TWI454521B - Aqueous liquid compositions, aqueous coating liquids, functional coating films and composites - Google Patents
Aqueous liquid compositions, aqueous coating liquids, functional coating films and composites Download PDFInfo
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- TWI454521B TWI454521B TW101104500A TW101104500A TWI454521B TW I454521 B TWI454521 B TW I454521B TW 101104500 A TW101104500 A TW 101104500A TW 101104500 A TW101104500 A TW 101104500A TW I454521 B TWI454521 B TW I454521B
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- acid
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- aqueous
- polymer
- liquid composition
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- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- UVZICZIVKIMRNE-UHFFFAOYSA-N thiodiacetic acid Chemical compound OC(=O)CSCC(O)=O UVZICZIVKIMRNE-UHFFFAOYSA-N 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- ODBLHEXUDAPZAU-UHFFFAOYSA-N threo-D-isocitric acid Natural products OC(=O)C(O)C(C(O)=O)CC(O)=O ODBLHEXUDAPZAU-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- LBLYYCQCTBFVLH-UHFFFAOYSA-M toluenesulfonate group Chemical group C=1(C(=CC=CC1)S(=O)(=O)[O-])C LBLYYCQCTBFVLH-UHFFFAOYSA-M 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 description 1
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Description
本發明係關於一種環境負荷較少之水性液狀組成物。更詳細而言,本發明係關於一種可形成於各種產業領域中有用之功能性塗佈膜之水性液狀組成物及水性塗佈液、藉由該水性塗佈液形成之功能性塗佈膜、以及使該功能性塗佈膜與基材一體化而成之複合材料。
近年來,嘗試利用藉由以具備各種功能之溶液、漿料或糊劑(以下,亦統稱為「漿料」)等液狀組成物作為功能性塗佈液並塗佈該功能性塗佈液而形成之塗佈膜的各種功能。此種嘗試係於塗料、油墨、塗層劑(coat agent)、磁體、陶瓷、建材、接著劑、液晶彩色濾光片、醫藥品、電子材料、及蓄電裝置等各種領域中進行。
例如,包含導電性材料、黏合劑樹脂、硬化劑、及溶劑等之糊狀導電性塗佈液可用作導電性接著劑、導電性塗料、導電性油墨等(非專利文獻1)。又,錄音帶、錄影帶、軟性磁碟等塗佈型磁記錄媒體係藉由將使次微米尺寸之磁性粒子均勻地分散於高分子溶液中而成之磁性塗料塗佈於聚酯等基膜(base film)上而製作。又,鋰離子二次電池之電極係將混合活性物質、導電材料、及黏合劑(結著材料)而製備之漿料塗佈於集電體箔上並加以乾燥而製作(非專利文獻2)。
為使如上所述之各種功能性塗佈液充分發揮其功能性,必
需使所形成之塗佈膜具備堅牢性與對基材之較高密接性。換言之,必需條件係塗佈液之狀態適於功能性表現,並且可形成對基材之密接性較高且具有耐久性之塗佈膜。因此,作為塗佈液之溶劑(分散媒),表現對基材之較高親和性並且容易乾燥之非水系(有機溶劑系)之溶劑絕對有利,從而廣泛應用於實際。
然而,通常有機溶劑之揮發性較高。因此,不僅對環境之負荷較大,而且亦必需考慮遺傳毒性,於安全性及作業性方面亦殘留有課題。近年來,於眾多產業領域中對環境保護及健康危害防止之意識正在提高。因此,對於存在如上所述之課題之有機溶劑之使用,對降低揮發性有機化合物(VOC,Volatile Organic Compounds)及無溶劑化等之要求日益高漲,而尋求向對環境或人較溫和之製品之轉換。
作為對環境或人較溫和之製品,水系製品或包含源自生物之原料之製品備受注目。該等製品作為擔負無溶劑化或脫石油製品之一部分作用者而受到期待。然而,於使用水代替有機溶劑作為溶劑之情形時,開始產生各種問題。例如水系塗佈液存在塗膜形成能差於有機溶劑系之塗佈液之問題。又,含有填充料之漿料狀之水系塗佈液存在若填充料處於帶電狀態則容易於漿料中凝集之問題。進而,由於溶劑與填充料之比重差較大,故而亦存在填充料容易沈澱而難以均勻分散之問題。進而,發現可代替先前之源自石油之原料的發揮塗膜形成能或分散能之源自生物之原料並不容易。
