TWI819997B - 乙烯-乙烯醇系共聚物組成物丸粒及該乙烯-乙烯醇系共聚物組成物丸粒的製造方法 - Google Patents
乙烯-乙烯醇系共聚物組成物丸粒及該乙烯-乙烯醇系共聚物組成物丸粒的製造方法 Download PDFInfo
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- TWI819997B TWI819997B TW105142179A TW105142179A TWI819997B TW I819997 B TWI819997 B TW I819997B TW 105142179 A TW105142179 A TW 105142179A TW 105142179 A TW105142179 A TW 105142179A TW I819997 B TWI819997 B TW I819997B
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- Prior art keywords
- ethylene
- vinyl alcohol
- alcohol copolymer
- resin
- pellets
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Abstract
本發明之目的係提供著色減低的乙烯-乙烯醇系共聚物組成物丸粒。本發明之乙烯-乙烯醇系共聚物組成物丸粒,含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C),對於該丸粒以分光色差計利用穿透法進行測定而得之黃色度(Yellow Index,YI)値為10以下。
Description
本發明關於著色受到抑制的乙烯-乙烯醇系共聚物組成物丸粒及該乙烯-乙烯醇系共聚物組成物丸粒的製造方法。
乙烯-乙烯醇系共聚物(以下有時稱為「EVOH樹脂」。)係易於排列的結構,因存在於高分子側鏈的羥基彼此間的氫鍵而有非常強的分子間作用力,所以結晶性高,而且即使在非晶部分,分子間作用力仍高,因此氧氣等氣體分子難以通過EVOH樹脂,使用EVOH樹脂而得之薄膜等展現優異的氣體阻隔性。
人們已利用EVOH樹脂之優異的氣體阻隔性,將其成形為食品包裝材料、醫藥品包裝材料、工業藥品包裝材料、農藥包裝材料等之薄膜或片或者瓶等容器等來利用。
EVOH樹脂如上述展現優異的氣體阻隔性,但不耐水,若被水潤濕或處於濕度高的狀況下,其氣體阻隔性降低。因此,使用於加壓加熱用之包裝材料等時,一般會將EVOH樹脂層配置於中間層並以聚烯烴樹脂層等予以包夾而做成多層結構。而且,就EVOH樹脂層而言也會在EVOH樹脂中混合尼龍等聚醯胺系樹脂,提高對於水的耐久性。
然而,由於在EVOH樹脂中混合聚醯胺系樹脂會使熱穩定性降低,所以在熔融混練時或熔融成形時變得易於形成熱劣化物、交聯物,而有成形物變色、魚眼(樹脂的微小粒)產生之情形。
就改善加熱熔融時之熱穩定性的技術而言,例如,有人於專利文獻1提案:一種樹脂組成物,由乙烯-乙酸乙烯酯共聚物皂化物(A)、利用末端調整劑調整末端COOH基之數目(x)與末端CONRR´基(惟,R為碳數1~22之烴基,R´為H或碳數1~22之烴基)之數目(y)之比例而得之末端調整聚醯胺系樹脂(B)、受阻苯酚系化合物(C)、及脂肪族羧酸鹼土金屬鹽(D)構成。專利文獻1記載:藉由在EVOH樹脂與聚醯胺系樹脂之混合物中加入脂肪族羧酸鹼土金屬鹽,熱穩定性提高,凝膠之產生受到抑制,長時運轉(long-run)成形變得可能。
另一方面,就減低熱熔融時之EVOH樹脂組成物著色之方法而言,一般係調整在利用擠製機使其熔融而製造丸粒時的製造條件。例如,專利文獻2記載:在將混合有EVOH樹脂與聚烯烴系樹脂的樹脂組成物或混合有EVOH樹脂與聚醯胺系樹脂的樹脂組成物予以加熱熔融之際,使擠製機之螺桿長L(mm)與螺桿外徑D(mm)之比(L/D)、熔融擠製時之比能量、每一根模頭噴嘴之吐出量、加工溫度為特定範圍。專利文獻2記載:藉由使加熱熔融時之擠製條件為特定範圍,可獲得無凝膠產生、無著色之丸粒。 [先前技術文獻] [專利文獻]
[專利文獻1]日本特開平6-345919號公報 [專利文獻2]日本特開2003-276021號公報
[發明所欲解決之課題] 然而,專利文獻1記載的樹脂組成物在利用擠製機進行加熱熔融時有著色之傾向,得到的成形物有難以適用於要求透明性之用途之問題。又,專利文獻2記載的技術也無法獲得充分的著色抑制效果,需要進一步改良。
是以,本發明之目的係提供著色減低的乙烯-乙烯醇系共聚物組成物丸粒。 [解決課題之手段]
本案發明人鑑於上述實情努力進行了探討,結果了解到:含有EVOH樹脂、聚醯胺系樹脂及鹼土金屬鹽的樹脂組成物,從擠製機擠出後比其熔融混練時更會產生著色。從擠製機擠出後樹脂丸粒亦持續高溫狀態。本案發明人著眼於含有EVOH樹脂、聚醯胺系樹脂及鹼土金屬鹽的樹脂丸粒若為高溫則容易著色,並發現可藉由將剛從擠製機之模頭(吐出口之模具)吐出的樹脂溫度控制為低以獲得著色少的樹脂丸粒,乃至完成本發明。
亦即,本發明採以下(1)~(6)之構成。 (1)一種乙烯-乙烯醇系共聚物組成物丸粒,含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C),對於該丸粒以分光色差計利用穿透法進行測定而得之黃色度(Yellow Index,YI)値為10以下。 (2)如(1)之乙烯-乙烯醇系共聚物組成物丸粒,其中,該乙烯-乙烯醇系共聚物(A)與該聚醯胺系樹脂(B)之質量比((A)/(B))為60/40~98/2。 (3)如(1)或(2)之乙烯-乙烯醇系共聚物組成物丸粒,其中,該鹼土金屬鹽(C)之含有比例,相對於該乙烯-乙烯醇系共聚物(A)與該聚醯胺系樹脂(B)之總量,以金屬換算計為10~200ppm。 (4)如(1)至(3)中任一項之乙烯-乙烯醇系共聚物組成物丸粒,更含有抗氧化劑。 (5)一種乙烯-乙烯醇系共聚物組成物成形體,係如(1)至(4)中任一項之乙烯-乙烯醇系共聚物組成物丸粒熔融成形而得。 (6)一種乙烯-乙烯醇系共聚物組成物丸粒之製造方法,係以分光色差計利用穿透法進行測定時的黃色度(YI)値為10以下的乙烯-乙烯醇系共聚物組成物丸粒之製造方法, 包括以下步驟:使用熔融混練裝置將含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C)的樹脂組成物予以熔融混練; 使剛從該熔融混練裝置吐出的乙烯-乙烯醇系共聚物組成物股線之溫度為268℃以下。 [發明之效果]
