TW201335252A - 聚烯烴微多孔膜的製造方法 - Google Patents
聚烯烴微多孔膜的製造方法 Download PDFInfo
- Publication number
- TW201335252A TW201335252A TW101148975A TW101148975A TW201335252A TW 201335252 A TW201335252 A TW 201335252A TW 101148975 A TW101148975 A TW 101148975A TW 101148975 A TW101148975 A TW 101148975A TW 201335252 A TW201335252 A TW 201335252A
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- Prior art keywords
- film
- solvent
- polyolefin
- drying
- plasticizer
- Prior art date
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 48
- 238000001035 drying Methods 0.000 claims abstract description 47
- 239000004014 plasticizer Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000009835 boiling Methods 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 14
- 238000001125 extrusion Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000012982 microporous membrane Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000004898 kneading Methods 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 18
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 15
- 238000009826 distribution Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- -1 polyethylene Polymers 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 238000007664 blowing Methods 0.000 description 5
- 229940057995 liquid paraffin Drugs 0.000 description 5
- 239000012188 paraffin wax Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 229920001903 high density polyethylene Polymers 0.000 description 3
- 239000004700 high-density polyethylene Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000011342 resin composition Substances 0.000 description 3
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 2
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- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
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- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
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- 239000004743 Polypropylene Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
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- 238000007654 immersion Methods 0.000 description 1
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- 230000010220 ion permeability Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
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- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
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- 239000007773 negative electrode material Substances 0.000 description 1
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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- 230000000452 restraining effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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Abstract
本發明之課題,是在聚烯烴微多孔膜的製造方法中,抑制因萃取溶劑的不均一乾燥所造成之膜的不均一化,並且實現高速乾燥而實現聚烯烴微多孔膜的高速連續生產。本發明之解決手段,是在藉由擠壓成形將由聚烯烴樹脂與可塑劑所構成之組成物成形為膜狀並進行延伸後,以溶劑來萃取並去除可塑劑,然後進行乾燥之聚烯烴微多孔膜的製造方法中,在可塑劑萃取後且進行乾燥前,使膜緊密接觸於輥或是將膜的寬度機械地限制,在維持對輥的緊密接觸或是寬度的限制之狀態下,藉由使溶劑沸點以上之溫度的液體(熱介質)接觸於膜,而將膜加熱乾燥。
Description
本發明係關於可適合地作為例如過濾膜或各種電池或電容器的分隔器之聚烯烴微多孔膜的製造方法。詳細而言,係關於藉由實現溶劑的高速乾燥,可實現高速連續生產,並且得到優異品質與優異均一性之聚烯烴微多孔膜的製造方法。
微多孔膜,以往既已使用作為電池用分隔器或電解電容器用分隔器等材料。近年來,尤其在鋰離子蓄電池用途的需求增加下,係強烈地期望可達到分隔器的高速生產。
由於在鋰離子蓄電池中使用電解液和正負極活性物質等藥劑,所以考量到耐藥品性,分隔器的材質一般是使用聚烯烴系聚合物,尤其是便宜的聚乙烯或聚丙烯。對於鋰離子蓄電池等之非水電解液系電池用途的分隔器,以往既已要求防電極短路功能、高離子穿透性、電池捲繞時的組裝加工性、電池安全性、及可靠度等作為其基本性能。此外,近年來伴隨著電池的大型化、高能量密度化、高輸出化,對於品質均一化之要求更形強烈。
聚烯烴微多孔膜的製造方法,為人所知者有一種將由聚烯烴樹脂與可塑劑所構成之組成物熔融捏揉,並從模具中擠壓而成形為膜狀,在擠壓成形後,對膜進行單軸或雙軸延伸,延伸後以溶劑從膜中萃取前述可塑劑,使溶劑乾
燥,並可因應必要在乾燥後進一步進行延伸或熱處理之方法(日本特開平5-156058號公報、日本特開平11-60789號公報、日本特開2010-235707號公報)。
此外,關於可塑劑萃取後之溶劑的乾燥,為人所知者有一種在乾燥輥上將膜的寬度機械地限制之狀態下,以乾燥輥速度35~50m/min的條件下進行乾燥之方法(日本特開2011-42805公報)。
[專利文獻1]日本特開平5-156058號公報
