TW201842031A - 樹脂組成物、其之製造方法及使用此之成形體 - Google Patents
樹脂組成物、其之製造方法及使用此之成形體 Download PDFInfo
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- TW201842031A TW201842031A TW107108810A TW107108810A TW201842031A TW 201842031 A TW201842031 A TW 201842031A TW 107108810 A TW107108810 A TW 107108810A TW 107108810 A TW107108810 A TW 107108810A TW 201842031 A TW201842031 A TW 201842031A
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- resin composition
- ethylene
- ester
- vinyl alcohol
- aforementioned
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Abstract
本發明係揭示含有乙烯-乙烯醇共聚物及非離子表面活性劑之樹脂組成物中,前述乙烯-乙烯醇共聚物之乙烯單位含量為15~60莫耳%,皂化度為90莫耳%以上,以前述乙烯-乙烯醇共聚物為所含有之主成分,含有3~400ppm之前述非離子表面活性劑的樹脂組成物。又,係藉由熔融混練含有非離子表面活性劑,水及前述乙烯-乙烯醇共聚物之混合物而製造前述樹脂組成物。藉由使用所得之樹脂組成物,可得增加熔融成形時之吐出量,且具有優良外觀之成形體。
Description
本發明係有關含有乙烯-乙烯醇共聚物之樹脂組成物,其之製造方法及使用此之成形體。
乙烯-乙烯醇共聚物(以下簡稱「EVOH」)為具有優良氧等之氣體遮蔽性、透明性、保香姓、耐油性、非帶電性、機械強度等之高分子材料。因此EVOH被無法使用於容器等成形品之用途。使用EVOH之成形體一般係藉由熔融成形法製造。故要求提升EVOH於熔融成形時之生產性及熔融成形後具有優良外觀(不會發生變黃等之著色)等。
專利文獻1曾提案含有EVOH、水滑石及高級脂肪酸之金屬鹽的樹脂組成物。藉由該樹脂組成物可得不僅增加熔融成形時之吐出量,提升生產效率,且具有阻塞或魚眼較少之良好品質的薄膜等之成形品。但由前述樹脂組成物熔融成形所得之成形品會有著色問題。
專利文獻2及專利文獻3曾提案EVOH含有羧酸、磷酸等之酸,或鹼金屬鹽、鹼土類金屬鹽等之金屬鹽的各種樹脂組成物。又,專利文獻2及專利文獻3曾記載此等樹脂組成物共有優良外觀及熔融成形時之安定性。但此等樹脂組成物於熔融成形時之生產性不足。
專利文獻4曾記載含有含0.3重量%以上之表面活性劑的EVOH薄膜之蔬果物用包裝袋。專利文獻4又記載,藉由併用EVOH與表面活性劑,可解除使蔬果枯萎之蔬果包裝體內部的結露情形。但製告專利文獻4所記載之蔬果用包裝袋時,除了熔融成形時之生產性不足外,熔融成形所得之成形品外觀也不良。 [先前技術文獻] [專利文獻]
[專利文獻1]日本特開平01-308440號公報 [專利文獻2]日本特開2001-146539號公報 [專利文獻3]日本國際公開第2011/118648號 [專利文獻4]日本特開2013-193759號公報
[發明所欲解決之課題]
為了解決上述課題,本發明之目的為提供可得熔融成形時之吐出量較多,且外觀優良之成形體的樹脂組成物及其之製造方法。又,目的為提供使用此類樹脂組成物所得之成形體及多層結構體。 [解決課題之方法]
上述課題可藉由提供含有乙烯-乙烯醇共聚物及非離子表面活性劑之樹脂組成物中,前述乙烯-乙烯醇共聚物之乙烯單位含量為15~60莫耳%,皂化度為90莫耳%以上,以前述乙烯-乙烯醇共聚物為所含有之主成分,含有3~400ppm之前述非離子表面活性劑的樹脂組成物而解決。
前述非離子表面活性劑較佳為,由醚型、胺基醚型、酯型、酯-醚型及醯胺型所成群中所選出之至少一種。前述非離子表面活性劑更佳為,由聚氧烷烷基醚、聚氧烷烯基醚、聚氧乙烯苯乙烯化苯基醚、聚氧烷烷基胺、聚氧烷烯基胺、聚氧烷烷基酯、聚氧烷烯基酯、山梨糖醇酐烷基酯、山梨糖醇酐烯基酯、聚氧乙烯山梨糖醇酐烷基酯、聚氧乙烯山梨糖醇酐烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯及高級脂肪酸所成群中所選出之至少一種。
