TWI670177B - 液體濾器用基材及其製造方法 - Google Patents
液體濾器用基材及其製造方法 Download PDFInfo
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- TWI670177B TWI670177B TW104119808A TW104119808A TWI670177B TW I670177 B TWI670177 B TW I670177B TW 104119808 A TW104119808 A TW 104119808A TW 104119808 A TW104119808 A TW 104119808A TW I670177 B TWI670177 B TW I670177B
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Abstract
本發明之實施形態係提供一種液體濾器用基材,其具有含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層,泡點為0.40Mpa以上0.80Mpa以下,透水性能為1.0ml/min.cm2以上4.0ml/min.cm2以下。
Description
本揭示關於液體濾器用基材及其製造方法。
近年來,電子機器越來越小型、高性能化進展,特別地以個人電腦、智慧型手機為代表的數位機器、攜帶型終端係達成飛躍的進化。於牽引、支撐其的各式各樣之技術中,半導體產業的技術革新已完成大的任務者係周知之事實。於近年的半導體產業中,形成配線圖型尺寸小於20nm的領域之開發競争,加快各公司最先端生產線之構築。
微影步驟係以半導體零件製造來形成圖型之步驟。隨著近年的圖型微細化,不僅微影步驟所使用的藥液本身之性質形狀,而且塗布在晶圓上的藥液之操作,亦要求非常高度的技術。
高度地調製之藥液係在塗布到晶圓上的緊鄰之前,經緻密的濾器所過濾,去除對於圖型形成或良率造成大的影響之顆粒。於最先端的小於20nm之圖型形成中,要求能
補集未達約10nm的顆粒,濾器廠商各公司係進行全力的開發。
一般地,液體濾器係以由聚乙烯、聚四氟乙烯、尼龍、聚丙烯等之樹脂所成的多孔質膜作為基材,加工成筒匣形體而使用。從與藥液的相容性或捕集性能、處理能力、壽命等之觀點來看,基材係按照目的之用途而靈活運用。最近,特別重視減低來自基材的溶出物,多使用聚乙烯微多孔膜作為基材。
作為聚乙烯微多孔膜之代表的製造方法,可舉出相分離法或延伸法。相分離法係藉由高分子溶液的相分離現象來形成細孔之技術,例如有特開平2-251545號公報中所記載,藉由熱誘發相分離的熱誘發相分離法,及利用高分子對於溶劑的溶解度特性之非溶劑誘發相分離法。又,組合熱誘發相分離與非溶劑誘發相分離之兩者的技術,更且藉由延伸來調整孔構造之形式或大小,亦可使變化(variation)增大。延伸法例如係將經成形為薄片狀的聚乙烯原料薄片予以延伸,調整速度、倍率、溫度等之延伸條件,延長結晶構造中的非品質部分,邊形成微原纖維邊在層狀層之間形成微細孔之方法(例如參照特開2010-053245號公報、特開2010-202828號公報、特開平7-246322號公報、特開平10-263374號公報)。
然而,若要有效果地捕集未達約10nm的微細顆粒,則反而液體透過性有惡化之傾向。即,捕集性能與液體透過性係處於權衡關係。
又,於液體濾器的長期使用中,由於對於聚烯烴微多孔膜重複施加壓力,多孔質構造變化,液體透過性亦有徐徐降低之情況。為了解決如此的長期安定使用之問題,例如亦考慮使聚烯烴微多孔膜成為剛直的構成。然而,於剛直的聚烯烴微多孔膜中,亦對於捕集性能及液體透過性造成影響。
而且,於如前述公報記載的習知技術中,沒有對於未達約10nm的微細顆粒,捕集性能及液體透過性優異,更且於長期的使用中亦實現安定的液體透過性之提案。
因此,本揭示係為了解決上述問題,目的在於提供液體濾器用基材及其製造方法,其係一邊對於未達約10nm的微細顆粒具有優異的捕集性能,一邊具有優異的液體透過性,而且在長期使用中具有安定之液體透過性。
為了解決上述問題,具體之手段包含以下之態樣。
1.一種液體濾器用基材,其具有含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層,泡點為0.40Mpa以上0.80Mpa以下,透水性能為1.0ml/min.cm2以上4.0ml/min.cm2以下。
2.如上述1記載之液體濾器用基材,其中相對於前述B層的全部固體成分之合計質量,前述B層中的前述填料之含量為40質量%以上80質量%以下。
3.如上述1或上述2記載之液體濾器用基材,其空孔率為50%以上且未達75%。
4.如上述1~3中任一項記載之液體濾器用基材,其厚度為7μm以上25μm以下。
5.如上述1~4中任一項記載之液體濾器用基材,其中前述構成A層及B層的聚烯烴係由混合有重量平均分子量為90萬以上的超高分子量聚乙烯與重量平均分子量為20萬~80萬且密度為0.92~0.96g/cm3的高密度聚乙烯之聚乙烯組成物所構成。
6.如上述1~5中任一項記載之液體濾器用基材,其中前述B層中的前述填料之平均粒徑為0.2μm~2.0μm。
7.一種液體濾器用基材之製造方法,其係如上述1~6中任一項記載之液體濾器用基材之製造方法,具有:調製含有聚烯烴及溶劑的第1溶液(上述A層形成用液)之步驟,調製含有聚烯烴、溶劑及填料的第2溶液(上述B層形成用液)之步驟,將前述第1溶液經熔融混煉而得之熔融混煉物與前述第2溶液經熔融混煉而得之熔融混煉物,自模頭共擠出,冷卻固化而得到多層的凝膠狀成形物之步驟,在至少一方向中延伸前述多層的凝膠狀成形物之步驟,與於至少一方向中延伸之步驟的前或後,去除前述多層的凝膠狀成形物中之溶劑的至少一部分之步驟。
