所述異氰酸酯反應性組分。亦揭示了形成層壓結構之方法及所述層壓結構本身。
Description
本發明係關於雙組分黏合劑組合物。黏合劑組合物包括(A)異氰酸酯組分及(B)異氰酸酯反應性組分,其中異氰酸酯組分(A)基於磷酸酯多元醇。黏合劑組合物適合與傳統的層壓技術(即,在施加到基板之前預混合兩種組分)及相對較新的層壓技術(即,較高反應性之系統,其中在將基板集合在一起以混合組分之前將各組分施加到單獨的基板上)一起使用。此外,黏合劑組合物可以為無溶劑的或基於溶劑的。本發明之黏合劑組合物顯示出改進之黏合強度、耐溫性及耐化學性,同時保持延長的使用壽命,並且可用於食品包裝、藥物包裝及工業層壓。
黏合劑組合物適用於多種目的。例如,黏合劑組合物用於將基板黏合在一起以形成複合膜,即層壓材料,所述基板諸如聚乙烯、聚丙烯、聚酯、聚醯胺、金屬、金屬化物、紙或塞璐芬(cellophane)。此等類型之黏合劑通常稱為「層壓黏合劑」。
一種特定種類之層壓黏合劑包含雙組分基於聚胺甲酸酯之黏合
劑。通常,雙組分基於聚胺甲酸酯之層壓黏合劑包含:異氰酸酯組分,其包括含異氰酸酯之預聚物及/或聚異氰酸酯;及異氰酸酯反應性組分,其包括多元醇。預聚物可藉由使過量異氰酸酯與每分子含有兩個或兩個以上羥基之聚醚及/或聚酯反應而獲得。異氰酸酯反應性組分包括每分子用兩個或兩個以上羥基引發之聚醚及/或聚酯。這兩種組分通常以預定比率組合,或「預混合」,且隨後施加到第一基板(「載體幅材」)之表面上。隨後,將第一基板之表面與第二基板之表面集合在一起以形成層壓結構。最近,已經開發出較快固化之雙組分系統,其中將各組分單獨施加到基板之表面上。然後將各基板之表面集合在一起,使得兩種組分混合,藉此形成層壓結構。可將另外基板層添加到層壓結構中,其中另外的黏合劑組合物層位於各連續基板之間。隨後,在室溫或高溫下固化黏合劑,藉此使基板黏合在一起。
此類層壓黏合劑可廣泛用於製造包裝工業中使用之膜/膜及膜/箔層壓材料,特別用於食品包裝、藥物包裝及工業層壓,其中通常在高溫下曝露於腐蝕性化學品。為改進黏合劑之耐溫性及耐化學性,有時使用黏合促進劑,諸如矽烷偶聯劑、鈦酸酯偶聯劑、鋁酸鹽偶聯劑,以及環氧樹脂、磷酸及磷酸酯。這些黏合促進劑各有優點及缺點。
最近,磷酸酯多元醇已經用於層壓黏合劑組合物以改進耐溫性及耐化學性,特別在金屬層壓結構中,諸如基於箔及金屬化膜之層壓結構中。磷酸酯多元醇通常以小於異氰酸酯反應性組分之15重量%摻入異氰酸酯反應性組分中。然而,磷酸酯多元醇之添加加速了異氰酸酯組分及異氰酸酯反應性組分之間的反應,因此縮短了使用壽命。縮短之使用壽命會影響層壓材料之品質及一致性,並且在維護及清潔方面產生潛在的困難。結果,具有延長之使用壽命(通常大於40分鐘)的黏合劑更有利。
因此,期望雙組分層壓黏合劑表現出改進之耐溫性及耐化學性,
同時保持延長的使用壽命。
因此,揭示了這種雙組分層壓黏合劑組合物及其製造方法。本發明之黏合劑組合物適合與傳統的層壓技術(即,預混合)及相對較新的層壓技術(即,較高的反應性系統)一起使用。此外,黏合劑組合物可以為無溶劑的或基於溶劑的。
在一些實施例中,本發明之黏合劑組合物包括(A)異氰酸酯組分,其包括異氰酸酯封端之預聚物,所述預聚物為以下之反應產物:聚異氰酸酯及包括磷酸酯多元醇之異氰酸酯反應性混合物。本發明之黏合劑組合物進一步包括(B)異氰酸酯反應性組分多元醇組分,其包括多元醇。
在一些實施例中,揭示了用於製備雙組分黏合劑調配物之方法。在一些實施例中,所述方法包括藉由使聚異氰酸酯與包括磷酸酯多元醇之混合物反應來製備包括異氰酸酯封端之預聚物的異氰酸酯組分及製備包括多元醇的異氰酸酯反應性組分。所述方法進一步包括以約1.0至約5.0之化學計量比(NCO/OH)混合異氰酸酯組分及異氰酸酯反應性組分。
在一些實施例中,揭示了用於形成層壓結構之方法。在一些實施例中,所述方法包括將以約1.0至約5.0之化學計量比(NCO/OH)混合異氰酸酯組分及異氰酸酯反應性組分以形成雙組分黏合劑組合物,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物。所述方法進一步包括將黏合劑組合物施加到第一基板之表面上,使第一基板之表面與第二基板之表面接觸,並固化黏合劑組合物以將第一基板黏合到第二基板上。在其他實施例中,所述方法包括將異氰