前述樹脂組成物又以另含有金屬元素換算下10~500ppm之鹼金屬鹽為佳。
前述樹脂組成物又以另含有0.005~1質量%之由防氧化劑,紫外線吸收劑、可塑劑、防帶電劑、滑劑及填充劑所成群中所選出之至少一種的添加劑為佳。
前述樹脂組成物中前述EVOH又以含有二種乙烯單位含量不同之EVOH為佳。
含有前述樹脂成物之成形體為本發明之較佳實施態樣。又,具有由前述樹脂成物所形成之層與前述EVOH以外之熱塑性樹脂所形成之層的多層結構體也為本發明之較佳實態樣。
上述課題也可藉由提供熔融混練含有前述非離子表面活性劑、水及前述EVOH之混合物的前述樹脂組成物之製造方法而解決。此時前述混合物中,相對於前述EVOH100質量份之水含量較佳為0.1~50質量份。又以將含有前述非離子表面活性劑之水溶液或水分散體加入前述EVOH而得前述混合物為佳。 [發明之效果]
本發明之樹脂組成物具有優良外觀。又,使用該樹脂組成物可增加溶融成形時之吐出量。特別是既使低溫下也可確保一定吐出量。藉由使用此類樹脂組成物可以良好生產性製造外觀優良之成形體多層結構體。又,藉由本發明之製造方法可簡便製造前述樹脂組成物。 [實施發明之形態]
下面將詳述本發明之樹脂組成物、成形體及多層結構體。
[樹脂組成物] 本發明之樹脂組成物為,含有乙烯-乙烯醇共聚物及非離子表面活性劑之物中,前述乙烯-乙烯醇共聚物之乙烯單位含量為15~60莫耳%,皂化度為90莫耳%以上,以前述乙烯-乙烯醇共聚物為所含有之主成分,含有3~400ppm之前述非離子表面活性劑之物。
(EVOH) 本發明之樹脂組成物所含有的EVOH為,含有乙烯單位及乙烯醇單位之共聚物。前述EVOH可以已知之方法製造。例如使乙烯與乙烯酯共聚合得乙烯-乙烯醇共聚物後,使用鹼觸媒等使該共聚物皂化而得前述EVOH。前述乙烯酯如,乙酸乙烯酯、丙酸乙烯酯、三甲基乙酸乙烯酯等之脂肪酸乙烯酯,較佳為乙酸乙烯。前述EVOH於不阻礙本發明之效果的範圍內,可含有乙烯及乙烯醇以外之共聚合成分。此類其他共聚物如,來自乙烯基矽烷化合物之單位。此來自乙烯基矽烷化合物之單位如,來自乙烯三甲氧基矽烷、乙烯基三乙氧基矽烷、乙烯基三(β-甲氧基-乙氧基)矽烷或γ-甲基丙烯氧基丙基甲氧基矽烷之單位。此等之中較佳為來自乙烯基三甲氧基矽烷或乙烯基三乙氧基矽烷之單位。另外前述EVOH可含有來自其他共聚合成分之丙烯、丁烯等之α-烯烴;(甲基)丙烯酸或(甲基)丙烯酸甲酯等之不飽和羧酸或其酯;及N-乙烯基吡咯烷酮等之乙烯基吡咯烷酮之單位。前述EVOH中乙烯單位及乙烯醇單位以外之共聚合成分的含量較佳為10莫耳%以下,又以5莫耳%以下為佳,更佳為1莫耳%以下。
前述EVOH之乙烯單位含量需為15~60莫耳%。藉此可得優良之熔融成形性與阻氣性同時成立之樹脂組成物。前述乙烯含有率未達15莫耳%時,會降低樹脂組成物熔融成形時之長期運行性,且會降低所得成形體之耐水性,耐熱水性及高濕度下之阻氣性。前述乙烯含有率較佳為20莫耳%以上,又以超過20莫耳%為佳,更佳為22莫耳%以上。又,前述乙烯含有率超過60莫耳%時,會降低所得成形體之阻氣性。前述乙烯含有率較佳為50莫耳%以下。
前述EVOH之皂化度需為90莫耳%以上。藉此可得具有優良阻氣性之樹脂組成物。前述皂化度未達90莫耳%時,會降低所得成形體之阻氣性且使外觀惡化。前述皂化度較佳為95莫耳%以上,更佳為99莫耳%以上。前述EVOH之乙烯單位含量及皂化度可藉由溶劑係使用DMSO-d6
之1
H-NMR測定而求取。
前述EVOH之熔融流動率(溫度210℃、荷重2160g,以下將熔融流動率簡稱為MFR)較佳為0.1~200g/10分鐘。前述EVOH之MFR為此範圍時,前述樹脂組成物可得良好成形性及加工性,且所得成形體具有良好外觀。前述EVOH之MFR又以0.5g/10分鐘以上為佳,更佳為1g/10分鐘以上,特佳為3g/10分鐘以上。另外前述EVOH之MFR又以50g/10分鐘以下為佳,更佳為30g/10分鐘以下,特佳為15g/10分鐘以下,最佳為10g/10鐘以下。本發明之熔融流動率係依據JIS K 7210測定。
