TW201634539A - 複合膜的製造方法 - Google Patents
複合膜的製造方法 Download PDFInfo
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- TW201634539A TW201634539A TW104143188A TW104143188A TW201634539A TW 201634539 A TW201634539 A TW 201634539A TW 104143188 A TW104143188 A TW 104143188A TW 104143188 A TW104143188 A TW 104143188A TW 201634539 A TW201634539 A TW 201634539A
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- composite film
- hot air
- drying
- temperature
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Classifications
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Abstract
一種複合膜的製造方法,具有:在多孔質基材的單面或是雙面,將含有樹脂的塗抹液塗抹而形成塗抹層的塗抹過程;及使前述塗抹層與凝固液接觸使前述樹脂凝固,而獲得在前述多孔質基材的單面或是雙面具備含有前述樹脂的多孔質層的複合膜的凝固過程;及將前述複合膜沖水的沖水過程;及將前述複合膜以搬運速度30m/min以上一邊搬運一邊從前述複合膜將水除去,使用具備內含接觸式加熱手段及熱風送風手段的乾燥手段的乾燥裝置,將前述複合膜與前述接觸式加熱手段接觸並且將從前述熱風送風手段被送風的熱風與前述複合膜接觸而從前述複合膜將水除去的乾燥過程。
Description
本發明,是有關於複合膜的製造方法。
習知,已知在電池隔件、氣體過濾器、液體過濾器等的多孔質基材上具有多孔質層的複合膜。此複合膜的製造方法,已知將包含樹脂的塗抹液塗抹在多孔質基材上而形成塗抹層,浸漬在凝固液使塗抹層中的樹脂凝固,經過沖水及乾燥來製作多孔質層的方法之濕式製法(例如專利文獻1參照)。濕式製法,已知是可以將包含樹脂的多孔質層良好地多孔化的製法。
[專利文獻1]日本專利第5134526號公報
在多孔質基材上將具有多孔質層的複合膜由濕式製法量產的話,將長條的多孔質基材朝塗抹、凝固、沖水及乾燥的各過程依序搬運將這些的過程連續實施較佳,若從提高生產性的觀點,是在各過程提高多孔質基材的搬運速度較佳。但是,將多孔質基材的搬運速度提高的方式實施乾燥過程的話,會具有:設在多孔質基材上的多孔質層會剝離、在複合膜發生短縮、變形、皺褶的情況。至此為止,濕式製法的乾燥過程中的為了解決上述課題的最佳的手段未被提案。
本發明的實施例,是以上述狀況為基礎。
本發明的實施例的目的是提供一種複合膜的製造方法,可由較高的生產效率將高品質的複合膜製造。
將前述課題解決用的具體手段,包含以下的態樣。
[1]一種複合膜的製造方法,具有:在多孔質基材的單面或是雙面,將含有樹脂的塗抹液塗抹而形成塗抹層的塗抹過程;及使前述塗抹層與凝固液接觸使前述樹脂凝固,而獲得在前述多孔質基材的單面或是雙面具備含有前述樹脂的多孔質層的複合膜的凝固過程;及將前述複合膜沖水的沖水過程;及將前述複合膜由搬運速度30m/min以上一邊搬運一邊從前述複合膜將水除去,使用具備內含接觸式加熱手段及熱風送風手段的乾燥手段的乾燥
裝置,將前述複合膜與前述接觸式加熱手段接觸並且將從前述熱風送風手段被送風的熱風與前述複合膜接觸從前述複合膜將水除去的乾燥過程。
[2]如[1]的製造方法,其中,前述多孔質基材,是在105℃下放置30分鐘時的機械方向的熱收縮率是10%以下且寬度方向的熱收縮率是5%以下。
[3]如[1]或[2]的製造方法,其中,前述接觸式加熱手段,其與前述複合膜接觸的面的溫度是105℃以下,前述熱風,其在前述熱風送風手段的送風口中的溫度是105℃以下。
[4]如[1]~[3]項中任一項的製造方法,其中,前述熱風,其在前述熱風送風手段的送風口中的風速是5m/sec以上30m/sec以下。
[5]如[1]~[4]項中任一項的製造方法,其中,前述乾燥裝置,是具備2個以上的前述乾燥手段,在前述乾燥裝置具有2個以上的前述接觸式加熱手段,是藉由與前述複合膜接觸的面的溫度的異同被分為2個以上的群,構成與前述第一群的下游側相鄰接的群也就是第二群的前述接觸式加熱手段的前述面的溫度,是比構成前述複合膜的搬運方向的最上游側也就是第一群的前述接觸式加熱手段的前述面的溫度更高。
[6]如[1]~[5]項中任一項的製造方法,其中,對於前述複合膜的前述接觸式加熱手段的總接觸長是30m以下。
[7]如[1]~[6]項中任一項的製造方法,其中,前述乾燥裝置,是具備前述乾燥手段被配置於內部的具有搬入口及搬出口的外殼,從前述搬入口至前述搬出口為止的前述複合膜的搬運長度是50m以下。