酸酯組分均勻地施加到第一基板之表面上,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物,將異氰酸酯反應性組分均勻地施加到第二基板之表面上,使第一基板及第二基板集合一起,藉此使異氰酸酯組分與多元醇組分混合並反應,以在第一基板與第二基板之間形成黏合劑組合物,並固化黏合劑組合物以將第一基板與第二基板黏合。
雙組分黏合劑組合物中的其他視情況選用之組分包含但不限於界面活性劑、流平劑、消泡劑、流變改質劑、有色顏料、黏合促進劑(例如,磷酸酯及環氧樹脂)及其類似物及其任何組合。
此外,可將溶劑諸如乙酸乙酯、甲基乙基酮、甲苯及其組合摻入本發明之雙組分黏合劑組合物中以形成基於溶劑之黏合劑。
本文亦揭示了包括本發明之雙組分黏合劑組合物之層壓結構。
如上所述,根據本發明之雙組分黏合劑組合物包括異氰酸酯組分及異氰酸酯反應性組分。
異氰酸酯組分
在一些實施例中,異氰酸酯組分包括異氰酸酯封端之預聚物。在一些實施例中,異氰酸酯封端之預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物。
在一些實施方案中,異氰酸酯組分包括異氰酸酯封端之預聚物及選自由以下組成之群之異氰酸酯:芳族異氰酸酯、脂族異氰酸酯、環脂族異氰酸酯及其組合。
合適之芳族異氰酸酯包含但不限於1,3-及1,4-伸苯基二異氰酸酯、1,5-伸萘基二異氰酸酯、2,6-甲苯二異氰酸酯、2,4-甲苯二異氰酸酯(2,4-TDI)、2,4'-二苯基甲烷二異氰酸酯(2,4'-MDI)、4,4'-二苯基甲烷二異氰酸酯、聚合異氰酸酯及其組合。
合適之脂族聚異氰酸酯在直鏈或支鏈伸烷基殘基中有利地具有3至16個碳原子,較佳4至12個碳原子,並且合適之環脂族或環脂族二異氰酸酯在伸環烷基殘基中有利地具有4至18個碳原子,較佳6至15個碳原子。本領域中熟習此項技術者充分理解環脂族二異氰酸酯同時意指環及脂族鍵結NCO基團,諸如異佛爾酮二異氰酸酯。與此相反,環脂族二異氰酸酯應理解為意指僅具有直接鍵結到環脂族環上之NCO基團之彼等,例如H12MDI。
合適之脂族及環脂族異氰酸酯包含環己烷二異氰酸酯、甲基環己烷二異氰酸酯、乙基環己烷二異氰酸酯、丙基環己烷二異氰酸酯、甲基二乙基環己烷二異氰酸酯、丙烷二異氰酸酯、丁烷二異氰酸酯、戊烷二異氰酸酯、己烷二異氰酸酯、庚烷二異氰酸酯、辛烷二異氰酸酯、壬烷二異氰酸酯、壬烷三異氰酸酯(諸如4-異氰酸酯基甲基-1,8-辛烷二異氰酸酯(TIN))、癸烷二異氰酸酯及癸烷三異氰酸酯、十一烷二異氰酸酯及十一烷三異氰酸酯及十二烷二異氰酸酯及十二烷三異氰酸酯、異佛酮二異氰酸酯(IPDI)、二異氰酸六亞甲酯(HDI)、二異氰酸基二環己基甲烷(H12MDI)、2-甲基戊烷二異氰酸酯(MPDI)、2,2,4-三甲基六亞甲酯二異氰酸/2,4,4-三甲基六亞甲酯二異氰酸(TMDI)、降冰片烷二異氰酸酯(NBDI)、苯二甲二異氰酸酯(XDI)、四甲基二甲苯二異氰酸酯及二聚體、三聚體及其組合。
根據本發明,另外異氰酸酯,諸如4-甲基-環己烷1,3-二異氰酸酯、2-丁基-2-乙基伸戊酯二異氰酸、3(4)-異氰酸酯基甲基-1-甲基環己酯異氰酸酯、2-異氰酸酯基丙基環己基異氰酸酯、2,4'-亞甲基雙(環己基)二異氰酸酯及1,4-二異
氰酸-4-甲基-戊烷亦適用。
用於產生異氰酸酯封端之預聚物之磷酸酯多元醇可經由羥基封端之化合物與磷酸或聚磷酸的反應來製造。合適之羥基封端之化合物包含聚酯多元醇、聚己內酯多元醇、聚醚多元醇、聚碳酸酯多元醇、基於天然油之多元醇及其混合物與共聚物。羥基封端之化合物之平均OH值可以為5至2,000mg KOH/g,或14至850mg KOH/g,或56至500mg KOH/g,或110至450。羥基封端之化合物之平均官能度可以為1.0至6.0,或1.8至4.0,或2.0至4.0。羥基封端之化合物之平均分子量可以為25至12,000g/mol,或250至6,000g/mol,或350至3,000g/mol。在一些實施例中,磷酸酯多元醇可以經由羥基封端之化合物、磷酸或聚磷酸及諸如甲基二苯基二異氰酸酯之聚異氰酸酯之反應來製造。
如所討論,合適之異氰酸酯封端之預聚物為化學計量比(NCO/OH)大於1,或在2與6之間,或在2.5與4.0之間的聚異氰酸酯及異氰酸酯反應性混合物之反應產物。聚異氰酸酯選自芳族異氰酸酯、脂族異氰酸酯及環脂族異氰酸酯。異氰酸酯反應性混合物包括以異氰酸酯反應性混合物重量計之至少1%之磷酸酯多元醇,或2%至25%之磷酸酯多元醇,或以異氰酸酯反應性混合物之重量計之4%至10%之磷酸酯多元醇。
(B)異氰酸酯反應性組分