依本發明,可提供黃色度(YI)値為10以下的著色減低的乙烯-乙烯醇系共聚物組成物丸粒,所以也可理想地用於要求透明性的成形物。
以下,就本發明之構成詳細地說明,但該等係例示理想的實施態樣之一例,並不限於該等內容。 另外,本說明書中,所有以質量表示的百分率或份,同以重量表示的百分率或份。
本發明之乙烯-乙烯醇系共聚物組成物丸粒之特徵為:含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C),且對於該丸粒以分光色差計利用穿透法進行測定而得之黃色度(YI)値為10以下。 以下就各成分加以說明。
<乙烯-乙烯醇系共聚物(A)> 本發明使用的乙烯-乙烯醇系共聚物(EVOH樹脂)為公知的樹脂,為非水溶性之熱塑性樹脂。EVOH樹脂,通常係將乙烯酯系單體與乙烯共聚合而得到乙烯-乙烯酯系共聚物,並將其予以皂化而得。亦即,以乙烯結構單元與乙烯醇結構單元為主,並包含皂化步驟後殘存的些許量之乙烯酯結構單元。在上述共聚合時,可採用溶液聚合法等公知的聚合法。
上述乙烯酯系單體,例如可列舉:乙酸乙烯酯、甲酸乙烯酯、丙酸乙烯酯、戊酸乙烯酯、丁酸乙烯酯、異丁酸乙烯酯、三甲基乙酸乙烯酯、癸酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯、叔碳酸(versatic acid)乙烯酯等脂肪族乙烯酯、苯甲酸乙烯酯等芳香族乙烯酯等;通常為碳數3~20,較佳為碳數4~10,尤佳為碳數4~7之脂肪族乙烯酯。其中,從經濟的觀點,使用乙酸乙烯酯較佳。該等通常單獨使用,但視需要也可同時使用多種。
EVOH樹脂之乙烯含量係在乙烯與乙烯酯系單體聚合時決定,於皂化前後並未有變化。根據ISO14663測得的乙烯結構單元之含有率通常為20~60莫耳%,較佳為25~50莫耳%,尤佳為25~45莫耳%。乙烯含量若過低,有耐衝擊性、加工性降低之傾向;若過高,有氣體阻隔性、耐溶劑性降低之傾向。
EVOH樹脂之皂化度為利用滴定法(JIS K6726)(惟,使用EVOH樹脂均勻地溶解於水/甲醇溶劑而得之溶液)測得之値,通常為90~100莫耳%,較佳為95~100莫耳%,尤佳為98~100%。皂化度若過低,有氣體阻隔性降低之傾向。
EVOH樹脂之熔體流動速率(以下有時稱為MFR。),以在210℃、負載2160g測得的値計,通常為0.1~100g/10分鐘,較佳為1~50g/10分鐘,更佳為2~40g/10分鐘。該値過高或過低時有加工性降低之傾向。
EVOH之熔點,以利用差示掃描熱量計(DSC)以升降溫速度10℃/min測得之値計,通常為100~220℃,較佳為120~210℃,更佳為140~200℃。
另外,本發明,除了乙烯與乙烯酯以外,尚可在不損害對於EVOH樹脂要求的特性之範圍(例如,未達10莫耳%)共聚合能共聚合的乙烯性不飽和單體,上述單體可列舉下列者。例如,可列舉:丙烯、1-丁烯、異丁烯等烯烴類、或2-丙烯-1-醇、3-丁烯-1-醇、4-戊烯-1-醇、5-己烯-1-醇、3,4-二羥基-1-丁烯、5-己烯-1,2-二醇等含有羥基的α-烯烴類、或其醯基化物、酯化物;酯化物可列舉3,4-二醯氧基-1-丁烯,尤其3,4-二乙醯氧基-1-丁烯等。又,可列舉:2-亞甲基丙烷-1,3-二醇、3-亞甲基戊烷-1,5-二醇等羥烷基亞乙烯類;1,3-二乙醯氧基-2-亞甲基丙烷、1,3-二丙醯氧基-2-亞甲基丙烷、1,3-二丁醯氧基-2-亞甲基丙烷等二乙酸羥烷基亞乙烯酯類。又,可列舉丙烯酸、甲基丙烯酸、巴豆酸、苯二甲酸(酐)、馬來酸(酐)、伊康酸(酐)等不飽和酸類或其鹽、及碳數1~18之單或二烷基酯類。又,可列舉丙烯醯胺、碳數1~18之N-烷基丙烯醯胺、N,N-二甲基丙烯醯胺、2-丙烯醯胺丙磺酸或其鹽、及丙烯醯胺丙基二甲基胺或其酸鹽或其4級鹽等丙烯醯胺類、甲基丙烯醯胺、碳數1~18之N-烷基甲基丙烯醯胺、N,N-二甲基甲基丙烯醯胺、2-甲基丙烯醯胺丙磺酸或其鹽、甲基丙烯醯胺丙基二甲基胺或其酸鹽及其4級鹽等甲基丙烯醯胺類。又,可列舉N-乙烯基吡咯烷酮、N-乙烯基甲醯胺、N-乙烯基乙醯胺等N-乙烯基醯胺類、丙烯腈、甲基丙烯腈等氰化乙烯類、碳數1~18之烷基乙烯基醚、羥烷基乙烯基醚、烷氧基烷基乙烯基醚等乙烯基醚類、氯乙烯、偏二氯乙烯、氟乙烯、偏二氟乙烯、溴乙烯等鹵化乙烯類、三甲氧基乙烯基矽烷等乙烯基矽烷類、及乙酸烯丙酯、氯丙烯、三甲基-(3-丙烯醯胺-3-二甲基丙基)-氯化銨、丙烯醯胺-2-甲基丙磺酸、碳酸乙烯基伸乙酯、甘油單烯丙醚等。又,也可經胺甲酸酯化、縮醛化、氰乙基化、氧伸烷基化等「後改性」。 尤其就需要延伸加工、真空・壓縮空氣成形等之二次成形性的用途而言,宜使用共聚合有含有羥基的α-烯烴類的EVOH,尤其於側鏈具有1,2-二醇的EVOH。
本發明使用之EVOH樹脂中因應目的也可包含其他熱塑性樹脂。包含其他熱塑性樹脂時,其他熱塑性樹脂之含量相對於樹脂組成物全體通常低於30質量%。
又,因應目的也可在不損害本發明之效果之範圍包含其他摻合劑成分。該等摻合劑之添加量相對於樹脂組成物通常低於5質量%。其他摻合成分,例如可列舉滑石、碳酸鈣、雲母、玻璃纖維等填料、石蠟油等塑化劑、抗氧化劑、熱穩定劑、光穩定劑、紫外線吸收劑、氧吸收劑、中和劑、潤滑劑、防霧劑、抗結塊劑、滑爽劑、交聯劑、交聯助劑、著色劑、阻燃劑、分散劑、界面活性劑、乾燥劑、抗靜電劑、抗菌劑、硬化劑、發泡劑、結晶成核劑、生物降解用添加劑、螢光增白劑、矽烷偶聯劑等,可含有任意摻合劑1種或2種以上。