依照本發明之一實施形態,提供液體濾器用基材及其製造方法,其係一邊對於未達約10nm的微細顆粒具有優異的捕集性能,一邊具有優異的液體透過性,而且在長期使用中具有安定之液體透過性。
以下,對於本發明之實施形態,依順序說明,惟此等之說明及實施例係例示本發明之實施形態者,並非限制本發明之實施形態的範圍。
再者,於本說明書全體中,在數值範圍使用「~」時,各數值範圍包含其上限值與下限值。
又,關於聚烯烴微多孔膜,所謂「長度方向」,就是意指聚烯烴微多孔膜之長度方向,所謂「寬度方向」,就是意指與聚烯烴微多孔膜的長度方向正交之方向。以下,將「寬度方向」亦稱為「TD」,將「長度方向」亦稱為「MD」。
本發明之實施形態的液體濾器用基材具有含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層。即,本發明之實施形態的
液體濾器用基材係由具備A層與B層至少各1層的層合聚烯烴微多孔膜所構成。層合聚烯烴微多孔膜的液體濾器用基材係泡點為0.40Mpa以上0.80Mpa以下,透水性能為1.0ml/min.cm2以上4.0ml/min.cm2以下。
依照如此本發明之實施形態,可提供液體濾器用基材,其係一邊對於未達約10nm的微細顆粒具有優異的捕集性能,一邊具有優異的液體透過性,而且在長期使用中具有安定之液體透過性。
以下,說明各構成之詳細。
(層合聚烯烴微多孔膜)
於本揭示中,液體濾器用基材之層合聚烯烴微多孔膜係具備含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層之層合聚烯烴微多孔膜。
層合聚烯烴微多孔膜只要是具備A層與B層至少各1層即可,其層合數及層合順序係沒有特別的限定。
關於層合數,從製造上之觀點來看,更佳為2層~3層。
關於層合順序,例如較佳為A層/B層、A層/B層/A層、B層/A層/B層、A層/A層/B層、或A層/B層/B層。
再者,於本發明之實施形態的層合聚烯烴微多孔膜中,在不妨礙本發明之實施形態的效果之範圍內,亦可更
層合A層及B層以外之第三層。
(A層)
於本揭示中,A層係含有聚烯烴的微多孔膜狀之層。
此處,所謂的「微多孔膜狀」,就是意指聚烯烴的原纖維構成三次元的網絡構造,在內部具有多數的微細孔,成為此等微細孔經連結之構造,氣體或液體可從一側之面往另一側之面通過的膜構造。
作為聚烯烴,例如可舉出聚乙烯、聚丙烯、聚丁烯、聚甲基戊烯等之均聚物或共聚物、或此等的2種以上之混合物。其中,較佳為聚乙烯。
作為聚乙烯,宜為高密度聚乙烯、及高密度聚乙烯與超高分子量聚乙烯之混合物等。高密度聚乙烯係指重複單位的乙烯以直鏈狀結合之結晶性的聚乙烯,依據JIS K6748(1995)的密度定義為0.92g/cm3以上之聚乙烯。
作為本發明之實施形態所用的聚烯烴,較佳為使用含有5質量%以上的重量平均分子量為60萬以上的超高分子量聚乙烯之聚乙烯組成物,更佳為含有7質量%以上的超高分子量聚乙烯之聚乙烯組成物,特佳含有13質量%~27質量%的超高分子量聚乙烯之聚乙烯組成物。
又,藉由適量摻合2種以上的聚乙烯,隨著延伸時的原纖維化而形成網絡網狀構造,具有使空孔發生率增加之效用。摻合2種以上的聚乙烯後之平均重量平均分子量較佳為35萬~250萬。特別地,較佳為混合有上述重量平
均分子量為90萬以上的超高分子量聚乙烯與重量平均分子量為20萬~80萬且密度為0.92~0.96g/cm3的高密度聚乙烯之聚乙烯組成物。此時,高密度聚乙烯的聚乙烯組成物中之比例較佳為95質量%以下,更佳為93質量%以下,特佳為87質量%~73質量%。又,高分子量聚乙烯在聚乙烯組成物中之比例較佳為5質量%以上,更佳為7質量%以上,特佳為13質量%~27質量%。
再者,重量平均分子量係藉由將聚烯烴微多孔膜的試料在鄰二氯苯中加熱溶解,以GPC(Waters公司製,Alliance GPC2000型,管柱:GMH6-HT及GMH6-HTL),在管柱溫度135℃、流速1.0mL/分鐘之條件下進行測定而得。
(B層)
於本揭示中,B層係含有聚烯烴及填料的微多孔膜狀之層。B層之「微多孔膜狀」亦與A層同樣,但於由聚烯烴原纖維所成的三次元網絡構造之中,以捕捉有填料之形式存在。
B層所用的聚烯烴係可使用與A層所用的聚烯烴同樣者。其中,使用相同的聚烯烴來形成A層與B層者,於提高兩層的接著性之觀點中較佳。特別地,作為A層與B層之聚烯烴,較佳為使用混合有上述超高分子量聚乙烯與高密度聚乙烯之聚乙烯組成物。
B層所用的填料係可使用無機物或有機物之任一者。
對於填料,要求在製造層合聚烯烴微多孔膜的過程中不溶解,而且在液體濾器中亦不溶解於被處理液之性質形狀。
作為無機物填料,例如可舉出氫氧化鋁、氫氧化鎂、氫氧化鈣、氫氧化鉻、氫氧化鋯、氫氧化鈰、氫氧化鎳、氫氧化硼等之金屬氫氧化物;氧化鋁或氧化鋯、氧化鎂等之金屬氧化物;碳酸鈣、碳酸鎂等之碳酸鹽;硫酸鋇或硫酸鈣等之硫酸鹽;矽酸鈣、滑石等之黏土礦物等等。其中,無機填料較佳為由金屬氫氧化物及金屬氧化物之至少一者所構成。
上述各種填料係可各自單獨使用或組合2種以上使用。又,亦可使用經由矽烷偶合劑等所表面修飾之無機填料。