在一些實施例中,異氰酸酯反應性組分包括羥基封端之化合物。在一些實施例中,異氰酸酯反應性組分包括選自由以下組成之群之羥基封端之化合物:聚酯多元醇、聚己內酯多元醇、聚醚多元醇、聚碳酸酯多元醇、基於天然油之多元醇及其組合。
羥基封端之化合物之平均OH值可以為5至2,000mg KOH/g,或14至850mg KOH/g,或56至500mg KOH/g,或110至450。羥基封端之化合物之平均官能度可以為2.0至6.0,或2.0至4.0,或2.0至3.0。羥基封端之化合
物之平均分子量可以為25至12,000g/mol,或250至6,000g/mol,或350至3,000g/mol。此外,低分子量聚二醇,諸如乙二醇、二甘醇、三羥甲基丙烷、二丙二醇、三丙二醇及三異丙醇胺亦可以包含在異氰酸酯反應性組分中。
層壓
預期分別調配本發明無溶劑黏合劑組合物之異氰酸酯組分及多元醇組分且儲存直至期望形成層壓結構。較佳地,異氰酸酯組分及多元醇組分在25℃下呈液態。即使組分在25℃下為固體,但可接受視需要加熱組分以使其呈液態。可以根據各種方法形成包括本發明之黏合劑組合物的層壓結構。
在一些實施例中,層壓結構可以藉由在將混合之組合物施加到基板之前預混合異氰酸酯及異氰酸酯反應性組分來形成。此類方法包括將異氰酸酯組分及異氰酸酯反應性組分以約1.0至約5.0之化學計量比(NCO/OH)混合以形成雙組分黏合劑組合物,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物。所述方法進一步包括將黏合劑組合物施加到第一基板之表面上,使第一基板之表面與第二基板之表面接觸,並固化黏合劑組合物以將第一基板黏合到第二基板上。
在其他實施例中,層壓結構可以用相對較新之層壓技術(即,較高反應性之系統,其中在將基板集合在一起以混合組分之前將各組分施加到單獨的基板上)形成。此類方法包括將異氰酸酯組分均勻地施加到第一基板之表面上,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物;將異氰酸酯反應性組分均勻地施加到第二基板之表面上。較佳地,各基板上之各組分之層的厚度為0.5μm至2.5μm。藉由控制施加到各基板之層的厚度,組分之比率可得到控制。所述方法進一步包括將第一基板及第二基板集合在一起,藉此使異氰酸酯組分
及多元醇組分混合並反應,以在第一基板及第二基板之間形成黏合劑組合物,並固化黏合劑組合物以將第一基板及第二基板黏合。當使第一與第二基板集合在一起且使組分彼此接觸時,異氰酸酯組分與異氰酸酯反應性組分開始混合且反應。此標誌著固化製程之開始。當第一及第二基板穿過各種其他輥且最終到達重繞輥時,實現進一步混合及反應。因為基板各自比穿過各輥之其他基板採取更長或更短路徑,所以進一步混合及反應在第一及第二基板穿過輥時進行。以此方式,兩個基板相對於彼此移動,使各別基板上的組分混合。可固化混合物隨後固化或使其固化。
在一些實施例中,溶劑(諸如乙酸乙酯、甲基乙基酮、甲苯及其組合)可以摻入本發明之雙組分黏合劑組合物中以形成基於溶劑之黏合劑。
在一些實施例中,添加劑可視情況包含於黏合劑組合物中。此類添加劑之實例包含但不限於界面活性劑、流平劑、消泡劑、流變改質劑、有色顏料、黏合促進劑(例如,磷酸酯及環氧樹脂)及其類似物及其組合。
層壓結構中合適之基板包含膜,諸如紙、織造及非織造織物、聚合物膜、金屬箔及金屬塗層(金屬化)之聚合物膜。一些膜視情況具有上面用墨水打印影像之表面,所述墨水可與黏合劑組合物接觸。基板被分層以形成層壓結構,其中根據本發明之黏合劑組合物將基板中之一或多者黏合在一起。
現將藉由描述說明本發明黏合劑組合物及現有黏合劑組合物之實例(說明性實例「IE」、比較實例「CE」,統稱為「實例」)來進一步詳細解釋本發明。然而,本發明之範疇當然不限於所述實例。
使用表1中識別之原材料製備實例。
黏合強度量測
對切成15mm寬條帶且在配備有50N測力計之Thwing AlbertTM QC-3A剝離測試儀上以4吋/分鐘之速率對1吋條帶進行牽拉的層壓樣品進行90° T-剝離測試。當層壓材料中之兩個膜分離(剝離)時,記錄牽拉期間的力之平均值。若膜中之一者拉伸或斷裂,則記錄最大力或斷裂時的力。本文中之值為三個分離樣品條帶之平均值。失效模式(FM)或失效之模式(MOF)記錄如下:「FS」表示膜拉伸;「FT」表示膜撕裂或斷裂;「DL」表示分層(次級膜與初級膜分離);「AT」表示黏合劑轉移(黏合劑不能黏附到初級膜並轉移到次級膜);「AS」表示黏合劑裂開或黏合失效(黏合劑存在於初級膜及次級膜兩者上);「MT」表示金屬從金屬化膜轉移到第二膜;「PMT」表示部分金屬轉移。製成層壓材料後,儘快測試初始或「濕」黏合。另外之T-剝離測試在指定之時間間隔進行,通