[8]如[1]~[7]項中任一項的製造方法,其中,前述接觸式加熱手段,其與前述複合膜接觸的面是含有氟系樹脂。
依據本發明的實施例的話,可提供一種複合膜的製造方法,可由較高的生產效率將高品質的複合膜製造。
10‧‧‧乾燥裝置
21‧‧‧外殼
22‧‧‧搬入口
23‧‧‧搬出口
31、32、33、34‧‧‧加熱滾子
41、42、43、44‧‧‧熱風送風手段
41a‧‧‧外殼
41b‧‧‧送風口
51、52、53、54‧‧‧乾燥手段
61‧‧‧驅動滾子
70‧‧‧複合膜
[第1圖]顯示本揭示的製造方法的一實施例的概念圖。
[第2圖]顯示本揭示的製造方法所使用的乾燥裝置的一例的概略圖。
[第3圖A]顯示熱風送風手段所具有的送風口的一例的概略圖。
[第3圖B]顯示熱風送風手段所具有的送風口的一例的概略圖。
在本說明書中使用「~」顯示的數值範圍,是包含各別被揭示於「~」的前後的數值的最小值及最大值的範圍。
本說明書的「過程」,不是只有獨立的過程,即使無法與其他的過程明確區別的情況,只要可達成其過程所期的目的的話,也被包含於本用語。
在本說明書中,「機械方向」,在呈長條狀被製造的多孔質基材及複合膜中是指長條方向的意思,「寬度方向」,是指與「機械方向」垂直交叉的方向的意思。「機械方向」也稱為「MD方向」,「寬度方向」也稱為「TD方向」。
以下,說明本發明的實施例。這些的說明及實施例只是例示本發明,不是限制本發明的範圍。
本揭示的製造方法,是製造具備:多孔質基材、及設在該多孔質基材的單面或是雙面的含有樹脂的多孔質層,的複合膜的方法。本揭示的製造方法,是將含有樹脂的塗抹液,塗抹在多孔質基材的單面或是雙面,在多孔質基材的單面或是雙面設置多孔質層的製造方法。本揭示的製造方法,是具有下述的過程。
‧在多孔質基材的單面或是雙面,將含有樹脂的塗抹液塗
抹而形成塗抹層的塗抹過程。
‧將塗抹層與凝固液接觸使樹脂凝固,而獲得在多孔質基材的單面或是雙面具備含有樹脂的多孔質層的複合膜的凝固過程。
‧將複合膜沖水的沖水過程。
‧從複合膜將水除去的乾燥過程。
本揭示的製造方法,是濕式製法的方法,在多孔質基材上設置多孔質層的製造方法。
本揭示的製造方法,是進一步,具有將在塗抹過程使用的塗抹液調製的塗抹液調製過程也可以。
第1圖,是顯示本揭示的製造方法的一實施例的概念圖。在第1圖中,複合膜的製造用的多孔質基材的滾子是被放置在圖內的左側,將複合膜捲取的滾子被放置在圖內的右側。第1圖所示的實施例,是具有:塗抹液調製過程、塗抹過程、凝固過程、沖水過程、及乾燥過程。本實施例,是將塗抹過程、凝固過程、沖水過程、及乾燥過程連續地依序進行。且,本實施例,是配合塗抹過程的實施時期進行塗抹液調製過程。各過程的詳細如後述。
本揭示的製造方法,若從複合膜的生產效率的觀點,乾燥過程的複合膜的搬運速度是30m/min以上。搬運速度愈快速附著於複合膜的水分除去愈困難,如何可以將複合膜的品質有效維持的方式足夠地乾燥是成為重要的重點。在此,在本揭示的製造方法中,乾燥過程,是使
用具有接觸式加熱手段及熱風送風手段的乾燥手段,將複合膜與接觸式加熱手段接觸,並且將從熱風送風手段被送風的熱風與複合膜接觸,從複合膜將水除去的過程。依據此乾燥過程的話,與乾燥手段是只有使用接觸式加熱手段的乾燥過程相比,多孔質層的剝離困難,與乾燥手段只有使用熱風送風手段的乾燥過程相比,在複合膜不易發生短縮、變形、及皺褶。因此,依據本揭示的製造方法的話,可以由較高的生產效率將高品質的複合膜製造。乾燥過程的複合膜的搬運速度是30m/min未滿的話,會具有生產效率差,在複合膜會發生短縮、變形、或是皺褶,多孔質層的剝離發生的情況。
依據本揭示的製造方法的話,因為乾燥手段是將接觸式加熱手段及熱風送風手段併設且使用兩者從複合膜將水除去,所以在乾燥過程所需要的時間可短縮,且不需要加長乾燥過程的搬運長度,可抑制製造設備的設置空間及設置成本。
以下,將本揭示的製造方法的各過程詳細說明。
本揭示的製造方法,是具有將用在塗抹過程的塗抹液調製的塗抹液調製過程也可以。本揭示的製造方法,是不具有塗抹液調製過程也可以,在塗抹過程中,供給已經被製造且被保管的塗抹液也可以。
塗抹液調製過程,是將含有樹脂的塗抹液調製的過程。塗抹液,是例如,將樹脂溶化在溶劑,依據需要進一步將無機充填料和有機充填料分散地調製。對於在塗抹液的調製所使用的樹脂和充填料等,即,多孔質層所包含的樹脂和充填料等,是在後述的[多孔質層]的項詳細說明。
在塗抹液的調製所使用的樹脂溶解的溶劑(以下也稱為「良溶劑」),可舉例N-甲基吡咯烷酮、二甲基乙酰胺、二甲基甲醯胺、二甲基甲醯胺等的極性醯胺溶劑。若從形成具有良好的多孔構造的多孔質層的觀點,將誘發相分離的相分離劑混合在良溶劑較佳。相分離劑,可舉例水、甲醇、乙醇、丙基醇、丁基醇、丁二醇、乙二醇、丙二醇、三丙二醇等。相分離劑,是由在塗抹時可以確保適切的塗抹液的黏度的範圍的量比的方式與良溶劑混合較佳。
在塗抹液的調製使用的溶劑,若從形成良好的多孔構造的觀點,包含良溶劑60質量%以上、相分離劑5質量%~40質量%的混合溶劑較佳。塗抹液,若從形成良好的多孔構造的觀點,樹脂是包含3質量%~15質量%的濃度較佳。
