TWI589627B - 一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜及其製法 - Google Patents
一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜及其製法 Download PDFInfo
- Publication number
- TWI589627B TWI589627B TW105121074A TW105121074A TWI589627B TW I589627 B TWI589627 B TW I589627B TW 105121074 A TW105121074 A TW 105121074A TW 105121074 A TW105121074 A TW 105121074A TW I589627 B TWI589627 B TW I589627B
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- Taiwan
- Prior art keywords
- polyester film
- visible light
- polyester
- nano
- jis
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Classifications
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Description
本發明為一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜及其製法,其特徵是該聚酯膜於可見光波段透光率低,但同時兼具高透明性、耐紫外線、低霧度、抗老化及阻隔紅外線等諸項優點。
受到全球暖化的影響,節能產品的需求日益強勁,推動節能及減低二氧化碳排放已成為各國政府施政的重要措施,因此開發高性能節能材料目前重要且迫切的課題。
隨著汽車持有數量的增加,消費者在關注價格、安全等因素的同時,對舒適性也提出了更高的要求。特別是夏天,遮陽、隔熱性能與車室隱密性需同時兼顧時,許多消費者提高了對車用隔熱膜的要求。希望能有高隔熱效果、低透光率之隔熱膜,得以應用在汽車側窗及後窗玻璃。
現用於透明視窗的隔熱貼膜中,其主要隔熱機制包含金屬反射塗層、有機染色塗層等技術。隔熱效果不外乎透過金屬反射塗層進行紅外線與紫外線的反射,但有產品反光性高的缺點;或透過有機染色塗層進行紅外線的吸收,藉以提供隔熱的效果,唯隔熱效果不佳,容易退色。另外,以電鍍或濺鍍金屬銀薄層,同時搭配介電材形成多層薄膜結構,藉由多層干射原理形成可見光區穿透加強,而紅外光區反射加強的光譜選擇性隔熱膜材,其設備投資及原料成本高且成品良率偏低。
為了實現節能減碳目的,在現有技術中例如,美國第5,385,751
號專利揭示一種使用化學氣相沉積法(Chemical Vapor Deposition)於透明玻璃基板上製作摻雜氟之氧化鎢紅外線阻隔材料。然而,由於係使用化學氣相沉積法,需要具備大型的製造裝置,因而其所需之製造成本較高,故仍有其缺點。
中國專利CN1320055和CN1286911是將聚酯切片混合黑色聚酯母粒及碳黑有機染料方式,經熔融擠出、拉伸成黑色薄膜,在製膜押出段經由精密的計量設備添加一定比例的黑色聚酯母粒可製備出黑色薄膜。但這種方法深受計量設備精度及穩定性所影響,往往因為計量誤差造成色差,而且容易退色。