該能夠含有的樹脂及摻合劑意指係對於樹脂成分均勻添加(係丸粒內部均勻添加)。
就上述熱穩定劑而言,基於提高熔融成形時之熱穩定性等各種物性之目的,也可添加:乙酸、丙酸、丁酸、月桂酸、硬脂酸、油酸、二十二酸等有機酸類或該等之鹼金屬鹽(鈉、鉀等)等鹼土金屬鹽以外之鹽;或硫酸、亞硫酸、碳酸、磷酸、硼酸等無機酸類、或該等之鹼金屬鹽(鈉、鉀等)、鋅鹽等鹼土金屬鹽以外之鹽等添加劑。該等之中,添加乙酸、包含硼酸及其鹽的硼化合物、乙酸鹽、磷酸鹽尤佳。
添加乙酸時,其添加量相對於EVOH樹脂100質量份通常為0.001~1質量份,較佳為0.005~0.2質量份,尤佳為0.01~0.1質量份。乙酸之添加量若過少,有無法充分獲得乙酸之含有效果之傾向;反之若過多,有變得難以獲得均勻的薄膜之傾向。
又,添加硼化合物時,其添加量,相對於EVOH樹脂100質量份以硼換算(灰化後以ICP發光分析法分析)計通常為0.001~1質量份,較佳為0.002~0.2質量份,尤佳為0.005~0.1質量份。硼化合物之添加量若過少,有時無法充分獲得硼化合物之添加效果;反之若過多,有變得難以獲得均勻的薄膜之傾向。
又,乙酸鹽、磷酸鹽(包括磷酸氫鹽)之添加量,相對於EVOH樹脂(A)100質量份以金屬換算(灰化後以ICP發光分析法分析)計通常為0.0005~0.1質量份,較佳為0.001~0.05質量份,尤佳為0.002~0.03質量份。該添加量若過少,有時無法充分獲得其含有效果;反之若過多,有變得難以獲得均勻的薄膜之傾向。另外,對於EVOH樹脂添加2種以上之鹽時,其總量宜在上述添加量之範圍內。
就於EVOH樹脂中添加乙酸、硼化合物、乙酸鹽、磷酸鹽的方法不特別限定,可列舉以下方法:i)使含水率20~80質量%之EVOH樹脂之多孔性析出物與添加物之水溶液接觸而使其含有添加物後予以乾燥之方法;ii)使EVOH樹脂之均勻溶液(水/醇溶液等)含有添加物後,股線狀地擠製到凝固液中,接著將得到的股線切斷而做成丸粒,再進行乾燥處理之方法;iii)一併混合EVOH樹脂與添加物後利用擠製機等予以熔融混練之方法;iv)於製造EVOH樹脂時,以乙酸等有機酸類中和在皂化步驟使用的鹼(氫氧化鈉、氫氧化鉀等),再藉由水洗處理調整殘存的乙酸等有機酸類、副生成的鹽之量的方法等。 為了更顯著地獲得本發明之效果,添加物之分散性優異的i)、ii)之方法較佳,使其含有有機酸及其鹽時併用iv)之方法較佳。
該EVOH樹脂通常以丸粒形狀流通市場,供應於各種熔融成形。該丸粒之形狀例如有球形、圓柱形、立方體形、直方體形等,但通常為球狀(橄欖球狀)或圓柱形,其大小,從後續作為成形材料使用時之便利性之觀點,當為球狀時直徑通常為1~6mm,較佳為2~5mm,高度通常為1~6mm,較佳為2~5mm,當為圓柱狀時底面之直徑通常為1~6mm,較佳為2~5mm,長度通常為1~6mm,較佳為2~5mm。
<聚醯胺系樹脂(B)> 本發明使用的聚醯胺系樹脂(B)為公知的樹脂,為非水溶性之熱塑性樹脂。
聚醯胺系樹脂,例如可列舉:聚己內醯胺(尼龍6)、聚-ω-胺基庚酸(尼龍7)、聚-ω-胺基壬酸(尼龍9)、聚十一醯胺(尼龍11)、聚月桂內醯胺(尼龍12)等脂肪族聚醯胺系樹脂。又共聚合聚醯胺系樹脂,可列舉:聚乙二胺己二醯胺(尼龍26)、聚四亞甲基己二醯胺(尼龍46)、聚六亞甲基己二醯胺(尼龍66)、聚六亞甲基癸二醯胺(尼龍610)、聚六亞甲基十二烷二醯胺(尼龍612)、聚八亞甲基己二醯胺(尼龍86)、聚十亞甲基己二醯胺(尼龍108)、己內醯胺/月桂內醯胺共聚物(尼龍6/12)、己內醯胺/ω-胺基壬酸共聚物(尼龍6/9)、己內醯胺/己二酸六亞甲基二胺共聚物(尼龍6/66)、月桂內醯胺/己二酸六亞甲基二胺共聚物(尼龍12/66)、乙二胺己二醯胺/己二酸六亞甲基二胺共聚物(尼龍26/66)、己內醯胺/己二酸六亞甲基二胺/癸二酸六亞甲基二胺共聚物(尼龍66/610)、己二酸伸乙胺/己二酸六亞甲基二胺/癸二酸六亞甲基二胺共聚物(尼龍6/66/610)等脂肪族共聚合聚醯胺、聚六亞甲基間苯二甲醯胺、聚六亞甲基對苯二甲醯胺、聚間苯二甲基己二醯胺、六亞甲基間苯二甲醯胺/對苯二甲醯胺共聚物、聚對伸苯基對苯二甲醯胺、聚對伸苯基3,4’-二苯基醚對苯二甲醯胺等芳香族共聚合聚醯胺、非晶性聚醯胺、對於上述聚醯胺系樹脂以亞甲基苄胺、間二甲苯二胺等之羧基、胺基進行末端改性而得之末端改性聚醯胺等。 該等聚醯胺系樹脂可單獨使用1種或組合2種以上使用。其中,從做成EVOH樹脂組成物並將其作為多層薄膜之中間層使用時之耐加壓加熱性之觀點,宜使用尼龍6。
聚醯胺系樹脂(B),以熔點通常為150~270℃,較佳為180~250℃,更佳為200~230℃者較理想。又,熔體流動速率(MFR)於230℃、負載2160g下通常為0.1~100g/10分鐘,較佳為1~50g/10分鐘,更佳為3~20g/10分鐘。
<鹼土金屬鹽(C)> 本發明使用的鹼土金屬鹽(C),例如可列舉:鹼土金屬之乙酸鹽、丙酸、丁酸、月桂酸、硬脂酸、油酸、二十二酸等之脂肪族羧酸鹽、檸檬酸鹽等有機酸鹽;鹼土金屬之硼酸鹽、鹼土金屬之碳酸鹽、鹼土金屬之碳酸氫鹽、鹼土金屬之磷酸鹽等無機酸鹽等。 鹼土金屬之乙酸鹽,例如可列舉乙酸鎂、乙酸鈣、乙酸鋇等。 鹼土金屬之碳酸鹽,例如可列舉碳酸鈣、碳酸鎂、碳酸鋇等。 鹼土金屬之碳酸氫鹽,例如可列舉碳酸氫鈣、碳酸氫鎂、碳酸氫鋇等。 鹼土金屬之磷酸鹽,例如可列舉磷酸二氫鈣、磷酸一氫鎂、磷酸氫鋇等。 該等鹼土金屬鹽可單獨含有1種或以組合2種以上之方式含有。 其中,從EVOH樹脂之生產性之觀點,較佳為水溶性鹽。再者,從將EVOH樹脂組成物予以熔融成形時之成形性之觀點,鹼土金屬鹽以使用有機酸鹽較佳,使用碳數1~6之脂肪族羧酸鹽更佳,特佳係使用乙酸鎂。