前述EVOH可為由二種以上之EVOH的混合物所形成。此時之乙烯含有率、皂化度及MFR之值為,由添加質量比算出之平均值。就生產成本及所得製品之均勻性的觀點,本發明之樹脂組成物較佳為含有一種EVOH。又,就使阻塞性與各種機械物性同時成立之觀點,本發明之樹脂組成物較佳為含有二種乙烯單位含量不同之EVOH。此時二種EVOH之乙烯單位含量差異較佳為5莫耳%以上,差異更佳為10莫耳%以上。又,相對於乙烯單位含量較低之EVOH的乙烯單位含量較高之EVOH的質量比較佳為1/99~99/1,更佳為5/95~95/5。
本發明之樹脂組成物係以前述EVOH為所含有之主成分。此主成分係指質量基準下含量最多之成分。本發明之樹脂組成物中前述EVOH之含量較佳為55質量%以上。前述含量未達55質量%時,前述樹脂組成物之阻氣性及成形性恐不足。前述含量又以80質量%以上為佳,更佳為90質量%以上,特佳為95質量%以上,最佳為99質量%以上。
(非離子表面活性劑) 本發明之樹脂組成物為,含有3~400ppm之非離子表面活性劑。前述樹脂組成物可藉由含有一定量之非離子表面活性劑,而增加熔融成形時之樹脂的吐出量。特別是既使前述樹脂組成物含有前述EVOH以外之其他成分時,也不會受此類成分影響,可增加樹脂之吐出量,同時既使熔化後之樹脂為低溫也可確保一定之吐出量。又令人驚訝係前述樹脂成物藉由含有一定量之非離子表面活性劑,可抑制熔融成形時該樹脂成物著色。詳細原因雖不明確,但推測如下所述。一般EVOH含有金屬離子時,已知藉由該金屬離子與EVOH反應,會促進EVOH熱惡化而使EVOH發生變黃等之著色情形。因此推測藉由非離子表面活性劑阻礙此類反應等,可抑制EVOH熱劣化。
前述樹脂組成物所含有之非離子表面活性劑無特別限定,但較佳為由醚型、胺基醚型、酯型、酯-醚型及醯胺型所成群中所選出之至少一種。此等非離子表面活性劑可單獨使用,或二種以上併用。
前述醚型之非離子表面活性劑較佳為,聚氧烷烷基醚、聚氧烷烯基醚、聚氧乙烯苯乙烯化苯基醚。
聚氧烷烷基醚及聚氧烷烯基醚較佳如下述式(1)所示之物。
式中,R為碳數6~22之直鏈或支鏈之烷基或烯基,A為各自獨立之碳數2~4之伸烷基,n係表示聚氧烷單位之縮合度,為1~30。
上述式(1)中R之碳數為8~18。A之碳數較佳為2或3。n較佳為2~25,更佳為3~20。
聚氧烷烷基醚具體如,聚氧乙烯己基醚、聚氧乙烯庚基醚、聚氧乙烯辛基醚、聚氧乙烯-2-乙基己基醚、聚氧乙烯壬基醚、聚氧乙烯癸基醚、聚氧乙烯月桂醚、聚氧乙烯十四烷基醚、聚氧乙烯十六烷基醚、聚氧乙烯硬脂醚、聚氧乙烯二十烷基醚等之聚氧乙烯烷基醚、聚氧丙烯硬脂醚等之聚氧丙烯烷基醚、聚氧乙烯聚氧丙烯烷基醚等。
聚氧烷烯基醚具體如,聚氧乙烯油醚等之聚氧乙烯烯基醚等。
聚氧乙烯苯乙烯化苯基醚具體如,聚氧乙烯單苯乙烯化苯基醚、聚氧乙烯二苯乙烯化苯基醚、聚氧乙烯三苯乙烯化苯基醚等。前述聚氧乙烯苯乙烯化苯基醚之環氧乙烷附加數較佳5~30莫耳。
前述胺基醚型之非離子表面活性劑較佳如,聚氧烷烷基胺、聚氧烷烯基胺等。聚氧烷烷基胺較佳如,椰油烷基胺-氧化乙烯附加物、聚氧乙烯硬脂胺、聚氧乙烯月桂胺、聚氧乙烯聚氧丙烯月桂胺、聚氧乙烯硬脂胺等。聚氧烷烯基胺較佳如,聚氧乙烯油基胺等。前述聚氧烷烷基胺之乙氧化物附加數較佳為1~40莫耳。
前述酯型之非離子表面活性劑較佳如,聚氧烷烷基酯、聚氧烷烯基酯、山梨糖醇酐烷基酯、山梨糖醇酯烯基酯、聚氧乙烯山梨糖醇酐烷基酯、聚氧乙烯山梨糖醇烯烴酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯等。
聚氧烷烷基酯及聚氧烷烯基酯較佳如下述式(2)所示之物。
式中,R、A及n之定義與上述式(1)相同。較佳範圍為,R之碳數為8~18,A之碳數為2或3,n為7~14。n為前述範圍時,可使良好之吐出量與外觀同時成立。
聚氧烷烷基酯具體如,聚氧乙烯單月桂酸酯、聚環乙烷二月桂酸酯、聚氧乙烯單棕櫚酸酯、聚氧乙烯單硬脂酸酯、眾環氧乙烷二硬脂酸酯等。
聚氧烷烯基酯具體如,聚氧乙烯油酸酯、聚乙二醇二油酸酯等。
山梨糖醇酐烷基酯具體如,山梨糖醇酐單辛酸酯、山梨糖醇酐單月桂酸酯、山梨糖醇酐單棕櫚酸酯、山梨糖醇酐單硬脂酸酯、山梨糖醇酐二硬脂酸酯、山梨糖醇酐三硬脂酸酯、山梨糖醇酐單月桂酸酐等。
山梨糖醇酐烯基酯具體如,山梨糖醇酐單油酸酯、山梨糖醇酐三油酸酯、山梨糖醇酐倍半油酸酯等。
聚氧乙烯山梨糖醇酐烷基酯具體如,聚氧乙烯山梨糖醇酐單月桂酸酯、聚氧乙烯山梨糖醇酐單棕櫚酸酯、聚氧乙烯山梨糖醇酐單硬脂酸酯、聚氧乙烯山梨糖醇酐三硬脂酸酯、聚氧乙烯山梨糖醇酐三異硬脂酸酯、聚氧乙烯山梨糖醇酐單月桂酸脂等。