作為有機物填料,例如可例示交聯聚丙烯酸、交聯聚丙烯酸酯、交聯聚甲基丙烯酸、交聯聚甲基丙烯酸酯、交聯聚甲基丙烯酸甲酯、交聯聚矽氧(聚甲基倍半矽氧烷等)、交聯聚苯乙烯、交聯聚二乙烯基苯、苯乙烯-二乙烯基苯共聚物交聯物、聚醯亞胺、三聚氰胺樹脂、酚樹脂、苯并胍胺-甲醛縮合物等之各種交聯高分子微粒子;聚碸、聚丙烯腈、芳香族聚醯胺、聚縮醛、熱塑性聚醯亞胺等之耐熱性高分子微粒子等。又,此等之構成有機微粒子的有機樹脂(高分子)亦可為前述例示的材料之混合物、改性物、衍生物、共聚物(無規共聚物、交替共聚物、嵌段共聚物、接枝共聚物)、交聯物(前述的耐熱性高分子之情況)。
於本揭示中,在被處理液中含有凝膠狀顆粒時,從提高該凝膠狀顆粒的捕集性能之觀點來看,填料之平均粒徑較佳為0.2μm~2.0μm。
填料之平均粒徑若為0.2μm以上,則在以延伸、熱處理形成空孔時,容易形成良好的多孔質構造,可使泡點及透水性能成為更良好。從如此的觀點來看,填料之平均粒徑更佳為0.4μm以上。另一方面,填料之平均粒徑若為2.0μm以下,則容易以恰當的尺寸形成空孔,可進一步提高凝膠狀顆粒的捕集性能。從如此的觀點來看,填料之平均粒徑更佳為1.0μm以下。
填料之平均粒徑係使用雷射繞射式粒度分布測定裝置進行測定,自體積粒度分布中的中心粒徑(D50)所求得之值。
於本揭示中,B層中的前述填料之含量,相對於B層的全部固體成分之合計質量,較佳為40質量%以上80質量%以下。
填料之含量若為40質量%以上,則容易得到良好的泡點與透水性能。從如此的觀點來看,填料之含量更佳為45質量%以上。另一方面,填料之含量若為80質量%以下,則在樹脂中填料變良好地分散,難以發生缺陷,而且薄膜的機械強度有上升之傾向。從如此的觀點來看,填料之含量更佳為75質量%以下。
-透水性能(水流量)-
本發明之實施形態的液體濾器用基材(層合聚烯烴微多孔膜)之特徵為流量特性優異。
液體濾器用基材之透水性能係在90kPa的差壓下1.0ml/min.cm2~4.0ml/min.cm2。液體濾器用基材之透水性能若未達1.0ml/min.cm2,則得不到作為未達約10nm的顆粒用之液體濾器的充分透水性能,可能發生液體過濾的生產性降低之問題或為了維持送液量(生產性)而能量負荷增大之問題等。從如此的觀點來看,透水性能更佳為1.5ml/min.cm2以上。另一方面,液體濾器用基材之透水性能若超過4.0ml/min.cm2,則無法充分地補集未達約10nm的微小顆粒,可能發生不展現充分的捕集性能之問題。從如此的觀點來看,透水性能較佳為3.5ml/min.cm2以下。
透水性能係藉由以下之方法所求得之值。
將液體濾器用基材(層合聚烯烴微多孔膜)浸漬於乙醇中,於室溫下使乾燥後,載置於直徑37mm的不透鋼製透液單元(透液面積Scm2)上。以少量(0.5ml)的乙醇濕潤透液單元上的液體濾器用基材後,以90kPa的差壓使經預先計量的純水V(100ml)穿透,計測純水全量穿透所需要的時間T1(min)。測定係在24℃的環境中進行。使用所得之值,藉由以下之式算出。
透水性能(Vs)=V/(T1×S)
-泡點-
本發明之實施形態的液體濾器用基材(層合聚烯烴微多孔膜)之特徵為高度地補集未達約10nm的顆粒(更佳為數nm的顆粒)。
所謂的泡點,就是指對於與液體(本實施形態中為乙醇)接觸的狀態下之液體濾器用基材(層合聚烯烴微多孔膜)給予壓力,使空氣(泡)自一面朝向另一面通過孔時所必要的壓力(MPa),為依據ASTM E-128-61所測定之值。
液體濾器用基材之泡點為0.40MPa以上0.80MPa以下。本發明之實施形態的液體濾器用基材(層合聚烯烴微多孔膜)係泡點為0.40MPa以上0.80MPa以下之範圍,而且發揮如上述的良好透水性能。
液體濾器用基材之泡點若比0.40MPa低,則無法充分地補集如上述的微小顆粒,不展現充分的捕集性能。從如此的觀點來看,泡點更佳為0.45MPa以上。另一方面,液體濾器用基材之泡點若比0.80MPa,則透水性能會顯著地不足,於長期使用中有可能發生無法實現安定的液體透過性之情況。從如此的觀點來看,泡點更佳為0.70MPa以下。
再者,於本揭示中,必須將上述透水性能及泡點調整至恰當的範圍。作為控制此等物性之手法,並沒有特別的限定,例如可舉出調整A層與B層所用的聚乙烯樹脂之平均分子量、B層中的填料之含量、混合複數的聚乙烯樹脂而使用時其混合比率、原料中的聚乙烯樹脂濃度、於原料中混合複數的溶劑時其混合比率、為了榨出所擠出的多
層凝膠狀成形物(薄片狀物)內部之溶劑用的加熱溫度、擠壓力、延伸倍率、延伸後熱處理時的熱處理(熱定型)溫度、在萃取溶劑中的浸漬時間等之製造條件等。特別地,雖然於以下的製造方法之說明中亦顯示,但可藉由以下而適宜獲得:A層與B層所用的超高分子量聚乙烯係在各層的全部聚乙烯組成物中之質量比例為1%~35%,填料之含量係在全部組成物中的質量比例為40%~80%,為了榨出所擠出的多層凝膠狀成形物(薄片狀物)內所含有的溶劑之一部分而邊加熱至40℃~100℃邊施予合適的擠壓力,使總延伸倍率(縱延伸倍率與橫延伸倍率之積)成為20倍~60倍,或使熱定型時的熱定型溫度成為110℃~140℃等。
-空孔率-
於本揭示中,液體濾器用基材(層合聚烯烴微多孔膜)之空孔率較佳為50%以上且未達75%,更佳為50%以上75%以下,尤佳為60%以上75%以下。該聚烯烴微多孔膜之空孔率為50%以上時,在透水性能進一步提高之點較佳。另一方面,空孔率為75%以下時,液體濾器用基材的力學強度成為更良好,在操縱性亦提高之點較佳。
此處,液體濾器用基材的層合聚烯烴微多孔膜之空孔率(ε)係藉由下述式算出。
ε(%)={1-Ws/(ds.t)}×100
Ws:聚烯烴微多孔膜的單位面積重量(g/m2)
ds:聚烯烴的真密度(g/cm3)
t:聚烯烴微多孔膜的膜厚(μm)
-厚度-