本發明中,乙烯-乙烯醇系共聚物(A)與聚醯胺系樹脂(B)之質量比((A)/(B))較佳為60/40~98/2。可藉由使乙烯-乙烯醇系共聚物(A)與聚醯胺系樹脂(B)之質量比為前述範圍以獲得耐加壓加熱性優異之EVOH樹脂組成物。乙烯-乙烯醇系共聚物(A)與聚醯胺系樹脂(B)之質量比更佳為70/30~95/5,又更佳為80/20~90/10。
又,鹼土金屬鹽(C)之含有比例,相對於乙烯-乙烯酯系共聚物(A)與聚醯胺系樹脂(B)之總量,以金屬換算計較佳為10~200ppm,更佳為10~100ppm,又更佳為10~50ppm。鹼土金屬鹽(C)之含有比例若過多,有丸粒中產生凝膠或發泡、著色,或成形性變得不穩定之傾向;若過少,有熔融黏度變得容易上升之傾向。
本發明之乙烯-乙烯醇系共聚物組成物丸粒中宜摻合抗氧化劑。可藉由含有抗氧化劑以提高成形加工時之熱穩定性。
抗氧化劑可列舉苯酚系抗氧化劑、胺系抗氧化劑、胺基醚系抗氧化劑、磷系抗氧化劑、硫系抗氧化劑等。
苯酚系抗氧化劑,例如可列舉:2,6-二第三丁基-對甲酚、2,6-二第三丁基-4-乙基苯酚、2,6-二環己基-4-甲基苯酚、2,6-二異丙基-4-乙基苯酚、2,6-二第三戊基-4-甲基苯酚、2,6-二第三辛基-4-正丙基苯酚、2,6-二環己基-4-正辛基苯酚、2-異丙基-4-甲基-6-第三丁基苯酚、2-第三丁基-4-乙基-6-第三辛基苯酚、2-異丁基-4-乙基-6-第三己基苯酚、2-環己基-4-正丁基-6-異丙基苯酚、苯乙烯化混合甲酚、DL-α-生育酚、β-(3,5-二第三丁基-4-羥基苯基)丙酸硬脂酯等單環苯酚化合物;2,2´-亞甲基雙(4-甲基-6-第三丁基苯酚)、4,4´-亞丁基雙(3-甲基-6-第三丁基苯酚)、4,4´-硫雙(3-甲基-6-第三丁基苯酚)、2,2´-硫雙(4-甲基-6-第三丁基苯酚)、4,4´-亞甲基雙(2,6-二第三丁基苯酚)、2,2´-亞甲基雙[6-(1-甲基環己基)-對甲酚]、2,2´-亞乙基雙(4,6-二第三丁基苯酚)、2,2´-亞丁基雙(2-第三丁基-4-甲基苯酚)、3,6-二氧雜八亞甲基雙[3-(3-第三丁基-4-羥基-5-甲基苯基)丙酸酯]、三乙二醇雙[3-(3-第三丁基-5-甲基-4-羥基苯基)丙酸酯]、1,6-己二醇雙[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]、2,2´-硫代二伸乙基雙[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]等2環苯酚化合物;1,1,3-參(2-甲基-4-羥基-5-第三丁基苯基)丁烷、1,3,5-參(2,6-二甲基-3-羥基-4-第三丁基苄基)異氰尿酸酯、1,3,5-參[(3,5-二第三丁基-4-羥基苯基)丙醯氧基乙基]異氰尿酸酯、參(4-第三丁基-2,6-二甲基-3-羥基苄基)異氰尿酸酯、1,3,5-三甲基-2,4,6-參(3,5-二第三丁基-4-羥基苄基)苯等3環苯酚化合物;肆[亞甲基-3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]甲烷、季戊四醇-肆[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]等4環苯酚化合物;雙(3,5-二第三丁基-4-羥基苄基膦酸乙基)鈣、雙(3,5-二第三丁基-4-羥基苄基膦酸乙基)鎳等含磷苯酚化合物;等。
胺系抗氧化劑,例如可列舉:雙(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、琥珀酸二甲酯與1-(2-羥基乙基)-4-羥基-2,2,6,6-四甲基哌啶乙醇之縮聚物、N,N´,N´´,N´´´-肆-[4,6-雙-{丁基-(N-甲基-2,2,6,6-四甲基哌啶-4-基)胺基}-三-2-基]-4,7-二氮雜癸烷-1,10-二胺、二丁基胺-1,3,5-三-N,N´-雙(2,2,6,6-四甲基-4-哌啶基-1,6-六亞甲基二胺)與N-(2,2,6,6-四甲基-4-哌啶基)丁基胺之縮聚物、聚[{6-(1,1,3,3-四甲基丁基)胺基-1,3,5-三-2,4-二基}{(2,2,6,6-四甲基-4-哌啶基)亞胺基}六亞甲基{(2,2,6,6-四甲基-4-哌啶基)亞胺基}]、肆(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、2,2,6,6-四甲基-4-哌啶基苯甲酸酯、雙-(1,2,6,6-五甲基-4-哌啶基)-2-(3,5-二第三丁基-4-羥基苄基)-2-正丁基丙二酸酯、雙-(N-甲基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、1,1´-(1,2-乙烷二基)雙(3,3,5,5-四甲基哌酮)、(混合2,2,6,6-四甲基-4-哌啶基/十三烷基)-1,2,3,4-丁烷四羧酸酯、(混合1,2,2,6,6-五甲基-4-哌啶基/十三烷基)-1,2,3,4-丁烷四羧酸酯、混合[2,2,6,6-四甲基-4-哌啶基/β,β,β´,β´-四甲基-3,9-{2,4,8,10-四氧雜螺(5,5)十一烷}二乙基]-1,2,3,4-丁烷四羧酸酯、混合[1,2,2,6,6-五甲基-4-哌啶基/β,β,β´,β´-四甲基-3,9-{2,4,8,10-四氧雜螺(5,5)十一烷}二乙基]-1,2,3,4-丁烷四羧酸酯、N,N´-雙(3-胺基丙基)乙二胺-2,4-雙[正丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)胺基]-6-氯-1,3,5-三縮合物、聚[6-N-啉基-1,3,5-三-2,4-二基][(2,2,6,6-四甲基-4-哌啶基)亞胺基]六亞甲基[(2,2,6,6-四甲基-4-哌啶基)醯亞胺]、N,N´-雙(2,2,6,6-四甲基-4-哌啶基)六亞甲基二胺與1,2-二溴乙烷之縮合物、N-(2,2,6,6-四甲基-4-哌啶基)-2-甲基等。