塗抹過程,是在多孔質基材的單面或是雙面,將含有樹脂的塗抹液塗抹而形成塗抹層的過程。朝多孔質基材的
塗抹液的塗抹,是藉由塗抹試驗機、模具塗抹機、反向滾子塗抹機、凹板塗抹機等的塗抹手段進行。塗抹量,是雙面合計為例如10mL/m2~60mL/m2。
塗抹過程的一實施例,是使用:透過多孔質基材被相面對配置的將一方的面塗抹的第一塗抹手段、及將另一方的面塗抹的第二塗抹手段,將塗抹液同時塗抹在多孔質基材的雙面的形態。
塗抹過程的一實施例,是使用:在多孔質基材的搬運方向被分離配置的將一方的面塗抹的第一塗抹手段、及將另一方的面塗抹的第二塗抹手段,將塗抹液每次單面地依序塗抹在多孔質基材的雙面的形態。
凝固過程,是將塗抹層與凝固液接觸使被包含於塗抹層的樹脂凝固,而獲得在多孔質基材的單面或是雙面具備多孔質層的複合膜的過程。將塗抹層與凝固液接觸的方法,是將具有塗抹層的多孔質基材,浸漬在凝固液較佳,具體而言,通過放入了凝固液的槽(凝固槽)較佳。
凝固液,一般是使用於塗抹液的調製的良溶劑及相分離劑、及水的混合溶液。良溶劑及相分離劑的混合比,是配合使用於塗抹液的調製的混合溶劑的混合比的話,生產性較佳。凝固液的水的含有量,若從多孔構造的形成及生產性的觀點,是40質量%~80質量%較佳。凝固液的溫度是例如10℃~50℃。
沖水過程,是由將在複合膜所包含的溶劑(塗抹液的溶劑、及凝固液的溶劑)除去的目的,將複合膜沖水的過程。沖水過程,是將複合膜在水浴中搬運的過程較佳。沖水用的水的溫度,是例如0℃~70℃。
乾燥過程,是由將在沖水後的複合膜所包含的水除去的目的而進行的過程。
乾燥過程中的複合膜的搬運速度,若從複合膜的生產效率的觀點,是30m/min以上。前述搬運速度,更佳是40m/min以上,進一步較佳是50m/min以上。另一方面,前述搬運速度的上限,若從確保乾燥時間的觀點,是100m/min以下較佳。
實施乾燥過程的乾燥裝置,是具備內含接觸式加熱手段及熱風送風手段的乾燥手段。乾燥裝置,是具備前述乾燥手段1個或是2個以上,若從乾燥效率的觀點,具備前述乾燥手段2個以上較佳。
接觸式加熱手段,具體而言,可舉例加熱滾子、加熱皮帶、熱板等。接觸式加熱手段是加熱滾子或是加熱皮帶的情況,加熱滾子或是加熱皮帶的外周面是與複合膜接觸的面。
在本揭示的製造方法中,乾燥裝置,不具備
外殼也可以,但是若從將複合膜的周圍的溫度及濕度控制的觀點,具備外殼較佳。
在以下將乾燥裝置的實施例,一邊參照圖面一邊說明,但是本揭示的製造方法當然不被限定於這些的例。以下,舉例接觸式加熱手段的其中一例的加熱滾子說明乾燥裝置的實施例。以下說明的乾燥裝置的實施例,其接觸式加熱手段也適用在加熱滾子以外的手段(例如加熱皮帶、熱板)的乾燥裝置。接觸式加熱手段是例如加熱皮帶或是熱板的實施例,是藉由將以下的說明中的加熱滾子31~34,換成加熱皮帶31~34或是熱板31~34就可以實施。
如第2圖所示的乾燥裝置10,是具備:外殼21、及被配置於外殼21的內部的乾燥手段51~54、及將複合膜70搬運用的驅動滾子61。外殼21,是具有:將複合膜70搬入用的搬入口22、及將複合膜70搬出用的搬出口23。外殼21,是例如金屬製。驅動滾子61,是藉由無圖示的馬達及控制部旋轉速度被控制。
乾燥裝置10是,為了將外殼21內部的溫度及濕度控制的目的,進一步具備溫度感測器、濕度感測器及排氣導管也可以。
在乾燥裝置10中,從搬入口22至搬出口23為止的複合膜70的搬運長度,若從省空間的觀點,是50m以下較佳,40m以下更佳,30m以下進一步較佳。另一方面,前述搬運長度,若從確保乾燥時間的觀點,是
5m以上較佳,10m以上更佳。
在外殼21內部,未限定乾燥手段51、52、53及54並列的方向。如第2圖所示,在外殼21的上面附近及下面附近之間使複合膜70往復的方式並列也可以,其以外例如,在外殼21的左側面附近及右側面附近之間使複合膜70往復的方式並列也可以。
乾燥手段51,是具備1個加熱滾子及1個熱風送風手段。乾燥手段51所具備的加熱滾子31及熱風送風手段41,是例如,被配置於將複合膜70挾在其間地相面對的位置。加熱滾子31及熱風送風手段41的位置關係,不限定於將複合膜70挾於其間地相面對的位置,從熱風送風手段41被送風的熱風可與和加熱滾子31接觸的複合膜70碰觸的位置關係即可。
乾燥手段51,是在加熱滾子31及熱風送風手段41之外,進一步具有朝複合膜70施加熱的其他的熱發生手段(例如遠紅外線照射手段等)也可以。
乾燥手段52~54、加熱滾子32~34及熱風送風手段42~44的形態,也與乾燥手段51、加熱滾子31及熱風送風手段41的形態同樣。
在第2圖中,顯示具有4個乾燥手段的乾燥裝置的例,但是乾燥手段的個數不限定於此,可從1個或是2個以上選擇。在第2圖中例示了,1個乾燥手段,是對於接觸式加熱手段1個,具備熱風送風手段1個的形態例,但是1個乾燥手段,是對於接觸式加熱手段1個,具
備熱風送風手段2個以上也可以。
加熱滾子31~34的外徑,是例如,10cm~200cm。加熱滾子31~34的寬度,是配合欲製造的複合膜的寬度選擇較佳,例如,10cm~300cm。