美國專利US20060178254曾揭示一種如何製作鎢氧化物和複合鎢氧化物之方法,該專利文獻雖揭示可以獲得有效阻隔紅外線之光學特性之鎢氧化物和複合鎢氧化物,但由於其熱處理之製作程序較為複雜,於大量生產時需分別控制每一熱處理步驟之最佳條件因而其成品品質不穩定,不易掌控品質。
傳統上生產高隔熱且低透光效果之隔熱膜,至少需於基材上分別處理隔熱層以賦與隔熱功能;另處理有色層以遮蔽可見光,降低光透過率。如為塑膠基材,在歷經上述繁複製程後,不僅基材熱收縮嚴重,各處理層也因熱履歷時間長,影響層間密著,產品品質不穩定,良率差,製造成本亦不具競爭優勢。
本發明要解決的問題是:現有技術中,經由雙軸延伸製程生產聚酯薄膜時,對於低透光率及高紅外線阻隔要求無法兼顧,在原料中加入一定比例之機能性微粒,常影響聚酯膜的光學性能,霧度增加,應用於透明視窗貼膜大為受限。
本發明的主要目的在於揭示一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜,物性具備可見光穿透率(依JIS K7705測試標準)介於5~50%、紅外線阻隔率(依JIS R3106測試標準)至少90%,且霧度值(依JIS K7705測試標準)小於1.5%。
本發明的透明聚酯膜,可為聚對苯二甲酸乙二酯膜(PET膜)、聚萘二甲酸乙二醇脂膜(PEN膜)聚氯乙烯膜(PVC膜)、聚碳酸酯膜(PC膜)、聚丙烯膜(PP膜)、聚碳酸酯膜(PC膜)、聚乙烯膜(PE膜)或尼龍膜(Nylon膜),優選為PET膜,一般選用厚度為12~75μm,常用厚度為23~50μm。
本發明的透明聚酯膜成分中,含有粒徑介於10~90nm的隔熱漿料及/或粒徑介於20~80nm的黑色色漿,有助於透明聚酯膜同時滿足透明性及紅外線阻隔性的需求,其中隔熱漿料成份為CsxNyWO3-ZClC,與一般透明隔熱材料使用摻銻二氧化錫(ATO)或氧化銦錫(ITO)比較,紅外線阻絕性能大幅提升。
本發明的透明聚酯膜製法,適用於製得物性具備可見光穿透率介於5~50%、紅外線阻隔率至少90%且霧度值小於1.5%的聚酯膜,包括以下步驟:(1)配製黏度介於50~200cps的奈米隔熱漿料;(2)配製黏度介於30~120cps的奈米黑色色漿;(3)取乙二醇單體及對苯二甲酸或對苯二甲酸二甲酯為聚合原料;且基於聚合原料的重量,取製備的奈米隔熱漿料5~40wt%及/或奈米黑色色漿0.005~0.1wt%參予酯化、聚縮合反應,製得聚酯粒;(4)進行聚酯膜加工,在270~290℃溫度下,將聚酯粒擠出成透明聚酯膜。
本發明的聚酯膜,是由一種以上(含一種)的二元羧酸及一種以上的二元醇為原料,優選為選用對苯二甲酸和乙二醇為原料,且同時加入奈米隔熱漿料及奈米黑色色漿參予反應,或擇一加入奈米隔熱漿料或奈米黑色色漿參予反應,再使用經過酯化、聚縮合反應製得的膠粒進行雙軸拉伸聚酯膜加工,而延伸製得聚酯膜。
尤其是,本發明的聚酯膜,包含隔熱漿料及奈米黑色色漿,色相均勻且不易退色,還具備隔熱效果,可見光的穿透率低於50%,但高於5%,紅外線阻隔率至少90%,且霧度值小於1.5%。
本發明的聚酯膜製法,包括以下步驟:1.製備奈米隔熱漿料:2.製備奈米黑色色漿:3.製作聚酯粒:將步驟1及步驟2製備的奈米隔熱漿料與奈米黑色色漿,加入到聚合原料單體或聚合原料單體混合物之中,接著,進行酯化反應或酯交換反應,製得聚酯粒;及4.使用步驟3的聚酯粒進行聚酯膜加工,製得透明聚酯膜。