胺基醚系抗氧化劑,例如可列舉:雙(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯、雙(1-甲氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-乙氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-丙氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-丁氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-戊氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-己氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-庚氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-壬氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-癸氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(1-十二烷氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯等。
磷系抗氧化劑,例如可列舉:亞磷酸三苯酯、亞磷酸二苯基異癸酯、亞磷酸苯基二異癸酯、4,4´-亞丁基-雙(3-甲基-6-第三丁基苯基二(十三烷基))亞磷酸酯、環新戊四基雙(壬基苯基)亞磷酸酯、環新戊四基雙(二壬基苯基)亞磷酸酯、環新戊四基參(壬基苯基)亞磷酸酯、環新戊四基參(二壬基苯基)亞磷酸酯、10-(2,5-二羥基苯基)-10H-9-氧雜-10-磷雜菲(phosphaphenanthrene)-10-氧化物、二異癸基季戊四醇二亞磷酸酯、參(2,4-二第三丁基苯基)亞磷酸酯等。
硫系抗氧化劑,例如可列舉:硫代二丙酸二月桂酯、硫代二丙酸二(十三烷)酯、硫代二丙酸二硬脂酯、季戊四醇肆(3-十二烷基硫代丙酸酯)、4,4-硫雙(2-第三丁基-5-甲基苯酚)雙-3-(十二烷基硫代)丙酸酯、3,3´-硫代二丙酸二肉豆蔻酯、月桂基-硬脂基-3,3´-硫代二丙酸酯、新戊四基肆(3-月桂基硫代丙酸酯)等。
該等抗氧化劑可單獨使用1種或併用2種以上。其中,從成形加工時之熱穩定性之觀點,較佳係使用苯酚系抗氧化劑,更佳係使用受阻苯酚系抗氧化劑。
抗氧化劑之含量,相對於EVOH系樹脂(A)與聚醯胺系樹脂(B)之總量100質量份,較佳為0.1~200ppm,更佳為1~100ppm,又更佳為1~50ppm。抗氧化劑之含量若為前述範圍,成形加工時之熱穩定性變得良好。
可在不損及本發明之效果之範圍對於本發明之乙烯-乙烯醇系共聚物組成物丸粒摻合其他添加物。 其他添加物,例如可列舉:塑化劑、穩定劑、填料、著色劑、潤滑劑、抗結塊劑、抗靜電劑等。
本發明之乙烯-乙烯醇系共聚物組成物丸粒之特徵為:使用分光色差計利用穿透法進行測定而得之黃色度(YI)値為10以下。 藉由黃色度(YI)値為10以下,可確保樹脂丸粒之透明性。黃色度(YI)値為8以下更佳。 該測定,例如可將丸粒填充於直徑35mm×高度30mm之圓柱型玻璃製單元而製作成測定用樣品,並依據JISZ-8722對於該樣品以分光色差計利用穿透法進行測定。
<乙烯-乙烯醇系共聚物組成物丸粒之製造方法> 本發明之乙烯-乙烯醇系共聚物組成物丸粒之製造方法不特別限定。 摻合上述(A)~(C)成分之方法,可列舉:(1)於預先摻合有乙烯-乙烯醇系共聚物(A)與鹼土金屬鹽(C)之組成物中摻合聚醯胺系樹脂(B)之方法,(2)於預先摻合有聚醯胺系樹脂(B)與鹼土金屬鹽(C)之組成物中摻合乙烯-乙烯醇系共聚物(A)之方法,(3)一併摻合乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C)之方法等。就EVOH樹脂之物性改善效果與生產性之觀點,較佳為(1)之方法。 另外,該(1)之方法,可列舉:i)使含水率20~80質量%之EVOH樹脂之多孔性析出物與鹼土金屬鹽(C)之水溶液接觸後予以乾燥之方法;ii)使EVOH樹脂之均勻溶液(水/醇溶液等)含有鹼土金屬鹽(C)後,股線狀地擠製到凝固液中,接著將獲得之股線切斷而做成丸粒,並予以乾燥之方法;iii)一併混合EVOH樹脂與鹼土金屬鹽(C)後以擠製機等予以熔融混練之方法。就EVOH樹脂之物性改善效果與生產性之觀點,較佳為i)之方法。
本發明之乙烯-乙烯醇系共聚物組成物丸粒,可藉由以下方式獲得:以上述方式摻合乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C),將獲得之組成物利用熔融混練裝置予以熔融混練,並將剛從熔融混練裝置吐出之樹脂溫度調節成比以往更低。
本案發明人著眼於將含有EVOH樹脂、聚醯胺系樹脂及鹼土金屬鹽的樹脂組成物熔融混練時,因在高溫狀態與空氣接觸而導致著色加劇。其原因推測係:為了各種的物性改善而需要在EVOH樹脂與聚醯胺系樹脂之樹脂組成物中摻合鹼土金屬鹽,但該鹼土金屬鹽會成為觸媒而容易使樹脂組成物之劣化加劇。因此,本案發明人著眼於剛從擠製機吐出之溫度,發現藉由將該溫度調整成比以往更低,可抑制EVOH樹脂與聚醯胺系樹脂之樹脂組成物之劣化加劇,並獲得著色少的樹脂丸粒,乃至完成本發明。
熔融混練裝置,可列舉混練機、擠製機、混合輥、班布里混合機、Kneader-Rudder捏合機、Plasto Mill混練機等,尤其使用能夠連續處理且混合效率優異的擠製機之方法較理想。
擠製機可使用單軸擠製機、雙軸擠製機中之任一種,其中,雙軸擠製機,尤其螺桿旋轉方向為同方向之雙軸擠製機,就可藉由適度的剪切而獲得充分的混練之觀點較為理想。