於本揭示中,液體濾器用基材(層合聚烯烴微多孔膜)之膜厚較佳為7μm~25μm,更佳為10μm~20μm。液體濾器用基材之膜厚為7μm以上時,容易得到充分的力學強度,在容易得到聚烯烴微多孔膜之加工時等的操縱性及濾器筒匣的長期使用時之耐久性之點較佳。另一方面,液體濾器用基材之膜厚為25μm以下時,在以單膜容易得到充分的透水性能之點較佳。再者,於指定大小的濾筒中,容易得到更多的過濾面積,將聚烯烴微多孔膜加工而得到液體濾器用基材時的濾器之流量設計及構造設計變容易之點亦較佳。
例如,假想將濾筒收容在相同大小的殼體內時,由於濾材(包含濾器用基材的構成材料全體)之厚度愈薄,愈可增大濾材面積,故作為液體濾器,高流量.低過濾壓力之設計成為可能。即,作為液體濾器,欲維持相同流量時,過濾壓力變低,維持相同過濾壓力時,流量變高之設計係成為可能。特別地,由於過濾壓力變低,所一旦捕集的顆粒,因繼續在濾材內部暴露於過濾壓力下而隨著時間的經過自濾材內部與過濾液一起被擠出而漏出的機率係顯著降低。又,過濾的液體中所溶存的氣體,因過濾前後的壓力差(過濾後的壓力降低)而出現微小氣泡的機率係顯著降
低。再者,亦可期待藥液等之過濾對象物的過濾良率之提高,或長時間高度地維持彼等之品質的效果。
另一方面,濾材之厚度愈薄,濾材之強度或耐久性能愈降低,但例如只要是在濾器設計中為可能,則亦可一邊藉由與粗孔的高強度支持體複合化(例如進行疊合折入等之加工)而補強,一邊調整耐久性與流量之設計。
-液體濾器-
上述本發明之實施形態的液體濾器用基材,係可在適宜進行與藥液的親和性賦予加工後,加工成筒匣形體,作為液體濾器使用。
液體濾器係用於自含有由有機物及/或無機物所成的顆粒之被處理液中,去除該顆粒之器具。顆粒係在被處理液中以固體狀或凝膠狀存在。於本實施形態中,適合於去除粒徑未達約10nm(較佳為數nm)之顆粒的情況。又,液體濾器不僅可用於半導體之製造步驟,亦可例如用於顯示器製造及研磨等之其他製造步驟中。
作為液體濾器用基材,例如熟知由聚四氟乙烯及/或聚丙烯所成之多孔質基材。
與聚四氟乙烯多孔質基材比較下,上述本發明之實施形態的聚烯烴微多孔膜所成的基材係與藥液的親和性較良好。因此,例如濾器與藥液的親和性賦予加工變容易。又,於濾器殼體內裝填濾筒,填充藥液時,不易在濾筒內出現空氣滯留,藥液的過濾良率變良好。再者,由於聚乙
烯樹脂本身不含鹵素元素,使用過的濾筒之處理為容易,亦具有能減低環境負荷等之效果。
本發明之實施形態的液體濾器用基材(層合聚烯烴微多孔膜)只要至少具有A層及B層,而且得到上述泡點及透水性能之方法,則可以任何的方法來製造。於本發明之實施形態中,較佳為藉由具有以下所示之步驟(I)~步驟(V)的液體濾器用基材之製造方法來製造。即,(I)對於A層,調製至少含有聚烯烴(較佳為含有5質量%以上的聚烯烴之聚烯烴組成物,更佳為上述聚乙烯組成物)及溶劑的第1溶液之步驟,(II)對於B層,調製至少含有聚烯烴(較佳為含有5質量%以上的聚烯烴之聚烯烴組成物,更佳為上述聚乙烯組成物)溶劑及填料的第2溶液之步驟,(III)將上述步驟(I)的第1溶液經熔融混煉而得之熔融混煉物與上述步驟(II)的第2溶液經熔融混煉而得之熔融混煉物,自模頭(較佳為扁平模頭)共擠出,冷卻固化而得到多層的凝膠狀成形物之步驟,(IV)在至少一方向中延伸前述多層的凝膠狀成形物之步驟,(V)於至少一方向中延伸之步驟的前或後,去除前述多層的凝膠狀成形物中之溶劑的至少一部分之步驟。
於上述中,步驟(IV)及步驟(V)亦可任一者先進行,但
較佳為依順序實施下述,可更良好地製造。
(VI)於至少一方向中延伸多層的凝膠狀成形物之前,自多層的凝膠狀成形物中預先榨出一部分的溶劑之步驟,(VII)於至少一方向中延伸已榨出溶劑後之多層的凝膠狀成形物之步驟,(VIII)自延伸後的中間成形物之內部來萃取洗淨溶劑之步驟。
於步驟(I)中,調製含有A層中所含有的聚烯烴(較佳為含有5質量%以上的聚烯烴之聚烯烴組成物,更佳為上述聚乙烯組成物)及溶劑(較佳為大氣壓下沸點是210℃以上之不揮發溶劑)的第1溶液(用於形成上述A層之溶液)。此處,溶液較佳為熱可逆的溶膠-凝膠溶液,即藉由使聚烯烴在溶劑中加熱溶解而溶膠化,調製熱可逆的溶膠-凝膠溶液。
作為步驟(I)中的溶劑,只要是可充分膨潤或溶解聚烯烴者,則沒有特別的限制,但較佳為使用大氣壓下的沸點是210℃以上之不揮發溶劑或該不揮發溶劑與大氣壓下的沸點未達210℃之揮發溶劑的混合溶劑。作為不揮發溶劑,例如可舉出流動石蠟、石蠟油、礦油、蓖麻油或組合2種以上的此等之溶劑等。其中,作為不揮發溶劑,較佳為流動石蠟。作為揮發溶劑,例如較佳可舉出四氫萘、乙二醇、十氫萘、甲苯、二甲苯、二乙基三胺、乙二胺、二甲基亞碸、己烷或組合2種以上的此等之溶劑等。
於步驟(I)之溶液中,從控制液體濾器用基材(層合聚
烯烴微多孔膜)的液體透過性與作為濾材的捕集性能之觀點來看,聚烯烴之濃度,相對於溶液的全部質量,較佳為10質量%~45質量%,更佳為13質量%~25質量%。聚烯烴之濃度若為10質量%以上,則良好地維持力學強度,操縱性亦優異,更且可在聚烯烴微多孔膜之製膜中壓低切斷的發生頻率。又,聚烯烴之濃度若為45質量%以下,則容易形成空孔。
於步驟(II)中,調製含有B層中所含有的聚烯烴(較佳為含有5質量%以上的聚烯烴之聚烯烴組成物,更佳為上述聚乙烯組成物)、溶劑與填料的第2溶液(用於形成上述B層之溶液)。步驟(II)係可與上述步驟(I)同時地實施。
又,步驟(II)所用的溶劑及溶劑之含量、聚烯烴及聚烯烴之濃度係與上述步驟(I)同樣。