加熱滾子31~34的外周面的材質,是例如可舉例不鏽鋼、金屬電鍍、陶瓷、矽橡膠、氟系樹脂等。若從抑制複合膜附著於加熱滾子31~34的觀點,加熱滾子31~34的外周面是含有氟系樹脂較佳。氟系樹脂,是例如,可舉例聚四氟乙烯(PTFE)、全氟烷基氟樹脂(PFA)、四氟化乙烯‧六氟化丙烯共聚物(FEP)等。
加熱滾子31~34的外周面的溫度,若從抑制在複合膜70發生短縮、變形、皺褶的觀點,105℃以下較佳,100℃以下更佳,95℃以下進一步較佳。另一方面,前述溫度,若從將複合膜70乾燥的觀點,65℃以上較佳。
加熱滾子31~34,是可以將外周面的溫度各別控制較佳。加熱滾子31~34的外周面的溫度,是全部相同也可以,一部分相同也可以,彼此相異也可以。
加熱滾子31~34,若從抑制在複合膜70發生短縮、變形、皺褶的觀點,外周面的溫度是分開成不同的複數群較佳。由外周面的溫度的異同所產生的各群的例,是例如,可舉例下述(i)~(iii)。在以下的說明,T31、T32、T33、及T34,各別是加熱滾子31的外周面的溫度、加熱滾子32的外周面的溫度、加熱滾子33的外周面
的溫度、及加熱滾子34的外周面的溫度的意思。
(i)將加熱滾子31作為第一群,將加熱滾子32及33作為第二群,將加熱滾子34作為第三群。加熱滾子32的外周面的溫度、及加熱滾子33的外周面的溫度,是相同。
前述(i)的情況,第二群的外周面的溫度是比第一群的外周面的溫度更高,且,第三群的外周面的溫度是比第二群的外周面的溫度更低較佳。即,T31<T32=T33>T34的關係較佳。第一群的外周面的溫度、及第三群的外周面的溫度,是相同或相異也可以,相異的情況時,第三群的外周面的溫度是比第一群的外周面的溫度更高較佳。
(ii)將加熱滾子31及32作為第一群,將加熱滾子33及34作為第二群。加熱滾子31的外周面的溫度、及加熱滾子32的外周面的溫度,是相同。加熱滾子33的外周面的溫度、及加熱滾子34的外周面的溫度,是相同。
前述(ii)的情況,第二群的外周面的溫度是比第一群的外周面的溫度更高較佳。即,T31=T32<T33=T34的關係較佳。
將(iii)加熱滾子31作為第一群,將加熱滾子32作為第二群,將加熱滾子33作為第三群,將加熱滾子34作為第四群。
前述(iii)的情況,第二群的外周面的溫度是比第一群的外周面的溫度更高,且,第三群的外周面的
溫度是比第二群的外周面的溫度更高,且,第四群的外周面的溫度是比第三群的外周面的溫度更低較佳。即,T31<T32<T33>T34的關係較佳。第一群的外周面的溫度、及第四群的外周面的溫度,是相同或相異也可以,相異的情況時,第四群的外周面的溫度是比第一群的外周面的溫度更高較佳。第二群的外周面的溫度、及第四群的外周面的溫度,是相同或相異也可以,相異的情況時,第四群的外周面的溫度是比第二群的外周面的溫度更高較佳。
在上述(i)~(iii)的其中任一,構成與第一群的下游側相鄰接的群也就是第二群的加熱滾子的外周面的溫度,是比構成複合膜的搬運方向的最上游側也就是第一群的加熱滾子的外周面的溫度更高較佳。
在上述中,說明了加熱滾子的數量是4個的情況的例,但是乾燥裝置所具備的加熱滾子的數量不限定於此。對應乾燥裝置所具備的加熱滾子的全數量,增減被包含於上述(i)~(iii)的各群的加熱滾子的數量即可。
對於複合膜70的加熱滾子31~34的總接觸長,若從抑制在複合膜70發生短縮、變形、皺褶的觀點、及抑制多孔質層的剝離的觀點,30m以下較佳,20m以下更佳,10m以下進一步較佳。另一方面,前述總接觸長,若從乾燥效率的觀點,是1m以上較佳,3m以上更佳。前述總接觸長,是無關於乾燥裝置所具備的加熱滾子的個數,在上述範圍較佳。
加熱滾子31~34,是藉由馬達旋轉的驅動滾
子也可以,隨著複合膜70的搬運而旋轉的從動滾子也可以。
加熱滾子31~34,是驅動滾子的情況,可以將旋轉速度各別控制較佳。若從抑制在複合膜70發生短縮、變形、皺褶的觀點、及抑制多孔質層的剝離的觀點,加熱滾子31~34的旋轉速度,是以加熱滾子31為基準被調節在±5%以下的範圍較佳。加熱滾子31~34的旋轉速度的調節例,是例如,可舉例下述(a)及(b)。當然,加熱滾子31~34的旋轉速度,是全部相同也可以。
(a)對於加熱滾子31的旋轉速度,將加熱滾子32的旋轉速度調節至101%,將加熱滾子33的旋轉速度調節至102%,將加熱滾子34的旋轉速度調節至103%。
(b)對於加熱滾子31的旋轉速度,將加熱滾子32的旋轉速度調節至101%,將加熱滾子33的旋轉速度調節至101%,將加熱滾子34的旋轉速度調節至100%。
接著說明熱風送風手段41~44。熱風送風手段41~44,是例如,在具有將空氣吸入的吸氣口及將熱風吹出的送風口的外殼的內部,具備電熱器或是蒸氣加熱器或是熱媒加熱器、及送風用風扇。前述外殼,是例如,具有相面對於加熱滾子的圓弧狀的曲面,在此曲面被配置有1個或是複數個送風口。前述外殼,是例如金屬製。
熱風送風手段41~44,是將包含從送風口吹出的熱風的暖氣,從吸氣口吸氣,進行溫度調節和露點調節,將空氣循環使用較佳。