所述奈米隔熱漿料的成分,基於漿料組成物總重量,包含以下成分,且以下各成分的總和為100%:a)隔熱微粒(分子式為CsxNyWO3-ZClC)10~50wt%;來源得購自南亞塑膠工業股份有限公司的製品;b)乙二醇30~70wt%;及
c)分散助劑5~40wt%。
所述奈米隔熱漿料的具體做法,包括:
1.使用分子式為CsxNyWO3-ZClC的複合金屬鎢氧氯化物粉體為隔熱微粒;其中,Cs為銫;N為錫(Sn)、銻(Sb)或鉍(Bi);W為鎢;O為氧;x、y、z、c均為正數,且符合以下條件:x≦1.0;y≦1.0;y/x≦1.0;z≦0.6;及c≦0.1;
2.將步驟1的隔熱微粒(CsxNyWO3-ZClC)分散在乙二醇中,製得隔熱微粒溶液;於乙二醇溶劑中,加入所述隔熱微粒,經均勻攪拌成後,靜置濕潤;為了使隔熱微粒均勻分散,所述隔熱微粒溶液可以添加適量的分散助劑;其中,所述分散助劑可選自陰離子型、非離子型以及高分子分散劑之一種以上,其中以高分子分散劑為佳,因為高分子分散劑是具有多個錨固基團之共聚合物,可選自聚羧酸酯、磺酸型聚酯多元醇、聚磷酸酯、聚胺酯、改性聚丙烯酸酯類聚合物之一種或一種以上。陰離子型分散劑可選自丙烯酸類陰離子型分散劑,包括聚丙烯酸銨(共)聚合物、聚丙烯酸鈉(共)聚合物、苯乙烯-丙烯酸(共)聚合物、羧酸鈉鹽共聚合物等。非離子型分散劑可選自脂肪醇乙氧基化合物、聚氧乙烯烷基醚等。
3.對步驟1製備的隔熱微粒溶液,以濕式研磨機進行研磨分散,直至隔熱微粒的平均粒徑介於10~90nm,且隔熱微粒溶液的黏度介於50~200cps,得到奈米隔熱漿料。
所述奈米黑色色漿的成分,基於色漿漿料組成物總重量,包含以下成分,且以下各成分的總和為100%:
a)碳黑微粒5~25wt%;b)乙二醇40~75wt%;及c)分散助劑10~50wt%。
所述奈米黑色色漿的具體做法,包括:
1.使用碳黑為黑色微粒;來源得購自Orion、Cabot、Mitsubishi等廠家的碳黑製品;
2.將步驟1的碳黑分散在乙二醇中,製得黑色微粒溶液;於乙二醇溶劑中,加入所述碳黑微粒,經均勻攪拌成後,靜置濕潤;為了使隔熱微粒均勻分散,所述隔熱微粒溶液可以添加適量的分散助劑;其中,所述分散助劑可選自陰離子型、非離子型以及高分子分散劑之一種以上,其中以高分子分散劑為佳。所用陰離子型、非離子型以及高分子分散劑,同上述奈米隔熱漿料製程所用分散劑。
3.對步驟1製備的黑色微粒溶液,以濕式研磨機進行研磨分散,直至碳黑微粒的平均粒徑介於20~80nm,且黑色微粒溶液的黏度介於30~120cps,得到奈米黑色色漿。
所述製作聚酯粒的具體做法,包括:1.取乙二醇單體及對苯二甲酸或對苯二甲酸二甲酯為聚合原料;2.基於上述聚合原料的重量,取製備的奈米隔熱漿料5~40wt%及奈米黑色色漿0.005~0.1wt%;其中,奈米隔熱漿料的用量,優選為5~30wt%,最優選為25~30wt%;3.將步驟2的奈米隔熱漿料與奈米黑色色漿,依序加入攪拌中的乙二醇單體中,再加入對苯二甲酸或對苯二甲酸二甲酯,在250~285℃下,進行酯
化反應100~140分鐘(min),酯化反應結束後,降壓30~45分鐘(min);4.接著,在銻或鈦催化劑作用下進行聚縮合反應,溫度從280℃降至260℃左右,反應160~240分鐘(min),最後生成聚酯融熔體和副產物,副產物通過精餾予以去除後,聚酯融熔體經過冷卻、切粒製得聚酯粒。