[專利文獻2]日本特開平11-60789號公報
[專利文獻3]日本特開2010-235707號公報
[專利文獻4]日本特開2011-42805號公報
先前技術中,在製膜速度慢的時期中,可塑劑萃取後之溶劑的乾燥步驟中之缺失較不明顯。因此,觀念上作為乾燥方法,係有人提出依據熱風所進行之乾燥、接觸於加熱輥、以及浸漬於加熱介質等各種方法(專利文獻1),但具體的方法係廣泛地採用乾燥裝置為簡易構造之將熱風吹送至加熱輥上之方法。
惟當製膜速度增快時,從乾燥開始至乾燥結束為止之
薄膜路徑增長,在乾燥步驟中,已乾燥部分和未乾燥部分之絕對長度亦分別增長。由於膜的些許厚度不均,使得較薄部分於短時間內被乾燥,較厚部分則花費較多時間乾燥。除此之外,已乾燥部分會產生收縮,未乾燥部分則維持該長度,使得未乾燥部分從加熱輥中浮起,而使未乾燥部分的乾燥時間進一步增長。
此外,微多孔膜在半乾燥狀態下,會因拉普拉斯力所造成的負壓而使空孔被破壞,當乾燥時間增長時,空孔率會降低。因此,不均一的乾燥乃成為使空孔率與厚度的均一性惡化之因素。
另一方面,以縮短從乾燥開始至乾燥結束為止之薄膜路徑者為目的,欲縮短乾燥時間者,當使加熱輥的溫度成為遠較溶劑沸點更高之溫度時,溶劑在加熱輥的表面上急速氣化,使膜從加熱輥中浮起,導致加熱效率的降低。因此,亦難以藉由提高加熱輥的溫度來縮短乾燥時間。
本發明者們係鑒於上述課題而進行精心探討,結果發現到並非依據加熱輥及熱風之乾燥,而是在維持使膜緊密接觸於低溫輥之狀態下或是維持將膜的寬度機械地限制之狀態下,藉由使液體的熱介質接觸於膜來進行加熱及乾燥,如此可解決上述課題,因而完成本發明。
亦即,本發明之第1主旨,係存在於一種聚烯烴微多孔膜的製造方法,其係具有:(a)將至少含有聚烯烴樹
脂與可塑劑之組成物熔融捏揉,並從模具中擠壓而成形為膜狀之步驟,(b)在前述擠壓成形後,將所得之膜至少往單軸方向進行延伸之步驟,(c)在前述延伸後,以溶劑從膜中萃取前述可塑劑並藉此去除之步驟,以及(d)在前述萃取後,使膜乾燥之步驟之聚烯烴微多孔膜的製造方法,其特徵為:在萃取步驟後且乾燥步驟前,使膜緊密接觸於較溶劑的沸點更低溫之輥,在維持膜緊密接觸於輥之狀態下,藉由使與溶劑沸點以上之溫度的聚烯烴呈疏液性之液體接觸於膜,而將膜加熱乾燥。
此外,本發明之第2主旨,係存在於一種聚烯烴微多孔膜的製造方法,其係具有:(a)將至少含有聚烯烴樹脂與可塑劑之組成物熔融捏揉,並從模具中擠壓而成形為膜狀之步驟,(b)在前述擠壓成形後,將所得之膜至少往單軸方向進行延伸之步驟,(c)在前述延伸後,以溶劑從膜中萃取前述可塑劑並藉此去除之步驟,以及(d)在前述萃取後,使膜乾燥之步驟之聚烯烴微多孔膜的製造方法,其特徵為:在萃取步驟後且乾燥步驟前,將膜的寬度機械地限制,在維持膜之寬度的機械限制之狀態下,藉由使與溶劑沸點以上之溫度的聚烯烴呈疏液性之液體接觸於膜,而將膜加熱乾燥。
本發明中,在萃取步驟後乾燥步驟前,使膜緊密接觸於低溫輥或是將膜的寬度機械地限制,並在維持該狀態下
進行乾燥,藉此可防止因乾燥所造成之膜在寬度方向上的收縮。
在使膜緊密接觸於輥時,輥的溫度必須設為未達溶劑沸點之溫度。當輥的溫度為溶劑沸點以上之溫度時,溶劑在輥表面上急速氣化而使膜無法緊密接觸於輥,故不佳。
將膜的寬度機械地限制之手段,較佳為夾箝式的拉幅裝置。此外,亦可為在使膜緊密接觸於輥之狀態下將兩端部機械地限制之方法。
本發明中,係以與聚烯烴呈疏液性之液體作為熱介質,並藉由使溶劑沸點以上之溫度的熱介質接觸於膜而將膜加熱,使溶劑蒸發並去除來進行乾燥。以高溫的液體直接將膜加熱,可在短時間內將足夠的熱賦予至膜,而縮短乾燥時間。此外,由於以液體的熱介質來進行加熱,即使未乾燥部分從輥浮起,加熱效率亦不會降低,而能夠實現高速乾燥。再者,藉由選擇與聚烯烴呈疏液性之液體作為熱介質,使熱介質不會進入於膜中,且即使些許的熱介質進入於膜中,由於與聚烯烴呈疏液性,所以不會產生因拉普拉斯力所造成的負壓,而無破壞空孔之疑慮。
用作為熱介質之與聚烯烴呈疏液性之液體,較佳為比熱較大之水。
使膜接觸於前述熱介質之方法,可列舉出使膜通過熱介質中之方法,和將熱介質吹送至膜之方法等。此外,為了抑制溶劑在輥表面上氣化而使膜從傳送輥浮起之情形,當將熱介質吹送至膜時,液體的熱介質,較佳係從輥的相
反側接觸於膜。