於嘗試水系漿料中之填充料之分散及穩定化之情形時,可考慮分散劑之使用、填充料之表面處理、微膠囊化、超音波處理、聚合物中之極性基導入等各種方法。該等方法中,若考慮製造製程或塗佈系統之簡單化、以及成本方面,則分散劑之使用較為有利。作為水系漿料中所使用之分散劑,可考慮塗料領域中所使用之聚羧酸鹽或磷酸系胺鹽(非專利文獻3)、作為高分子分散劑之聚丙烯酸醯胺(非專利文獻4)等。但是,若考慮降低環境負荷,則分散劑較佳為對環境較溫和之天然物系物質。提出於非水電解質二次電池之電極之製造時使用羧甲基纖維素作為水系分散劑(專利文獻1)。然而,羧甲基纖維素於其分散效果方面尚留有改良之餘地。又,為形成堅固之塗佈膜,必需使用石油系黏合劑樹脂。因此,期望一種雖為源自生物之物質之天然系聚合物,但亦可表現不遜色於使用石油系黏合劑樹脂之情形之密接性的天然系聚合物之利用技術。
作為所期待之水系漿料之用途,可考慮近年來其成長尤為顯著之二次電池或電容器等蓄電裝置電極板用塗佈液。電極板係使電極層或集電體等單位構件一體化而成之會給蓄電裝置之性能帶來較大影響之電極構件。因此,為延長蓄電裝置之充放電循環壽命並且實現高能量密度化,提出使電極板薄膜大面積化。例如於專利文獻2及3中記載有將使金屬氧化物、硫化物、鹵化物等正極活性物質粉末、導電性材料、及黏合劑分散或溶解於適當之溶劑中而獲得之糊狀塗佈液
塗佈於包含鋁等金屬箔之集電體之表面,形成塗佈膜層而獲得之正極電極板。
又,電池之負極電極板或電容器之可極化電極板係將混合碳質材料等活性物質與使黏合劑溶解於適當之溶劑中而成者而獲得之糊狀塗佈液塗佈於集電體上,形成塗佈膜層而獲得。塗佈液之製備中所使用之黏合劑必需對於非水電解液而言電化學性穩定,不會於電池或電容器之電解液中溶出,不會因電解液而嚴重膨潤,可溶於某些溶劑等。
另一方面,塗佈各種樹脂溶液而形成集電體之素材金屬即鋁等金屬材料表面之保護皮膜。然而,所形成之保護皮膜雖對金屬表面之密接性優異,但存在對有機溶劑之耐久性不充分之問題。
進而,將上述糊狀塗佈液塗佈於集電體而獲得之電池或電容器之電極板之塗佈膜層存在對集電體之密接性或可撓性不充分之問題。又,對集電體之接觸電阻較大,於電池或電容器之組裝時或充放電時,有時會產生塗佈膜層之剝離、脫落、龜裂等。
如上所述,於先前之電池或電容器中存在電極層與集電體(基板)之密接性較低,電極層與集電體之間之電阻較高之問題。為解決該等問題而提出各種塗佈液。藉由以提出之各種塗佈液所形成之塗佈膜層可使密接性不良之問題得到不斷改善。然而,電極層與集電體之間之電阻進一步變高,因此仍未達到問題之解決。又,近年來,對於上述蓄電裝置及該
等之關聯製品亦要求考慮環境之製造步驟。因此,尋求一種使用對環境負荷較少之成分之塗佈液。
[專利文獻1]日本專利特開2009-238720號公報
[專利文獻2]日本專利特開昭63-10456號公報
[專利文獻3]日本專利特開平3-285262號公報
[非專利文獻1]藤山光美:「第一章,導電性填充料之混練‧分散不良要因及其對策」、「導電性填充料之新混練‧分散技術及其不良對策」技術資訊協會,第20頁,2004年
[非專利文獻2]立花和宏:「鋰離子二次電池用正極漿料之調整與塗佈.乾燥及電極動作之理解」,Material stage,技術資訊協會,第8卷,第12號,第72頁~第75頁,2009年
[非專利文獻3]城清和:「水系塗料用分散劑之技術開發」,JETI,第44卷,第10號,第110頁~第112頁,1996年
[非專利文獻4]神谷秀博:「水系中之微粒子凝集.分散行為之評價與控制」,Material stage,第2卷,第1號,第54頁~第60頁,2002年
本發明之目的在於提供一種含有對環境之負荷較少之廉
價材料,即便長期保存亦可維持適度之黏度,可形成具有對基材之優異密接性、耐久性、耐溶劑性、及耐水性並且能發揮以導電性或親水性為代表之各種功能之功能性塗佈膜的水性液狀組成物及水性塗佈液。
又,本發明之目的在於提供一種具有對基材之優異密接性、耐久性、耐溶劑性、及耐水性並且可發揮以導電性或親水性為代表之各種功能之功能性塗佈膜及其形成方法。
進而,本發明之目的在於提供一種使具有耐久性、耐溶劑性、及耐水性並且可發揮以導電性或親水性為代表之各種功能之功能性塗佈膜密接於基材而成之複合材料。
又,本發明之目的在於提供一種使耐久性及耐溶劑性優異並且導電性良好之導電性塗佈膜密接於集電體而成之電極板用構件及電極板、及包含該電極板之具有放電容量較大或內部電阻較低等特性之蓄電裝置。
上述目的係藉由以下所示之本發明而達成。即,根據本發明,可提供一種含有包含水之水系介質、具有羥基及/或胺基之聚合物、及膦醯基丁烷三羧酸之水性液狀組成物。
於本發明中,較佳為進而含有聚合物酸,且上述聚合物酸為含有羧基之乙烯系單體之均聚合體及/或含有羧基之乙烯系單體與不含羧基之乙烯系單體之共聚合體;較佳為上述聚合物酸為選自由聚丙烯酸、聚順丁烯二酸、及聚衣康酸所組成之群中之至少一種。又,較佳為進而含有聚烷二醇及/或
聚環氧烷。
較佳為上述聚合物為選自由多糖、聚胺基酸、聚乙烯醇、聚烯丙胺、聚乙烯胺、聚脒、聚乙烯亞胺及該等之衍生物所組成之群中之至少一種;較佳為上述多糖為選自由海藻酸、澱粉、纖維素、甲殼素、聚葡萄胺糖(chitosan)、果膠及該等之衍生物所組成之群中之至少一種;較佳為上述聚胺基酸為選自由聚離胺酸、聚鳥胺酸、聚精胺酸、聚組胺酸、魚精蛋白、明膠及膠原蛋白所組成之群中之至少一種。
較佳為上述聚合物(A)與上述膦醯基丁烷三羧酸(B)之質量比為A/B=1/5~5/1;較佳為上述聚合物之重量平均分子量為5,000~200萬;較佳為上述聚合物與上述膦醯基丁烷三羧酸之合計之固形份濃度為0.1~40質量%。
較佳為進而含有導電性材料;較佳為上述導電性材料為選自由乙炔黑、科琴黑、石墨、爐黑、單層或多層碳奈米纖維、及單層或多層碳奈米管所組成之群中之至少一種。
又,根據本發明,可提供一種含有上述水性液狀組成物之水性塗佈液。進而,根據本發明,可提供一種藉由上述水性塗佈液形成之功能性塗佈膜。較佳為功能性塗佈膜之利用JIS K7194測定之表面電阻率為3,000 Ω/□以下。
根據本發明,可提供一種包括將上述水性塗佈液加熱至80℃以上之步驟之功能性塗佈膜之形成方法。又,根據本發明,可提供一種包含基材、及一體地配設於上述基材上之上述功能性塗佈膜的複合材料。較佳為基材為選自由金屬、玻