熱風送風手段41~44所具備的送風口,是例如,可舉例如第3圖A及第3圖B所示的形態例。第3圖A及第3圖B,是顯示熱風送風手段41所具有的送風口的一例的概略圖,顯示在外殼41a設在相面對於加熱滾子31的面的送風口41b。如第3圖A所示的送風口41b,其開口部的形狀是圓形,複數個是呈格子狀周期地被並列設置。如第3圖B所示的送風口41b,是開口部的形狀,是與複合膜70的搬運方向垂直交叉的方向長的長方形,複數個是在複合膜70的搬運方向由規定的間隔被並列設置。
送風口41b的開口部及加熱滾子的距離,是例如2cm~15cm,5cm~10cm較佳。
來自送風口41b的送風方向,是熱風到達複合膜70為止的距離最短的方向較佳,即,將開口部及加熱滾子連結的最短距離的方向較佳。
從熱風送風手段41~44被送風的熱風的送附口中的溫度,若從抑制在複合膜70發生短縮、變形、皺褶的觀點、及抑制多孔質層的剝離的觀點,是105℃以下較佳,100℃以下更佳,95℃以下進一步較佳。另一方面,前述溫度,若從將複合膜70乾燥的觀點,65℃以上較佳。
從熱風送風手段41~44被送風的熱風的送附口中的風速,若從抑制在複合膜70發生短縮、變形、皺褶的觀點、及抑制多孔質層的剝離的觀點,30m/sec以下
較佳,25m/sec以下更佳。另一方面,前述風速,若從乾燥效率的觀點,5m/sec以上較佳,10m/sec以上更佳。
熱風送風手段41~44,其送附口中的熱風的溫度,是全部相同也可以,一部分相同也可以,彼此相異也可以。熱風送風手段41~44,是送附口中的熱風的風速,是全部相同也可以,一部分相同也可以,彼此相異也可以。
在乾燥裝置10的下游側的隨後中,進一步,加熱滾子是單獨被設置1個或是設置複數個也可以,將從乾燥裝置10被搬出的複合膜70與該加熱滾子接觸使進一步乾燥也可以。
在乾燥裝置10的下游側的隨後中,由將複合膜70熱緩和的目的設置1個或是複數個加熱滾子也可以。上述的目的用的加熱滾子,是外周面溫度為60℃~130℃較佳。
在乾燥裝置10的上游側的之前,將複合膜70挾入從複合膜70將水分除去用的上下一對的壓輥,及/或,朝複合膜70將風吹附將水分甩開用的空氣噴嘴,是各別設置1個或是複數個也可以。
本揭示的製造方法,是採用下述的實施例也可以。
‧塗抹液調製過程的一部分,是由從塗抹液的調製用溶劑將異物除去的目的,在將該溶劑與樹脂混合前進行通過過濾器的處理。在此處理使用的過濾器的保留粒子徑,是例
如0.1μm~100μm。
‧在實施塗抹液調製過程的槽桶設置攪拌機,由攪拌機將時常塗抹液攪拌,來抑制塗抹液中的固態成分的沈降。
‧將從塗抹液調製過程至塗抹過程中運送塗抹液的配管作成循環式,在配管內使塗抹液循環來抑制塗抹液中的固態成分的凝集。此情況,將配管內的塗抹液的溫度一定地控制較佳。
‧在從塗抹液調製過程至塗抹過程將運送塗抹液的配管的中途處設置過濾器,將塗抹液中的凝集物及/或異物除去。
‧從塗抹液調製過程至塗抹過程中供給塗抹液的泵,是設置無脈動定量泵。
‧在塗抹過程的上游,配置靜電除去裝置,將多孔質基材表面除電。
‧在塗抹手段的周圍設置外殼,將塗抹過程的環境保持清淨,且,將塗抹過程的氣氛的溫度及濕度控制。
‧在塗抹手段的下游配置將塗抹量檢出的感測器,修正塗抹過程中的塗抹量。
以下,說明複合膜的多孔質基材及多孔質層的詳細。
在本揭示中多孔質基材,是指在內部具有空孔或空隙的基材的意思。這種基材,是可舉例:微多孔膜;由纖維
狀物所構成的不織布、紙等的多孔性薄片;在這些微多孔膜和多孔性薄片將其他的多孔性的層積層1層以上的複合多孔質薄片;等。在本揭示中,若從複合膜的薄膜化及強度的觀點,微多孔膜較佳。微多孔膜,是在內部具有多數的微細孔,這些微細孔是成為被連結的構造,使氣體或是液體可從一方的面朝另一方的面通過的膜的意思。
多孔質基材的材料,是具有電絕緣性的材料較佳,有機材料及無機材料皆可以。
多孔質基材的材料,若從在多孔質基材賦予關閉功能的觀點,是熱可塑性樹脂較佳。關閉功能,是在複合膜被適用於電池隔件的情況時電池溫度昇高時,藉由構成材料溶解將多孔質基材的孔閉塞而將離子的移動遮斷,來防止電池的熱暴走的功能。熱可塑性樹脂,是融點200℃未滿的熱可塑性樹脂,特別是聚烯烴較佳。
多孔質基材,是包含聚烯烴的微多孔膜(也稱為「聚烯烴微多孔膜」)較佳。聚烯烴微多孔膜,是例如,可舉例被適用在習知的電池隔件的聚烯烴微多孔膜,從此中選擇具有足夠的力學特性及物質透過性者較佳。
聚烯烴微多孔膜,若從使發生關閉功能的觀點,包含聚乙烯較佳,聚乙烯的含有量,是對於聚烯烴微多孔膜的全質量為95質量%以上較佳。
聚烯烴微多孔膜,是被曝在高溫時若從賦予不容易地破膜程度的耐熱性的觀點,是包含聚乙烯及聚丙烯的聚烯烴微多孔膜較佳。這種聚烯烴微多孔膜,可舉例
聚乙烯及聚丙烯在1個層混在的微多孔膜。在這種微多孔膜中,若從兼容關閉功能及耐熱性的觀點,包含95質量%以上的聚乙烯及5質量%以下的聚丙烯較佳。且,若從兼容關閉功能及耐熱性的觀點,聚烯烴微多孔膜是具備2層以上的積層構造,至少1層是包含聚乙烯,至少1層是包含聚丙烯的構造的聚烯烴微多孔膜也較佳。
