TWI483843B - 容器用樹脂包覆金屬板 - Google Patents
容器用樹脂包覆金屬板 Download PDFInfo
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- TWI483843B TWI483843B TW101135552A TW101135552A TWI483843B TW I483843 B TWI483843 B TW I483843B TW 101135552 A TW101135552 A TW 101135552A TW 101135552 A TW101135552 A TW 101135552A TW I483843 B TWI483843 B TW I483843B
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Description
本發明是有關於一種例如用於食品罐裝的罐體及蓋等的容器用樹脂包覆金屬板。
先前,作為用於食品罐裝的金屬罐用原材料的無錫鋼(Tin Free Steel,TFS)、鋁等金屬板,為了提高耐蝕性、耐久性、耐候性等而實施塗裝。但是,實施該塗裝的步驟不僅燒接處理複雜,而且必需大量的處理時間,還存在排放大量的溶劑的問題。
因此,為了解決該等問題,而開發在經加熱的金屬板上積層熱塑性樹脂膜而成的膜層壓金屬板代替塗裝鋼板,目前在工業上用作食品罐裝用原材料。
食品罐裝用原材料除了加工性、密接性等基本特性外,若為二片罐用途,則要求深拉伸成形性、加工-蒸煮(retort)後密接性或耐蝕性、創意性等各種功能。使膜層壓金屬板多功能化的方法可選擇:(1)在膜內添加具有欲附加的功能的改質劑,使膜本身多功能化的方法;(2)不對膜進行改質,而在膜表面塗佈具有欲附加的功能的改質劑或包含改質劑的樹脂的方法的任一種方法。
上述(1)在膜中直接添加改質劑的方法,在大量生產具有固定功能的膜的情況下,是生產效率高、收益性高的方法。但是由於食品罐裝的形狀或內容物的種類多種多樣,並且對每種罐裝所要求的功能不同,因此該方法並不
恰當。原因是,每當改變賦予膜的功能時,需要清洗樹脂的擠出裝置、或澆鑄鼓(casting drum)、冷卻輥等,而必須長時間停止生產線,從而導致生產效率明顯降低。
另一方面,上述(2)在膜的表面塗佈包含改質劑的樹脂的方法,容易變更附加在膜上的功能,因此可應對食品罐裝的多樣性需求。原因是藉由對裝入了包含改質劑的塗佈液的罐進行清洗、交換,而可快速地應對。
此種在膜表面塗佈包含改質劑的樹脂的方法例如可列舉專利文獻1。專利文獻1是在金屬板與膜之間形成以環氧樹脂為主成分,且包含三聚氰胺樹脂、嵌段異氰酸酯化合物、著色劑的樹脂層的方法。
然而,環氧樹脂雖然富有反應性、且與金屬板的密接性優異,但存在深拉伸成形性劣化的缺點,因此無法獲得可用作二片罐用原材料的膜。即便欲將專利文獻1的樹脂包覆金屬板成形為深拉伸罐(Draw-Redraw cans,DRD罐),環氧樹脂亦無法追隨罐高度方向的伸長變形,而導致限制原材料的變形,並在拉伸步驟中導致原材料斷裂。
為了提高密接性,在專利文獻2~專利文獻5中揭示對膜進行樹脂塗佈的方法。專利文獻2~專利文獻5是聚酯樹脂與環氧樹脂的複合系、或以環氧樹脂為主成分的構成。因此,與專利文獻1同樣,深拉伸成形性困難,無法適用於二片罐用途。另外,專利文獻2~專利文獻5中所記載的實施例中,並未揭示對製罐加工性或深拉伸成形性進行評價的例子,因此亦可明白,這些例子並未考慮要求
深拉伸加工的二片罐用途。
[專利文獻1]日本專利特開2007-185915號公報
[專利文獻2]日本專利特開平4-266984號公報
[專利文獻3]日本專利特開平8-199147號公報
[專利文獻4]日本專利特開平10-183095號公報
[專利文獻5]日本專利特開2002-206079號公報
本發明是鑒於上述情況而成,目的是提供一種可應對食品罐裝原材料所要求的多種特性的容器用樹脂包覆金屬板。
本發明者等人為了解決課題而進行銳意研究,結果獲得以下發現。
在金屬板的至少單面具有以聚酯樹脂為主成分的多層結構的樹脂包覆層。並且,將含有(i)聚酯樹脂、(ii)酚樹脂、(iii)金屬烷氧化物系化合物及/或金屬螯合化合物、(iv)環氧樹脂、(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上的樹脂層製成與金屬板的密接層,較佳為在其上層積層聚酯膜,藉此可獲得不但具有優異的深拉伸成形性、加工後密接性等基本特性,而且亦具有蒸煮處理環境下的創意性等多種優異的功能的容器用樹脂包覆金屬板。
本發明是基於以上的發現而成,其要旨如以下所述。
[1]一種容器用樹脂包覆金屬板,其特徵在於:在金屬板的至少單面,具有以聚酯樹脂為主成分的多層結構的樹脂包覆層(A),該樹脂包覆層(A)具有樹脂層(a1),該樹脂層(a1)與上述金屬板面密接,含有下述(i)~(v)的成分,並以聚酯樹脂為主成分:
(i)聚酯樹脂
(ii)酚樹脂
(iii)金屬烷氧化物系化合物及/或金屬螯合化合物
(iv)環氧樹脂
(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上。
[2]如[1]所述之容器用樹脂包覆金屬板,其中上述(iv)環氧樹脂是雙酚A以外的環氧樹脂。
[3]如上述[1]或[2]所述之容器用樹脂包覆金屬板,其中上述樹脂包覆層(A)包含:上述樹脂層(a1)、及形成於該樹脂層(a1)的上層的聚酯膜(a2)。
[4]如上述[1]至[3]中任一項所述之容器用樹脂包覆金屬板,其中形成上述樹脂層(a1)的樹脂成分的比率滿足下述:
(i)聚酯樹脂:50質量%~89質量%
(ii)酚樹脂:10質量%~45質量%
(iii)金屬烷氧化物系化合物及/或金屬螯合化合物:0.01質量%~10質量%
(iv)環氧樹脂:0.5質量%~20質量%
(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上:0.1質量%~10質量%。
[5]如上述[1]至[4]中任一項所述之容器用樹脂包覆金屬板,其中上述(i)聚酯樹脂的數量平均分子量為3000~100000,且是下述(i-1)~(i-3)中任一種以上:
(i-1)玻璃轉移溫度為0℃以上且小於35℃的聚酯樹脂
(i-2)玻璃轉移溫度為35℃以上且小於65℃的聚酯樹脂
(i-3)玻璃轉移溫度為65℃以上且小於100℃的聚酯樹脂。
[6]如上述[5]所述之容器用樹脂包覆金屬板,其中形成上述(i)聚酯樹脂的各聚酯樹脂的比率滿足下述:
玻璃轉移溫度為0℃以上且小於35℃的聚酯樹脂:30質量%~70質量%
玻璃轉移溫度為35℃以上且小於65℃的聚酯樹脂:10質量%~35質量%
玻璃轉移溫度為65℃以上且小於100℃的聚酯樹脂:10質量%~35質量%。
[7]如上述[1]至[6]中任一項所述之容器用樹脂包覆金屬板,其中上述(i)聚酯樹脂是含有源自雙酚酸的重複單元的聚酯樹脂。
[8]如上述[1]至[7]中任一項所述之容器用樹脂包覆金屬板,其中上述(iii)金屬烷氧化物系化合物及/或金屬螯
合化合物是鈦烷氧化物系化合物及/或鈦螯合化合物。
[9]如上述[2]至[8]中任一項所述之容器用樹脂包覆金屬板,其中上述聚酯膜(a2)是聚酯樹脂的結構單元的85質量%以上為對苯二甲酸乙二酯單元及/或萘二甲酸乙二酯單元的雙軸延伸聚酯膜,且該雙軸延伸聚酯膜含有無機粒子及/或有機粒子。
根據本發明,可獲得能應對食品罐裝用原材料所要求的多種特性的容器用樹脂包覆金屬板。並且,可容易附加食品罐裝所要求的多種功能的新的容器用樹脂包覆金屬板,是產業上有益的發明。
以下,對本發明的容器用樹脂包覆金屬板進行詳細地說明。
首先,對本發明中所用的金屬板進行說明。
本發明的金屬板可使用廣泛用作罐用材料的鋁板或軟鋼板等。特別是最佳為形成了下層包含金屬鉻、上層包含鉻氫氧化物的二層皮膜的表面處理鋼板(以下稱為無錫鋼(Tin Free Steel,TFS))等。
TFS的金屬鉻層、鉻氫氧化物層的附著量並無特別限定,就加工後密接性、耐蝕性的觀點而言,均以Cr換算計,金屬鉻層較理想為設為70mg/m2
~200mg/m2
的範圍、鉻氫氧化物層較理想為設為10mg/m2
~30mg/m2
的範圍。
並且,本發明的容器用樹脂包覆金屬板在金屬板的至
少單面,具有以聚酯樹脂為主成分的多層結構的樹脂包覆層(A)。該聚酯樹脂可使用與下述樹脂層(a1)中所說明的聚酯樹脂相同的聚酯樹脂。
並且,該樹脂包覆層(A)具有與上述金屬板面密接的樹脂層(a1),而且上述樹脂層(a1)以聚酯樹脂為主成分,並含有下述(i)~(v)的成分。如上所述,樹脂包覆層(A)以聚酯樹脂為主成分,此處,主成分是指樹脂包覆層(A)中含有50質量%以上的聚酯樹脂:
(i)聚酯樹脂
(ii)酚樹脂
(iii)金屬烷氧化物系化合物及/或金屬螯合化合物
(iv)環氧樹脂
(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上。
接著,對與金屬板面密接的樹脂層(a1)進行說明。
(i)聚酯樹脂
本案發明中,以聚酯樹脂為主成分,此處所謂主成分,是指樹脂層(a1)中含有50質量%以上的聚酯樹脂。
聚酯樹脂較佳為數量平均分子量為3000~100000,更佳為5000~30000,尤佳為10000~25000的範圍內。另外,數量平均分子量是藉由凝膠滲透層析(gel permeation chromatography)分析藉由與聚苯乙烯的比較所得的換算值。若數量平均分子量低於3000,則加工性變差,若數量平均分子量高於100000,則有塗料化時的黏度變高,而無
法恰當的塗裝的情況。
聚酯樹脂的玻璃轉移溫度較佳為0℃以上且小於100℃的範圍內。藉由將玻璃轉移溫度設為0℃以上且小於100℃的範圍,而樹脂的柔軟性、加工性或耐黏連性會適度地平衡,而適合於食品罐裝用途。
1種聚酯樹脂存在難以滿足多種要求性能的情況。在單獨使用時,例如在聚酯樹脂的玻璃轉移溫度為0℃以上且小於35℃時,會對樹脂層賦予柔軟性而加工性優異。但是,在膜上塗佈樹脂層後,若在捲曲的狀態下以超過玻璃轉移溫度的溫度長時間保持,則有導致膜產生黏連的擔憂。另外,由於玻璃轉移溫度低、且耐熱性不足,因此耐蒸煮性稍有劣化。
若玻璃轉移溫度為35℃以上且小於65℃,則膜不會產生黏連,而不會損及膜的美觀。若玻璃轉移溫度為65℃以上且小於100℃,則雖然黏連性優異,但由於皮膜變硬而加工性稍有劣化。
因此較佳為,聚酯樹脂藉由併用玻璃轉移溫度不同的多種樹脂,引出各種聚酯樹脂的良好性能,從而獲得取得了平衡的更優異的樹脂層。
另外,在併用玻璃轉移溫度不同的多種樹脂時,各聚酯樹脂的比率較佳為如以下所述:
玻璃轉移溫度為0℃以上且小於35℃的聚酯樹脂:30質量%~80質量%
玻璃轉移溫度為35℃以上且小於65℃的聚酯樹脂:10
質量%~35質量%
玻璃轉移溫度為65℃以上且小於100℃的聚酯樹脂:10質量%~35質量%。
藉由設為此種比率的範圍,而加工性與黏連性的平衡明顯提高。
另外,聚酯樹脂較佳為含有源自雙酚酸的重複單元。在作為用以製造聚酯樹脂的原料成分的單體組成物中含有雙酚酸時,與酚樹脂的反應性提高,並且硬化速度提高,結果耐蒸煮白化性提高。另外,以高比率使用以雙酚酸為必須單體的玻璃轉移溫度為0℃以上且小於35℃的聚酯,硬化性亦提高。如此,具有即便玻璃轉移溫度低而塗佈膜的黏連性亦優異等的特徵,因此聚酯樹脂較佳為含有源自雙酚酸的重複單元。
聚酯樹脂(i)可使用使多元酸成分與多元醇成分酯化反應而成的聚酯樹脂。
多元酸成分例如可使用:鄰苯二甲酸酐、間苯二甲酸、對苯二甲酸、琥珀酸、反丁烯二酸、己二酸、壬二酸、癸二酸、二聚酸等1種以上的二元酸及這些酸的低級烷基酯化物,根據需要可併用:苯甲酸、丁烯酸等一元酸,偏苯三甲酸酐、甲基環己烯三甲酸等三元以上的多元酸等。
多元醇成分主要可使用:乙二醇、二乙二醇、丙二醇、1,4丁二醇、新戊二醇、3-甲基戊二醇、1,4-己二醇、1,6-己二醇、環己烷二甲醇等二元醇,而且根據需要可併用:甘油、三羥甲基乙烷、三羥甲基丙烷、季戊四醇等三元以
上的多元醇。這些多元醇可單獨使用,或將2種以上加以混合而使用。