璃、天然樹脂、合成樹脂、陶瓷、木材、紙、纖維、不織布、織布、及皮革所組成之群中之至少一種;較佳為基材為選自由鋁、銅、鎳、及不鏽鋼所組成之群中之至少一種。
進而,根據本發明,可提供一種電極板用構件,其包含集電體、及配設於上述集電體之表面之導電性塗佈膜,且上述導電性塗佈膜為對塗佈於上述集電體之表面之上述水性液狀組成物進行加熱處理而形成者。再者,較佳為集電體為非水電解液二次電池用、電雙層電容器用、或鋰離子電容器用之集電體。
又,根據本發明,可提供一種包含上述電極板用構件、及配設於上述導電性塗佈膜之表面之活性物質層的電極板。進而,根據本發明,可提供一種包含上述電極板之蓄電裝置。該蓄電裝置可較佳地作為非水電解液二次電池、電雙層電容器、或鋰離子電容器。
本發明之水性液狀組成物及水性塗佈液包含對環境之負荷較少之廉價之材料,既便長期保存亦可維持適度之黏度。又,可形成具有對基材之優異之密接性、耐久性、耐溶劑性、及耐水性並且可發揮導電性、親水性、耐污染性、防黴/抗菌性、防臭性、及加工性等功能之功能性塗佈膜。
又,即便於本發明之水性液狀組成物及水性塗佈液含有導電性材料等填充料之情形時,填充料亦可良好地分散,而不易產生沈澱分離。進而,可期待本發明之水性液狀組成物及
水性塗佈液於電池、電子材料塗料、油墨、色劑(Toner)、橡膠/塑膠、陶瓷、磁體、接著劑、液晶彩色濾光片等多方面中之利用。
本發明之功能性塗佈膜係具有對基材之優異之密接性、耐久性、耐溶劑性、及耐水性並且可發揮導電性、親水性、耐污染性、防黴/抗菌性、防臭性、及加工性等功能者。又,本發明之功能性塗佈膜可製成對集電體與電極層之密接性較高,耐電解液性優異,與集電體之接觸電阻亦得到改良之導電性塗佈膜。進而,本發明之電極板用構件及電極板係耐久性及耐溶劑性優異並且集電體上密著有導電性良好之導電性塗佈膜者。因此,若使用本發明之電極板用構件及電極板,則可提供非水電解液二次電池、電雙層電容器、或鋰離子電容器等具有放電容量較大或內部電阻較低等特性之高性能之蓄電裝置。
其次,列舉用以實施本發明之形態,進一步詳細地說明本發明。本發明之水性液狀組成物含有包含水之水系介質、具有羥基及/或胺基之聚合物(以下,亦記為「OH/NH2
聚合物」)、及膦醯基丁烷三羧酸(以下,亦記為「PBTC,phosphonobutane tricarboxylic acid」)。藉由含有該等成分,可抑制存在進而含有之情況之導電性材料等填充料之沈澱分離,並且可確保較高之親水性。
本發明之水性液狀組成物藉由含有具備對導電性材料等
填充料之結著能或分散能及親水功能等之OH/NH2
聚合物及PBTC,可維持對填充料之結著性或分散性及親水性等功能性,並且環境性能亦優異。又,由於含有適量之水,較佳為包含水與水溶性醇類等有機溶劑之水系介質作為溶劑或分散媒,故而可抑制OH/NH2
聚合物或PBTC之析出,並且可維持適度之黏性。因此,本發明之水性液狀組成物可確保塗佈時之適用期(pot life),並且可抑制填充料之沈澱分離,且可實現塗佈性或分散穩定性。
本發明中之所謂「水性液狀組成物」,係指填充料等微小固體粒子高濃度地分散於水系介質中而成為漿料狀或糊狀者。
本發明之水性液狀組成物中含有水系介質。該水系介質係作為溶劑或分散媒發揮功能之成分。水系溶劑可僅為水,亦可為水與有機溶劑之混合溶劑。水較佳為蒸餾水,但根據用途亦可為通常之自來水。
有機溶劑較佳為可與水混和之溶劑。作為此種有機溶劑之具體例,可舉出:甲醇、乙醇、正丙醇、異丙醇(IPA,isopropyl alcohol)、正丁醇、第二丁醇、異丁醇、第三丁醇等醇類;乙酸甲酯、乙酸乙酯、乙酸正丙酯、乙酸異丙酯、乙酸正丁酯、乙酸異丁酯、乙酸甲氧基丁酯、溶纖劑乙酸酯(cellosolve acetate)、乙酸戊酯、乳酸甲酯、乳酸乙酯、乳酸丁酯等酯類;丙酮、甲基乙基酮、甲基異丁基酮、二異丁基酮、環己
酮等酮類;N-甲基-2-吡咯烷酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺等醯胺類;二甲基亞碸等亞碸類。其中,較佳為醇類,進而較佳為IPA。該等有機溶劑可單獨使用亦可組合兩種以上而使用。
水系介質之pH值較佳為7以下。其原因在於若水系介質之pH值超過7,則有時OH/NH2
聚合物之交聯不易進行。
於使用水與有機溶劑之混合溶劑作為水系介質之情形時,混合溶劑中所含之有機溶劑之比例較佳為1~70質量%,進而較佳為5~60質量%。例如,於使用IPA與水之混合溶劑之情形時,混合溶劑中所含之IPA之比例較佳為1~40質量%,進而較佳為5~40質量%。
本發明之水性液狀組成物中所含之OH/NH2
聚合物與PBTC係藉由加熱而反應、交聯。因此,就反應效率而言,較佳為於加熱前之狀態下兩者均勻地混合。因此,OH/NH2
聚合物較佳為於100℃以下可溶於pH值1~14之水或包含水與有機溶劑之水系介質。
作為OH/NH2
聚合物之具體例,可舉出:多糖、聚胺基酸、聚乙烯醇、聚烯丙胺、聚乙烯胺、聚脒、及聚乙烯亞胺等聚合物;該等聚合物之衍生物;該等之混合物等。
作為上述衍生物之具體例,可舉出:上述聚合物之羧基化物、二醇化物、甲苯磺醯化物、硫氧化物、磷氧化物、醚化物、烷基化物、及該等之鹽等。該等衍生物可藉由先前公知
之方法合成。取代基之導入率較佳為每一構成聚合物之單體單元為0.1~6。若未達0.1,則有時不易表現所導入之取代基之特性,若超過6,則有時聚合物之交聯變得不充分。
上述OH/NH2
聚合物之具體例中,多糖具有為天然物或源自天然物之優點。尤其是多糖中,海藻酸、澱粉、纖維素、甲殼素、聚葡萄胺糖、及果膠就容易大量獲取之方面而言較佳。多糖可為天然物,亦可為合成物。作為源自天然之多糖,可例示:源自海草之海藻酸、馬鈴薯澱粉、棉花纖維素、源自甲殼類之聚葡萄胺糖等。
OH/NH2
聚合物中,較佳為甲殼素、聚葡萄胺糖、纖維素及該等之衍生物,進而較佳為聚葡萄胺糖、聚葡萄胺糖衍生物、陽離子化聚葡萄胺糖及該等之鹽(以下,亦簡記為「聚葡萄胺糖類」)。聚葡萄胺糖類由於(i)其本身具有抗菌性等各種獨特之特性;(ii)利用PBTC之交聯性良好;(iii)容易與包含纖維、金屬、或玻璃等之基材相互作用而密接性較高,故而尤佳。