被包含於聚烯烴微多孔膜的聚烯烴,其重量平均分子量是10萬~500萬的聚烯烴較佳。聚烯烴的重量平均分子量是10萬以上的話,可以在微多孔膜賦予足夠的力學特性。另一方面,聚烯烴的重量平均分子量是500萬以下的話,微多孔膜的關閉特性良好,且微多孔膜的成形容易。
聚烯烴微多孔膜的製造方法,可舉例:將熔融的聚烯烴樹脂從T-模具壓出而薄片化,將此結晶化處理之後延伸,接著熱處理而作成微多孔膜的方法;將流動石蠟等的可塑劑一起熔融的聚烯烴樹脂從T-模具壓出,將此冷卻薄片化,延伸之後,將可塑劑抽出,熱處理而作成微多孔膜的方法;等。
由纖維狀物所構成的多孔性薄片,可舉例由:聚對苯二甲酸乙二醇酯等的聚酯;聚乙烯、聚丙烯等的聚烯烴;芳香族聚醯胺、聚醯亞胺、聚醚磺、聚磺、聚醚酮,聚醚醯亞胺等的耐熱性樹脂;纖維素;等的纖維狀物所構成的不織布、紙等的多孔性薄片。耐熱性樹脂,是指融點是200℃以上的樹脂,或是不具有融點的分解溫度
是200℃以上的樹脂。
複合多孔質薄片,可舉例在由微多孔膜和纖維狀物所構成的多孔性薄片,將功能層積層的薄片。這種複合多孔質薄片,若從藉由功能層進一步附加功能的觀點較佳。功能層,若從例如賦予耐熱性的觀點,可舉例由耐熱性樹脂所構成的多孔性的層、和由耐熱性樹脂及無機充填料所構成的多孔性的層。耐熱性樹脂,可舉例從芳香族聚醯胺、聚醯亞胺、聚醚磺、聚磺、聚醚酮及聚醚醯亞胺所選擇的1種或是2種以上的耐熱性樹脂。無機充填料,可舉例氧化鋁等的金屬氧化物;氫氧化鎂等的金屬氫氧化物;等。複合化的手法,可舉例在微多孔膜和多孔性薄片將功能層塗抹的方法、將微多孔膜和多孔性薄片及功能層由黏著劑接合的方法、將微多孔膜和多孔性薄片及功能層熱壓合的方法等。
多孔質基材的寬度,若從朝本揭示的製造方法的適合性的觀點,0.1m~3.0m較佳。
多孔質基材的厚度,若從機械強度的觀點,是5μm~50μm較佳。
多孔質基材,是在105℃下放置30分鐘時的熱收縮率,是在MD方向為10%以下較佳,5%以下更佳,在TD方向為5%以下較佳,3%以下更佳。
多孔質基材的斷裂伸度,若從機械強度的觀點,在MD方向為10%以上較佳,20%以上更佳,在TD方向為10%以上較佳,20%以上更佳。多孔質基材的斷裂
伸度,是在溫度20℃的氣氛中,使用拉伸試驗機,由拉伸速度100mm/min進行拉伸試驗而求得。
多孔質基材的格利值(JIS P8117:2009),若從機械強度及物質透過性的觀點,是50秒/100cc~800秒/100cc較佳。
多孔質基材的空孔率,若從機械強度、處理性能、及物質透過性的觀點,是20%~60%較佳。
多孔質基材的平均孔徑,若從物質透過性的觀點,是20nm~100nm較佳。多孔質基材的平均孔徑,是依照ASTM E1294-89使用細孔徑分布計器所測量的值。
在本揭示中多孔質層,是在內部具有多數的微細孔,這些微細孔是成為被連結的構造,使氣體或是液體可從一方的面朝另一方的面通過的層。
多孔質層,是複合膜被適用在電池隔件的情況,可與電極黏著的黏著性多孔質層較佳。黏著性多孔質層,是與只有多孔質基材的單面相比,雙面較佳。
多孔質層,是將含有樹脂的塗抹液塗抹而形成。因此,多孔質層,是含有樹脂。多孔質層,若從多孔化的觀點,是將含有樹脂及充填料的塗抹液塗抹而形成較佳。因此,多孔質層,是含有樹脂及充填料較佳。充填料,是無機充填料及有機充填料皆可以。充填料,若從多
孔質層的多孔化及耐熱性的觀點,是無機粒子較佳。以下,說明在塗抹液及多孔質層所含有的樹脂等的成分。
多孔質層所包含的樹脂,無種類的限定。多孔質層所包含的樹脂,是具有將充填料固定化的功能者(接合劑樹脂)較佳。多孔質層所包含的樹脂,若從朝濕式製法的適合性的觀點,是疏水性樹脂較佳。多孔質層所包含的樹脂,是複合膜被適用在電池隔件的情況,電解液穩定,電氣化學性穩定,具有將無機粒子固定化的功能,可與電極黏著也較佳。多孔質層的樹脂是包含1種也可以包含2種以上也可以。
多孔質層所包含的樹脂,是例如,可舉例聚氟化亞乙烯、聚氟化亞乙烯共聚物、苯乙烯-丁二烯共聚物、丙烯腈和甲基丙烯腈等的乙烯腈類的均聚物或是共聚物、聚氧化乙烯和聚環氧丙烷等的聚醚類。其中,聚氟化亞乙烯及聚氟化亞乙烯共聚物(也稱為「聚氟化亞乙烯系樹脂」)較佳。
聚氟化亞乙烯系樹脂,可舉例氟化亞乙烯的均聚物(即聚氟化亞乙烯);氟化亞乙烯及其他的可共聚合的單體的共聚物(聚氟化亞乙烯共聚物);這些的混合物。可與氟化亞乙烯共聚合的單體,是例如,可舉例四氟代乙烯、六氟丙烯、三氟矽乙烯、三氯乙烯、氟化乙烯等,可以使用1種類或是2種類以上。聚氟化亞乙烯系樹脂,可
藉由乳化聚合或是懸濁聚合製造。
多孔質層所包含的樹脂,若從耐熱性的觀點,是耐熱性樹脂(融點是200℃以上的樹脂,或是不具有融點的分解溫度是200℃以上的樹脂)較佳。耐熱性樹脂,是例如,可舉例聚醯胺(耐綸)、全芳香族聚醯胺(芳族聚醯胺)、聚醯亞胺、聚醯胺醯亞胺、聚磺、聚酮、聚醚酮、聚醚磺、聚醚醯亞胺、纖維素、及這些的混合物。其中,若從多孔構造的形成的容易度、與無機粒子的粘合性、耐氧化性等的觀點,全芳香族聚醯胺較佳。全芳香族聚醯胺之中,若從成形容易的觀點,甲基型全芳香族聚醯胺較佳,特別是聚間苯二甲醯胺較佳。