擠製機之螺桿有效長(L/D),通常為10~100,較佳為15~70,更佳為40~60。L/D若過小,有熔融混練變得不充分,均勻分散性變得不充分之情形。另一方面,L/D若過大,有因過度剪切或過度滯留而引起因剪切發熱所致之分解之傾向。擠製機之螺桿之捏合區之L/D,當捏合區有多數個時以其總和計,通常為3~15,較佳為5~10,尤佳為5~8。捏合區之L/D為上述範圍時,有變得容易調節成後述所希望之溫度之傾向。
螺桿轉速,通常為100~1000rpm,較佳為300~800rpm,更佳為400~600rpm。螺桿轉速若過小,有吐出變得不穩定之傾向;若過大,無法使剛從擠製機吐出的樹脂溫度成為268℃以下,丸粒有產生著色之情形。
模頭(吐出口之模具)之形狀通常為圓形。其直徑之大小通常為1~10mm,較佳為3~5mm,尤佳為3.5~4.5mm。該直徑過大時,由於股線不穩定,有生產性降低之傾向;過小時,有變得難以調整成後述所希望之溫度之傾向。
擠製機內之熔融時之組成物之溫度,通常為150~300℃,較佳為180~290℃,更佳為200~280℃。組成物之溫度若過低,熔融混練變得不充分,有無法獲得均勻的樹脂丸粒之情形。另一方面,組成物之溫度若過高,無法將剛從擠製機吐出的樹脂溫度調低,丸粒有產生著色之情形。 另外,組成物之溫度調整,通常可藉由適宜地設定擠製機內之缸筒之溫度、及螺桿轉速以進行。
剛從擠製機等熔融混練裝置吐出之樹脂丸粒(股線狀之混練物)之溫度為較以往更低的溫度。該溫度,通常為聚醯胺系樹脂(B)之熔點+5~48℃,較佳為聚醯胺系樹脂(B)之熔點+10~40℃,特佳為聚醯胺系樹脂(B)之熔點+20~30℃。該熔點,例如可藉由對於聚醯胺系樹脂以差示掃描熱量分析計(DSC)進行測定以獲得。 又,剛從擠製機等熔融混練裝置吐出的樹脂丸粒(股線狀之混練物)之溫度,通常為268℃以下,較佳為230~266℃,更佳為240~266℃。可藉由將剛吐出之丸粒(股線)之溫度調整於該範圍以獲得著色產生減低的乙烯-乙烯醇系共聚物組成物丸粒。
將剛吐出之樹脂溫度調整於上述範圍之方法不特別限定,當使用擠製機作為熔融混練裝置時,可列舉:調整擠製機之轉筒溫度之方法、降低擠製機之模頭(吐出口之模具)緊鄰之溫度之方法、對於剛從擠製機之模頭吐出之丸粒吹送冷風之方法、將剛從擠製機之模頭吐出之股線予以水冷之方法、使用擠製機之螺桿之捏合區之數目少的螺桿之方法、使用擠製機之螺桿之捏合區之L/D小的螺桿之方法、加大擠製機之模頭(吐出口之模具)直徑之方法等;可藉由調節該等要素以綜合地調整剛吐出之樹脂溫度。
對於以上述方式獲得之乙烯-乙烯醇系共聚物組成物丸粒以分光色差計利用穿透法進行測定時之黃色度(YI)値為10以下,可獲得著色減低的成形體。
另外,本發明中,熔融擠製時之比能量(kWh/kg)較佳為0.1~0.5之範圍。比能量若未達0.1,有熔融混練無法充分進行之情形;反之若超過0.5,有樹脂組成物熱劣化而導致著色,或獲得之丸粒所形成的成形物中常產生魚眼之情形。另外,該値可藉由將擠製機之螺桿馬達之電力値除以擠製機之吐出量以求得。
本發明之乙烯-乙烯醇系共聚物組成物丸粒,可藉由熔融成形製作成例如膜、片等薄膜、袋、杯、盤、管、瓶、槽等中空容器、蓋材等各種成形物。
該熔融成形方法,例如可列舉T模擠製、充氣吹脹擠製、吹塑成形、熔融紡紗、異型擠製等擠製成形法、射出成形法等。該熔融成形溫度通常為190~250℃。
可將本發明之乙烯-乙烯醇系共聚物組成物丸粒予以熔融成形並以單層之形式形成各種成形物,但從在水存在下使用時防止氣體阻隔性降低、提高機械強度等觀點,較佳係以對於EVOH樹脂組成物層疊層EVOH樹脂以外之熱塑性樹脂層而得之多層結構體之形式供應於各種成形物。
構成EVOH樹脂以外之熱塑性樹脂層的熱塑性樹脂(以下,有時稱為「其他熱塑性樹脂」。),具體而言,可列舉:直鏈狀低密度聚乙烯、低密度聚乙烯、超低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、乙烯-α-烯烴(碳數4~20之α-烯烴)共聚物等聚乙烯系樹脂、聚丙烯、丙烯-α-烯烴(碳數4~20之α-烯烴)共聚物等聚丙烯系樹脂、乙烯-乙酸乙烯酯共聚物、離子聚合物、乙烯-丙烯(嵌段及無規)共聚物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物聚丁烯、聚戊烯等烯烴之均聚物或共聚物、或將該等烯烴之均聚物或共聚物以不飽和羧酸或其酯接枝改性而得者等廣義之聚烯烴系樹脂;聚酯系樹脂;聚醯胺系樹脂(亦包括共聚合聚醯胺);聚氯乙烯;聚偏二氯乙烯;丙烯酸系樹脂;聚苯乙烯;乙烯酯系樹脂;聚酯彈性體;聚胺酯彈性體;氯化聚乙烯;氯化聚丙烯;芳香族或脂肪族多酮;進一步將該等還原而得之多元醇類。 其中,基於抑制樹脂組成物之氣體阻隔性降低之目的,較佳係使用疏水性樹脂,具體而言聚烯烴系樹脂為較佳,尤其聚乙烯系樹脂、聚丙烯系樹脂為較佳。
上述EVOH樹脂組成物層及其他熱塑性樹脂層,也可於多層結構體中各具有2層以上。
上述EVOH樹脂組成物層及其他熱塑性樹脂層,也可進一步在EVOH樹脂組成物層與其他熱塑性樹脂層之間介隔黏著樹脂層。 黏著樹脂層,例如可列舉藉由加成反應或接枝反應等使不飽和羧酸或其酸酐化學性地鍵結至烯烴系聚合物(上述之聚烯烴系樹脂)而得之含有羧基的改性烯烴系聚合物。具體而言,可列舉選自馬來酸酐接枝改性聚乙烯、馬來酸酐接枝改性聚丙烯、馬來酸酐接枝改性乙烯-丙烯(嵌段及無規)共聚物、馬來酸酐接枝改性乙烯-丙烯酸乙酯共聚物、馬來酸酐接枝改性乙烯-乙酸乙烯酯共聚物等中之1種或2種以上之混合物為較佳。此時,熱塑性樹脂中含有的不飽和羧酸或其酸酐之量通常為0.001~3質量%,較佳為0.01~1質量%,尤佳為0.03~0.5質量%。改性物中之改性量若少,有黏著性變得不充分之傾向;反之若多,會引起交聯反應,有成形性變差之傾向。
另外,其他熱塑性樹脂層、黏著樹脂層中也可含有通常會摻合的公知的抗氧化劑、抗靜電劑、塑化劑、潤滑劑、成核劑、抗結塊劑、蠟等。