聚葡萄胺糖為可藉由例如使存在於蟹或蝦之甲殼類之外皮中之甲殼素脫乙醯化而獲得者,其本身為眾所周知之材料。可製造各種脫乙醯化度、各種分子量之聚葡萄胺糖類,亦可自市場較容易地獲取。
作為聚乙烯醇(以下,亦簡記為「PVA,polyvinyl alcohol」),可使用利用先前公知之方法製造之任一者,聚合度或皂化度等並無限定。又,亦可為與其他單體之共聚合
物。進而,針對聚烯丙胺、聚乙烯胺、聚乙烯亞胺及聚脒,亦可使用利用先前公知之方法製造之任一者,聚合度等並無限定。又,亦可為與其他單體之共聚合物。
聚胺基酸可為天然物,亦可為合成物。作為聚胺基酸之具體例,可舉出:聚離胺酸、聚鳥胺酸、聚精胺酸、聚組胺酸、魚精蛋白、明膠及膠原蛋白等。
於使用聚乙烯胺、聚脒、聚葡萄胺糖、及纖維素衍生物等分子內具有胺基之聚合物之情形時,於該等聚合物中添加酸,與胺基發生造鹽反應,藉此抗菌性及水溶解性提高。於本發明中,亦可使用該等聚合物之鹽。
作為上述造鹽反應中所使用之酸,只要為某種程度溶解於水系介質中之酸即可。具體而言,可舉出:鹽酸、甲酸、乙酸、丙酸、丁酸、牛磺酸、吡咯烷酮羧酸、檸檬酸、蘋果酸、乳酸、羥基丙二酸、丙二酸、丁二酸、己二酸、苯甲酸、水楊酸、胺基苯甲酸、鄰苯二甲酸、維生素C等有機酸。其中,較佳為乳酸、蘋果酸、檸檬酸等天然存在之有機酸。
此種酸之使用量因聚葡萄胺糖之脫乙醯化度、聚乙烯胺及聚脒之鹼度或酸之當量而變化,因此無法一概地規定。但是,較佳為設為可使所生成之鹽保持水溶性之使用量。酸之使用量較佳為相對於聚乙烯胺、聚脒、聚葡萄胺糖或纖維素衍生物中之1個胺基,為約0.8~2莫耳之範圍。
OH/NH2
聚合物之重量平均分子量較佳為5,000~200萬。若未達5,000,則存在交聯產物變弱之傾向。另一方面,若
OH/NH2
聚合物之重量平均分子量超過200萬,則於使用水性液狀組成物作為塗佈液之情形時,有時不易形成均勻之塗膜。
於OH/NH2
聚合物為聚葡萄胺糖類之情形時,聚葡萄胺糖類之重量平均分子量較佳為5,000以上,進而較佳為3萬~100萬。若重量平均分子量未達5,000,則有時所形成之皮膜之強度變得不充分。又,於含有導電性材料之情形時,有時導電性材料之分散性變得不充分。另一方面,若聚葡萄胺糖類之重量平均分子量超過100萬,則有時水性液狀組成物之黏度變得過高而必需較低地控制聚葡萄胺糖類之濃度。又,漿料之黏度上升而變得不易提高導電性材料之固形份濃度,故而欠佳。
本發明之水性液狀組成物中所含之OH/NH2
聚合物之比例相對於水性液狀組成物100質量份,較佳為0.1~40質量份,進而較佳為0.5~20質量份。
本發明之水性液狀組成物中含有PBTC。PBTC係作為OH/NH2
聚合物之交聯劑而發揮功能。因此,於使用本發明之水性液狀組成物作為塗佈液時,PBTC有助於所形成之塗佈膜之堅牢性提高。又,除作為交聯劑之功能以外,亦可有助於所形成之塗佈膜之親水性、抗菌/防黴性、防臭性等之表現。PBTC為公知之物質,通常使用於螯合劑、抗垢劑、清潔劑、漂白劑、防腐劑、消毒劑、摻雜劑等用途中。再者,PBTC可以Dequest 7000(Thermphos公司製造)等商品名自
市場獲取。
本發明之水性液狀組成物中所含之PBTC之比例相對於水性液狀組成物100質量份,較佳為1~40質量份,進而較佳為1~20質量份。
本發明之水性液狀組成物中所含之OH/NH2
聚合物(A)與PBTC(B)之質量比較佳為A/B=1/5~5/1。若A/B之值未達1/5,則存在OH/NH2
聚合物之交聯變得不充分之傾向。另一方面,若A/B之值超過5/1,則有時就成本績效(cost performance)之方面而言不利。
於本發明之水性液狀組成物中,OH/NH2
聚合物與PBTC之合計之固形份濃度較佳為0.1~40質量%。於OH/NH2
聚合物之重量平均分子量較大,溶液黏度較高之情形時,有時會產生將上述固形份濃度設為0.1質量%左右之必要。但是,若上述固形份濃度未達0.1質量%,則有時難以穩定地形成塗佈膜。另一方面,若上述固形份濃度超過40質量%,則有時不易獲得均勻之水性液狀組成物。
(聚合物酸)
較佳為本發明之水性液狀組成物中進而含有聚合物酸。該聚合物酸為含有羧基之乙烯系單體之均聚合體及/或含有羧基之乙烯系單體與不含羧基之乙烯系單體之共聚合體。藉由含有此種聚合物酸,可進一步提高所形成之塗佈膜對基材之密接性,並且所形成之塗佈膜之親水功能亦進一步提高。
聚合物酸較佳為含有源自含有羧基之乙烯系單體之構成
單元20莫耳%以上,重量平均分子量較佳為5000以上。若源自含有羧基之乙烯系單體之構成單元之含有比例未達20莫耳%,則存在水溶性降低,並且所形成之塗佈膜對基材之密接性降低之傾向。又,若重量平均分子量未達5000,則有時所形成之塗佈膜之強度變得不充分。
作為含有羧基之乙烯系單體之具體例,可舉出:丙烯酸、甲基丙烯酸、順丁烯二酸、衣康酸、反丁烯二酸、丁烯酸、丙烯酸β-羧乙酯、甲基丙烯酸β-羧乙酯等。
作為不含羧基之乙烯系單體,可使用苯乙烯類、丙烯酸酯類、甲基丙烯酸酯類、丙烯醯胺類、烷酸乙烯酯及丙烯腈類。作為苯乙烯類之具體例,可舉出:苯乙烯、甲基苯乙烯、乙烯基甲苯、乙烯基乙苯、乙烯基萘等。作為丙烯酸酯類及甲基丙烯酸酯類之具體例,可舉出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸異丙酯等脂肪族(C1
~C30
)之醇酯類;(甲基)丙烯酸環己酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸甲基環己酯等脂環族醇之酯類;(甲基)丙烯酸羥基乙酯、(甲基)丙烯酸羥基丙酯等含有羥基之(甲基)丙烯酸酯;(甲基)丙烯酸二甲基胺基乙酯、(甲基)丙烯酸二乙基胺基乙酯等含有胺基之(甲基)丙烯酸酯;(甲基)丙烯酸羥基乙酯之鄰苯二甲酸酯類;(甲基)丙烯酸縮水甘油酯等含有縮水甘油基之(甲基)丙烯酸酯等。
作為丙烯醯胺類之具體例,可舉出:丙烯醯胺、甲基丙烯醯胺、二丙酮丙烯醯胺、N-羥甲基丙烯醯胺、N,N-二甲基