聚氧乙烯山梨糖醇酐烯基酯具體如,聚氧乙烯山梨糖醇酐單油酸酯、聚氧乙烯山梨糖醇酐三油酸酯等。
甘油烷基酯具體如,甘油單硬脂酸酯、甘油單肉豆蔻酸酯等。
甘油烯基酯具體如,甘油單油酸酯等。
聚甘油烷基酯具體如,二甘油月桂酸酯、四甘油硬脂酸酯、聚甘油月桂酸酯、聚甘油硬脂酸酯等。
聚甘油烯基酯具體如,聚甘油油酸酯等。
前述酯-醚型之非離子表面活性劑較佳為,聚氧乙烯山梨糖醇酐烷基酯、聚氧乙烯山梨糖醇酐烯基酯等。
前述醯胺型之非離子表面活性劑較佳為高級脂肪酸醯胺,更佳為高級脂肪酸烷醇醯胺。
高級脂肪酸烷醇醯胺如,高級脂肪酸單或二烷醇醯胺,具體如己酸單或二乙醇醯胺、辛酸單或二乙醇醯胺、癸酸單或二乙醇醯胺、月桂酸單或二乙醇醯胺、棕櫚酸單或二乙醇醯胺、硬脂酸單或二乙醇醯胺、油酸單或二乙醇醯胺、椰油脂肪酸單或雙乙醇醯胺,或構成此等之乙醇醯胺被丙醇醯胺或丁醇醯胺取代之物等。
高級脂肪酸烷醇醯胺以外之高級脂酸醯胺如,己酸醯胺、辛酸醯胺、癸酸醯胺、月桂酸醯胺、棕櫚酸醯胺、硬脂酸醯胺、油酸醯胺等。
非離子表面活性劑更佳為,由聚氧烷烷基醚,聚氧烷烯基醚、聚氧烷苯乙烯化苯基醚、聚氧烷烷基胺、聚氧烷烯基胺、聚氧烷烷基酯、聚氧烷烯基酯、山梨糖醇酐烷基酯、山梨糖醇酐烯基酯、聚氧乙烯山梨糖醇酐烷基酯、聚氧乙烯山梨糖醇酐烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯及高級脂肪酸醯胺所成群中所選出之至少一種。
特別是就得到具有優良外觀之成形體的觀點,非離子表面活性劑較佳為醚型或酯型,其中就著色之觀點更佳為由聚氧烷烷基醚、聚氧烷烯基醚、聚氧烷烷基酯、聚氧烷烯基酯、甘油烷基酯、聚甘油烷基酯及聚甘油烯基酯所成群中所選出之至少一種。此等可單獨使用或複數種組合。
本發明之樹脂組成物中非離子表面活性劑的含量為3~400ppm。該含量未達3ppm時,將無法得到充分之增加前述樹脂組成物之吐出量的效果,且無法得到充分抑制著色之效果。前述含量較佳為10ppm以上,更佳為50ppm以上。又,前述含量超過400ppm時不利於經濟面,且概括所有樹脂的結果供給擠壓機之樹脂會不足,也會降低前述樹脂組成物之吐出量,同時會拉長擠壓機內前述樹脂組成物之滯留時間而傾向使樹脂變黃。前述含量較佳為300ppm以下,更佳為150ppm以上。
(鹼金屬鹽) 前述樹脂組成物較佳為另含有鹼金屬鹽。相對於其他樹脂藉由此類含有鹼金屬鹽之樹脂組成物可具有良好接著性。特別是具有由前述樹脂組成物所形成之層與由前述乙烯-乙烯醇共聚物以外之熱塑性樹脂所形成之層的多層結構體,可提升層間接著性。又令人驚訝的係藉由使用一定量之非離子表面活性劑,可抑制因鹼金屬鹽而使EVOH熱劣化,且可提升接著性。
形成前述鹼金屬鹽之鹼金屬如,鋰、鈉、鉀,但較佳為鈉及鉀。上述鹼金屬鹽如,鋰、鈉、鉀等之脂肪族羧酸鹽、芳香族羧酸鹽、碳酸鹽、鹽酸鹽、硝酸鹽、硫酸鹽、磷酸鹽、金屬錯合物等。此等之中就易取得之觀點等更佳為乙酸鈉、乙酸鉀、碳酸鈉、碳酸鉀、磷酸鈉及磷酸鉀。
本發明之樹脂組成物較佳為,金屬元素換算下含有10~500ppm之鹼金屬鹽。鹼金屬鹽之含量又以30ppm以上為佳,更佳為100ppm以上。又,前述含量又以400ppm以下為佳,更佳為300ppm以下。鹼金屬鹽之含量為上述下限以上時,以前述樹脂組成物作為構成多層結構體之層的材料用時,可提升層間之接著性。另外金屬鹽之含量為上述上限以下時,可抑制前述樹脂組成物著色。
(其他成分) 前述樹脂組成物於不限礙本發明之效果的範圍內,可含有前述EVOH及非離子表面活性劑以外之其他成分。前述樹脂成物中其他成分之含量較佳0.005~45質量%。該含量又以20質量%以下為佳,更佳為10質量%以下,特佳為5質量%以下,最佳為1質量%以下。又,使用二種以上之成分時合計含量可為前述範圍。
前述樹脂組成物較佳為含有由防氧化劑,紫外線吸收劑、可塑劑、防帶電劑、滑劑及填充劑所成群中所選出之至少一種之添加劑。前述樹脂組成物中該添加劑之含量較佳為0.005~50質量%。該含量又以20質量%以下為佳,更佳為10質量%以下,特佳為5質量%以下,最佳為1質量%以下。
上述防氧化劑如,N,N’-己烷-1,6-二基雙[3-(3,5-二-tert-丁基-4-羥基苯基)丙醯胺]、N,N’-1,6-己烷二基雙{N-(2,2,6,6-四甲基-4-哌啶基)-甲醯胺}、2,5-二-t-丁基氫醌、2,6-二2,2’-伸甲基-雙-(4-甲基-6-t-丁基苯酚)、十八烷基-3-(3’,5’-二-t-丁基-4’-羥基苯基)丙酸酯、4,4’-硫基雙-(6-t-丁基苯酚)等。