填料在第2溶液中的含量,相對於聚烯烴與填料之合計質量,較佳為40質量%以上80質量%以下,更佳為45質量%以上75質量%以下。
步驟(III)係將步驟(I)及步驟(II)所調製的第1溶液及第2溶液在各自的混煉器中熔融混煉,自模頭(較佳為扁平模頭)共擠出各自所得之熔融混煉物,冷卻固化而得到多層狀的凝膠狀成形物。較佳為將熔融混煉物在聚烯烴的熔點至「熔點+65℃」之溫度範圍中,自模頭(較佳為扁平模頭)共擠出而得到擠出物,其次冷卻前述擠出物而得到多層的凝膠狀成形物。
作為扁平模頭,可舉出多歧管型、供料頭型、堆疊板
型。作為成形物,較佳賦形為薄片狀。
冷卻係可在水溶液或有機溶劑中淬冷,也可澆鑄在經冷卻的金屬輥上。一般地,冷卻係採用在水或在溶膠-凝膠溶液時的揮發性溶劑中之淬冷的方法。冷卻溫度較佳為10℃~40℃。
再者,較佳為在水浴的表層設置水流,製作多層的凝膠狀成形物。藉此,自在水浴中凝膠化的成形物(例如薄片)之中所放出而浮遊在水面上的混合溶劑,係可不再度附著於成形物。
步驟(IV)係在一方向或二方向(例如MD及TD)中延伸多層的凝膠狀成形物之步驟。於在一方向或二方向(例如MD及TD)中延伸之步驟的前或後,可設置步驟(V),於步驟(V)中去除多層的凝膠狀成形物中之溶劑的至少一部分。
又,步驟(VI)係於至少一方向中延伸多層的凝膠狀成形物之前,預先榨出多層的凝膠狀成形物內之溶劑的一部分之步驟。於步驟(VI)中,例如藉由通過上下2個帶或輥之間隙等之方法,對於多層的凝膠狀成形物之面施加壓力,可適宜地實施。
榨出的溶劑量必須藉由液體濾器用基材所要求的液體透過性及過濾對象物之捕集性能來調整,該調整係可藉由上下的帶或輥間之擠壓力、榨出步驟之溫度、擠壓次數而調整至恰當的範圍。
再者,多層的凝膠狀成形物所受到的壓力,當以帶等
之面狀體進行時較佳為調整至0.1MPa~2.0MPa,當以輥等進行時較佳為調整至2kgf/m~45kgf/m。
榨出溫度較佳為10℃~100℃。
又,擠壓次數由於取決於設備的容許空間,可無特別地限制地實施。再者,視需要於溶劑的榨出前,可進行一段或複數段的預備加熱,自成形物(例如薄片)內去除一部分的溶劑。此時,預備加熱溫度較佳為50℃~100℃。
步驟(VII)係於至少一方向中延伸經前述步驟(VI)榨出溶劑後之多層的凝膠狀成形物,而製作中間成形物之步驟。此處,步驟(VII)之延伸較佳為雙軸延伸,亦可採用將縱延伸及橫延伸分別實施之逐次雙軸延伸,或將縱延伸及橫延伸同時實施之同時雙軸延伸的任一方法。又,亦較佳為在縱方向中複數次延伸後於橫方向中延伸之方法、在縱方向中延伸後於橫方向中複數次延伸之方法、在逐次雙軸延伸後更在縱方向及/或橫方向中1次或複數次延伸之方法。
總延伸倍率(=縱延伸倍率與橫延伸倍率之積),從控制聚烯烴微多孔膜的液體透過性與過濾對象物的捕集性能之觀點來看,較佳為20倍~60倍,更佳為20倍~50倍。延伸倍率若為60倍以下,則在層合聚烯烴微多孔膜的製膜中,壓低切斷的發生頻率。又,延伸倍率若為20倍以上,則更抑制厚度不均之發生。如前述較佳為延伸係在使溶劑以合適的狀態殘存之狀態下進行。延伸溫度較佳為80℃~125℃。
又,於(VII)的延伸步驟之後亦可進行熱定型處理。熱定型處理時的熱定型溫度,從控制液體濾器用基材的液體透過性與過濾對象物的捕集性能之觀點來看,較佳為110℃~140℃。熱定型溫度若為140℃以下,則液體濾器用基材的過濾對象物之捕集性能更優異。熱定型溫度若為110℃以上,則可良好地維持透過性能。
步驟(VIII)係自經延伸的中間成形物之內部來萃取洗淨溶劑之步驟。此處,步驟(VIII)為了自經延伸的中間成形物(延伸薄膜)之內部來萃取溶劑,較佳為以二氯甲烷等之鹵化烴、己烷等之烴等的溶劑進行洗淨。
當在滯留溶劑的槽內浸漬中間成形物而洗淨時,洗淨花費20秒~150秒之時間者,由於得到雜質的溶出少之液體濾器用基材(層合聚烯烴微多孔膜)而較佳,更佳為30秒~150秒,特佳為30秒~120秒。再者,為了進一步提高洗淨的效果,較佳為將槽分成數段,自層合聚烯烴微多孔膜之搬送步驟的下游側注入洗淨溶劑,使洗淨溶劑朝向步驟搬送的上游側流動,使下游槽的洗淨溶劑之純度比上游層者更高。
又,取決於對於液體濾器用基材的要求性能,亦可藉由退火處理進行熱定型。再者,從在步驟的搬送性等之觀點來看,退火處理較佳為在50℃~150℃實施,更佳為在50℃~140℃實施。
藉由此製法,可提供液體濾器用基材,其兼具優異的液體透過性與優異的過濾對象物之捕集性能,而且在長期
使用中具有安定的液體透過性。
再者,於本揭示中,液體濾器用基材之製造方法係不限定於上述者。例如,於上述步驟(III)中,不藉由扁平模頭等的共擠出,亦可為分別設置A層用的模頭與B層用的模頭,以各模頭擠出多層的凝膠狀成形物後,貼合兩成形物,製作層合凝膠狀薄片之方法。又,也可分別預先製作A層的微多孔膜與B層的微多孔膜,使用接著劑等接著A層與B層而成為液體濾器用基材。
以下,藉由實施例更具體地說明本發明之一實施形態,本實施形態只要不超出其主旨,則不受以下之實施例所限定。再者,只要沒有特別預先指明,則「份」係以質量基準。
(透水性能(水流量))
預先在乙醇中浸漬層合聚烯烴微多孔膜,於室溫下乾燥。將此層合聚烯烴微多孔膜固定於直徑37mm的不透鋼製之透液單元(透液面積Scm2)。以少量(0.5ml)的乙醇濕潤透液單元上的該層合聚烯烴微多孔膜後,以90kPa的差壓使經預先計量的純水V(100ml)穿透,計測純水全量穿透時所需要的時間T1(min)。自該純水的液量與純水之穿透所需要的時間,藉由以下之式計算90kPa差壓下的每單位