常在1天及7天後進行。
袋中煮沸(Boil-in-Bag)測試程序
層壓材料由Prelam Al及GF-19或GF-10製成。將9"×12"(23cm×30.5cm)層壓板中之一個摺疊,得到約9"×6"(23cm×15.25cm)之雙層,使得一層的PE膜與另一層的PE膜接觸。在切紙機上修剪邊緣,得到約5"×7"(12.7cm×17.8cm)之摺疊片。兩個長邊及一個短邊在邊緣處熱封,得到內部尺寸為4"×6"(10.2cm×15.2cm)之成品小袋。熱封在177℃(350℉)下在276kpa(40PSI)之液壓下進行1秒。各測試製造兩個或三個小袋。
小袋經由開口邊緣用100±5ml之1:1:1調味汁(等重量份之番茄醬、醋及植物油之共混物)填充。避免將填充物濺到熱封區域,因為這可能導致熱封在測試期間失效。在填充之後,將小袋之頂部以最小化小袋內空氣滯留的方式密封。
在小袋之所有四個側面上檢查密封完整性以確保在密封中沒有會導致小袋在測試期間洩漏的缺陷。丟棄並更換任何可疑小袋。在一些情況下,標記層壓材料中的缺陷以識別在測試期間是否產生新的另外缺陷。
鍋中裝滿三分之二之水使其並滾沸。沸騰之鍋蓋上蓋子,以最小化水及蒸汽損失。在測試期間觀察鍋以確保存在足夠之水以維持沸騰。將小袋置於沸水中並保持30分鐘。移除小袋並將隧道、起泡、分層或洩漏之程度與經標記之先前存在的缺陷中之任一者進行比較。記錄觀察結果。將小袋切開,倒空,並用肥皂及水沖洗。從小袋中切出一個或多個1"(2.54cm)條帶,並且根據前述標準黏合強度測試,以10吋/分鐘量測層壓材料黏合強度。其在取出小袋內容物後儘快完成。檢查小袋的內部並記錄任何其他視覺缺陷。
化學老化試驗程序
層壓材料由上述Prelam Al/GF-19及92 LBT/GF-19製成。將9"×12"
(23cm×30.5cm)層壓板中之一個摺疊,得到約9"×6"(23cm×15.25cm)的雙層,使得一層的PE膜與另一層的PE膜接觸。在切紙機上修剪邊緣,得到約5"×7"(12.7cm×17.8cm)的摺疊片。兩個長邊及一個短邊在邊緣處熱封,得到內部尺寸為4"×6"(10.2cm×15.2cm)的成品小袋。熱封在177℃(350℉)下在276kpa(40PSI)之液壓下進行1秒。各測試製造兩個或三個小袋。
小袋經由開口邊緣用100±5ml之1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充。避免將填充物濺到熱封區域,因為這可能導致熱封在測試期間失效。在填充之後,將小袋之頂部以最小化小袋內空氣滯留的方式密封。
在小袋之所有四個側面上檢查密封完整性以確保在密封中沒有會導致小袋在測試期間洩漏的缺陷。丟棄並更換任何可疑小袋。在一些情況下,標記層壓材料中的缺陷以識別在測試期間是否產生新的另外缺陷。
然後將含有1:1:1調味汁之小袋放置在設定為50℃(122。℉)之對流烘箱中持續100小時。在老化之後移除小袋並將隧道、起泡、分層或洩漏之程度與經標記之先前存在的缺陷中之任一者進行比較。記錄觀察結果。將小袋切開,倒空,並用肥皂及水沖洗。從小袋中切出一個或多個1"(2.54cm)條帶,並且根據上述標準黏合強度測試量測層壓材料黏合強度。其在取出小袋內容物後儘快完成。檢查小袋的內部並記錄任何其他視覺缺陷。
使用壽命量測
藉由Brookfield DV-II黏度計在給定溫度下測定無溶劑黏合劑之使用壽命。黏合劑在給定溫度下之使用壽命定義為黏合劑在所述溫度下達到4,000cps所需之時間,並在Brookfield DV-II黏度計上量測。
基於溶劑之黏合劑之使用壽命藉由使用#2 Zahn Cup在室溫下量測黏合劑的黏度來測定。黏合劑在室溫下之使用壽命定義為當藉由#2 Zahn Cup
量測時黏合劑達到黏度所花費之時間,液體從杯中完全排出將花費超過25秒。
表2顯示了由異氰酸酯組分及異氰酸酯反應性組分分解之所選實例的詳細組成。
在所有實施例中,異氰酸酯組分與異氰酸酯反應性組分之化學計量比保持在1.25。
說明性實例1(「IE1」)
使用由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器來產生磷酸酯多元醇。在N2吹掃下,首先將98.1公克VORANOLTM CP 450裝載到反應器中。在攪拌下,將1.9公克聚磷酸逐滴添加到反應器中。在