上述紫外線級收劑如,伸乙基-2-氰基-3,3’-二笨基丙烯酸酯、2-(2’-羥基-5’-甲基苯基)苯并三唑、2-(2’-羥基-5’-甲基苯基)苯并三唑、2-(2’-羥基-5’-甲基苯基)苯并三唑、2-(2’-羥基-3’-t-丁基-5’-甲基苯基)-5-氯苯并三唑、2-羥基-4-甲氧基二苯甲酮、2,2’-二羥基-4-甲氧基二苯甲酮、2-羥基-4-辛氧基二苯甲酮等。
上述可塑劑如,酞酸二甲酯、酞酸二乙酯、酞酸二辛酯、蠟、流動石蠟、磷酸酯等。
上述防帶電劑如,季戊四醇單硬脂酸酯、山梨糖醇酐棕櫚酸酯、硫酸化聚烯烴類、聚氧乙烯、聚乙二醇(商品名:碳蠟)等。
上述滑劑如,伸乙基雙硬脂醯胺、丁基硬脂酸脂等。
上述填充劑如,玻璃纖維、矽灰石、矽酸鈣、滑石、蒙脫石等。
前述樹脂組成物可含有其化成分用之EVOH以外的熱塑性樹脂。熱塑性樹脂如,聚烯烴[聚乙烯、聚丙烯、聚(1-丁烯)、聚(4-甲基-1-戊烯)、乙烯-丙烯共聚物、乙烯與碳數4以上之α-烯烴的共聚物、烯烴與馬來酸酐之共聚物、乙烯-乙烯基酯共聚物、乙烯-丙烯酸酯共聚物,或以不飽和羧或其衍生物使此等被接枝改質所得之改質聚烯烴等];尼龍(尼龍6、尼龍66、尼龍6/66共聚物等);聚氯乙烯;聚偏氯乙烯;聚酯;聚苯乙烯;聚丙烯腈;聚胺基甲酸酯;聚縮醛;改質聚乙烯醇等。前述樹脂組成物中EVOH以外之熱塑性樹脂的含量較佳為45質量%以下,又以20質量%以下為佳,更佳為10質量%以下,特佳為5質量%以下,最佳為1質量%以下。
就熱安定性及調整粘度之觀點,前述樹脂組成物可含有其他成分用之各種酸等之化合物。此化合物如,羧酸、磷酸化合物及硼化合物等,具體例如下所述。又,此等化合物可預先含於EVOH中。 羧酸:草酸、琥珀酸、苯甲酸、檸檬酸、乙酸、乳酸等 磷酸化合物:磷酸、亞磷酸等各種之酸或其鹽等 硼化合物:硼酸、硼酸酯、硼酸鹽、氫化硼等
前述樹脂組成物之MFR較佳為,與前述EVOH相同之範圍。藉由使前述樹脂組成物之MFR為此類範圍所得之效果也與EVOH時相同。
(樹脂成物之製造方法) 本發明之樹脂組成物的製造方法無特別限制,例如熔融混練含有前述EVOH、非離子表面活性劑及必要時之其他成分的混合物之方法。
熔融混練前述EVOH、非離子表面活性劑等可使用揑和混練機、擠壓機、混合輥、班伯里混合機等已知之混合裝置或混練裝置進行。非離子表面活性劑之態樣如,粉末等之固體、熔融物、水溶液等之溶液及水分散液等之分散液等。此態樣之非離子表面活性劑可與前述EVOH及其他成分混合。非離子表面活性劑之態樣較佳為溶液及分散液。熔融混練含有前述EVOH及非離子表面活性劑等之混合物時的溫度,可因應所使用之EVOH的熔點等適當調節。一般為120℃~300℃。
又以藉由熔融混練含有前述非離子表面活性劑、水及前述EVOH之混合物,而製造前述樹脂組成物之方法為佳。前述混合物中水之含量相對於前述EVOH100質量份較佳為0.1~50質量份,更佳為0.5~50質量份。該含量未達0.1質量份時,恐易使所得之樹脂組成物著色。又,前述含量超過50質量份時,恐會使前述EVOH與水產生相分離而易使由擠壓機吐出之樹脂組成物發泡。前述混合物中水之含量係指,單獨添加之量及與其他成分同時添加之量的合計量,也包括因吸濕等而含於前述非離子表面活性劑及前述EVOH中之水。與其他成分同時添加之方法如,以溶液或水分散液狀使用前述非離子表面活性劑之方法,或如後述使用前述EVOH含有一定水量之物的方法。
前述製造方法較佳為,將含有前述非離子表面活性劑之水溶液或水分散液加入前述EVOH而得前述混合物。藉由以水溶液或水分散體狀添加前述非離子表面活性劑,易使該非離子表面活性劑分散於前述EVOH中。
前述製造方法可為,將前述非離子表面活性劑加入熔融前之前述EVOH中,或將前述非離子表面活性劑加入熔融後之前述EVOH中。就生產性之觀點又以後者為佳。
熔融混練含有前述非離子表面活性劑、水及前述EVOH之混合物方法如,將前就EVOH導入擠壓機機後,相對於熔融後之該EVOH添加非離子表面活性劑及必要時之其他成分再混練、吐出之方法。此時可將含水率5~40質量%之前述EVOH導入擠壓機。