丙烯醯胺等。作為烷酸乙烯酯之具體例,可舉出:乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、苯甲酸乙烯酯等。又,作為丙烯腈類之具體例,可舉出:丙烯腈、甲基丙烯腈等。
聚合物酸較佳為選自由聚丙烯酸、聚順丁烯二酸、及聚衣康酸所組成之群中之至少一種。藉由含有此種聚合物酸,可進一步提高所形成之塗佈膜對基材之密接性,並且所形成之塗佈膜之親水功能亦進一步提高。
本發明之水性液狀組成物中所含之聚合物酸之比例相對於水性液狀組成物100質量份,較佳為0.1~40質量份,進而較佳為0.5~20質量份。
較佳為本發明之水性液狀組成物中含有聚烷二醇及/或聚環氧烷。聚烷二醇係藉由使環氧乙烷、環氧丙烷、環氧丁烷等環氧烷開環聚合而獲得之非離子性化合物。又,聚環氧烷係聚烷二醇中聚合度相對較高之高分子量型之非離子性化合物。藉由含有聚烷二醇及/或聚環氧烷,可賦予所形成之塗佈膜更高之可撓性或親水性。
作為聚烷二醇,較佳為聚乙二醇、聚丙二醇、聚丁二醇。又,作為聚環氧烷,較佳為聚環氧乙烷、聚環氧丙烷、聚氧化四亞甲基醚(polytetramethylene oxide)、聚環氧乙烷與聚環氧丙烷之無規或嵌段共聚合物等。該等可以PEO(住友精化公司製造)、Alkox(明成化學工業公司製造)等商品名自市場獲取。
本發明之水性液狀組成物中所含之聚烷二醇與聚環氧烷之合計之含有比例相對於水性液狀組成物100質量份,較佳為0.1~40質量份,進而較佳為0.5~20質量份。
較佳為本發明之水性液狀組成物中含有導電性材料。藉由含有導電性材料,可形成電接觸性提高之塗佈膜。如此形成之塗佈膜可較佳地作為鋰二次電池或電容器等蓄電裝置中所使用之集電體之塗佈膜。即,可形成具有良好導電性之塗佈膜,因此可降低電極層之內部電阻,並且可提高容量密度。
導電性材料較佳為選自由乙炔黑、科琴黑、石墨、爐黑、單層或多層碳奈米纖維及單層或多層碳奈米管所組成之群中之至少一種。
本發明之水性液狀組成物中所含之導電性材料之比例相對於水性液狀組成物100質量份,較佳為0.1~30質量份,進而較佳為1~20質量份。
本發明之水性液狀組成物藉由選擇含有適當之OH/NH2
聚合物、聚合物酸、聚烷二醇及聚環氧烷等,可用作環境負荷較少,具有優異之功能性之水性塗佈液。具體而言,可期待本發明之水性液狀組成物於塗料、油墨、磁體、陶瓷、蓄電裝置、接著劑、電子材料、液晶彩色濾光片、醫藥品、化妝品、香料等各種領域中之利用。例如,藉由含有碳黑等導電性材料,可用作用以製成形成於鋰離子二次電池或電容器等
蓄電裝置之集電體之表面之導電性塗佈膜的導電性塗佈液。
本發明之水性塗佈液為含有上述水性液狀組成物者。再者,亦可僅將上述水性液狀組成物直接用作塗佈液。又,亦可根據用途以成為適當之稀釋倍率之方式利用水系介質稀釋而使用。
若對將本發明之水性塗佈液塗佈於金屬材料等之基材之表面而形成之塗佈膜進行加熱乾燥,則PBTC作為OH/NH2
聚合物之交聯劑發揮作用,而可形成對基材表面具有非常優異之密接性,並且具有耐溶劑性及耐水性之塗佈膜。
水性塗佈液中所含之各成分之比例於將水性塗佈液之總體設為100質量份之情形時,分別如下所述。OH/NH2
聚合物較佳為0.1~40質量份,進而較佳為0.5~20質量份。PBTC較佳為1~40質量份,進而較佳為1~20質量份。聚合物酸較佳為0.1~40質量份,進而較佳為0.5~20質量份。聚烷二醇與聚環氧烷之合計較佳為0.1~40質量份,進而較佳為0.5~20質量份。導電性材料較佳為0.1~30質量份,進而較佳為1~20質量份。再者,水性塗佈液之固形份比例較佳為0.1~40質量%。
若OH/NH2
聚合物之比例未達0.1質量份,則有時所形成之塗佈膜之強度或密接性不足,而存在構成塗佈膜之成分變得容易脫落之傾向。另一方面,若OH/NH2
聚合物之比例超過40質量份,則存在變得不易獲得均勻之溶液之傾向。若
PBTC之比例未達1質量份,則有時交聯之程度變得不充分,而存在所形成之塗佈膜之交聯密度較低,於對基材之密接性、對有機溶劑之不溶解性、非膨潤性之方面上變得不充分之傾向。另一方面,若PBTC之比例超過40質量份,則存在所形成之塗佈膜之可撓性降低之傾向,並且有時就成本方面而言變得不利。若導電性材料之比例未達0.1質量份,則有時所形成之塗佈膜之導電性不足。另一方面,若導電性材料之比例超過30質量份,則有時其他成分不足而所形成之塗佈膜之性能降低。
於形成導電性塗佈膜之情形時,於將水性塗佈液之總體設為100質量份之情形時,較佳為含有OH/NH2
聚合物1~10質量份、PBTC 1~10質量份、聚合物酸0.1~20質量份、聚烷二醇與聚環氧烷之合計0.1~10質量份及導電性材料1~15質量份。
水性塗佈液中亦可含有除PBTC以外之交聯劑(其他交聯劑)等成分。作為其他交聯劑,可舉出除PBTC以外之多元酸類。具體而言,可使用多元酸;多元酸之酸酐;多元酸之一部分或全部之羧基之鹽(銨鹽或胺鹽);多元酸之一部分或全部之羧基之烷基酯、醯胺、醯亞胺、或醯胺醯亞胺;藉由N-羥基琥珀醯亞胺、N-羥基磺基琥珀醯亞胺、或該等之衍生物對該等化合物之羧基之1個以上進行修飾而成之衍生物等。作為多元酸之衍生物,較佳為若加熱則會生成多元酸之化合物。
更具體而言,較佳為使用以下所示之多元酸或其衍生物(例如酸酐)。
<二元酸>草酸、丙二酸、丁二酸、甲基丁二酸、戊二酸、甲基戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、順丁烯二酸、甲基順丁烯二酸、反丁烯二酸、甲基反丁烯二酸、衣康酸、黏康酸、檸康酸、戊烯二酸、乙炔二甲酸、酒石酸、蘋果酸、刺孢青黴酸、麩胺酸、麩胱甘肽、天冬醯胺酸、胱胺酸、乙醯胱胺酸、二甘醇酸、亞胺基二乙酸、羥基乙基亞胺基二乙酸、硫代二甘醇酸、亞硫醯基二甘醇酸、磺醯基二甘醇酸、聚氧化乙烯二甘醇酸(PEG酸,polyethylene oxide diglycol acid)、吡啶二甲酸、吡二甲酸、環氧丁二酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、四氯鄰苯二甲酸、萘二甲酸、四氫鄰苯二甲酸、甲基四氫鄰苯二甲酸、環己烷二甲酸、二苯基碸二甲酸、二苯基甲烷二甲酸;<三元酸>檸檬酸、1,2,3-丙烷三甲酸、1,2,4-丁烷三甲酸、2-膦醯基-1,2,4-丁烷三甲酸、偏苯三甲酸、1,2,4-環己烷三甲酸;<四元酸>乙二胺四乙酸、1,2,3,4-丁烷四甲酸、均苯四甲酸、1,2,4,5-環己烷四甲酸、1,4,5,8-萘四甲酸;<六元酸>1,2,3,4,5,6-環己烷六甲酸。