聚酯樹脂(i)的市售品例如可列舉:東洋紡績(股)製造的Vylon 300、Vylon 500、Vylon 560、Vylon 600、Vylon 630、Vylon 650、Vylon 670、Vylon GK 130、Vylon GK 140、Vylon GK 150、Vylon GK 190、Vylon GK 330、Vylon GK 590、Vylon GK 680、Vylon GK 780、Vylon GK 810、Vylon GK 890,尤尼吉可(Unitika)(股)製造的Elitel UE-3220、Elitel UE-3500、Elitel UE-3210、Elitel UE-3215、Elitel UE-3216、Elitel UE-3620、Elitel UE-3240、Elitel UE-3250、Elitel UE-3300,東亞合成(股)製造的ARONMELT PES-310、ARONMELT PES-318、ARONMELT PES-334等。
(ii)酚樹脂
藉由添加酚樹脂,而會引起交聯反應,並形成立體網狀結構,因此可獲得使皮摸的耐蝕性或耐蒸煮性提高的效果。
樹脂層(a1)中進一步添加酚樹脂作為成分(ii)。可列舉:使苯酚、間甲酚、間乙基苯酚、3,5-二甲苯酚、間甲氧基苯酚等三官能酚化合物,或對甲酚、鄰甲酚、對第三丁基苯酚、對乙基苯酚、2,3-二甲苯酚、2,5-二甲苯酚、間甲氧基苯酚等各種二官能性酚,與甲醛在鹼觸媒存在下合成而成的產物。這些酚化合物可使用1種或將2種以上加以混合而使用。另外,亦可使用藉由碳數為1~12的醇類將酚樹脂中所含有的羥甲基的一部分或全部醚化而成的
形態的產物。
(iii)金屬烷氧化物系化合物及/或金屬螯合化合物
金屬烷氧化物系化合物及/或金屬螯合化合物會與(i)聚酯樹脂、(ii)酚樹脂、(iv)環氧樹脂引起反應。各樹脂的官能基與金屬烷氧化物系化合物及/或金屬螯合化合物之間進行交聯反應。該交聯反應與無金屬烷氧化物系化合物及/或金屬螯合化合物的情形相比,其皮膜的硬化速度明顯更快,因此結果可藉由極少的熱能表現出優異的密接性、加工性、耐蒸煮性、耐蝕性。例如,已存在的層壓罐是在將膜層壓後以180℃以上溫度實施數秒~數分鐘燒接,然後利用後加熱使樹脂皮膜硬化,而確保上述各種要求性能的罐。但是,本發明中,含有金屬烷氧化物系化合物及/或金屬螯合化合物時的樹脂層進行熱融著層壓時,僅藉由1秒左右的短時間加熱便使樹脂層充分硬化,可獲得與實施後加熱者同等以上的性能。因此,不需要製造製程中的後加熱步驟,而尤其提高製造效率。此外,亦可降低二氧化碳的排放,可成為實用上極為有用的技術。而且,藉由在皮膜中摻入金屬,而提高皮膜的強度,結果大幅地提高耐衝擊性或耐蝕性。根據以上理由,較佳為上述樹脂層(a1)含有金屬烷氧化物系化合物及/或金屬螯合化合物。
金屬烷氧化物系化合物及/或金屬螯合物系化合物例如可列舉:鋁、鈦、錫、鋯等的烷氧化物金屬化合物、及乙醯乙酸配位於金屬的金屬螯合化合物等。其中較佳為使用鈦烷氧化物系化合物及/或鈦螯合化合物。以下,對其理
由進行說明。
藉由金屬烷氧化物系化合物及/或金屬螯合化合物、與聚酯樹脂及/或酚樹脂連續地進行交聯反應,而在樹脂層內形成分子鏈的立體網狀結構。藉此可最有效地抑制因蒸煮處理環境下的水蒸氣或熱水的滲透所導致的變色。
所謂因水蒸氣所導致的變色,是在蒸煮殺菌處理中,以樹脂層本身發生白濁的方式變色的現象,被稱為蒸煮白化。由於會使罐外面的創意性受損,因此是可使消費者的購買意願降低的大問題。發明者等人進行銳意研究,結果認為原因是,藉由水蒸氣滲透至包覆罐體的樹脂層內,而在樹脂層的界面及界面附近形成液胞,由於液胞部而使光發生散射。因此,為了改善特性,重要的是抑制樹脂層的界面及界面附近的液胞形成。即,侵入至樹脂中的水蒸氣擴散至樹脂中,而到達與金屬板的界面。在蒸煮處理剛開始後,由於填充至罐內的內容物為接近常溫的狀態,因此自罐的外部至內部產生溫度梯度。即,擴散至樹脂中的水蒸氣隨著接近金屬板而冷卻,而在該界面及界面附近發生液化,成為冷凝水而形成液胞。由於液胞在蒸煮處理後亦會殘留於界面及界面附近,因此會導致光的散射,而可見到樹脂表面發生白濁。因此,為了抑制蒸煮白化,只要抑制界面及界面附近的液胞的形成即可。
另一方面,蒸煮處理裝置除了如上所述使用水蒸氣作為加熱介質的蒸煮處理裝置以外,有使用熱水作為加熱介質的蒸煮裝置。為使用熱水作為加熱介質的蒸煮裝置時,
由於與因水蒸氣所導致的變色不同的機制,而產生樹脂層本身變色而創意性劣化的問題。其原因認為,在蒸煮處理的初始階段,聚酯分子鏈的交聯反應未充分進行時,滲透至樹脂層內的水以聚酯的羰基末端基為觸媒促進聚酯分子鏈的水解反應,從而在樹脂層內形成大的液胞。
本發明者等人對上述2種變色現象進行銳意研究,結果可知,在使用鈦烷氧化物系化合物及/或鈦螯合物系化合物作為金屬烷氧化物系化合物及/或金屬螯合化合物時,在熱融著層壓階段可充分形成因鈦烷氧化物系化合物及/或鈦螯合物系化合物、與聚酯樹脂及/或酚樹脂的交聯反應所形成的聚酯分子鏈的網狀結構,其結果可最有效地抑制這2種的變色現象。並且認為,聚酯分子鏈的網狀結構可抑制水蒸氣及熱水滲透至樹脂內並到達界面,並且可藉由提高樹脂強度及彈性模數而抑制液胞的形成及成長。另外,藉由分子鏈網狀結構形成所伴隨的羰基末端基量的減少,亦可抑制急遽的水解反應。因此,金屬烷氧化物系化合物及/或金屬螯合化合物較佳為使用鈦烷氧化物系化合物及/或鈦螯合化合物。
(iv)環氧樹脂
環氧樹脂主要使皮膜的密接性提高。特佳為酚醛清漆型環氧樹脂。酚醛清漆型環氧樹脂的市售品可列舉:DIC(Dainippon Ink & Chemicals,DIC)(股)公司製造的EPICRON N-665、EPICRON N-670、EPICRON N-673、EPICRON N-680、EPICRON N-690、EPICRON N-695、
EPICRON N-730、EPICRON N-740、EPICRON N-770、EPICRON N-865、EPICRON N-870,陶氏化學(Dow Chemical)(股)公司製造的XD-7855,旭化成環氧(Asahi Kasei Epoxy)(股)公司製造的ECN-1273、ECN-1299等。聯苯型環氧樹脂可列舉:三菱化學(股)製造的YL6121H、YX7399。
另外,環氧樹脂較佳為雙酚A以外的環氧樹脂。原因是擔憂雙酚A的內分泌擾亂作用。
(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上
聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂與三聚氰胺樹脂等相比,硬化速度更快,在可形成強韌的皮膜的方面更優異。與包含聚酯/三聚氰胺系、環氧/三聚氰胺系等的樹脂組成物相比,硬化特性更優異,因此在層壓鋼板的耐蒸煮性、耐蝕性及加工性等的方面,可發揮特別優異的性能。
作為聚胺樹脂,若例示特別具有代表性的聚胺樹脂,則脂肪族胺可列舉:二乙三胺、三乙三胺、三乙五胺,脂環式聚胺可列舉異佛酮二胺等。另外,為了改善作業性或低刺激化、提高機械物性,亦可列舉:使脂肪族聚胺與環氧樹脂或丙烯腈加成、或使甲醛與苯酚反應而改質的產物等。芳香族聚胺可列舉:間苯二胺、二胺基二苯基磺酸、二胺基二苯基甲烷等。市售品可列舉:DIC(股)製造的EPICRON EXB-353、日本氣體產品(Air Products Japan)
(股)製造的Ancamine 2596、Ancamine 2605等。
聚醯胺基胺樹脂、聚醯胺樹脂為例如藉由油脂脂肪酸與聚胺的脫水縮合反應而合成的化合物。市售品可列舉:三洋化成的POLYMIDE L-15-3、POLYMIDE L-45-3,日本氣體產品(股)製造的Ancamide 2137、SUNMIDE 330、SUNMIDE X-2000等。
樹脂層(a1)的組成(質量%)
形成樹脂層(a1)的樹脂成分的比率較佳為滿足下述:
(i)聚酯樹脂:50質量%~89質量%
(ii)酚樹脂:10質量%~45質量%
(iii)金屬烷氧化物系化合物及/或金屬螯合化合物:0.01質量%~10質量%
(iv)環氧樹脂:0.5質量%~20質量%
(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上:0.1質量%~10質量%。
若(i)聚酯樹脂的比率低於50質量%,則加工性惡化,若聚酯樹脂的比率超過89質量%,則有硬化性不足而耐蒸煮性降低的情況。聚酯樹脂的比率更佳為55質量%~85質量%的範圍。
若(ii)酚樹脂的比率低於10質量%,則硬化性不足而耐蒸煮性劣化,若酚樹脂的比率超過45質量%,則有加工性惡化的情況。酚樹脂的比率更佳為20質量%~40質量%。
若(iii)金屬烷氧化物系化合物及/或金屬系螯合化合
物的比率低於0.01質量%,則無法獲得所期待的快速硬化性等效果,另外若比率超過10質量%,則樹脂皮膜變硬而加工性劣化,此外,亦有在塗佈液製作時引起凝膠化的情況。比率更佳為0.1質量%~7質量%。
若(iv)環氧樹脂的比率低於0.5質量%,則密接性降低,結果是耐蝕性劣化,若環氧樹脂的比率超過20質量%,則有導致耐蒸煮白化性降低的情況。環氧樹脂的比率更佳為2質量%~7質量%。
若(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上的比率低於0.1質量%,則硬化性不足而耐蒸煮性劣化,若比率超過10質量%,則有加工性惡化的情況。比率更佳為1質量%~4質量%。
樹脂層(a1)的附著量
樹脂層(a1)的附著量較佳為規定為0.1g/m2
以上5.0g/m2
以下的範圍。在附著量小於0.1g/m2
時,有無法均勻地包覆金屬板表面,而膜厚變得不均勻的情況。另一方面,若附著量超過5.0g/m2
,則有樹脂的凝聚力變得不充分,而導致樹脂層的強度降低的擔憂。其結果,在製罐加工時,樹脂層凝聚破壞而膜剝離,並以此為起點而導致罐體部斷裂。
根據以上所述,附著量較佳為0.1g/m2
以上5.0g/m2
以下,更佳為0.1g/m2
以上3.0g/m2
以下,尤佳為0.5g/m2
以上2.5g/m2
。
著色劑
而且,藉由在樹脂層(a1)中添加染料、顏料等著色劑,而可隱藏基底的金屬板,並賦予樹脂獨自的多樣的色調。例如藉由添加碳黑作為黑色顏料,而可隱藏基底的金屬色,並且可對食品罐裝賦予黑色所具有的高級感。
碳黑的粒徑可使用5nm~50nm的範圍的粒徑,若考慮到在聚酯樹脂中的分散性或發色性,較佳為5nm~30nm的範圍。
除了黑色顏料以外,亦可藉由添加白色顏料而隱藏基底的金屬光澤,並且可使印刷面鮮豔化,並獲得良好的外觀。所添加的顏料必須在容器成形後可發揮出優異的創意性,就該觀點而言,可使用二氧化鈦等無機系顏料。由於著色力強、且亦富有展延性,因此在容器成形後亦可確保良好的創意性,因此較佳。
在期望容器表面具有閃耀色時,較佳為使用黃色的有機系顏料。由於透明性優異並且著色力強,而且富有展延性,因此在容器成形後亦可獲得具有閃耀色的外觀。若例示本發明中可使用的有機系顏料,則可列舉:色指數(簡稱:C.I.)為顏料黃12、顏料黃13、顏料黃14、顏料黃16、顏料黃17、顏料黃55、顏料黃81、顏料黃83、顏料黃139、顏料黃180、顏料黃181、顏料黃183、顏料黃191、顏料黃214中的至少1種。特別是就色調(閃耀色)的鮮豔性、耐熱水變色性等的觀點而言,更佳為使用C.I.顏料黃180、顏料黃214。
此外,紅顏料可列舉:C.I.顏料紅101、顏料紅177、
顏料紅179、顏料紅187、顏料紅220、顏料紅254,藍顏料可列舉:C.I.顏料藍15、顏料藍15:1、顏料藍15:2、顏料藍15:3,紫顏料可列舉:C.I.顏料紫19,橙顏料可列舉:C.I.顏料橙64,綠顏料可列舉:C.I.顏料綠7等。
以上的著色劑的調配比率在構成樹脂層(a1)的樹脂層的全部固體成分中,較佳為含有0.1質量%~70質量%。
硬化觸媒
樹脂層(a1)中除了上述成分(i)~成分(v)及著色劑外,可添加促進交聯的硬化觸媒。例如可使用:磷酸等無機酸,十二烷基苯磺酸、甲苯磺酸等有機酸及藉由胺等對這些酸進行嵌段而成的產物。硬化觸媒的調配比率在構成樹脂層(a1)的樹脂層的全部固體成分中,較佳為0.01質量%~5質量%。
另外,樹脂層(a1)中可添加先前公知的潤滑劑、消泡劑、均化劑、顏料、二氧化矽等抗黏連劑等。另外,硬化輔助劑可併用三聚氰胺樹脂、苯并胍胺樹脂、異氰酸酯樹脂等其他的硬化劑,這些硬化輔助劑可根據膜的乾燥條件、層壓條件而併用恰當的硬化輔助劑。
接著,對形成於樹脂層(a1)的上層的樹脂層(聚酯膜)(a2)進行說明。
樹脂包覆層(A)較佳為在樹脂層(a1)的上層形成以聚酯樹脂為主成分的樹脂層(a2)作為最上層,更佳為樹脂層(a2)為聚酯膜(a2)。