所述兼具低可見光及高紅外線阻隔之聚酯膜的具體做法,包括:1.取本發明的聚酯粒為原料;2.進行雙軸拉伸聚酯膜加工,在270~290℃的溫度下擠出、延伸成膜;及3.完成定型後,即製得兼具低可見光及高紅外線阻隔之聚酯膜。
本發明的聚酯膜,具有紅外線阻隔性佳、霧度低、耐候性佳及抗老化性能佳的優點,可見光的穿透率低於50%,但高於5%,紅外線阻隔率至少90%,且霧度值小於1.5%,極適合應用於建築玻璃、車用玻璃及防農作物過度日曬之農業用膜上,提供絕佳隔熱效果,也解決了傳統隔熱膜濺鍍、濕式塗佈製程繁複、成本高、品質欠佳的缺點。
本發明的聚酯膜物性,是通過下列測試方法進行評估:
採用日商HORIBA LB-500動態光散射原理粒徑分析儀,量測經研磨分散後之奈米隔熱漿及奈米黑色色漿之微粒粒徑。
採用日商Tokyo Denshoku Co.,Ltd.產製的型號為TC-HⅢ的光穿透率測試機(Haze Meter),依JIS K7705測試標準,測試聚酯膜的光透過率。
可見光穿透率越高,則代表聚酯膜的透明性越佳。
採用日商HOYA產製的型號為LT-3000紅外線通過率測試機,依JIS R3106測試標準,測試聚酯膜的紅外線通過率,再以100%扣去紅外線通過率即為紅外線(IR cut%)阻隔率。
測試結果為紅外線阻隔率愈高,代表聚酯膜的隔熱效果越佳。
採用日商Tokyo Denshoku Co.,Ltd.產製的型號為TC-HⅢ的光穿透率測試機(Haze Meter),依JIS K7705測試標準,測試聚酯膜的光透過率。
霧度值越小,則代表聚酯膜的清澈度越佳。
採用ATLAS TECHNOLOGY Co.出品的型號為ATLAS UV TEST的耐候試驗機,燈管波長:UVB 313nm,試驗溫度:50~60℃,照射週期:每週期包括照射4小時,接著蒸濕4小時,試驗時間1000小時,照射能量:0.71w/m2。再以分光儀測量變色值(DE)。
DE值越小,代表耐候(光)越佳。
本發明的聚酯膜物性,以下列實施例1~8及比較例1-12具體比較及說明,但本發明的範疇不以此為限。
製得38μm厚度聚酯薄膜,其中,取乙二醇單體及對苯二甲酸或對苯二甲酸二甲酯為聚合原料;且基於上述聚合原料的重量,取製備的奈米隔熱
漿料30wt%,且隔熱微粒(CsxNyWO3-ZClC)的粒徑為10nm;取黑色色漿0.005wt%,且碳黑微粒的粒徑為20nm,參予酯化、聚縮合反應,製得聚酯粒;然後進行聚酯膜加工,在270~290℃溫度下,將聚酯粒擠出並延伸成38μm透明聚酯膜。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,但隔熱微粒(CsxNyWO3-ZClC)的粒徑改為65nm;黑色色漿用量改為0.01wt%,且碳黑微粒的粒徑改為50nm。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,但隔熱微粒(CsxNyWO3-ZClC)的粒徑改為90nm;黑色色漿用量改為0.05wt%,且碳黑微粒的粒徑改為80nm。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,但隔熱漿料用量改為25wt%,隔熱微粒(CsxNyWO3-ZClC)的粒徑改為10nm;黑色色漿用量改為0.05wt%,且碳黑微粒的粒徑改為50nm。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,但隔熱漿料用量改為25wt%,隔熱微粒(CsxNyWO3-ZClC)的粒徑改為65nm;黑色色漿用量改為0.07wt%,且碳黑微粒的粒徑改為50nm。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,但隔熱漿料用量改為25wt%,隔熱微粒(CsxNyWO3-ZClC)的粒徑改為90nm;黑色色漿用量改為0.07wt%,且碳黑微粒的粒徑改為80nm。該聚酯薄膜物性測試列於表1中。