室溫下混合30分鐘後,將反應器溫度升至100℃。在100℃下1小時後,將反應產物冷卻至室溫以用於製備異氰酸酯組分。
異氰酸酯組分:在另一個實驗室玻璃反應器中,首先裝載129.23公克在45℃下預熔的ISONATETM 125M。將反應器之溫度設定為50℃。在攪拌下,將264.04公克ISONATETM 143L裝入反應器中。混合10分鐘後,將51.16公克來自步驟1之基於VORANOLTM CP 450之磷酸酯多元醇裝入反應器中。若溫度超過75℃,則施加冷卻。在將反應器溫度冷卻至50℃至60℃之間之後,將113.49公克VORANOLTM 220-260添加到反應器中。將反應在75℃再保持2小時,然後添加98.07公克乙酸乙酯。在75℃再混合0.5小時後,獲得澄清低黏度預聚物。發現預聚物具有12.4%之NCO含量及84%之固體含量。
異氰酸酯反應性組分:使用由配備有機械攪拌之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器來產生異氰酸酯反應性組分。將反應器之溫度設定在65℃。在N2吹掃及攪拌下,將518.24公克中間體88X102裝入反應器中,然後添加0.98公克磷酸、8.2公克在65℃下預熔的TMP、984.0公克ADCOTETM 86-116及137.76公克乙酸乙酯。然後將反應器之溫度升至70℃。在70℃下混合45分鐘後,獲得澄清低黏度液體。發現混合物具有76.9%之固體含量、41之OH值及890cps之室溫黏度。
層壓:1649.2公克異氰酸酯反應性組分、656公克異氰酸酯組分及1346.5公克乙酸乙酯以獲得50%固體溶液。然後將所述溶液以1.7磅/令之塗層重量施加到Prelam Al上,然後使用Nordmeccanica LABO COMBITM中試層壓機將其與高助滑LLDPE膜(GF-19)層壓。將相同之黏合劑以1.78磅/令之塗層重量施加到92LBT上,然後將其與GF-19層壓。PE及箔之間之黏合強度在層壓後立即量測,並且在層壓後間隔1天、7天及14天量測。7天後,使用層壓結構製造小袋,並用1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充,
用於袋中煮沸及熱老化測試。黏合強度及失效模式之結果總結在表3中。
比較實例1(「CE1」)
異氰酸酯組分:使用由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器來產生異氰酸酯組分。首先裝載129.23公克在45℃下預熔的ISONATETM 125M。將反應器之溫度設定為50℃。在攪拌下,將264.04公克ISONATETM 143L裝入反應器中。混合10分鐘後,將51.16公克VORANOLTM CP 450裝入反應器中。若溫度超過75℃,則施加冷卻。在將反應器溫度冷卻至50℃至60℃之間之後,將113.49公克VORANOLTM 220-260添加到反應器中。將反應在75℃再保持2小時,然後添加98.07公克乙酸乙酯。在75℃下再混合0.5小時後,獲得澄清低黏度預聚物。發現預聚物具有12.5%之NCO含量及84%之固體含量。
異氰酸酯反應性組分:使用由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器來產生異氰酸酯反應性組分。將反應器之溫度設定在65℃。在N2吹掃及攪拌下,將518.24公克中間體88X102裝入反應器中,然後添加0.98公克磷酸、8.2公克在65℃下預熔的TMP、984.0公克ADCOTETM 86-116及137.76公克乙酸乙酯。然後將反應器之溫度升至70℃。在70℃下混合45分鐘後,獲得澄清低黏度液體。發現混合物具有76.9%之固體含量、41之OH值及890cps之室溫黏度。
層壓:1649.2公克異氰酸酯反應性組分、656公克異氰酸酯組分及1346.5公克乙酸乙酯以獲得50%固體溶液。然後將所述溶液以1.75磅/令之塗層重量施加到Prelam Al上,然後使用Nordmeccanica LABO COMBITM中試層壓機將其與高助滑LLDPE膜(GF-19)層壓。將相同之黏合劑以1.82磅/令之塗層重量施加到92LBT上,然後將其與GF-19層壓。PE及箔之間之黏合強度在層壓後立即量測,且在層壓後間隔1天、7天及14天量測。7天後,使用層壓結構製