再者,亦可併用以下所示之其他多元酸。例如,異檸檬酸、烏頭酸、氮基三乙酸、羥基乙基乙二胺三乙酸、羧基乙基硫代丁二酸、對稱苯三甲酸(trimesic acid,1,3,5-苯三甲酸)等
三元酸;乙二胺N,N'-丁二酸、1,4,5,8-萘四甲酸、戊烯四甲酸、己烯四甲酸、麩胺酸二乙酸、順丁烯二醯化甲基環己烯四甲酸、呋喃四甲酸、二苯甲酮四甲酸、酞菁四甲酸、1,2,3,4-環丁烷四甲酸、環戊烷四甲酸等單環式四羧酸類;二環[2,2,1]庚烷-2,3,5,6-四甲酸、二環[2,2,2]辛烷-2,3,5,6-四甲酸等多環式四羧酸類之四元酸;二伸乙基三胺五乙酸等五元酸等。
水性塗佈液中所含之其他多元酸之比例較佳為相對於OH/NH2
聚合物設為0.01~200質量%。
作為除多元酸以外之其他交聯劑,例如可舉出:乙二醇二縮水甘油醚、聚乙二醇二縮水甘油醚、甘油聚縮水甘油醚等環氧化合物;甲苯二異氰酸酯、二甲苯二異氰酸酯、六亞甲基二異氰酸酯、苯基二異氰酸酯等異氰酸酯化合物;利用酚類、醇類、活性亞甲基類、硫醇類、醯胺類、醯亞胺類、胺類、咪唑類、脲類、胺基甲酸類、亞胺類、肟類、亞硫酸類等之阻斷劑對該等異氰酸酯化合物進行阻斷而成之嵌段異氰酸酯化合物;乙二醛、戊二醛、二醛澱粉等醛化合物;聚乙二醇二丙烯酸酯、聚乙二醇二甲基丙烯酸酯、己二醇二丙烯酸酯等(甲基)丙烯酸酯化合物;羥甲基三聚氰胺、二羥甲基脲等羥甲基化合物;乙酸氧鋯、碳酸氧鋯、乳酸鈦等有機酸金屬鹽;三甲醇鋁、三丁醇鋁、四乙醇鈦、四丁醇鈦、四丁醇鋯、乙醯丙酮酸二丙醇鋁、雙(乙醯丙酮酸)二甲醇鈦、雙(乙基乙醯乙酸)二丁醇鈦等金屬烷氧化物化合物;乙烯基甲氧基矽烷、乙烯基乙氧基矽烷、3-縮水甘油氧基丙基三甲
氧基矽烷、3-縮水甘油氧基丙基三乙氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-異氰酸酯丙基三乙氧基矽烷、咪唑矽烷等矽烷偶合劑;甲基三甲氧基矽烷、四乙氧基矽烷、甲基三乙氧基矽烷等矽烷化合物;碳化二醯亞胺化合物等。該等交聯劑之含有比例較佳為設為OH/NH2
聚合物之0.01~200質量%。
又,藉由於水性塗佈液中含有非離子性有機化合物及/或界面活性劑,亦可有效實現對纖維處理之適應性提高或處理物之質感提高。非離子性有機化合物與界面活性劑之合計之含有比例為OH/NH2
聚合物之1~50質量%左右。
作為非離子性有機化合物,例如可舉出:甘油、季戊四醇、三羥甲基丙烷、葡萄糖、果糖、甘露醇、乳糖及海藻糖等。
作為界面活性劑,可舉出:陽離子性界面活性劑、非離子性界面活性劑及兩性界面活性劑。更具體而言,可舉出:氯化膽鹼、聚氧乙烯十二烷基胺、聚氧乙烯十八烷基胺、二甲基十二烷基甜菜鹼、烷基二胺基乙基甘胺酸、乙基硫酸羊毛脂脂肪酸胺基乙基二甲基銨、氧乙烯烷醚、烷基糖苷、烷基聚糖苷、蔗糖脂肪酸酯、甘油烷基醚、甘油烷基酯等。再者,亦可併用兩種以上非離子性有機化合物或界面活性劑。
非離子性有機化合物與界面活性劑之合計之含有比例較佳為相對於OH/NH2
聚合物(例如聚葡萄胺糖類)為1~50質量%。又,非離子性有機化合物之含有比例較佳為相對於
OH/NH2
聚合物(例如聚葡萄胺糖類)為1~20質量%。再者,界面活性劑之含有比例較佳為相對於OH/NH2
聚合物(例如聚葡萄胺糖類)為1~20質量%。藉由設為上述含有比例,可提高所形成之塗佈膜之耐水性與經濟效果之平衡性。
本發明之水性塗佈液中亦可於不妨礙本發明之目的之範圍內添加作為OH/NH2
聚合物之溶解助劑之低級一元羧酸、己二酸二醯肼等二醯肼類、防腐劑、防黴劑、有機溶劑、微粒子填充料、油劑等。
本發明之水性塗佈液雖然含有交聯成分,但是即便於5~30℃之溫度下放置1個月以上亦不易稠化或凝膠化。因此,可確保適用期,並且可用作一液型之處理劑。又,藉由對將本發明之水性塗佈液塗佈於物品(基材)表面而形成之塗佈膜進行加熱乾燥,可形成耐水性優異之功能性塗佈膜。再者,藉由以80℃以上,較佳為120℃~200℃之極限溫度進行加熱乾燥,可形成堅固地密著於物品(基材)表面之功能性塗佈膜。
於水性塗佈液不含填充料等之溶液之情形時,藉由將OH/NH2
聚合物、PBTC、聚合物酸、聚烷二醇及/或聚環氧烷等添加於水系介質中,可製備水性塗佈液。將各成分添加於水系介質(溶劑)中之順序並無特別限定。攪拌亦可於室溫下進行,但亦可視需要進行加熱。
另一方面,於分散有導電性材料之水性塗佈液之情形時,可藉由將OH/NH2
聚合物、PBTC、導電性材料、聚合物酸、聚烷二醇及/或聚環氧烷以成為上述比例之方式添加於水系
介質(分散媒)中,使用先前公知之混合機進行混合分散而製備水性塗佈液。作為混合機,可使用球磨機、砂磨機、顏料分散機、磨碎機、超音波分散機、均質機、行星式混合機、霍巴特型混合機(Hobart mixer)等。再者,亦較佳為使用混合機預先將導電性材料混合,繼而添加OH/NH2
聚合物、PBTC及其他任意成分而均勻混合之方法。藉由採取該等方法,可較容易地製備均勻之水性塗佈液。
本發明之功能性塗佈膜係藉由對將上述水性塗佈液塗佈於被塗佈物(基材)之表面而形成之塗佈膜進行加熱乾燥而形成。水性塗佈液之塗佈量並無特別限制,只要為所形成之功能性塗佈膜之厚度成為通常0.05~100μm,較佳為0.1~10μm,進而較佳為0.1~5μm,尤佳為0.1~2μm之量即可。作為基材,可舉出:鋁或銅等金屬、玻璃、天然樹脂、合成樹脂、陶瓷、木材、紙、纖維、織布、不織布、皮革等。其中,較佳為鋁箔或銅箔等蓄電裝置用集電體。