時間(min).單位面積(cm2)之透水量Vs,將此當作透水性能(ml/min.cm2)。測定係在24℃的溫度環境下進行。
Vs=V/(T1×S)
(泡點)
層合聚烯烴微多孔膜之泡點係依據ASTM E-128-61,於測定溶劑使用乙醇進行測定。
(厚度)
以接觸式的膜厚計(Mitutoyo公司製)測定層合聚烯烴微多孔膜的膜厚20點,將此等平均而求得。此處,接觸端子係使用底面為直徑0.5cm的圓柱狀者。測定壓力為0.1N。
(空孔率)
層合聚烯烴微多孔膜之空孔率(ε)係藉由下述式算出。
ε(%)={1-Ws/(ds.t)}×100
Ws:層合聚烯烴微多孔膜的單位面積重量(g/m2)
ds:聚烯烴的真密度(g/cm3)
t:層合聚烯烴微多孔膜的膜厚(μm)
再者,層合聚烯烴微多孔膜的單位面積重量,係自樣品切出10cm×10cm,測定其質量,將質量除以面積而求得單位面積重量。
(固體捕集性能)
使含有0.0045質量%的金膠體(平均粒徑3nm)之水溶液100ml以差壓10kPa通過層合聚烯烴微多孔膜而進行過濾。自過濾前的金膠體水溶液100ml之質量(M1)與通過層合聚烯烴微多孔膜的濾液之質量(M2)的差,依照下述式求得金膠體的捕集率。
再者,固體捕集性能之評價係將捕集率為90%以上時判斷為最良好(AA),將捕集率為80%以上且未達90%時判斷為良好(A),將捕集率未達80%時判斷為不良(B)。
捕集率(%)=((M1-M2)/(M1×45×10-6))×100
(透水量變化率(送液安定性))
預先在乙醇中浸漬層合聚烯烴微多孔膜,於室溫下乾燥。將此層合聚烯烴微多孔膜以0.5mm間隔重疊5片,固定於直徑37mm的不透鋼製之透液單元(透液面積Scm2)上,以少量(0.5ml)的乙醇濕潤透液單元上的該層合聚烯烴微多孔膜。然後,於40kPa的差壓下使純水200ml穿透層合聚烯烴微多孔膜,計測全量穿透層合聚烯烴微多孔膜所需要的時間(T1),其後立即開放差壓狀態。繼續,使用相同樣品,重複於40kPa的差壓下使純水200ml穿透,立即開放差壓之操作100次。計測第100次的純水200ml之穿透所需要的時間(T100),藉由以下之式算出透水量變化率(%)。
再者,評價係將透水量變化率為10%以下時判斷為最
良好(AA),將透水量變化率超過10%且15%以下時判斷為良好(A),將透水量變化率超過15%時判斷為不良(B)。再者,透水量變化率若良好,則亦可理解在長期使用中能維持良好的多孔質構造。
透水量變化率(%)=(T100-T1)/T1×100
(實施例1)
作為A層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE1)20質量%與重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE2)80質量%,以樹脂組成總量成為17質量份之方式,摻混預先準備的流動石蠟83質量份,調製聚乙烯溶液A。
作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)5質量%、重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE4)20質量%與由平均粒徑0.8μm的氫氧化鎂所成之填料75質量%,以固體成分總質量成為35質量份之方式,摻混預先準備的流動石蠟65質量份,調製聚乙烯溶液B。
將所得之聚乙烯溶液A與聚乙烯溶液B供給至供料頭,於溫度175℃熔融混煉而各自成為混煉物,自模頭共擠出此2個混煉物,成形為多層薄片狀,將所成形的多層薄片在水浴中冷卻至20℃,同時製作層凝膠狀薄片(基礎膠帶)。此時,在水浴的表層設置水流,自在水浴中凝膠化的多層薄片之中所放出而浮遊在水面上的溶劑,係不再
度附著於多層薄片。
將所製作的基礎膠帶,在經加熱至40℃的輥上邊施加20kgf/m的推壓邊搬送,而自基礎膠帶內去除流動石蠟的一部分。然後,將基礎膠帶在長度方向(MD)中於溫度90℃下以倍率4倍進行延伸,繼續在寬度方向(TD)中於溫度105℃下以倍率7倍進行延伸而雙軸延伸。然後,立即在128℃進行熱處理(熱定型)。
其次,一邊將經雙軸延伸的基礎膠帶在分成2槽的二氯甲烷浴中各自各30秒連續浸漬,一邊萃取流動石蠟。此處,將開始浸漬側當作第1槽,將結束浸漬側當作第2槽時,洗淨溶劑的純度為(低)第1層<第2槽(高)。
然後,在45℃乾燥去除二氯甲烷,邊在經加熱至120℃的輥上搬送邊進行退火處理,而得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係粒徑3nm的金膠體粒子之捕集率為90%以上,顯示優異的捕集性能,送液安定性與液體透過性亦優異。
表1中顯示上述的製造條件,表2中顯示所得之層合聚烯烴微多孔膜的物性。再者,關於以下的實施例及比較例,亦同樣地顯示於表1及表2中。
(實施例2)
作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)7.5質量%、重量平均分子量為30
萬且密度為0.96g/cm3之高密度聚乙烯(PE4)29.5質量%與氫氧化鎂(填料)63質量%,以固體成分總質量成為35質量份之方式,摻混預先準備的流動石蠟65質量份,調製聚乙烯溶液B。
除了於實施例1中,換成上述的聚乙烯溶液B以外,與實施例1同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係粒徑3nm的金膠體粒子之捕集率為90%以上,顯示優異的捕集性能,送液安定性與液體透過性亦優異。
(實施例3)