造小袋,並用1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充,用於袋中煮沸及熱老化測試。黏合強度及失效模式之結果總結在表3中。
說明性實例2(「IE2」)
異氰酸酯組分:如IE1中所示,98.1公克VORANOLTM CP 755與1.9公克聚磷酸反應形成磷酸酯多元醇。磷酸酯多元醇用於合成異氰酸酯組分。
向由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器中裝入在45℃下預熔融的61.30公克ISONATETM 125M。將反應器之溫度設定為50℃。在攪拌下,將24.90公克MOR-FREETM 218裝入反應器中,然後添加46.66公克ADCOTETM x111-43及6.22公克磷酸酯多元醇。若溫度超過75℃,則施加冷卻。在80℃下反應4小時後,將13.91公克ISONATETM 143L添加到反應器中。在80℃下再混合1小時後,獲得澄清低黏度預聚物。發現預聚物具有之13.9% NCO含量。
層壓:將100公克VORANOLTM CP 755與153公克異氰酸酯組分混合。然後將所述混合物以1.15磅/令之塗層重量施加到Prelam Al上,然後使用Nordmeccanica Labocombi中試層壓機將其與高助滑LLDPE膜(GF-19)層壓。將相同之黏合劑以1.15磅/令之塗層重量施加到92LBT上,然後將其與GF-19層壓PE及箔之間之黏合強度在層壓後立即量測,並且在層壓後間隔4小時、1天及7天量測。7天後,使用層壓結構製造小袋,並用1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充,用於袋中煮沸及熱老化測試。黏合強度及失效模式之結果總結在表3中。
說明性實例3(「IE3」)
異氰酸酯組分:如IE1中所示,98.1公克VORANOLTM CP 450與1.9公克聚磷酸反應形成磷酸酯多元醇。磷酸酯多元醇用於合成異氰酸酯組分。
向由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻
璃反應器中裝入在45℃下預熔融的63.88公克ISONATETM 125M。將反應器之溫度設定為50℃。在攪拌下,將24.06公克MOR-FREETM 218裝入反應器中,然後添加45.12公克ADCOTETM x111-43及6.02公克磷酸酯多元醇。若溫度超過75℃,則施加冷卻。在80℃下反應4小時後,將13.91公克ISONATETM 143L添加到反應器中。在80℃下再混合1小時後,獲得澄清低黏度預聚物。發現預聚物具有之13.9% NCO含量。
層壓:將100公克VORANOLTM CP 755與153公克異氰酸酯組分混合。然後將所述混合物以1.10磅/令之塗層重量施加到Prelam Al上,然後使用Nordmeccanica LABO COMBITM中試層壓機將其與高助滑LLDPE膜(GF-19)層壓。將相同之黏合劑以1.10磅/令之塗層重量施加到92LBT上,然後將其與GF-19層壓。PE及箔之間之黏合強度在層壓後立即量測,並且在層壓後間隔4小時、1天及7天量測。7天後,使用層壓結構製造小袋,並用1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充,用於袋中煮沸及熱老化測試。黏合強度及失效模式之結果總結在表3中。
比較實例2(「CE2」)
異氰酸酯組分:向由配備有機械攪拌器之4頸燒瓶及溫度控制器組成之實驗室玻璃反應器中裝入在45℃下預熔融的62.96公克ISONATETM 125M。將反應器之溫度設定為50℃。在攪拌下,將30.81公克MOR-FREETM 218裝入反應器中,然後添加46.23公克ADCOTETM x111-43。若溫度超過75℃,則施加冷卻。在80℃下反應4小時後,將14.00公克ISONATETM 143L添加到反應器中。在80℃下再混合1小時後,獲得澄清低黏度預聚物。發現預聚物具有之13.5% NCO含量。
層壓:將90公克VORANOLTM CP 755、10公克MOR-FREETM 88-138與153公克異氰酸酯組分混合。然後將所述混合物以1.10磅/令之塗層重量
施加到Prelam Al上,然後使用Nordmeccanica LABO COMBITM中試層壓機將其與高助滑LLDPE膜(GF-19)層壓。將相同之黏合劑以1.10磅/令之塗層重量施加到92LBT上,然後將其與GF-19層壓。PE及箔之間之黏合強度在層壓後立即量測,並且在層壓後間隔4小時、1天及7天量測。7天後,使用層壓結構製造小袋,並用1:1:1調味汁(等重量份之番茄醬、醋及植物油的共混物)填充,用於袋中煮沸及熱老化測試。黏合強度及失效模式之結果總結在表3中。