根據本發明之聚烯烴微多孔膜的製造方法,可實現高速連續生產,防止因膜的收縮所造成之空孔率的降低,而提升空孔率或膜壓之均一性。此外,於乾燥時可抑制聚烯烴之配向的緩和,而防止強度的降低。
以下係詳細說明本發明的實施形態。本發明所使用之聚烯烴,可使用乙烯、丙烯、1-丁烯、4-甲基-1-戊烯、1-己烯、1-辛烯等之烯烴的單聚物或共聚物。當中,特佳為可藉由高延伸來提高結晶化度,且價格低之高密度聚乙烯。
使用高密度聚乙烯時,重量平均分子量(由凝膠滲透層析法所測定)較佳為1萬以上,尤佳為5萬以上。當分子量過小時,熔融成形的熔融張力變小,使成形性惡化,或是延伸性惡化,而有形成低強度之疑慮。重量平均分子量的上限,只要是可熔融成形且可得到均一的樹脂組成物之範圍者即可,並無特別限制,通常為100萬以下,較佳為70萬以下。
本發明中所使用之可塑劑,為在與聚烯烴樹脂混合時,於聚烯烴樹脂的熔點以上時可形成均一溶液之非揮發性溶劑。具體而言,可例示出流動石蠟或石蠟等之烴類、鄰
苯二甲酸二辛酯或鄰苯二甲酸二丁酯等之酯類、十八烯醇或十八烷醇等之高級醇。此等當中,特佳為容易取得且容易處理之流動石蠟或石蠟。
本發明中所使用之聚烯烴樹脂與可塑劑之比率,為了不會產生微相分離,只要是在萃取可塑劑並去除後可成為微多孔膜之充分比率即可。具體而言,聚烯烴樹脂的含有比率為10~70重量%,特佳為20~50重量%。
聚烯烴樹脂與可塑劑之熔融捏揉,可使用多軸擠壓機或單軸擠壓機等,藉由通常的方法來進行。
由聚烯烴樹脂與可塑劑所構成之組成物中,可因應目的而添加抗氧化劑、結晶核劑、抗帶電劑、難燃劑、潤滑劑、紫外線吸收劑等之添加劑。
熔融捏揉後之樹脂組成物,係藉由擠壓成形而成形為薄片狀或薄膜狀(以下合稱為「膜狀」)。擠壓成形,可使用T模具(平板模具)來擠壓成膜狀,或是使用圓形模具等來擠壓成筒狀並加工為膜狀。擠壓成形後之膜的厚度,較佳為1~500μm,特佳為5~100μm。當膜厚過薄時,強度容易不足,過厚時,於使用在電池分隔器時,會有分隔器的佔有體積變得過大之疑慮。
藉由擠壓成形所得之膜,至少往單軸方向進行延伸。所謂至少往單軸方向進行延伸,是指機械方向上的單軸延伸,寬度方向上的單軸延伸,同步雙軸延伸,逐次雙軸延伸。此外,延伸不限於單段延伸,亦可進行多段或多數次延伸。延伸方法並無特別限制,可為輥延伸或使用拉幅機
之延伸。此外,為了實現高強度,特佳為雙軸延伸。
延伸溫度,可為一般方法中所使用之溫度。例如可在聚烯烴樹脂組成物的熔點(Tm)以下(Tm-50)℃以上之範圍內進行延伸。
延伸倍率並無特別限制,於單軸延伸時,通常為2~20倍,特佳為4~10倍。於雙軸延伸時,以面積倍率計通常為2~400倍,特佳為4~200倍。
延伸後,從膜中萃取可塑劑並去除。萃取可塑劑之方法,係將微多孔膜連續地送入至注滿萃取溶劑之槽中,花費可去除可塑劑之充分時間來浸漬於槽中,然後使附著的溶劑乾燥而進行。此時可適用下列一般所知的手段,亦即:依序將微多孔膜送入至藉由多段地分割槽內部而形成濃度差之各槽中之多段法,以及從相對於微多孔膜的行進方向呈相反之方向來供給萃取溶劑以形成濃度梯度之逆向流法,如此可提高萃取效率,故較佳。從微多孔膜中實質地去除可塑劑乃為重要。此外,當在未達溶劑沸點的範圍內將萃取溶劑的溫度加溫時,可促進可塑劑與溶劑之擴散而提高萃取效率,故更佳。
本發明所使用之萃取溶劑,只要是相對於聚烯烴為不良溶劑,相對於可塑劑為良溶劑,且沸點低於聚烯烴樹脂的熔點者即可。溶劑的沸點,尤佳係未達100℃。此般溶劑的具體例,當可塑劑為流動石蠟或石蠟時,可列舉出正己烷或環己烷等之烴類、二氯甲烷或1,1,1-三氯乙烷等之鹵化烴類、乙醇或異丙醇等之醇類、四氫呋喃或二***等
之醚類、丙酮或丁酮等之酮類。此等當中,從取得和處理之容易性來看,特佳為二氯甲烷或環己烷。
萃取可塑劑後,在乾燥步驟前,使膜緊密接觸於冷卻輥或是將膜的寬度機械地限制。
在使膜緊密接觸於冷卻輥時,冷卻輥的表面溫度,係設為溶劑的沸點以下且不會激烈地產生溶劑的冷凝或結露之溫度。具體而言,當溶劑為二氯甲烷時,較佳為0~40℃,尤佳為35℃左右。
在將膜的寬度機械地限制時,機械地限制之方法,較佳為藉由以多數個夾箝來握持膜的兩端部,並配合膜的移動使該夾箝移動之拉幅裝置所進行之方法。此外,在使膜緊密接觸於輥上之狀態下以帶狀物將膜的兩端部予以按壓之方法,亦可將膜的寬度機械地限制。