作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)9質量%、重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE4)35質量%與氫氧化鎂(填料;平均粒徑0.8μm)56質量%,以固體成分總質量成為30質量份之方式,摻混預先準備的流動石蠟70質量份,調製聚乙烯溶液B。
除了於實施例1中,換成上述的聚乙烯溶液B以外,與實施例1同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係粒徑3nm的金膠體粒子之捕集率為90%以上,顯示優異的捕集性能,送液安定性與液體透過性亦優異。
(實施例4)
作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)12質量%、重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE4)48質量%與氫氧化鎂(填料;平均粒徑0.8μm)40質量%,以固體成分總質量成為26質量份之方式,摻混預先準備的流動石蠟74質量份,調製聚乙烯溶液B。
除了於實施例1中,換成上述的聚乙烯溶液B以外,與實施例1同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係粒徑3nm的金膠體粒子之捕集率為80%以上,顯示優異的捕集性能,送液安定性與液體透過性亦優異。
(比較例1)
作為A層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE1)20質量%與重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE2)80質量%,以樹脂組成總量成為17質量份之方式,摻混預先準備的流動石蠟83質量份,調製聚乙烯溶液A。作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)13質量%、重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE4)49質量%與平均粒徑0.8μm的氫氧化鎂所成之填料38質量%,以固體成分總質量成為24質量份之方式,摻混預先準備的流動石蠟76質量份,調製聚乙烯溶液B。
除了於實施例1中,換成上述的聚乙烯溶液B及聚乙烯溶液B以外,與實施例1同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係泡點低,而且粒徑3nm的金膠體粒子之捕集率未達80%,送液安定性不充分。
(比較例2)
作為A層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE1)17質量%與重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE2)83質量份,以樹脂組成總量成為17質量份之方式,摻混預先準備的流動石蠟83質量份,調製聚乙烯溶液A。
作為B層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE3)17質量%與重量平均分子量為56萬且密度為0.96g/cm3之高密度聚乙烯(PE4)83質量%,以固體成分總質量成為25質量份之方式,摻混預先準備的流動石蠟72質量份與十氫萘3質量份,調製聚乙烯溶液B。
將所得之聚乙烯溶液A與聚乙烯溶液B供給至供料頭,於160℃熔融混煉而各自成為混煉物,自模頭共擠出此2個混煉物,成形為多層薄片狀,將所成形的多層薄片在水浴中冷卻至25℃,同時製作層凝膠狀薄片(基礎膠帶)。此時,在水浴的表層設置水流,自在水浴中凝膠化的多層薄片之中所放出而浮遊在水面上的溶劑,係不再度
附著於多層薄片。
將所製作的基礎膠帶,在55℃ 10分鐘,更且在95℃ 10分鐘使乾燥,而自基礎膠帶內去除十氫萘。然後,將基礎膠帶在經加熱至85℃的輥上邊施加20kgf/m的推壓邊搬送,而自基礎膠帶內去除流動石蠟的一部分。然後,將基礎膠帶在長度方向(MD)中於溫度100℃下以倍率5.8倍進行延伸,在寬度方向(TD)中於溫度100℃下以倍率14倍進行延伸而雙軸延伸。然後,立即在118℃進行熱處理(熱定型)。
其次,一邊將經雙軸延伸的基礎膠帶在分成2槽的二氯甲烷浴中各自各30秒連續浸漬,一邊萃取流動石蠟。此處,將開始浸漬側當作第1槽,將結束浸漬側當作第2槽時,洗淨溶劑的純度為(低)第1層<第2槽(高)。
然後,在45℃乾燥去除二氯甲烷,邊在經加熱至110℃的輥上搬送邊進行退火處理,而得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係金膠體粒徑3nm的金膠體粒子之捕集率為80%以上,雖然顯示優異的捕集性能,但送液安定性與透水性能不充分。
(比較例3)
作為A層用的溶液,混合重量平均分子量440萬之超高分子量聚乙烯(PE1)20質量%與重量平均分子量30萬且密度為0.96g/cm3之高密度聚乙烯(PE2)80質量%,以樹脂
組成總量成為17質量份之方式,摻混預先準備的流動石蠟83質量份,調製聚乙烯溶液A。
作為B層用的溶液,混合重量平均分子量440萬之超高分子聚乙烯(PE3)30質量%與重量平均分子量為56萬且密度為0.96g/cm3之高密度聚乙烯(PE4)70質量%,以固體成分總量成為32質量份之方式,摻混預先準備的流動石蠟53質量份及十氫萘15重量部,調製聚乙烯溶液B。