對於基於溶劑之黏合劑,與CE1相比,IE1顯示出顯著改進之黏合強度及改進之耐化學性及耐溫性。對於無溶劑黏合劑,雖然IE2及IE3具有更長之使用壽命(CE2之使用壽命的兩倍),但與基於含有磷酸酯多元醇的異氰酸酯反應性組分的CE2相比,說明性實例顯示類似的黏合堆積。此外,IE2及IE3亦顯示類似或更好之黏合強度以及耐化學性及耐溫性。
除了上文所描述之實施例之外,特定組合之許多實施例亦在本發明之範疇內,下文描述其中一些實施例:
實施例1.一種雙組分黏合劑組合物,其包括:(A)異氰酸酯組分,其包括異氰酸酯封端之預聚物,所述預聚物為以下之反應產物:
聚異氰酸酯;及包括磷酸酯多元醇之異氰酸酯反應性混合物;及(B)包括多元醇之異氰酸酯反應性組分。
實施例2.如前述或後續實施例中任一項所述之雙組分黏合劑組合物,其中聚異氰酸酯選自由以下組成之群:芳族異氰酸酯、脂族異氰酸酯、環脂族異氰酸酯及其組合。
實施例3.如前述或後續實施例中任一項所述之雙組分黏合劑組合物,其中磷酸酯多元醇為羥基封端之化合物與(聚)磷酸之反應產物。
實施例4.如前述或後續實施例中任一項所述之雙組分黏合劑組合物,其中磷酸酯多元醇為羥基封端之化合物、(聚)磷酸及另一聚異氰酸酯之反應產物。
實施例5.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物選自由以下組成之群:聚酯多元醇、聚己內酯多元醇、聚醚多元醇、聚碳酸酯多元醇、基於天然油之多元醇及其組合與共聚物。
實施例6.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有5至2,000mg KOH/g之平均OH值。
實施例7.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有14至850mg KOH/g之平均OH值。
實施案8.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有56至500mg KOH/g之平均OH值。
實施例9.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有1.0至6.0之平均官能度。
實施例10.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有1.8至4.0之平均官能度。
實施例11.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有2.0至4.0之平均官能度。
實施例12.如實施例3所述之雙組分黏合劑組合物,其中所述羥基封端之化合物具有25至12,000g/mol之平均分子量。
實施例13.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有250至6,000g/mol之平均分子量。
實施例14.如實施例3所述之雙組分黏合劑組合物,其中羥基封端之化合物具有350至3,000g/mol之平均分子量。
實施例15.如前述或後續實施例所述之雙組分黏合劑組合物,其中磷酸酯多元醇佔異氰酸酯反應性混合物總重量之至少-1重量%。
實施例16.如前述或後續實施例所述之雙組分黏合劑組合物,其中磷酸酯多元醇佔異氰酸酯反應性混合物總重量之2至25重量%。
實施例17.如前述或後續實施例所述之雙組分黏合劑組合物,其中磷酸酯多元醇佔異氰酸酯反應性混合物總重量之4至10重量%。
實施例18.如前述或後續實施例所述之雙組分黏合劑組合物,其中聚異氰酸酯及異氰酸酯反應性混合物以至少1之化學計量比(NCO/OH)存在。
實施例19.如前述或後續實施例所述之雙組分黏合劑組合物,其中聚異氰酸酯及異氰酸酯反應性混合物以2.0至6.0之化學計量比(NCO/OH)存在。
實施例20.如前述或後續實施例所述之雙組分黏合劑組合物,其中聚異氰酸酯及異氰酸酯反應性混合物以2.5至4.0之化學計量比(NCO/OH)存在。
實施例21.如前述或後續實施例所述之雙組分黏合劑組合物,其
中異氰酸酯反應性組分之多元醇選自由以下組成之群:聚酯多元醇、聚己內酯多元醇、聚醚多元醇、聚碳酸酯多元醇、基於天然油之多元醇及其組合。