在使膜緊密接觸於冷卻輥或是將膜的寬度機械地限制後,在維持對冷卻輥的緊密接觸或是膜之寬度的限制之狀態下,藉由使液體狀的熱介質接觸於膜而將膜加熱,以進行溶劑的乾燥。熱介質所使用之液體,必須與聚烯烴呈疏液性。由於熱介質所使用之液體與聚烯烴呈疏液性,所以熱介質的液體不會進入於聚烯烴微多孔膜中。熱介質所使用之液體,具體而言,較佳為水。
熱介質之液體的沸點,係設為萃取溶劑的沸點以上。
使膜接觸於熱介質的液體之方法,可列舉出將膜浸漬於熱介質中之方法,使膜通過充填有熱介質的液體之槽中之方法,將熱介質吹送至膜之方法等。
在將熱介質吹送至膜時,較佳係從傳送輥側的相反面側吹送至膜。當從輥側吹送熱介質時,溶劑在輥表面上急速氣化,而產生膜從輥中浮起之疑慮。
以下係藉由實施例來更詳細說明本發明的實施形態,但本發明並不限定於此等實施例。
使用雙軸擠壓機,將聚烯烴樹脂材料(將2,6-二-三級丁基對甲酚0.3重量份乾式摻合於高密度聚乙烯(重量平均分子量30萬,重量平均分子量/數量平均分子量為7,密度0.956)100重量份者)30重量份與流動石蠟(37.78℃時的動態黏度75.9cSt)70重量份熔融捏揉,並從平板模具(衣架型模具)中,將樹脂混合物擠壓至表面溫度控制在40℃之冷卻輥上,而得厚度1.1mm的薄片狀微多孔膜前驅物。
接著使用拉幅式同步雙軸延伸機,在119℃中將所得之薄片狀微多孔膜前驅物延伸為5×5倍,而得寬度1,000mm、厚度40μm之均一的膜狀微多孔膜前驅物。
使所得之膜狀微多孔膜前驅物與二氯甲烷(溶劑)進行約2分鐘的逆向流接觸,以萃取流動石蠟(可塑劑)並去除。
在萃取流動石蠟並去除後,使用第1圖的乾燥裝置,
以製膜速度70m/分進行加熱乾燥。具體而言,使萃取流動石蠟並去除後之聚乙烯微多孔膜1,於位置2上緊密接觸於溫度控制在35℃之冷卻輥3,並在維持緊密接觸之狀態下,從噴嘴4吹送溫度65℃的溫水,以加熱去除二氯甲烷。
乾燥後之微多孔膜的厚度以及空孔率在寬度方向上的分布,係以下列方法來測定,並於第1表及第3圖顯示該結果。
使用Mitutoyo Litematic VL-50A-B(測定件號碼:120060),以微多孔膜之寬度的中心為基準,在寬度方向上以10mm的間距來測定厚度。
以微多孔膜之寬度的中心為基準,在寬度方向上,每隔20mm裁切20mm×20mm的樣本,並測定微多孔膜的重量(μg)。接著從上述20mm×20mm之樣本的重量以及對應於此之從3點所求取的平均厚度(將中心的厚度Tc加權2倍後之加權平均)中,依循下列式來算出空孔率。
上述式中,係使用結晶化度85~90%之聚乙烯的密度(0.995g/cm3)來計算。
除了使用第2圖的乾燥裝置,並以製膜速度120m/分來進行加熱乾燥之外,其他與實施例1相同。具體而言,使聚乙烯微多孔膜11通過水12中,在維持以拉幅裝置13限制寬度方向之狀態下,以約60℃的溫水14來加熱。以拉幅裝置開始限制寬度方向之位置上的水15,控制在約25℃。所得之微多孔膜的厚度以及空孔率在寬度方向上的分布,係如第1表及第4圖所示。
除了以製膜速度10m/分,且將50℃的熱風吹送至40℃的加熱輥上來進行乾燥處理之外,其他與實施例1相同。所得之微多孔膜的厚度以及空孔率在寬度方向上的分布,係如第1表及第5圖所示。
除了將製膜速度設為20m/分之外,其他與比較例1相同。所得之微多孔膜的厚度以及空孔率在寬度方向上的分布,係如第1表及第6圖所示。
除了將製膜速度設為20m/分,且未以拉幅裝置13進行寬度方向上的機械限制之外,其他與實施例2相同。所得之微多孔膜的厚度以及空孔率在寬度方向上的分布,係如第1表及第6圖所示。
從實施例1、2中,可得知在本發明之方法中,即使製膜速度為高速的70m/分或120m/分,亦可得到厚度及空孔率為均一之微多孔膜。相對於此,當於加熱輥上吹送熱
風來進行乾燥時,當製膜速度為低速的10m/分時,可得到厚度及空孔率為均一之微多孔膜(比較例1),但當製膜速度為20m/分時,厚度及空孔率的變動增大,而大幅地損及品質的均一性及穩定性(比較例2)。此外,即使是浸漬於溫水之方法,在未進行寬度方向的機械限制時,寬度方向的收縮增大,此外,厚度及空孔率的變動亦增大。
本發明可應用在過濾膜或各種電池或電容器的分隔器等所使用之聚烯烴微多孔膜的高速生產。
1‧‧‧微多孔膜
2‧‧‧膜緊密接觸於冷卻輥之位置
3‧‧‧冷卻輥(控制在約35℃)
4‧‧‧噴嘴(約65℃的溫水)
5‧‧‧泵浦
6‧‧‧加熱器