多孔質層的充填料是包含無機粒子較佳。多孔質層所包含的無機粒子,是電解液穩定,且,電氣化學性穩定較佳。多孔質層的無機粒子是包含1種也可以包含2種以上也可以。
多孔質層所包含的無機粒子,是例如,可舉例氫氧化鋁、氫氧化鎂、氫氧化鈣、氫氧化鉻、氫氧化鋯、氫氧化鈰、氫氧化鎳、氫氧化硼等的金屬氫氧化物;二氧化矽、氧化鋁、氧化鋯、氧化鎂等的金屬氧化物;碳酸鈣、碳酸鎂等的碳酸鹽;硫酸鋇、硫酸鈣等的硫酸鹽;矽酸鈣、滑石等的黏土鑛物;等。其中,若從難燃性賦予和除電效果的觀點,金屬氫氧化物及金屬氧化物較佳。無
機粒子,是藉由有機矽烷偶合劑等被表面修飾者也可以。
多孔質層所包含的無機粒子的粒子形狀是任意,球形、橢圓形、板狀、針狀、不定形皆可以。無機粒子的一次粒子的體積平均粒徑,若從多孔質層的成形性、複合膜的物質透過性、及複合膜的滑動性的觀點,0.01μm~10μm較佳,0.1μm~10μm更佳。
多孔質層是含有無機粒子的情況,在樹脂及無機粒子的合計量中的無機粒子的比率,是例如30體積%~90體積%。
多孔質層,是含有有機充填料和其他的成分也可以。有機充填料,是例如,可舉例由交聯聚(甲基)丙烯酸、交聯聚(甲基)丙烯酸酯、交聯聚矽、交聯聚苯乙烯、交聯聚二乙烯基苯、苯乙烯-二乙烯苯共聚物交聯物、聚醯亞胺、三聚氰胺樹脂、酚樹脂、苯代三聚氰胺-甲醛縮合物等的交聯高分子所構成的粒子;由聚磺、聚丙烯腈、芳族聚醯胺、聚縮醛、熱可塑性聚醯亞胺等的耐熱性樹脂所構成的粒子;等。
多孔質層的厚度,若從機械強度的觀點,在多孔質基材的單面為0.5μm~5μm較佳。
多孔質層的空孔率,若從機械強度、處理性能、及物質透過性的觀點,30%~80%較佳。
多孔質層的平均孔徑,若從物質透過性的觀點,是20nm~100nm較佳。多孔質層的平均孔徑,是依照ASTM E1294-89使用細孔徑分布計器所測量的值。
複合膜的厚度,是例如5μm~100μm,電池隔件用的情況,例如5μm~50μm。
複合膜的格利值(JIS P8117:2009),若從機械強度及物質透過性的觀點,是50秒/100cc~800秒/100cc較佳。
複合膜的空孔率,若從機械強度、處理性能、及物質透過性的觀點,30%~60%較佳。
在本揭示中複合膜的空孔率,是藉由下述的式求得。多孔質基材的空孔率及多孔質層的空孔率也同樣。
空孔率(%)={1-(Wa/da+Wb/db+Wc/dc+...+Wn/dn)/t}×100
Wa、Wb、Wc、...、Wn,是構成材料a、b、c、...,n的質量(g/cm2),da、db、dc、...、dn,是構成材料a、b、c、...、n的真密度(g/cm3),t是膜厚(cm)。
複合膜的用途,是例如,可舉例電池隔件、電容器用薄膜、氣體過濾器、液體過濾器等,特別是最佳的用途,可舉例非水系二次電池用隔件。
以下舉例實施例,將本發明的實施例進一步具體說明。以下的實施例所示的材料、使用量、比率、處理程序等,只要不脫離本揭示的宗旨皆可以適宜變更。因此,本發明的實施例的範圍不應被解釋是藉由以下所示的具體例被限定。
適用在實施例及比較例的測量方法及評價方法,是如下述。
[膜厚]
多孔質基材的膜厚(μm),是以接觸式的厚度計(三豐社的LITEMATIC),測量10cm×30cm內的任意的20點,藉由將此平均而求得。測量端子是使用直徑5mm的圓柱狀者,在測量中使7g的荷重被外加的方式被調整。
將多孔質基材切出MD方向19cm×TD方向6cm的大小3枚,將此為試料。將試料的一端由夾子把持,在將庫內溫度保持在105℃的烤箱中,使MD方向成為重力方向的方式將試料吊下,在無張力狀態下放置了30分鐘。在30分鐘的熱處理的前及後,測量MD方向及TD方向各試料的長度,藉由下述式,將MD方向及TD方向的熱收縮率(%)算出,將試料3枚的平均值算出。
熱收縮率(%)=(熱處理前的長度-熱處理後的長度)÷熱處理前的長度×100
將複合膜的水分率由紅外線水分率計測量,將乾燥狀態如下述分類。
A:水分率是1%未滿。
B:水分率是1%以上3%未滿。
C:水分率是3%以上5%未滿。
D:水分率是5%以上。
在乾燥過程的前後測量複合膜的寬度,計算短縮率(%),如下述分類。
A:短縮率是3%未滿。
B:短縮率是3%以上5%未滿。
C:短縮率是5%以上。
在乾燥過程的隨後及捲取後,由目視觀察複合膜的外觀,將皺褶的發生如下述分類。
A:無皺褶。
B:在乾燥過程的隨後有輕微的皺褶。皺褶可藉由捲取消解。
C:在乾燥過程的隨後有皺褶。皺褶無法藉由捲取消解。
將複合膜由缺點檢査機檢查,檢出明缺點(比周邊部分明亮的部分)及暗缺點(比周邊部分暗的部分),藉由其大小(最大徑)及複合膜每100m2的個數,將多孔質層的剝離如下述分類。多孔質層剝離的話,被剝離的部分是作為明缺點被檢出。被剝離的多孔質層是附著在複合膜表面的話,附著的部分是作為暗缺點被檢出。
A:500μm以下的缺點是10個未滿,5mm以下的缺點是1個未滿。
B:500μm以下的缺點是10個以上50個未滿,5mm以下的缺點是1個未滿。
C:500μm以下的缺點是50個以上,5mm以下的缺點是1個以上。