同實施例2製得23μm厚度聚酯薄膜,隔熱微粒(CsxNyWO3-ZClC)的粒徑為65nm;黑色色漿用量為0.01wt%,且碳黑微粒的粒徑為50nm。該聚酯薄膜物性測試列於表1中。
同實施例2製得50μm厚度聚酯薄膜,隔熱微粒(CsxNyWO3-ZClC)的粒徑為65nm;黑色色漿用量為0.01wt%,且碳黑微粒的粒徑為50nm。該聚酯薄膜物性測試列於表1中。
製得38μm厚度聚酯薄膜,其中,聚酯反應中不加隔熱漿料及黑色色漿。該聚酯薄膜物性測試列於表1中。
同實施例1製得38μm厚度聚酯薄膜,其中,聚酯反應中隔熱漿料用量、隔熱微粒(CsxNyWO3-ZClC)的粒徑及碳黑微粒的粒徑相同;但,黑色色漿用量改為0.15wt%。
同實施例1製得38μm厚度聚酯薄膜,其中,聚酯反應中隔熱漿料用量相同,但隔熱微粒(CsxNyWO3-ZClC)的粒徑改為120nm;黑色色漿用量改為0.05wt%,且碳黑微粒的粒徑改為100nm。該聚酯薄膜物性測試列於表1中。
製得38μm厚度聚酯薄膜,但不添加黑色色漿,聚酯反應中隔熱漿料用量為5wt%,且隔熱微粒(CsxNyWO3-ZClC)的粒徑為65nm。該聚酯薄膜物性測試列於表1中。
同比較例4,不添加黑色色漿製得38μm厚度聚酯薄膜。但,聚酯反應中隔熱漿料含量改為10wt%。該聚酯薄膜物性測試列於表1中。
同比較例4,不添加黑色色漿製得38μm厚度聚酯薄膜。但,聚酯反應中隔熱漿料含量改為15wt%。該聚酯薄膜物性測試列於表1中。
同比較例4,不添加黑色色漿製得38μm厚度聚酯薄膜。但,聚酯反應中隔熱漿料含量改為65nm。該聚酯薄膜物性測試列於表1中。
製得38μm厚度聚酯薄膜,但不添加隔熱漿料;黑色色漿用量為0.005wt%,碳黑微粒的粒徑為50nm。該聚酯薄膜物性測試列於表1中。
同比較例8,不添加隔熱漿料製得38μm厚度聚酯薄膜。但,黑色色漿用量改為0.01wt%。該聚酯薄膜物性測試列於表1中。
同比較例8,不添加隔熱漿料製得38μm厚度聚酯薄膜。但,黑色色漿用量改為0.05wt%。該聚酯薄膜物性測試列於表1中。
同比較例8,不添加隔熱漿料製得38μm厚度聚酯薄膜。但,黑色色漿用量改為0.1wt%。該聚酯薄膜物性測試列於表1中。
同實施例2,製得製得38μm厚度聚酯薄膜,但隔熱漿料及黑色色漿不參予聚合,於加工延伸階段將隔熱漿料、黑色色漿及聚酯粒混合之後加熱延伸成38μm之聚酯薄膜,隔熱漿料用量為30wt%,粒徑65nm;黑色色漿用量為0.01wt%,粒徑50nm。該聚酯薄膜物性測試列於表1中。
1.從表1得知,比較例4~7製得的聚酯薄膜,未添加炭黑微粒,可見光穿透率偏高,無法達成低可見光穿透的效果。
2.從表1得知,比較例8~11製得的聚酯薄膜,未添加隔熱微粒,紅外線阻隔率偏低,無法達成高紅外線阻隔的效果。
3.從表1得知,實施例1~8製得的聚酯薄膜,同時添加隔熱微粒及炭黑微粒,對達成低可見光穿透及高紅外線阻隔效果,具有明顯成效。