11‧‧‧微多孔膜
12‧‧‧水
13‧‧‧拉幅裝置
14‧‧‧溫水(約60℃)
15‧‧‧水(約25℃)
16‧‧‧隔熱材
17‧‧‧加熱器
18‧‧‧冷卻器
19‧‧‧泵浦
第1圖為本發明的實施例1中所使用之乾燥裝置之概略圖。
第2圖為本發明的實施例2中所使用之乾燥裝置之概略圖。
第3圖為本發明的實施例1中所得之微多孔膜的厚度及空孔率的分布之圖表。
第4圖為本發明的實施例2中所得之微多孔膜的厚度及空孔率的分布之圖表。
第5圖為本發明的比較例1中所得之微多孔膜的厚度及空孔率的分布之圖表。
第6圖為本發明的比較例2中所得之微多孔膜的厚度
及空孔率的分布之圖表。
第7圖為本發明的比較例3中所得之微多孔膜的厚度及空孔率的分布之圖表。
1‧‧‧微多孔膜
2‧‧‧膜緊密接觸於冷卻輥之位置
3‧‧‧冷卻輥(控制在約35℃)
4‧‧‧噴嘴(約65℃的溫水)
5‧‧‧泵浦
6‧‧‧加熱器
Claims (4)
- 一種聚烯烴微多孔膜的製造方法,其係具有:(a)將至少含有聚烯烴樹脂與可塑劑之組成物熔融捏揉,並從模具中擠壓而成形為膜狀之步驟,(b)在前述擠壓成形後,將所得之膜至少往單軸方向進行延伸之步驟,(c)在前述延伸後,以溶劑從膜中萃取前述可塑劑並藉此去除之步驟,以及(d)在前述萃取後,使膜乾燥之步驟之聚烯烴微多孔膜的製造方法,其特徵為:在萃取步驟後且乾燥步驟前,使膜緊密接觸於較溶劑的沸點更低溫之輥,在維持膜緊密接觸於輥之狀態下,藉由使與溶劑沸點以上之溫度的聚烯烴呈疏液性之液體接觸於膜,而將膜加熱乾燥。
- 一種聚烯烴微多孔膜的製造方法,其係具有:(a)將至少含有聚烯烴樹脂與可塑劑之組成物熔融捏揉,並從模具中擠壓而成形為膜狀之步驟,(b)在前述擠壓成形後,將所得之膜至少往單軸方向進行延伸之步驟,(c)在前述延伸後,以溶劑從膜中萃取前述可塑劑並藉此去除之步驟,以及(d)在前述萃取後,使膜乾燥之步驟之聚烯烴微多孔膜的製造方法,其特徵為:在萃取步驟後且乾燥步驟前,將膜的寬度機械地限制,在維持膜之寬度的機械限制之狀態下,藉由使與溶劑沸點以上之溫度的聚烯烴呈疏液性之液體接觸於膜,而將膜加熱乾燥。
- 如申請專利範圍第1或2項所述之聚烯烴微多孔 膜的製造方法,其中與聚烯烴呈疏液性之液體為水。
- 如申請專利範圍第1至3項中任一項所述之聚烯烴微多孔膜的製造方法,其中(d)的乾燥步驟,係使與溶劑沸點以上之溫度的聚烯烴呈疏液性之液體,從膜之傳送輥的相反側接觸而藉此加熱膜。
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JP5952504B1 (ja) * | 2014-08-29 | 2016-07-13 | 住友化学株式会社 | 多孔質層、多孔質層を積層してなるセパレータ、および多孔質層またはセパレータを含む非水電解液二次電池 |
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HUE060294T2 (hu) * | 2014-12-11 | 2023-02-28 | Toray Industries | Mikropórusos poliolefin film, szeparátor akkumulátorhoz, és eljárások ezek elõállítására |
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CN110711497A (zh) * | 2015-03-27 | 2020-01-21 | 帝人株式会社 | 复合膜的干燥装置 |
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CN105131327B (zh) * | 2015-09-07 | 2019-07-02 | 广东工业大学 | 一种可控孔径的多孔薄膜的制造方法 |
US10770707B2 (en) * | 2015-12-04 | 2020-09-08 | Toray Industries, Inc. | Battery separator and method of manufacturing same |
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