[成形體] 含有由此所得之本發明樹脂組成物的成形體為本發明之較佳實施形態。該成形體可為僅由該樹脂組成物所形成之物,或具有由該樹脂組成物所形成之部分與由該樹脂組成物以外之物所形成的部分之物。
含有前述樹脂組成物之成形體如,顆粒、薄膜、薄片、容器(袋子、杯子、管子、盒子、瓶子等)、燃料容器、管子、纖維、飲食品用包裝材、容器用填裝材、醫療用輸液袋材、輪胎用軟管材、鞋用軟熱墊材、提袋內箱用內袋材、有機液體貯藏用槽材、有機液材輸送用管材、暖器用溫水管材(地板暖器用溫水管材等)、化妝品用包裝材、齒盒用包裝材、醫藥品用包裝材、包裝材用構件(蓋子、提袋內箱之活栓部分等)、農藥瓶、農藥用薄膜(溫室用薄膜、土壤燻蒸用薄膜)、穀物保管用袋、防水布、壁紙或化妝板、氫、氧等之氣體槽等。前述燃料容器如,汽車、摩托車、船舶、飛機、發電機、工業用機器、農業用機器等所搭載之燃料容器、將燃料補給此等燃料容器用之移動式容器、保管燃料用之容器等。燃料如汽油、其中代表例如甲醇、乙醇或摻混MTBE等之汽油即含氧汽油。另外如其他重油、輕油、燈油等。
前述成形體一般係藉由使前述樹脂組成物熔融成形而得。此等成形體可為了二次使用而粉碎後再度成形。又,可單軸或雙軸延伸為薄膜、薄片、纖維等。熔融成形法如,適用擠壓成形、吹塑擠壓、吹煉成形、熔融紡絲、射出成形等已知之任一種成形法。熔融成形時之熔融溫度較佳為150~130℃,更佳為200~250℃。藉由使用本發明之樹脂組成物,可抑制熔融成形後變黃等著色,或發生凝膠、突起、魚眼、條紋等。因此藉由使前述樹脂組成物熔融成形所得之成形體可具有優良外觀。又,製造薄膜時為了得到一定吐出量,一般的含有EVOH之組成物為,依序將供給部/壓縮部/計量部/模頭之溫度設定為例如175℃/200℃/210℃/210℃般,使壓縮部與計量部為溫度較高之溫度,但使用前述樹脂組成物時,既使供給部與壓縮部之溫度為比一般溫度低10℃以上之低溫條件下,也可得一定之吐出量。
該成形體較佳為,具有由前述樹脂組成物所形成之層與由EVOH以外之其他熱塑性樹脂所形成的層之多層結構體。前述樹脂組成物除了具有優良長期運行性,也可抑制熔融成形後變黃等著色,及抑制凝膠、突起、魚眼、條紋等。因此使用前述樹脂組成物與其他熱塑性樹脂藉由熔融成形可以良好生產性製造具有優良外觀之多層結構體。
前述多層結構之厚度結構無特別限定,但就成形性及成本等之觀點,相對於金屬厚度之前述樹脂組成物層的厚度比較佳為2~20%。前述多層結構體之層結構無特別限定,以其他熱塑性樹脂層為A,前述樹脂組成物層為B、接著性樹脂層為C時,例如可為A/B、A/B/A、A/C/B、A/C/B/C/A、A/B/A/B/A、A/C/B/C/A/C/B/C/A等之層結構。此等可另附加其他層。設置複數其他熱塑性樹脂層時,可使用不同之物或相同之物。另外可設置由成形時因裁切等而發生以碎屑所形成的回收樹脂層,或以由回收樹脂與其他熱塑性樹脂之摻混物所形成的層作為其他熱塑性樹脂層用。
上述接著性樹脂較佳為羧酸改質聚烯烴。羧酸改質聚烯烴較佳為使用烯烴系聚合物化學性鍵結乙烯性不飽和羧酸、其酯或其酐經化學性(例如加成反應、接枝反應等)結合所得的含有羧基之改質烯烴系聚合物。乙烯性不飽和羧酸、其酯或其酐如,馬來酸、富馬酸、衣康酸、馬來酸酐、衣康酸酐、馬來酸單甲基酯、馬來酸單乙基酯、馬來酸二乙基酯、富馬酸單甲基酯等,又以馬來酸酐為佳。此等接著性樹脂可單獨使用或二種以上混合使用。
前述其他熱塑性樹脂如,直鏈狀低密度聚乙烯、低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、乙烯-乙酸乙烯共聚物、乙烯-丙烯共聚物、聚丙烯、丙烯-α-烯經共聚物、聚丁烯、聚戊烯等之聚烯烴;聚對苯二甲酸乙二醇酯等之聚酯;聚酯彈性體;尼龍6、尼龍66等之聚醯胺;聚苯乙烯;聚氯乙烯、聚偏氯乙烯;丙烯酸系樹脂;乙烯酯系樹脂;聚胺基甲酸酯彈性體;聚碳酸酯;氯化聚乙烯;氯化聚丙烯。此等之中較佳為使用聚丙烯、聚乙烯、乙烯-丙烯共聚物、乙烯-乙酸乙烯共聚物、聚醯胺、聚苯乙烯及聚酯。
此等之中又以其他熱塑性樹脂層係使用聚烯烴層,接著性樹脂層係使用羧酸改質聚烯烴層為佳。藉由設置聚烯烴層除了可提升前述多層結構體之力學特性,也可提升耐濕性。特別是前述多層結構體之兩外層設置聚烯烴層時,可有效防止樹脂組成物吸濕而為佳。此時於不阻礙此類效果之範圍內可使聚烯烴添加回收樹脂。