藉由凹版印刷塗佈、凹版印刷反向塗佈、輥塗、邁耶棒式塗佈(Meyer bar coat)、刮塗(blade coat)、刀式塗佈(knife coat)、氣刀塗佈、刮刀式(comma)塗佈、槽模塗佈、滑動模塗佈(slide die coat)、浸漬塗佈、擠出塗佈、噴塗、刷塗等各種塗佈方法將水性塗佈液塗佈於基材之表面。其後,藉由加熱乾燥而形成功能性塗佈膜。若功能性塗佈膜之膜厚未達0.05 μm,則有時難以均勻地塗佈水性塗佈液。另一方面,
若超過100 μm,則有時功能性塗佈膜之可撓性降低。
加熱乾燥較佳為以80℃以上進行1秒鐘以上,更佳為以80℃以上250℃以下進行1秒以上60分鐘以下。若為該等條件,則可使塗佈液中之OH/NH2
聚合物等聚合物類充分交聯,可形成對基材之密接性及電化學穩定性提高之功能性塗佈膜。若加熱處理條件為未達80℃或未達1秒,則有時所形成之功能性塗佈膜之密接性及電化學穩定性降低。
本發明之水性液狀組成物及水性塗佈液於含有導電性材料之情形時,可較佳地作為構成二次電池或電容器等蓄電裝置用之電極板之導電性塗佈膜之形成材料。再者,藉由對塗佈於集電體10之表面之水性液狀組成物或水性塗佈液進行加熱乾燥,可獲得如圖1所示之包含集電體10及配設於該集電體10之表面之導電性塗佈膜12之電極板用構件14。導電性塗佈膜12之厚度通常為0.1~10μm,較佳為0.1~5μm,進而較佳為0.1~2μm。藉由於所形成之導電性塗佈膜12之上形成電池用正極電極層、電池用負極電極層、電容器用正極電極層、電容器用負極電極層或可極化電極層等活性物質層16,可製造如圖1所示之電極層-集電體間之電阻較小,環境負荷較少之蓄電裝置用之電極板20。
又,藉由使用以如上所述之方式製造之電極板,可獲得非水電解液二次電池、電雙層電容器、及鋰離子電容器等蓄電裝置。該蓄電裝置包含於集電體之表面配設有導電性塗佈膜
之電極板用構件,因此該蓄電裝置係具有放電容量較大或內部電阻較低等優異特性者。
導電性塗佈膜之表面電阻率較佳為3,000 Ω/□以下,進而較佳為2,000 Ω/□以下。若表面電阻率超過3,000 Ω/□,則內部電阻變高,因此難以獲得高效率且長壽命之電池或電容器。
導電性塗佈膜之表面電阻率係藉由以下所示之方法測定。將水性塗佈液塗佈於玻璃板上後,於200℃下乾燥1分鐘,而形成乾燥膜厚4μm之導電性塗佈膜。然後,依據JIS K 7194,藉由四探針法測定表面電阻率。再者,利用四探針法之表面電阻率測定可使用Mitsubishi Chemical Analytech公司製造之Loresta GP、MCP-T610,於25℃、相對濕度60%之條件下實施。
本發明之水性液狀組成物及水性塗佈液可較佳地作為設置於玻璃等之基材之表面之親水性塗佈膜的形成材料。藉由形成親水性塗佈膜,可賦予防灰暗性。親水性塗佈膜之厚度通常為0.1~10μm,較佳為0.1~5μm,進而較佳為0.1~2μm。
親水性塗佈膜與水之接觸角(θ)較佳為40°。親水性塗佈膜與水之接觸角(θ)係藉由以下所示之方法測定。將水性塗佈液塗佈於基材上後,於200℃下乾燥10秒鐘,形成乾燥膜厚0.7μm之親水性塗佈膜。然後,依據JIS K 2396,藉由液滴法測定水相對於親水性塗佈膜之接觸角。再者,利用液滴法之接觸角之測定可使用協和界面科學公司製造之接觸角計
Drop Master 100,於25℃、相對濕度60%之條件下實施。
本發明之複合材料包含基材、及一體地配設於該基材上之上述功能性塗佈膜。本發明之複合材料係親水性、導電性、抗菌/防臭性、質感、防灰暗性、紙力、染色性、耐水性、防污染性等優異之材料。再者,本發明之複合材料可藉由對於基材上塗佈上述水性液狀組成物或水性塗佈液而形成之塗佈膜進行加熱乾燥等而製造。
作為基材,可舉出:金屬、玻璃、天然樹脂、合成樹脂、陶瓷、木材、紙不織布、織布及皮革等。又,只要使用鋁、銅、鎳及不鏽鋼等金屬作為基材,則可提供作為蓄電裝置集電體有用之複合材料。
其次,列舉實施例進一步具體地說明本發明。再者,以下,記為「份」或「%」者係質量基準。
將各種水性液狀組成物之組成示於表1-1及1-2。再者,將羥基丙基聚葡萄胺糖簡稱為「HPC,hydroxypropyl chitosan」,將羥基丁基聚葡萄胺糖簡稱為「HBC,hydroxybutyl chitosan」,將甘油化聚葡萄胺糖簡稱為「GLYC,glycerylation chitosan」,將膦醯基丁烷三羧酸簡稱為「PBTC,phosphono butane tricarboxylic acid」,將異丙醇簡稱為「IPA,isopropyl alcohol」。
於離子交換水81份中添加聚葡萄胺糖(脫乙醯化度85%,重量平均分子量10萬)5份與50%PBTC水溶液(Thermphos公司製造,Dequest 7000)14份後,於室溫下攪拌溶解4小時,製備100份之水性液狀組成物。
設為表1-1及1-2所示之組成,除此以外,以與上述例1-1相同之方式製備水性液狀組成物。
於離子交換水65份中添加聚葡萄胺糖(脫乙醯化度85%,重量平均分子量10萬)10份與聚丙烯酸水溶液(束亞合成公司製造,JURYMER AC-10L(固形份40%,MW25,000))25份後,於室溫下攪拌24小時。然而,聚葡萄胺糖未溶解而無法獲得均勻之水性液狀組成物。
(1)導電性塗佈液
將乙炔黑10份與例1-1之水性液狀組成物90份加以調配,使用行星式混合機,以轉速60 rpm攪拌混合120分鐘而製備導電性塗佈液。
(2)導電性塗佈膜
使用刮刀式(comma)輥塗機將所製備之導電性塗佈液塗佈於厚度20μm之包含鋁箔之集電體之單面。利用110℃之烘箱加熱乾燥2分鐘,進而利用180℃之烘箱加熱乾燥2分鐘,而使膜厚1μm之導電性塗佈膜形成於集電體之單面上。
(3)溶解/膨潤性
製備於以碳酸伸乙酯(EC,ethylene carbonate):碳酸伸丙酯(PC,propylene carbonate):二甲氧基乙烷(DME,dimethoxy ethane)=1:1:2(體積比)調配之混合溶劑中溶解作為支援電解質之1莫耳之LiPF6
而成之溶液。將導電性塗佈膜浸漬於70℃之溶液中72小時後,觀察狀態。將導電性塗佈膜無變化者評價為溶解/膨潤性「良」。又,將導電性塗佈膜層剝離或膨潤者評價為溶解/膨潤性「不良」。將結果示於表2。
(4)表面電阻率