上述多層結構體含有至少1層本發明之EVOH樹脂組成物層即可,其構成不特別限定,但基於防止因水分導致之樹脂組成物之氣體阻隔性能降低之目的,本發明之EVOH樹脂組成物層宜為中間層。而且,其他熱塑性樹脂層宜為外側層。亦即,例如將多層結構體做成包裝物時,其他熱塑性樹脂層(尤其疏水性樹脂層)會成為與內包物接觸之層,及與外部空氣接觸之層。
多層結構體之層構成,令本發明之EVOH樹脂組成物層為a(a1、a2、・・・)且其他熱塑性樹脂層為b(b1、b2、・・・)時,通常為3~20層,較佳為3~15層,尤佳為3~10層。例如具體而言,可為b/a/b、a/b/a、a1/a2/b、a/b1/b2、b2/b1/a/b1/b2、b2/b1/a/b1/a/b1/b2等任意之組合。 又,該多層結構體可設置將在製造該多層結構體之過程產生的端部或不良品等再熔融成形而得之包含EVOH樹脂組成物與EVOH樹脂以外之熱塑性樹脂之混合物的再生(recycle)層。令該再生層為R時,多層結構體之層構成例如可列舉b/a/R、R/b/a、b/R/a/b、b/R/a/R/b、b/a/R/a/b、b/R/a/R/a/R/b等。 尤其設置再生層,就能有效地活用成形時產生的大量廢料之觀點,係工業上較佳。
多層結構中的各層之厚度,可依層構成、用途或容器形態、所要求之物性等予以調節。例如下列。另外,下列數値,當EVOH樹脂組成物層、黏著性樹脂層、其他熱塑性樹脂層中至少1種之層存在2層以上時,採用其中最厚的層之厚度。
本發明之EVOH樹脂組成物層通常為1~500μm,較佳為3~300μm,更佳為5~200μm。EVOH樹脂組成物層過薄時,有氣體阻隔性降低之傾向;EVOH樹脂組成物層過厚時,有獲得之成形物之柔軟性、二次加工性降低之傾向。 其他熱塑性樹脂層通常為10~6000μm,較佳為20~4000μm,尤佳為100~2000μm。其他熱塑性樹脂層過薄時,有獲得之成形物之剛性降低之傾向;其他熱塑性樹脂層過厚時,有獲得之成形物之柔軟性、二次加工性降低之傾向。 黏著性樹脂層通常為1~100μm,較佳為2~50μm,尤佳為5~40μm。 又,各層之厚度比,EVOH樹脂組成物層/其他熱塑性樹脂層之厚度比通常為0.005以上未達1,較佳為0.01以上未達1,尤佳為0.02~0.2,樹脂組成物層/黏著性樹脂層之厚度比通常為0.2~100,較佳為1~10,尤佳為1~5。
上述多層結構體也可進一步以公知的方法進行延伸處理。 另外,針對延伸,可為公知的延伸方法,例如可列舉單軸延伸、雙軸延伸等。加熱延伸方法,可採用輥延伸法、拉幅機延伸法、管狀延伸法、共射出延伸吹塑法、深抽拉成形法、真空成形法、壓縮空氣成形法、真空壓縮空氣成形法、柱塞輔助式真空壓縮空氣成形法等。雙軸延伸時也可採用同時雙軸延伸方式、逐次雙軸延伸方式中之任一方式。共射出延伸吹塑法之情況也可採用冷型坏法、熱型坏法中之任一方式。延伸溫度,以多層結構體之溫度(多層結構體附近之溫度)計,通常選自約80~200℃,較佳係選自約100~160℃之範圍。延伸倍率,以面積比計,通常為2~100倍,較佳為2~50倍。
經延伸處理的多層結構體中的各層之厚度例如下列。EVOH樹脂組成物層通常為0.1~200μm,較佳為1~100μm。其他熱塑性樹脂層通常為1~1000μm,較佳為3~500μm。黏著性樹脂層通常為0.1~50μm,較佳為1~30μm。又,各層之厚度比,EVOH樹脂組成物層/其他熱塑性樹脂層之厚度比通常為0.0002以上未達1,較佳為0.01以上未達1,EVOH樹脂組成物層/黏著性樹脂層之厚度比為0.2~100,較佳為1~10。
如上述獲得之多層結構體可加工成膜、片等薄膜、袋及杯、盤、管、瓶、槽等中空容器、蓋材等之形狀之容器。 該容器作為一般食品、以及美乃滋、調味醬等調味料、味噌等發酵食品、沙拉油等油脂食品、飲料、化妝品、醫藥品、農藥品、工業藥品等各種的包裝容器係有用。 [實施例]
以下,舉實施例具體地說明本發明,但本發明只要不超過其要旨,不限於實施例之記載。 另外,例中之「份」、「%」,除非特別說明否則意指質量基準。
(實施例1) 使用:利用使含水EVOH之多孔性析出物與鹼土金屬鹽(C)之水溶液接觸後予以乾燥之方法獲得之含有以金屬換算計為35ppm之乙酸鎂作為鹼土金屬鹽(C)的EVOH樹脂(A)(乙烯含量29莫耳%,皂化度99.6莫耳%,MFR4.1g/10分鐘(210℃,負載2160g),熔點185.6℃)85份,作為聚醯胺系樹脂(B)之係尼龍6的「NOVAMID 1028EN」(商品名,三菱工程塑膠(股)公司製,熔點220℃)15份,及作為抗氧化劑之受阻苯酚系化合物(季戊四醇-肆[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]「Irganox1010」(商品名,Ciba Geigy公司製))0.001份。 另外,EVOH樹脂(A)與聚醯胺系樹脂(B)之質量比(A)/(B)為85/15,鹼土金屬鹽(C)之含有比例,相對於EVOH樹脂(A)與聚醯胺系樹脂(B)之總量,以金屬換算計為30ppm。 將該等放入擠製機中,使用弱混練規格螺桿(日本製鋼所(股)公司製),於氮氣環境下,以螺桿轉速為500rpm,模頭之吐出口徑為4.0mm,擠製機之轉筒溫度(℃)成為C2/C3/C4/C5/C6/C7/C8/C9/C10/C11/C12/C13/C14/C15=100/230/230/230/ 230/230/230/230/230/230/230/210/210/210之方式進行加熱,製作乙烯-乙烯醇系共聚物組成物丸粒。 另外,該弱混練規格螺桿具有2處捏合區,該捏合區之L/D之總計為6.5。
針對經如上述方式熔融混練的丸粒,使用FLIR公司製「紅外線溫度計FLIRi3」(商品名)測定模頭出口之剛吐出之股線之溫度。 又,將丸粒填充於直徑35mm×高度30mm之圓柱型玻璃製單元,輕扣(tapping)3次後予以切齊,做成黃色度(YI)値測定用樣品。根據JISZ-8722,使用日本電色工業(股)公司製「分光色差計 SE6000」(商品名)測定獲得之YI値測定用樣品之黃色度(YI)値。 又,由擠製機之吐出量與螺桿馬達之電力値求得熔融擠製時樹脂組成物之比能量。 將該等結果示於表1。