實施例22.如前述或後續實施例所述之雙組分黏合劑組合物,其進一步包括選自由以下組成之群之溶劑:乙酸乙酯、甲基乙基酮、甲苯及其組合。
實施例23.如前述或後續實施例所述之雙組分黏合劑組合物,,其進一步包括選自由以下組成之群之添加劑:界面活性劑、流平劑、消泡劑、流變改質劑、有色顏料、黏合促進劑(例如,磷酸酯及環氧樹脂)及其中兩者或更多者之組合。
實施例24.一種用於製備雙組分黏合劑調配物之方法,其包括:藉由使聚異氰酸酯與包括磷酸酯多元醇之異氰酸酯反應性混合物反應來製備包括異氰酸酯封端之預聚物的異氰酸酯組分;製備包括多元醇之異氰酸酯反應性組分;將異氰酸酯組分及異氰酸酯反應性組分以約1.0至約5.0的化學計量比(NCO/OH)混合。
實施例25.一種用於形成層壓結構之方法,其包括:將異氰酸酯組分及異氰酸酯反應性組分以約1.0至約5.0之化學計量比(NCO/OH)混合以形成雙組分黏合劑組合物,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物;將黏合劑組合物施加到第一基板之表面上;使第一基板之表面與第二基板之表面接觸;及固化黏合劑組合物以將第一基板黏合到第二基板上。
實施例26.一種用於形成層壓結構之方法,其包括:將異氰酸酯組分均勻地施加到第一基板之表面,所述異氰酸酯組分包括異
氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物;將異氰酸酯反應性組分均勻地施加到第二基板之表面上;將第一基板與第二基板集合在一起,藉此使異氰酸酯組分與多元醇組分混合並反應,以在第一基板與第二基板之間形成黏合劑組合物;及固化黏合劑組合物以將第一基板與第二基板黏合。
實施例27.一種層壓結構,其包括如前述或後續實施例中任一項所述之雙組分黏合劑組合物。
Claims (8)
- 一種雙組分黏合劑組合物,其包括:(A)異氰酸酯組分,其包括異氰酸酯封端之預聚物,所述預聚物為以下之反應產物:聚異氰酸酯;及包括磷酸酯多元醇之異氰酸酯反應性混合物;及(B)包括多元醇之異氰酸酯反應性組分;其中所述磷酸酯多元醇為羥基封端之化合物及(聚)磷酸以及另一聚異氰酸酯之反應產物,所述磷酸酯多元醇佔所述異氰酸酯反應性混合物之總重量的至少1%重量。
- 如請求項1所述之雙組分黏合劑組合物,其中所述聚異氰酸酯及所述異氰酸酯反應性混合物以至少1之化學計量比(NCO/OH)存在。
- 如請求項1所述之雙組分黏合劑組合物,其中所述聚異氰酸酯及所述異氰酸酯反應性混合物以2.0至6.0之化學計量比(NCO/OH)存在。
- 如請求項1所述之雙組分黏合劑組合物,其進一步包括選自由以下組成之群之溶劑:乙酸乙酯、甲基乙基酮、甲苯及其組合。
- 如請求項1所述之雙組分黏合劑組合物,其進一步包括選自由以下組成之群之添加劑:界面活性劑、流平劑、消泡劑、流變改質劑、有色顏料、黏合促進劑及其中兩者或更多者之組合。
- 一種用於形成層壓結構之方法,其包括:將異氰酸酯組分及異氰酸酯反應性組分以約1.0至約5.0之化學計量比(NCO/OH)混合以形成雙組分黏合劑組合物,所述異氰酸酯組分包括異氰酸酯 封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物;將所述黏合劑組合物施加到第一基板之表面上;使所述第一基板之所述表面與第二基板之表面接觸;及固化所述黏合劑組合物以將所述第一基板黏合到所述第二基板;其中所述磷酸酯多元醇為羥基封端之化合物及(聚)磷酸以及另一聚異氰酸酯之反應產物,所述磷酸酯多元醇佔所述異氰酸酯反應性混合物之總重量的至少1%重量。
- 一種用於形成層壓結構之方法,其包括:將異氰酸酯組分均勻地施加到第一基板之表面,所述異氰酸酯組分包括異氰酸酯封端之預聚物,所述預聚物為聚異氰酸酯及包括磷酸酯多元醇的異氰酸酯反應性混合物的反應產物;將異氰酸酯反應性組分均勻地施加到第二基板之表面上;將所述第一基板與第二基板集合在一起,藉此使所述異氰酸酯組分與所述多元醇組分混合並反應,以在所述第一基板與所述第二基板之間形成黏合劑組合物;及固化所述黏合劑組合物以將所述第一基板與所述第二基板黏合;其中所述磷酸酯多元醇為羥基封端之化合物及(聚)磷酸以及另一聚異氰酸酯之反應產物,所述磷酸酯多元醇佔所述異氰酸酯反應性混合物之總重量的至少1%重量。
- 一種層壓結構,其包括如請求項1所述之雙組分黏合劑組合物。
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