聚酯膜(a2)組成
本發明中所使用的聚酯膜,就使蒸煮後的味特性良好的方面、抑制製罐步驟中的磨耗粉的產生的方面而言,較理想為以對苯二甲酸乙二酯及/或萘二甲酸乙二酯為主要構成成分。以對苯二甲酸乙二酯及/或萘二甲酸乙二酯為主要構成成分的聚酯,是聚酯的85質量%以上為以對苯二甲酸乙二酯及/或萘二甲酸乙二酯為構成成分的聚酯。更佳為90質量%以上,若如此則即便將飲料長期填充於金屬罐中,味特性亦良好,因此較理想。
另一方面,在不損及味特性的範圍內可將其他二羧酸成分、二醇成分進行共聚合,二羧酸成分例如可列舉:二苯基甲酸、5-鈉磺基間苯二甲酸、鄰苯二甲酸等芳香族二羧酸,草酸、琥珀酸、己二酸、癸二酸、二聚酸、順丁烯二酸、反丁烯二酸等脂肪族二羧酸,環己烷二甲酸等脂環族二羧酸,對羥基苯甲酸等羥基羧酸等。
二醇成分例如可列舉:乙二醇、丙二醇、丁二醇、戊二醇、己二醇、新戊二醇等脂肪族二醇,環己烷二甲醇等脂環族二醇,雙酚A、雙酚S等芳香族二醇,二乙二醇、聚乙二醇等。另外,芳香族二醇的雙酚A有內分泌擾亂作用之虞,因此較理想為不用作二醇成分。另外,這些二羧酸成分、二醇成分可併用2種以上。
另外,只要不妨礙本發明的效果,可將偏苯三甲酸、均苯三甲酸(trimesic acid)、三羥甲基丙烷等多官能化合物進行共聚合。
粒子
本發明中所用的聚酯膜可含有無機粒子及/或有機粒子。本發明中所用的聚酯膜中的粒子,在組成上為有機、無機均可,並無特別限制,就成形為膜時的突起形狀、耐磨耗性、加工性、味特性的觀點而言,體積換算平均粒徑較佳為0.005μm~5.0μm,特佳為0.01μm~3.0μm。另外,就耐磨耗性等的方面而言,較佳為下述式所示的相對標準偏差為0.5以下,更佳為0.3以下。
其中,
σ:相對標準偏差
D:數量平均粒徑(μm)
Di:粒徑(μm)
n:粒子個數(個)。
粒子的長徑/短徑比較佳為1.0~1.2。就突起硬度、耐磨耗性等的方面而言,莫氏硬度(Mohs hardness)較佳為小於7。
另外,為了充分表現這些效果,較佳為含有0.005質量%~10質量%的包含上述粒徑的粒子。
具體而言,無機粒子可列舉:濕式二氧化矽及乾式二氧化矽、膠體二氧化矽、矽酸鋁、氧化鈦、碳酸鈣、磷酸鈣、硫酸鋇、氧化鋁、雲母、高嶺土、黏土等。其中,較佳為粒子表面的官能基與聚酯反應而生成羧酸金屬鹽的粒子,具體而言,就與聚酯的親和性、耐磨耗性等的方面而言,相對於1g粒子,較佳為具有10-5
mol以上的官能基,更佳為具有2×10-5
mol以上的官能基。
另外,有機粒子可使用各種有機高分子粒子,其種類若為至少一部分對聚酯不溶的粒子,則可為任意組成的粒子。另外,此種粒子的原材料可使用:聚醯亞胺、聚醯胺醯亞胺、聚甲基丙烯酸甲酯、甲醛樹脂、酚樹脂、交聯聚苯乙烯、矽酮樹脂等各種原材料。其中,特佳為耐熱性高、且容易獲得粒度分布均勻的粒子的乙烯系交聯高分子粒子。
此種無機粒子及有機高分子粒子可單獨使用,較佳為併用2種以上而使用,藉由組合粒度分布、粒子強度等物性不同的粒子,而可獲得功能性更高的聚酯樹脂。
另外,在不妨礙本發明的效果的範圍內,可使用其他粒子、例如各種不定形的外部添加型粒子、及內部析出型粒子、或各種表面處理劑。而且,若聚酯膜為雙軸延伸聚酯膜,則就耐熱性、味特性的觀點而言較佳。雙軸延伸的方法可為同時雙軸延伸、逐次雙軸延伸的任一種,就使層壓性、成形性良好的方面而言,較佳為使延伸條件、熱處理條件特定化,並且膜的厚度方向的折射率為1.50以上。
而且,若厚度方向折射率為1.51以上、特別是1.52以上,則即便層壓時稍有不均,亦會同時具有成形性、耐衝擊性,而且可將面配向係數控制在特定範圍,因此較佳。
另外,雙軸延伸聚酯膜就在製罐步驟中拉伸成形後受到200℃~230℃左右的熱歷程後對頸部進行加工時的加工性、耐衝擊性的方面而言,較佳為藉由固體高分解能核磁共振(nuclear magnetic resonance,NMR)的結構解析中的羰基部的緩和時間為270msec以上。更佳為280msec以上,特佳為300msec以上。在不妨礙本發明的效果的範圍內,可使用其他粒子、例如各種不定形的外部添加粒子、及內部析出型粒子、或各種表面處理劑。
聚酯膜(a2)的厚度
本發明中所用的聚酯膜的厚度較佳為5μm~100μm。在聚酯膜的厚度小於5μm時,包覆性不充分而無法確保耐衝擊性與成形性。另一方面,若厚度超過100μm,則上述特性飽和,不但無法獲得任何的改善效果,而且在金屬表面上熱融著時所需要的熱能增大,因此導致損害經濟性。就此種觀點而言,更佳的聚酯膜的厚度為8μm~50μm,更佳為10μm~25μm。
接著,對本發明的容器用樹脂包覆金屬板的製造方法進行說明。
以聚酯為主成分的樹脂層(a1)的形成方法
作為一例,對在聚酯膜(a2)的表面形成聚酯樹脂層(a1)的方法進行敍述。
使成為主成分的聚酯樹脂溶解於有機溶劑中,並使本發明所規定的樹脂層(a1)的添加成分及任意添加成分溶解或分散於有機溶劑中而製備塗佈液。將該塗佈液在聚酯膜(a2)製膜時或製膜後塗佈於膜表面並乾燥,藉此形成樹脂層(a1)。
用以使聚酯樹脂溶解的有機溶劑可列舉:甲苯、二甲苯等芳香族烴溶劑,甲基乙基酮、環己酮等酮溶劑,乙酸乙酯、乙二醇單乙醚乙酸酯等酯系溶劑等,可適當選定這些有機溶劑的1種以上而使用。
上述塗佈液中可添加先前公知的潤滑劑、消泡劑、均化劑、顏料、二氧化矽等抗黏連劑等。另外,硬化輔助劑可併用三聚氰胺樹脂、苯并胍胺樹脂、異氰酸酯樹脂等其他硬化劑,這些硬化輔助劑可根據膜的乾燥條件、層壓條件而併用恰當的硬化輔助劑。
另外,亦可使本發明中所規定的交聯劑、硬化觸媒、作為著色劑的碳黑、偶氮系顏料等添加劑分散於有機溶劑中而使用。此時,若併用分散劑,則可賦予添加劑的均勻性,因此較佳。
將塗佈液塗佈於聚酯膜的方法可應用:輥塗機方式、模塗機方式、凹版(gravure)方式、凹版膠印(gravure offset)方式、噴霧塗佈方式等已知的塗裝方式,最佳為凹版輥塗法。塗佈液塗佈後的乾燥條件較佳為以80℃~170℃乾燥1秒~30秒,特別是以100℃~130℃乾燥5秒~30秒。乾燥後的樹脂層(a1)的附著量較佳為0.1g/m2
~5.0g/m2
的
範圍內。若附著量為0.1g/m2