(實施例2) 變更實施例1之熔融混練條件,使螺桿轉速為456rpm,擠製機之轉筒之溫度(℃)為C2/C3/C4/C5/C6/C7/C8/C9/C10/C11/C12/C13/C14/C15=100/230/230/230/ 230/240/240/240/240/240/240/240/240/240,除此以外,以與實施例1同樣方式進行,製作乙烯-乙烯醇系共聚物組成物丸粒。 求得模頭出口之剛吐出之股線之溫度、成形體之黃色度(YI)値、比能量,將結果示於表1。
(比較例1) 變更實施例1之熔融混練條件,使擠製機之轉筒之溫度(℃)為C2/C3/C4/C5/C6/C7/C8/C9/C10/C11/C12/C13/C14/C15=100/230/230/230/230/240/240/240/240/240/240/240/240/240,除此以外,以與實施例1同樣方式進行,製作乙烯-乙烯醇系共聚物組成物丸粒。 求得模頭出口之剛吐出之股線之溫度、成形體之黃色度(YI)値、比能量,將結果示於表1。
(比較例2) 將實施例1之螺桿變更為通常規格螺桿(日本製鋼所(股)公司製),並變更熔融混練條件,使擠製機之轉筒之溫度(℃)為C2/C3/C4/C5/C6/C7/C8/C9/C10/C11/ C12/C13/C14/C15=100/230/230/230/230/240/240/240/240/240/240/240/240/240,除此以外,以與實施例1同樣方式進行,製作乙烯-乙烯醇系共聚物組成物丸粒。另外,該通常規格螺桿具有2處捏合區,該捏合區之L/D之總計為10.25。 求得模頭出口之剛吐出之股線之溫度、成形體之黃色度(YI)値、比能量,將結果示於表1。
【表1】※比較例1之YI值經目視評價係和比較例2同等以上。
由表1之結果可知:實施例1、2之黃色度(YI)値為10以下,獲得著色受到抑制的乙烯-乙烯醇系共聚物組成物丸粒。相對於此,比較例1、2之黃色度(YI)値超過10,觀察到丸粒著色。 由此可知:可藉由將模頭出口之剛吐出之樹脂溫度調整為比以往更低,尤其調整為268℃以下,以獲得著色受到抑制的乙烯-乙烯醇系共聚物組成物丸粒。
本發明已詳細地且參照特定的實施態樣進行說明,但可在不脫離本發明的精神與範圍內加上各種變化、或修正係該技術領域中有通常知識者所顯而易見。本申請案係基於2015年12月24日提申之日本專利申請案(日本特願2015-251832),並將其內容引用於此作為參照。 [產業利用性]
使用乙烯-乙烯醇系共聚物組成物丸粒而得之成形物,氣體阻隔性優異而且著色受到抑制,於工業上極為有用。
Claims (11)
- 一種乙烯-乙烯醇系共聚物組成物丸粒,含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C),對於該丸粒以分光色差計利用穿透法進行測定而得之黃色度(Yellow Index,YI)值為10以下,該鹼土金屬鹽(C)包含相對於乙烯-乙烯酯系共聚物(A)與聚醯胺系樹脂(B)之總量,以金屬換算計為10~50ppm之鎂鹽,該聚醯胺系樹脂(B)的熔點為180~270℃,相對於該乙烯-乙烯酯系共聚物(A)與聚醯胺系樹脂(B)之總量100質量份,含有0.1~200ppm之抗氧化劑。
- 如申請專利範圍第1項之乙烯-乙烯醇系共聚物組成物丸粒,其中,該鎂鹽為碳數1~6之脂肪族羧酸鎂鹽。
- 如申請專利範圍第1項之乙烯-乙烯醇系共聚物組成物丸粒,其中,該鎂鹽為乙酸鎂、碳酸鎂、碳酸氫鎂及磷酸一氫鎂中之1種或2種以上之組合。
- 如申請專利範圍第1項之乙烯-乙烯醇系共聚物組成物丸粒,其中,該鹼土金屬鹽(C)的含有比例,相對於該乙烯-乙烯酯系共聚物(A)與該聚醯胺系樹脂(B)之總量,以金屬換算計為30~50ppm。
- 如申請專利範圍第1至4項中任一項之乙烯-乙烯醇系共聚物組成物丸粒,其中,該乙烯-乙烯醇系共聚物(A)與該聚醯胺系樹脂(B)之質量比((A)/(B))為60/40~98/2。
- 一種乙烯-乙烯醇系共聚物組成物成形體,係如申請專利範圍第1至5項中任一項之乙烯-乙烯醇系共聚物組成物丸粒熔融成形而得。
- 一種乙烯-乙烯醇系共聚物組成物丸粒之製造方法,係以分光色差計利用穿透法進行測定時的黃色度(YI)值為10以下的乙烯-乙烯醇系共聚物組成物丸粒之製造方法,包括以下步驟:使用熔融混練裝置將含有乙烯-乙烯醇系共聚物(A)、聚醯胺系樹脂(B)及鹼土金屬鹽(C)的樹脂組成物予以熔融混練;使剛從該熔融混練裝置吐出的乙烯-乙烯醇系共聚物組成物股線之溫度為268℃以下,該鹼土金屬鹽(C)包含相對於乙烯-乙烯酯系共聚物(A)與聚醯胺系樹脂(B)之總量,以金屬換算計為10~50ppm之鎂鹽,該聚醯胺系樹脂(B)的熔點為180~270℃,相對於該乙烯-乙烯酯系共聚物(A)與聚醯胺系樹脂(B)之總量100質量份,含有0.1~200ppm之抗氧化劑。
- 如申請專利範圍第7項之乙烯-乙烯醇系共聚物組成物丸粒之製造方法,其中,該鎂鹽為碳數1~6之脂肪族羧酸鎂鹽。
- 如申請專利範圍第7項之乙烯-乙烯醇系共聚物組成物丸粒之製造方法,其中,該鎂鹽為乙酸鎂、碳酸鎂、碳酸氫鎂及磷酸一氫鎂中之1種或2種以上之組合。
- 如申請專利範圍第7項之乙烯-乙烯醇系共聚物組成物丸粒之製造方法,其中,該鹼土金屬鹽(C)的含有比例,相對於該乙烯-乙烯酯系共聚物(A)與該聚醯胺系樹脂(B)之總量,以金屬換算計為30~50ppm。
- 如申請專利範圍第7至10中任一項之乙烯-乙烯醇系共聚物組成物丸粒之製造方法,其中,剛從擠製機等熔融混練裝置吐出之樹脂丸粒亦即股線狀之混練物之溫度為聚醯胺系樹脂(B)之熔點+5~48℃。
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