製造上述多層結構體之方法如下述方法。 (1)共擠壓前述樹脂組成物與其他熱塑性樹脂之方法 (2)將其他熱塑性樹脂熔融擠壓於由前述樹脂組成物所形成之成形體上的方法 (3)共射出前述樹脂組成物與其他熱塑性樹脂之方法 (4)使用接著劑層合由前述樹脂組成所形成之成形體與由其他熱塑性樹脂所形成之成形體的方法
此等方法之中較佳為(1)。本發明之樹脂組成物既使於高溫條件下熔融成形也可具有優良長期運行性,且可抑制熔融成形後著色。因此既使共擠壓該樹脂組成物與其他高熔點之熱塑性樹脂,也可得能抑制著色之外觀優良的多層結構體。共擠壓方法如,多歧管合流方式T模頭法、分程進料合流方式T模頭法、吹塑法等。
將上述共擠壓所得之多層結構體二次加工,可得例如下述成形體。 (1)藉由單軸或雙軸延伸多層結構體(薄片、薄膜等),且進行熱處理所得的多層延伸薄片或多層延伸薄膜 (2)藉由壓延多層結構體(薄片、薄膜等)所得之多層壓延薄片或多層壓延薄膜 (3)藉由使多層結構體(薄片、薄膜等)熱成形(真空成形、壓空成形、真空壓空成形等)所得之多層盒或多層杯狀容器 (4)藉由使多層結構體(管子等)伸縮吹煉成形所得之多層瓶、多層杯狀容器等。
此等二次加工所得之成形體較佳為,例如作為深度容器、杯狀容器、瓶等食物容器用。
下面將舉實施例更詳細說明本發明。
實施例1 (1)製作樹脂組成物顆粒 準備乙烯單位含量32莫耳%、皂化度99.98莫耳%、MFR3.8g/10分鐘(溫度210℃、荷重2160g)、含水率0.2質量%、含有鈉換算下200ppm之作為金屬鹽用之乙酸鈉的EVOH1。又,準備作為非離子表面活性劑用之分散聚氧乙烯(7)硬脂醚(非離子表面活性劑之化合物名中括弧內的數字係表示環氧乙烷單位之縮合度,以下相同)所得之水分散液(非離子表面活性劑之含量:10.0g/L)。摻混100質量份之EVOH1與1質量份之前述水分散液。以下條件熔融混練所得之混合物後,藉由顆粒化再乾燥,得樹脂組成物顆粒。 裝置:25mmφ雙軸擠壓機(東洋精機製作所製之「拉波普4C150」) L/D:25 螺旋:同方向完全咬合型 模頭孔數:2孔(3mmφ) 擠壓溫度:C1=200℃,C2至C5=220℃,模頭=220℃ 乾燥:真空乾燥90℃/2hr
(2)非離子表面活性劑定量 將樹脂組成物顆粒10g溶解於1,1,1,3,3,3-六氟-2-丙醇後,將該溶液滴入甲醇中。以濾器過濾此液體以去除析出物後濃縮。藉由使用Waters公司之「UPLC H-Class」測定所得之濃縮液,算出EVOH顆粒中非離子表面活性劑之含量。又,定量時係使用使用各非離子表面活性劑製作之檢量線。樹脂組成物顆粒中之聚氧乙烯(7)硬脂醚含量100ppm。
(3)評估吐出量 使用東洋精機製作所製之20mm擠壓機「D2020」(D=20mm、L/D=20、壓縮比=2.0、螺旋:全刮板),以下述條件由樹脂組成物顆粒得厚20μm之單層薄膜。此時將每一小時之單層薄膜的生產量評估為樹脂組成物之吐出量。吐出量為0.5kg/hr以上時具實用性。測定結果樹脂組成物之吐出量為1.6kg/hr。 單層薄膜製作條件 擠壓溫度:供給部/壓縮部/計量部/模頭 =160/180/210/210℃ 螺旋回轉數:40rpm 拉取輥溫度:80℃
(4)單層薄膜之外觀 以紙管捲取上述方法製作之單層薄膜,由肉眼以下述基準評估薄膜端面之著色。結果確認薄膜端面未著色。 A:確認未著色 B:稍有變黃 C:變黃但為可實用之程度 D:激烈變黃無法實用。
(5)多層結構體之接著性 使用樹脂組成物顆粒、直鏈狀低密度聚乙烯(LLDPE:三井化學公司製威特傑2022L)及接著性樹脂(SUMICA.ATOCHEM Co.Ltd製Bondine TX8030,以下簡稱為Ad),依下述得三種5層之多層薄膜(LLDPE/Ad/樹脂組成物/Ad/LLDPE=50μm/10μm/10μm/10μm/50μm)。所得之多層薄膜於多層製膜後立即由MD方向切出150mm、TD方向切出10mm,其次直接藉由自動夾具(島津製作所公司製DCS-50M)以T製剝離方式測定樹脂組成物層/Ad層間之剝離強度,再以下述基進行評估。結果接著強度為550g/15cm。 <多層製膜條件> 擠壓機: EVOH用:20mmφ擠壓機 實驗機ME型CO-EXT (東洋精機公司製) Ad用:25mmφ擠壓機 P25-18AC(大阪精機公司製) LLDPE用:32mmφ擠壓機 GF-32-A(塑料工學研究所公司製) EVOH擠壓溫度:供給部/壓縮部/計量部/模頭 =175/210/220/220℃ Ad擠壓溫度 :供給部/壓縮部/計量部/模頭 =100/160/220/220℃ LLDPE擠壓溫度:供給部/壓縮部/計量部/模頭 =150/200/210/220℃ 模頭:寬300mm衣架形模頭(塑料工學研究所公司製) <接著性判斷基準> A:600g/15cm以上 B:450g/15cm以上未達600g/15cm C:300g/15cm以上未達450g/15cm D:未達300g/15cm