~5.0g/m2
的範圍內,則連續均勻塗佈性優異,亦無創意性的問題,可確保耐蒸煮性、密接性,亦可消除膜捲取時的黏連性。在附著量小於0.1g/m2
時,有皮膜的連續性容易產生困難,並且難以表現物性與創意性的情況。另外,在蒸煮殺菌處理中對水蒸氣的阻隔性劣化,水分容易滯留在樹脂層(a1)/聚酯膜(a2)的界面,並可能引起蒸煮白化。另一方面,若附著量超過5.0g/m2
,則塗佈後的溶劑脫附性降低,作業性明顯降低,而且容易產生殘留溶劑的問題,從而存在膜捲取時的黏連性明顯降低的情況。附著量較佳的範圍是0.5g/m2
~2.5g/m2
的範圍。
將塗佈了樹脂層(a1)後的聚酯膜(a2)層壓於金屬板表面的方法
將塗佈了樹脂層(a1)的聚酯膜(a2),以樹脂層(a1)與金屬板面密接的方式層壓於金屬板表面。例如可使用:以超過膜的熔點的溫度對金屬板加熱,使用壓接輥(以下稱為層壓輥),使塗佈了樹脂層(a1)的聚酯膜(a2)與金屬板表面接觸並熱融著的方法。另外,此時如上所述,必須使用層壓輥使塗佈了樹脂層(a1)的聚酯膜面與金屬板接觸並熱融著。
關於層壓條件,以獲得本發明所規定的樹脂層的方式進行適當設定。例如較佳為,將層壓開始時的溫度設為至少膜的熔點以上,將以膜的熔點以上的溫度接觸的時間設為1msec~35msec的範圍,作為層壓時膜所受到的溫度
歷程。為了達成此種層壓條件,除了高速的層壓外,亦必須融著中的冷卻。層壓時的加壓並無特別規定,較佳面壓為9.8N/cm2
~294N/cm2
(1kgf/cm2
~30kgf/cm2
)。若該值過低,則即便到達樹脂界面的溫度為熔點以上,時間亦為短時間,因此熔融不充分,而難以獲得充分的密接性。另外,若加壓大,則層壓金屬板的性能上雖無不當,但施加於層壓輥的力大而必需設備上的強度,而導致裝置的大型化,因此不經濟。
以下,對本發明的實施例進行說明。
金屬板的製造
金屬板是使用鍍鉻的鋼板。對實施了冷軋、退火、調質軋壓的厚度0.18mm、寬度977mm的鋼板,進行脫脂、酸洗後進行鍍鉻處理,而製造鍍鉻的鋼板。鍍鉻處理是在包含CrO3
、F-
、SO4 2-
的鍍鉻浴中進行鍍鉻,中間沖洗後,在包含CrO3
、F-
的化學轉化處理液中進行電解。此時,調整電解條件(電流密度、電量等),將金屬鉻附著量與鉻氫氧化物附著量以Cr換算計分別調整為120mg/m2
、15mg/m2
。
罐內面側的樹脂包覆用膜的製造
在以表2所示的比率將表2所示的酸成分與二醇成分聚合而得的聚酯樹脂中,調配表2所示的粒子而製成樹脂組成物,根據常法將該樹脂組成物乾燥、熔融、擠出,在冷卻鼓上冷卻固化,而獲得未延伸膜,然後進行雙軸延伸、
熱固定,而獲得雙軸配向聚酯膜(a2)。
接著,以表1所示的比,將表1(表1-1及表1-2。以下相同。)所示的各聚酯樹脂、酚樹脂、金屬烷氧化物系化合物及/或金屬螯合化合物、環氧樹脂、聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂,溶解於甲苯與甲基乙基酮的混合溶劑中,而製作塗佈液。
此處,表示包含源自雙酚酸的重複單元的聚酯樹脂(i-1)的合成例。將作為酸成分的對苯二甲酸50質量份、間苯二甲酸112質量份、雙酚酸4.9質量份,作為多元醇成分的2-乙基-2-丁基-1,3-丁二醇50質量份、1,4-丁二醇99質量份、1,4-環己烷二甲醇48質量份,四丁醇鈦0.07質量份投入至2L燒瓶中,歷時4小時緩慢升溫至220℃為止,使水餾出進行酯化。使特定量的水餾出後,歷時30分鐘進行減壓聚合至10mmHg為止,並且升溫至溫度為250℃為止,接著在該1mmHg以下的狀態下進行50分鐘的後期聚合。接著,停止減壓聚合,在氮氣流下冷卻至220℃為止,添加偏苯三甲酸酐1.9質量份,在220℃下攪拌30分鐘進行羧基改質(後加成)後,取出樹脂,而獲得數量平均分子量22000、酸值5(mgKOH/g)、玻璃轉移溫度30℃的聚酯樹脂(i-1)。然後,冷卻至60℃以下為止,藉由甲基乙基酮/甲苯=50/50的混合溶液進行稀釋,而獲得不揮發成分40%的聚酯樹脂(i-1)溶液。
關於聚酯樹脂(i-2),例如可使用市售的聚酯樹脂即Vylon GK-250(數量平均分子量:10000、玻璃轉移溫度:
60℃、東洋紡績製造)。在甲基乙基酮/甲苯=50/50的混合溶劑中混合Vylon GK-250,而獲得不揮發成分40%的聚酯樹脂(i-2)溶液。
關於聚酯樹脂(i-3),例如可使用市售的聚酯樹脂即Vylon GK-640(數量平均分子量:18000、玻璃轉移溫度:79℃、東洋紡績製造)。在甲基乙基酮/甲苯=50/50的混合溶劑中混合Vylon GK-250,而獲得不揮發成分40%的聚酯樹脂(i-3)溶液。
另外,關於酚樹脂,是使用市售品TD2495(對甲酚型酚樹脂、50%正丁醇溶液、DIC(股)製造)等。
金屬螯合化合物是使用市售的TC-200(辛二醇鈦螯合物、松本精細化工(Matsumoto Fine Chemical)(股))等,金屬烷氧化物化合物是使用市售的ZA-65(丁醇鋯、松本精細化工(股))。
環氧樹脂是使用市售的EPICRON N-660(甲酚酚醛清漆型環氧樹脂、50%甲基乙基酮溶液、DIC(股)製造)、以及市售的YL6121H(聯苯型環氧樹脂、三菱化學(股)製造)。
另外,聚胺樹脂是使用市售品的EPICRON EXB-353(DIC(股)製造)。聚醯胺基胺樹脂是使用市售品的SUNMIDE328A(日本氣體產品製造)。聚醯胺樹脂是使用市售品的POLYMIDE L-15-3(三洋化成製造)。
在藉由上述方式獲得的雙軸配向聚酯膜(a2)的單側的面上,藉由凹版輥塗機以成為特定的乾燥膜厚的方式,
塗佈該塗佈液並乾燥,調整乾燥後的樹脂層(a1)的膜厚。乾燥溫度設為80℃~120℃的範圍。
罐外面側的樹脂包覆用膜的製造
在以表4所示的比率將表4所示的酸成分與二醇成分聚合而得的聚酯樹脂中,調配表4所示的粒子而製成樹脂組成物,根據常法將該樹脂組成物乾燥、熔融、擠出,在冷卻鼓上冷卻固化,而獲得未延伸膜,然後進行雙軸延伸、熱固定,而獲得雙軸配向聚酯膜(a2)。