除了於比較例2中,換成上述的聚乙烯溶液A及聚乙烯溶液B以外,與比較例2同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係金膠體粒徑3nm之捕集率為80%以上,雖然顯示優異的捕集性能,但泡點高而且送液安定性與透水性能亦不充分。
(比較例4)
作為A層用的溶液,混合重量平均分子量為440萬之超高分子量聚乙烯(PE1)20質量%與重量平均分子量為30萬且密度為0.96g/cm3之高密度聚乙烯(PE2)80質量%,以樹脂組成總量成為17質量份之方式,摻混預先準備的流動石蠟83質量份,調製聚乙烯溶液A。作為B層用的溶液,混合重量平均分子量440萬之超高分子聚乙烯(PE3)3.9質量%、重量平均分子量30萬且密度為0.96g/cm3之高密度聚乙烯(PE4)15.6質量%與平均粒徑0.8μm之氫氧化鎂(填料)80.5質量%,以固體成分總質量
成為34質量份之方式,摻混預先準備的流動石蠟66質量份,調製聚乙烯溶液B。
除了於實施例1中,換成上述的聚乙烯溶液A及聚乙烯溶液B以外,與實施例1同樣地,得到層合聚烯烴微多孔膜。
所得之層合聚烯烴微多孔膜係透水性能高,而且金膠體粒徑3nm之捕集率未達80%,送液安定性亦不充分。
日本申請案2014-130045之揭示係藉由參照其全體而併入本說明書中。
本說明書中所記載的全部文獻、專利申請案及技術規格係藉由參照各個文獻、專利申請案及技術規格而併入,
具體地以與各個記載的情況相同程度,藉由參照而併入本說明書中。
Claims (7)
- 一種液體濾器用基材,其具有含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層,泡點為0.40Mpa以上0.80Mpa以下,透水性能為1.0ml/min‧cm2以上4.0ml/min‧cm2以下,並且厚度為7μm以上25μm以下。
- 一種液體濾器用基材,其具有含有聚烯烴的微多孔膜狀之A層的至少1層、與含有聚烯烴及填料的微多孔膜狀之B層的至少1層,前述A層及前述B層中所含有的聚烯烴係由混合有重量平均分子量為90萬以上的超高分子量聚乙烯與重量平均分子量為20萬~80萬的高密度聚乙烯之聚乙烯組成物所構成,泡點為0.40Mpa以上0.80Mpa以下,透水性能為1.0ml/min‧cm2以上4.0ml/min‧cm2以下。
- 如請求項1或2之液體濾器用基材,其中相對於前述B層的全部固體成分之合計質量,前述B層中的前述填料之含量為40質量%以上80質量%以下。
- 如請求項1或2之液體濾器用基材,其空孔率為50%以上且未達75%。
- 如請求項2之液體濾器用基材,其厚度為7μm以上 25μm以下。
- 如請求項1或2之液體濾器用基材,其中前述B層中的前述填料之平均粒徑為0.2μm~2.0μm。
- 一種液體濾器用基材之製造方法,其係如請求項1~6中任一項之液體濾器用基材之製造方法,具有:調製含有聚烯烴及溶劑的第1溶液之步驟,調製含有聚烯烴、溶劑及填料的第2溶液之步驟,將前述第1溶液經熔融混煉而得之熔融混煉物與前述第2溶液經熔融混煉而得之熔融混煉物,自模頭共擠出,冷卻固化而得到多層的凝膠狀成形物之步驟,在至少一方向中延伸前述多層的凝膠狀成形物之步驟,與於至少一方向中延伸之步驟的前或後,去除前述多層的凝膠狀成形物中之溶劑的至少一部分之步驟。
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JP6573650B2 (ja) | 2017-09-15 | 2019-09-11 | 住友化学株式会社 | ガス分離方法 |
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US4778601A (en) * | 1984-10-09 | 1988-10-18 | Millipore Corporation | Microporous membranes of ultrahigh molecular weight polyethylene |
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US5786396A (en) * | 1996-08-21 | 1998-07-28 | Tonen Chemical Corporation | Method of producing microporous polyolefin membrane |
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JP5164413B2 (ja) * | 2007-04-04 | 2013-03-21 | 旭化成イーマテリアルズ株式会社 | 複合微多孔膜、電池用セパレータ、及び複合微多孔膜の製造方法 |
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US20130228519A1 (en) * | 2011-11-04 | 2013-09-05 | Ppg Industries Ohio, Inc. | Microporous material having filtration and adsorption properties and their use in fluid purification processes |
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