4.從表1得知,比較例1製得的聚酯薄膜,未添加隔熱微粒,也未添加炭黑微粒,與實施例2對照比較,可見光穿透率明顯較高且紅外線阻隔效果,明顯不足。
5.從表1得知,比較例2製得的聚酯薄膜,雖同時添加隔熱微粒及炭黑微粒,但添加細粒徑的奈米隔熱漿及奈米炭黑色漿超高量,只達到高紅外線阻隔效果,但可見光穿透率偏低,幾乎不透光。
6.從表1得知,比較例3製得的聚酯薄膜,同時添加隔熱微粒及炭黑微粒,但添加的奈米隔熱漿及奈米炭黑色漿的粒徑較大,雖達到低可見光穿透率及高紅外線阻隔效果,但聚酯薄膜之霧度值較高,影響聚酯膜的清徹度。
7.從表1得知,比較例12製得的聚酯薄膜,於加工延伸階段,將隔熱漿料及黑色色漿投入與聚酯粒混合,其濃度均勻性較差,影響可見光穿透、紅外線阻隔、霧度、QUV耐候特性等之穩定性,較實施例2差,且品質不穩定。
Claims (4)
- 一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜製法,用於製得物性具備可見光穿透率(依JIS K7705測試標準)介於5~50%、紅外線阻隔率(依JIS R3106測試標準)至少90%,且霧度值(依JIS K7705測試標準)小於1.5%的透明聚酯膜,包括以下步驟:(1)配製黏度介於50~200cps的奈米隔熱漿料;基於隔熱漿料組成物總重量,包含以下成分,且以下各成分的總和為100%:a)分子式為CsxNyWO3-ZClC的隔熱微粒10~50wt%,且平均粒徑介於10~90nm;其中,Cs為銫;N為錫(Sn)、銻(Sb)或鉍(Bi);W為鎢;O為氧;x、y、z、c均為正數,且符合以下條件:x≦1.0;y≦1.0;y/x≦1.0;z≦0.6;及c≦0.1;b)乙二醇30~70wt%;及c)分散助劑5~40wt%;選自陰離子型分散劑、非離子型分散劑以及高分子分散劑之一種以上;(2)配製黏度介於30~120cps的奈米黑色色漿;基於色漿漿料組成物總重量,包含以下成分,且以下各成分的總和為100%:a)碳黑微粒5~25wt%;平均粒徑介於20~80nm;b)乙二醇40~75wt%;及c)分散助劑10~50wt%;選自陰離子型分散劑、非離子型分散劑以及高分子分散劑之一種以上;(3)製作聚酯粒; a)取乙二醇單體及對苯二甲酸或對苯二甲酸二甲酯為聚合原料;且基於上述聚合原料的重量,取製備的奈米隔熱漿料5~40wt%及奈米黑色色漿0.005~0.1wt%參予反應;b)在250~285℃下,進行酯化反應100~140分鐘,酯化反應結束後,降壓30~45分鐘;c)在銻或鈦催化劑作用下,進行聚縮合反應,在溫度260℃左右,反應160~240分鐘,生成聚酯融熔體,通過精餾去除副產物後,再經過冷卻、切粒製得聚酯粒;(4)進行聚酯膜加工,在270~290℃溫度下,將聚酯粒擠出成透明聚酯膜。
- 如申請專利範圍第1項所述的透明聚酯膜製法,其中,在製作聚酯粒的步驟中,隔熱漿料的用量以5~30wt%取代。
- 如申請專利範圍第1項所述的透明聚酯膜製法,其中,在製作聚酯粒的步驟中,隔熱漿料的用量以25~30wt%取代。
- 一種低可見光穿透兼具高紅外線阻隔的透明聚酯膜,使用申請專利範圍第1項的的透明聚酯膜製法製得,且物性具備可見光穿透率(依JIS K7705測試標準)介於5~50%、紅外線阻隔率(依JIS R3106測試標準)至少90%,且霧度值(依JIS K7705測試標準)小於1.5%。
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