接著,以表3所示的比,將表3(表3-1與表3-2。以下相同。)所示的各聚酯樹脂、酚樹脂、金屬烷氧化物系化合物及/或金屬螯合化合物、環氧樹脂、聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂及著色劑,溶解於甲苯與甲基乙基酮的混合溶劑中進行溶解,而製作塗佈液。
此處,表示含有源自雙酚酸的重複單元的聚酯樹脂(i-1)的合成例。將作為酸成分的對苯二甲酸50質量份、間苯二甲酸112質量份、雙酚酸4.9質量份,作為多元醇成分的2-乙基-2-丁基-1,3-丁二醇50質量份、1,4-丁二醇99質量份、1,4-環己烷二甲醇48質量份、四丁醇鈦0.07質量份投入至2L燒瓶中,歷時4小時緩慢升溫至220℃為止,使水餾出進行酯化。使特定量的水餾出後,歷時30分鐘進行減壓聚合至10mmHg為止,並升溫至溫度為250℃為止,接著在該1mmHg以下的狀態下進行50分鐘後期聚合。接著,停止減壓聚合,在氮氣流下冷卻至220℃為止,添加偏苯三甲酸酐1.9質量份,在220℃下攪拌30分鐘進行羧基改質(後加成)後,取出樹脂,而獲得數量平均分子量22000、酸值5(mgKOH/g)、玻璃轉移溫度30℃
的聚酯樹脂(i-1)。然後,冷卻至60℃以下為止,並藉由甲基乙基酮/甲苯=50/50的混合溶液進行稀釋,而獲得不揮發成分40%的聚酯樹脂(i-1)溶液。
關於聚酯樹脂(i-2),例如可使用市售的聚酯樹脂即Vylon GK-250(數量平均分子量:10000、玻璃轉移溫度:60℃、東洋紡績製造)。在甲基乙基酮/甲苯=50/50的混合溶劑中混合Vylon GK-250,而獲得不揮發成分40%的聚酯樹脂(i-2)溶液。
關於聚酯樹脂(i-3),例如可使用市售的聚酯樹脂即Vylon GK-640(數量平均分子量:18000、玻璃轉移溫度:79℃、東洋紡績製造)。在甲基乙基酮/甲苯=50/50的混合溶劑中混合Vylon GK-250,而獲得不揮發成分40%的聚酯樹脂(i-3)溶液。
另外,關於酚樹脂(ii),是使用市售品TD2495(對甲酚型酚樹脂、50%正丁醇溶液、DIC(股)製造)等。
金屬螯合化合物是使用市售的TC-200(辛二醇鈦螯合物、松本精細化工(股))等,金屬烷氧化物化合物是使用市售的ZA-65(丁醇鋯、松本精細化工(股))。
環氧樹脂是使用市售的EPICRON N-660(甲酚酚醛清漆型環氧樹脂、50%甲基乙基酮溶液、DIC(股)製造)、及市售的YL6121H(聯苯型環氧樹脂、三菱化學(股)製造)。
另外,聚胺樹脂是使用市售品的EPICRON EXB-353(DIC(股)製造)。聚醯胺基胺樹脂是使用市售品的
SUNMIDE328A(日本氣體產品製造)。聚醯胺樹脂是使用市售品的POLYMIDE L-15-3(三洋化成製造)。
在藉由上述方式獲得的雙軸配向聚酯膜(a2)的單側的面上,藉由凹版輥塗機以成為特定的乾燥膜厚的方式,塗佈該塗佈液並乾燥,調整乾燥後的樹脂層(a1)的膜厚。乾燥溫度設為80℃~120℃的範圍。
容器用樹脂包覆金屬板的製造
使用圖1所示的金屬帶的層壓裝置,藉由金屬帶加熱裝置2對上述所得的鍍鉻的鋼板1進行加熱,藉由層壓輥3在鍍鉻的鋼板1的一個面層壓(熱融著)作為罐內面側的樹脂包覆層(A)的膜4a,並在另一面層壓(熱融著)作為罐外面側的樹脂包覆層(A)的膜4b。然後,藉由金屬帶冷卻裝置5進行水冷,而製造聚酯樹脂包覆金屬板。上述層壓輥3設為內部水冷式,在層壓中將冷卻水強制循環,進行膜黏接中的冷卻。將樹脂膜層壓於金屬板時,將與金屬板接觸的界面的膜溫度為膜的熔點以上的時間設為1msec~35msec的範圍內。
將根據以上方式製造的容器用樹脂包覆金屬板(本發明例)的單面側的皮膜剖面結構表示於圖2。
容器用樹脂包覆金屬板的評價
關於根據以上方式製造的容器用樹脂包覆金屬板的特性,藉由下述(1)~(7)的方法分別進行測定、評價。
(1)成形性
在容器用樹脂包覆金屬板上塗佈蠟後,沖裁直徑200mm的圓板,以拉伸比2.00獲得淺拉伸罐。接著,對該拉伸罐以拉伸比2.50再次進行拉伸加工。然後,根據常法進行凸起成形後,進行修整,接著實施縮頸-凸緣(neck in-flange)加工而將深拉伸罐成形。著眼於如此獲得的深拉伸罐的縮頸部,目視觀察膜的損傷程度。評價對象是罐的內外面。
(關於評分)
◎:成形後膜上亦未發現損傷亦未發現白化的狀態
○:成形後膜上未發現損傷,但發現部分白化的狀態
×:罐體破裂,無法成形
(2)耐蒸煮白化性
將上述(1)的成形性評價中可成形(○以上)的罐的底部(罐外面側)作為對象。在罐內充滿常溫的自來水後,將蓋合攏而密閉。然後,將罐底部朝下,而配置於蒸氣式蒸煮殺菌爐中,以125℃進行90分鐘的蒸煮處理。處理後,目視觀察罐底部外面的外觀變化。
(關於評分)
◎:外觀無變化
○:外觀稍有污點
×:外觀發生白濁(發生白化)
(3)耐熱水變色性
將上述(1)的成形性評價中可成形(○以上)的罐的底部(罐外面側)作為對象。在罐內充滿常溫的自來水後,將蓋合攏而密閉。然後,將罐底部朝下,而配置於熱水式蒸煮殺菌爐中,以125℃進行90分鐘蒸煮處理。處理後,目視觀察罐底部外面的外觀變化。
(關於評分)
◎:外觀無變化
○:外觀稍有變化(發生變色)
×:外觀變化(發生明顯的變色)
(4)成形後密接性1
將上述(1)的成形性評價中可成形(○以上)的罐作為對象。自罐體部切出剝離試驗用樣品(寬度15mm、長度120mm)。自切出的樣品的長邊側端部將膜的一部分剝離。將剝離的膜朝與所剝離的方向相反的方向(角度:180°)展開,使用拉伸試驗機,以拉伸速度30mm/min.進行剝離試驗,並評價每15mm寬度的密接力。評價對象是罐外面的罐體部。
(評分)
◎:10.0(N)/15(mm)以上
○:5.0(N)/15(mm)以上、且小於10.0(N)/15(mm)
×:小於5.0(N)/15(mm)
(5)成形後密接性2
將上述(1)的成形性評價中可成形(○以上)的罐作為對象。在罐的內部填充自來水後,將蓋合攏而密閉。接著,以130℃、90分鐘的條件實施蒸煮殺菌處理,自罐體部切出剝離試驗用樣品(寬度15mm、長度120mm)。自切出的樣品的長邊側端部將膜的一部分剝離。將剝離的膜朝與所剝離的方向相反的方向(角度:180°)展開,使用拉伸試驗機,以拉伸速度30mm/min.進行剝離試驗,並評價每15mm寬度的密接力。評價對象是罐內面的罐體部。