實施例2~23及比較例1~6 除了依表1與表2所示變更EVOH之種類、非離子表面活性劑之種類及含量外,與實施例1相同製作樹脂組成物顆粒、單層薄膜及多層結構體後,進行此等之分析及評估。結果如表2所示。
實施例34 與實施例1,相同準備EVOH1及非離子表面活性劑之水分散液。摻混100質量部份之EVOH1、1質量份之前述水分散液及作為防氧化劑用0.5質量份之N,N’-己烷-1,6-二基雙[3-(3,5-二-tert-丁基-4羥基苯基)丙醯胺]。除了使用由此所得之混合物外,與實施例1,相同製作樹脂組成物顆粒、單層薄膜及多層結構體後,進行此等之分析及評估。結果如表3所示。
實施例35~48 除了依表3所示變更非離子表面活性劑量與添加劑之種類及添加量外,與實施例34相同製作樹脂組成物顆粒、單層薄膜及多層結構體後,進行此等之分析及評估。結果如表3所示。
實施例49、50 除了以85質量份之EVOH1及15質量份之EVOH3(乙烯含量48莫耳%、皂化度99.98莫耳%,MFR15g/10分鐘(溫度210℃、荷量2160g)、含水率0.2質量%)取代100質量份之EVOH1,及使非離子表面活性劑之含量如表3所示外,與實施例1相同製作樹脂組成物之顆粒、單層薄膜及多層結構體後,進行此等之分析及評估。結果如表3所示。
實施例51 使用實施例1所得之樹脂組成顆粒,及使用三種5層共擠壓機,製作聚丙烯層(200μm)/接著性樹脂層(25μm)/樹脂組成物層(50μm)/接著性樹脂層(25μm)/聚丙烯層(200μm)之5層構成的多層薄膜。此時接著性樹脂係使用馬來酸酐改質聚丙烯。與實施例1相同評估所得之多層薄膜的外觀,確認薄膜端面未著色。
比較例7 除了使用比較例1所得之樹脂組成物顆粒外,與實施例51相同製作多層薄膜及進行外觀評估。結果薄膜端面激烈變黃無實用性。
Claims (11)
- 一種樹脂組成物,其為含有乙烯-乙烯醇共聚物及非離子表面活性劑, 前述乙烯-乙烯醇共聚物之乙烯單位含量為15~60莫耳%,皂化度為90莫耳%以上, 前述乙烯-乙烯醇共聚物係含有作為主成分, 且含有3~400ppm之前述非離子表面活性劑。
- 如請求項1之樹脂組成物,其中前述非離子表面活性劑為選自由醚型、胺基醚型、酯型、酯-醚型及醯胺型所成群之至少一種。
- 如請求項2之樹脂組成物,其中前述非離子表面活性劑為選自由聚氧烷烷基醚、聚氧烷烯基醚、聚氧乙烯苯乙烯化苯基醚、聚氧烷烷基胺、聚氧烷烯基胺、聚氧烷烷基酯、聚氧烷烯基酯、山梨糖醇酐烷基酯、山梨糖醇酐烯基酯、聚氧烷山梨糖醇酐烷基酯、聚氧乙烯山梨糖醇酐烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯及高級脂肪酸醯胺成群之至少一種。
- 如請求項1~3中任一項之樹脂組成物,其中另含有金屬元素換算下10~500ppm之鹼金屬鹽。
- 如請求項1~3中任一項之樹脂組成物,其中另含有0.005~1質量%之選自由防氧化劑、紫外線吸收劑、可塑劑、防帶電劑、滑劑及填充劑所成群之至少一種的添加劑。
- 如請求項1~3中任一項之樹脂組成物,其中前述乙烯-乙烯醇共聚物為含有二種乙烯單位含量不同之乙烯-乙烯醇共聚物。
- 一種成形體,其為含有如請求項1~6中任一項之樹脂組成物。
- 一種多層結構體,其為具有由如請求項1~6中任一項之樹脂組成物所形成之層與由前述乙烯-乙烯醇共聚物以外之熱塑性樹脂所形成之層。
- 一種如請求項1~6任一項之樹脂組成物的製造方法,其為熔融混練含有前述非離子表面活性劑、水及前述乙烯-乙烯醇共聚物之混合物。
- 如請求項9之製造方法,其中前述混合物中,相對於前述乙烯-乙烯醇共聚物100質量份的水之含量為0.1~50質量份。
- 如請求項9或10之製造方法,其中將含有前述非離子表面活性劑之水溶液或水分散體加入前述乙烯-乙烯醇共聚物中而取得前述混合物。
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