實施乾燥過程用的乾燥裝置,是準備第2圖所示的乾燥裝置。乾燥裝置的形態是如下述。
乾燥裝置,是在具有搬入口及搬出口的金屬製的外殼的內部,具備乾燥手段4個。4個乾燥手段是各別具有1個加熱滾子及1個熱風送風手段,該加熱滾子及該熱風送風手段,是被配置於將複合膜挾於其間地相面對的位置。4個加熱滾子的外周面是包含聚四氟乙烯。
4個熱風送風手段,是在具有將空氣吸入的吸氣口及將熱風吹出的送風口的外殼的內部,具備電熱器及送風用風扇。外殼,其相面對於加熱滾子的面是成為圓弧狀的曲面,在此曲面配置有送風口。熱風送風手段所具備的送風口,是如第3圖A所示的形態例被並列配置。
加熱滾子的外周面的溫度、從熱風送風手段被送風的熱風的送附口中的溫度及風速、對於複合膜的加熱滾子的總接觸長、以及乾燥裝置的搬運長度及搬運速度,是如表1所示。
多孔質基材,是準備長條狀的寬度1m的聚乙烯微多孔膜(PE膜)。該聚乙烯微多孔膜的物性如表1所示。
將聚間苯二甲醯胺(PMIA)溶解在溶劑(二甲基乙酰胺及三丙二醇的混合溶劑),在那使氫氧化鎂分散,而調製了黏度3000cP(公泊)的塗抹液。塗抹液的組成(質量比),是聚間苯二甲醯胺:氫氧化鎂:二甲基乙酰胺:三丙二醇
=4:16:48:32。
將由上述獲得的塗抹液(液溫20℃)塗抹在多孔質基材的雙面等量,在多孔質基材的雙面形成塗抹層。將塗抹層形成後的多孔質基材朝凝固槽搬運並浸漬在凝固液(水:二甲基乙酰胺:三丙二醇=40:36:24[質量比]、液溫30℃)使被包含於塗抹層的樹脂凝固,而獲得複合膜。
將複合膜,在被控制在水溫30℃的水浴中搬運並沖水,將沖水後的複合膜,通過乾燥裝置使乾燥。
將上述的各過程連續地實施,而獲得在聚乙烯微多孔膜的表背雙面具備多孔質層的複合膜。將被製造的複合膜的品質評價的結果如表1所示。且,對於以外的實施例及比較例也同樣地如表1所示。
除了將乾燥過程的各條件如表1變更以外,是與實施例1同樣地製作了複合膜。
除了將乾燥過程的各條件如表1變更以外,是與實施例1同樣地製作了複合膜。
除了將多孔質基材變更成具有如表1的物性的聚乙烯微多孔膜(PE膜),將乾燥過程的各條件如表1變更以外,是與實施例1同樣地製作了複合膜。
在塗抹液調製過程除了將聚間苯二甲醯胺變更成聚氟化亞乙烯(PVDF)以外,是與實施例1同樣地製作了複合膜。
將多孔質基材變更成聚對苯二甲酸乙二醇酯不織布(PET不織布)以外,是與實施例1同樣地製作了複合膜。
本說明書是參照2015年3月27日申請的日本申請第2015-67607號的整體。
本說明書的全部的文獻、日本專利申請、及技術規格,請參照各文獻、日本專利、及技術規格。
10‧‧‧乾燥裝置
21‧‧‧外殼
22‧‧‧搬入口
23‧‧‧搬出口
31、32、33、34‧‧‧加熱滾子
41、42、43、44‧‧‧熱風送風手段
51、52、53、54‧‧‧乾燥手段
61‧‧‧驅動滾子
70‧‧‧複合膜
Claims (8)
- 一種複合膜的製造方法,具有:在多孔質基材的單面或是雙面,將含有樹脂的塗抹液塗抹而形成塗抹層的塗抹過程;及使前述塗抹層與凝固液接觸使前述樹脂凝固,而獲得在前述多孔質基材的單面或是雙面具備含有前述樹脂的多孔質層的複合膜的凝固過程;及將前述複合膜沖水的沖水過程;及將前述複合膜以搬運速度30m/min以上一邊搬運一邊從前述複合膜將水除去,使用具備內含接觸式加熱手段及熱風送風手段的乾燥手段的乾燥裝置,將前述複合膜與前述接觸式加熱手段接觸並且將從前述熱風送風手段被送風的熱風與前述複合膜接觸而從前述複合膜將水除去的乾燥過程。
- 如申請專利範圍第1項的製造方法,其中,前述多孔質基材,其在105℃下放置30分鐘時的機械方向的熱收縮率是10%以下且寬度方向的熱收縮率是5%以下。
- 如申請專利範圍第1或2項的製造方法,其中,前述接觸式加熱手段,其與前述複合膜接觸的面的溫度是105℃以下,前述熱風,其在前述熱風送風手段的送風口中的溫度是105℃以下。
- 如申請專利範圍第1至3項中任一項的製造方法, 其中,前述熱風,其在前述熱風送風手段的送風口中的風速是5m/sec以上30m/sec以下。
- 如申請專利範圍第1至4項中任一項的製造方法,其中,前述乾燥裝置,是具備2個以上的前述乾燥手段,在前述乾燥裝置具有2個以上的前述接觸式加熱手段,是藉由與前述複合膜接觸的面的溫度的異同被分為2個以上的群,構成與前述第一群的下游側相鄰接的群也就是第二群的前述接觸式加熱手段的前述面的溫度,是比構成前述複合膜的搬運方向的最上游側也就是第一群的前述接觸式加熱手段的前述面的溫度更高。
- 如申請專利範圍第1至5項中任一項的製造方法,其中,對於前述複合膜的前述接觸式加熱手段的總接觸長是30m以下。
- 如申請專利範圍第1至6項中任一項的製造方法,其中,前述乾燥裝置,是具備前述乾燥手段被配置於內部的具有搬入口及搬出口的外殼,從前述搬入口至前述搬出口為止的前述複合膜的搬運長度是50m以下。
- 如申請專利範圍第1至7項中任一項的製造方法,其中,前述接觸式加熱手段,其與前述複合膜接觸的面是含 有氟系樹脂。
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