(評分)
◎:10.0(N)/15(mm)以上
○:5.0(N)/15(mm)以上、且小於10.0(N)/15(mm)
×:小於5.0(N)/15(mm)
(6)損傷部耐蝕性評價1
將上述(1)的成形性評價中可成形(○以上)的罐作為對象。如圖3所示,在罐外面的罐體部2個部位,切入到達基底鋼板的橫切損傷。接著,對於賦予了橫切損傷的罐,進行300小時的依據JISZ2371的鹽水噴霧試驗,測定來自損傷部的單側最大腐蝕寬度。將測定方法表示於圖4。評價對象是罐外面的罐體部。
(關於評分)
◎:單側最大腐蝕寬度小於0.5mm
○:單側最大腐蝕寬度為0.5mm以上且小於1.0mm
×:單側最大腐蝕寬度為1.0mm以上
(7)損傷部耐蝕性評價2
將上述(1)的成形性評價中可成形(○以上)的罐作為對象。如圖3所示,在罐內面的罐體部2個部位,切入到達基底鋼板的橫切損傷。接著,對罐的內部填充1.5%NaCl+1.5%檸檬酸鈉混合液後,將蓋合攏而密閉。接著,以130℃、90分鐘的條件實施蒸煮殺菌處理後,在溫度38℃的恆溫槽內經過20天。然後,將罐切開,測定來自橫切損傷部的單側最大腐蝕寬度。測定方法與(6)損傷部耐蝕性評價1相同。另外,評價對象是罐內面的罐體部。
(關於評分)
◎:單側最大腐蝕寬度小於1.0mm
○:單側最大腐蝕寬度為1.0mm以上且小於3.0mm
×:單側最大腐蝕寬度為3.0mm以上
將根據以上方式所得的結果表示於表5及表6。
根據表5、表6可知,本發明例在食品罐裝原材料所要求的成形性、耐蒸煮白化性、耐熱水變色性、成形後密接性、損傷部耐蝕性方面,具有良好的性能。相對於此,超出本發明的範圍的比較例的特性均劣化。
食品罐裝原材料可在以食品罐裝的罐體及蓋等為中心的世界的所有的市場中使用。
1‧‧‧金屬板(鍍鉻的鋼板)
2‧‧‧金屬帶加熱裝置
3‧‧‧層壓輥
4a、4b‧‧‧膜
5‧‧‧金屬帶冷卻裝置
圖1是表示金屬板的層壓裝置的主要部分的圖。(實施例1)
圖2是表示膜層壓金屬板的剖面結構的圖。(實施例1)
圖3是表示對罐體部所賦予的橫切損傷的位置的圖。(實施例1)
圖4是表示測定來自人工損傷的最大腐蝕寬度的方法的圖。(實施例1)
Claims (8)
- 一種容器用樹脂包覆金屬板,其特徵在於:在金屬板的至少單面,具有以聚酯樹脂為主成分的多層結構的樹脂包覆層(A),該樹脂包覆層(A)具有樹脂層(a1),該樹脂層(a1)與上述金屬板面密接,含有下述(i)~(v)的成分,並以聚酯樹脂為主成分:(i)聚酯樹脂,(ii)酚樹脂,(iii)金屬烷氧化物系化合物及/或金屬螯合化合物,(iv)環氧樹脂,(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上,其中形成上述樹脂層(a1)的樹脂成分的比率滿足下述:(i)聚酯樹脂:50質量%~89質量%,(ii)酚樹脂:10質量%~45質量%,(iii)金屬烷氧化物系化合物及/或金屬螯合化合物:0.01質量%~10質量%,(iv)環氧樹脂:0.5質量%~20質量%,(v)選自由聚胺樹脂、聚醯胺基胺樹脂、聚醯胺樹脂所組成的組群中的任一種以上:0.1質量%~10質量%。
- 如申請專利範圍第1項所述之容器用樹脂包覆金屬板,其中上述(iv)環氧樹脂是雙酚A以外的環氧樹脂。
- 如申請專利範圍第1項或第2項所述之容器用樹脂 包覆金屬板,其中上述樹脂包覆層(A)包含:上述樹脂層(a1)、及形成於該樹脂層(a1)的上層的聚酯膜(a2)。
- 如申請專利範圍第1項或第2項所述之容器用樹脂包覆金屬板,其中上述(i)聚酯樹脂的數量平均分子量為3000~100000,且為下述(i-1)~(i-3)中任一種以上:(i-1)玻璃轉移溫度為0℃以上且小於35℃的聚酯樹脂,(i-2)玻璃轉移溫度為35℃以上且小於65℃的聚酯樹脂,(i-3)玻璃轉移溫度為65℃以上且小於100℃的聚酯樹脂。
- 如申請專利範圍第4項所述之容器用樹脂包覆金屬板,其中形成上述(i)聚酯樹脂的各聚酯樹脂的比率滿足下述:玻璃轉移溫度為0℃以上且小於35℃的聚酯樹脂:30質量%~70質量%,玻璃轉移溫度為35℃以上且小於65℃的聚酯樹脂:10質量%~35質量%,玻璃轉移溫度為65℃以上且小於100℃的聚酯樹脂:10質量%~35質量%。
- 如申請專利範圍第1項或第2項所述之容器用樹脂包覆金屬板,其中上述(i)聚酯樹脂是含有源自雙酚酸的重複單元的聚酯樹脂。
- 如申請專利範圍第1項或第2項所述之容器用樹脂 包覆金屬板,其中上述(iii)金屬烷氧化物系化合物及/或金屬螯合化合物是鈦烷氧化物系化合物及/或鈦螯合化合物。
- 如申請專利範圍第3項所述之容器用樹脂包覆金屬板,其中上述聚酯膜(a2)是聚酯樹脂的結構單元的85質量%以上為對苯二甲酸乙二酯單元及/或萘二甲酸乙二酯單元的雙軸延伸聚酯膜,且該雙軸延伸聚酯膜含有無機粒子及/或有機粒子。
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AU2012313653B2 (en) | 2015-01-22 |
AU2012313653A1 (en) | 2014-04-24 |
CN103826846A (zh) | 2014-05-28 |
EP2762304A1 (en) | 2014-08-06 |
MY168765A (en) | 2018-12-04 |
WO2013046687A1 (ja) | 2013-04-04 |
JPWO2013046687A1 (ja) | 2015-03-26 |
US20140227529A1 (en) | 2014-08-14 |
EP2762304B1 (en) | 2016-06-08 |
US9751283B2 (en) | 2017-09-05 |
TW201318839A (zh) | 2013-05-16 |
EP2762304A4 (en) | 2015-06-03 |
CN103826846B (zh) | 2016-08-17 |
JP5541420B2 (ja) | 2014-07-09 |
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