使用刮刀式輥塗機將導電性塗佈液塗佈於聚對苯二甲酸乙二酯(PET,polyethylene terephthalate)膜上後,利用180℃之烘箱進行5分鐘乾燥處理而形成導電性塗佈膜(乾燥膜厚4 μm)。依據JIS K 7194,藉由四探針法測定所形成之導電性塗佈膜之表面電阻率。將結果示於表2。再者,利用四探針法之測定係使用Mitsubishi Chemical Analytech公司製造之Loresta GP、MCP-T610,於25℃、相對濕度60%之條件下實施。
使用表2所示之水性液狀組成物代替例1-1之水性液狀組成物,除此以外,以與上述實施例1相同之方式製備導電性塗佈液。又,以與實施例1相同之方式進行溶解/膨潤性之評價及表面電阻率之測定。將結果示於表2。再者,於比較例2中係使用聚偏二氟乙烯之
5%NMP(N-Methylpyrrolidone,N-甲基吡咯烷酮)溶液(聚偏二氟乙烯(PVDF,polyvinylidene fluoride)溶液)。
(1)正極電極板
使用刮刀式輥塗機將實施例1之導電性塗佈液塗佈於厚
度20 μm之包含鋁箔之集電體之單面。利用110℃之烘箱加熱乾燥2分鐘,進而利用180℃之烘箱加熱乾燥2分鐘,而使膜厚為1 μm之導電性塗佈膜形成於集電體之單面上。
藉由將LiCoO2
粉末(粒徑1~100 μm)90份、乙炔黑5份、及聚偏二氟乙烯之5%NMP溶液(PVDF溶液)50份加以混合,利用行星式混合機以轉速60 rpm攪拌混合120分鐘,而獲得漿料狀之包含正極活性物質之正極液。利用刮刀式輥塗機將所獲得之正極液塗佈於導電性塗佈膜之表面後,利用110℃之烘箱進行2分鐘乾燥處理,進而,利用180℃之烘箱乾燥2分鐘將溶劑除去,而於導電性塗佈膜上形成乾燥膜厚為100 μm之正極活性物質層。於5,000 kgf/cm2
之條件下進行加壓而使膜厚均勻後,於80℃之真空烘箱中進行48小時老化,將揮發分(水或溶劑等)充分地除去而獲得正極電極板。
(2)負極電極板
使用刮刀式輥塗機將實施例1之導電性塗佈液塗佈於銅箔集電體之單面。利用110℃之烘箱加熱乾燥2分鐘,進而利用180℃之烘箱加熱乾燥2分鐘,而使膜厚為1 μm之導電性塗佈膜形成於集電體之單面上。
將使焦炭(coal cokes)於1200℃下熱分解而獲得之碳粉末90份、乙炔黑5份、及聚偏二氟乙烯之5%NMP溶液(PVDF溶液)50份加以混合,利用行星式混合機以轉速60 rpm攪拌混合120分鐘,藉此獲得漿料狀之包含負極活性物質之負極
液。利用刮刀式輥塗機將所獲得之負極液塗佈於導電性塗佈膜之表面後,利用110℃之烘箱進行2分鐘乾燥處理,進而利用180℃之烘箱乾燥2分鐘將溶劑除去,而於導電性塗佈膜上形成乾燥膜厚為100μm之負極活性物質層。於5,000 kgf/cm2
之條件下進行加壓而使膜厚均勻後,於80℃之真空烘箱中進行48小時老化,將揮發分(水或溶劑等)充分地除去而獲得負極電極板。
(3)電池
經由包含具有三維孔隙結構(海綿狀)之寬度寬於正極電極板之聚烯烴系(聚丙烯、聚乙烯或該等之共聚合體)之多孔性膜之分隔件將正極電極板與負極電極板捲繞為螺旋狀而製作電極體。將所製作之電極體插入兼具負極端子之有底圓筒狀之不鏽鋼容器內,以AA尺寸組裝額定容量500 mAh之電池。將於以按照EC(碳酸伸乙酯):PC(碳酸伸丙酯):DME(二甲氧基乙烷)=1:1:2(體積比)總量成為1升之方式製備之混合溶劑中溶解作為支援電解質之1莫耳之LiPF6
而成者作為電解液注入至該電池中。
(4)充放電容量維持率
使用充放電測定裝置,於25℃之溫度條件下測定電池之充放電特性。分別對20微孔,以充電電流0.2 CA之電流值進行充電直至自充電方向電池電壓變為4.1 V為止,停歇10分鐘後,以相同電流進行放電直至2.75 V為止,停歇10分鐘後,以下,於同一條件下反覆100循環之充放電而測定充
放電特性。將第1循環之充放電容量值設為100之情形時的第100次充放電容量值(充放電容量維持率)為99%。
使用表3所示之導電性塗佈液代替實施例1之導電性塗佈液,除此以外,以與上述實施例20相同之方式製作電池。又,以與實施例20相同之方式測定充放電容量維持率。將結果示於表3。
使用刮刀式輥塗機將實施例1之導電性塗佈液塗佈於厚度20μm之包含鋁箔之集電體之單面。利用110℃之烘箱加熱乾燥2分鐘,進而利用180℃之烘箱加熱乾燥2分鐘,而使膜厚為0.5μm之導電性塗佈膜形成於集電體之單面上。
將比表面積1,500 m2
/g、平均粒徑10μm之高純度活性碳粉末100份及乙炔黑8份添入行星式混合機中,以總固形份濃度成為45%之方式添加聚偏二氟乙烯之5%NMP溶液(PVDF溶液)混合60分鐘。其後,以固形份濃度成為42%之方式利用NMP進行稀釋進而混合10分鐘而獲得電極
液。使用刮刀將所獲得之電極液塗佈於導電性塗佈膜上,利用送風乾燥機於80℃下乾燥30分鐘。其後,使用滾筒壓機進行加壓而獲得厚度80μm、密度0.6 g/cm3
之電容器用可極化電極板。
製作2片將所獲得之電容器用可極化電極板切取為直徑15 mm之圓形者,於200℃下乾燥20小時。使2片電極板之電極層面對向,於其間夾持直徑18 mm、厚度40μm之圓形纖維素製分隔件,收納於設置有聚丙烯製襯墊之不鏽鋼製硬幣型外裝容器(直徑20 mm,高度1.8 mm,不鏽鋼厚度0.25 mm)中。於硬幣型外裝容器中以不殘留空氣之方式注入電解液,經由聚丙烯製襯墊,於外裝容器上蓋上厚度0.2 mm之不鏽鋼蓋並固定,將容器密封,而製造直徑20 mm、厚度約2 mm之電容器。再者,使用使四氟硼酸四乙基銨以1莫耳/升之濃度溶解於碳酸伸丙酯中而成之溶液作為電解液。將所獲得之電容器之電容及內部電阻之測定結果示於表4。
使用表4所示之導電性塗佈液代替實施例1之導電性塗佈液,除此以外,以與上述實施例26相同之方式獲得電容器。又,測定所獲得之電容器之電容及內部電阻。將測定結果示於表4。
使用表4所示之導電性塗佈液代替實施例1之導電性塗佈液,除此以外,以與上述實施例26相同之方式獲得電容器。
測定所獲得之電容器之電容及內部電阻,設為評價實施例26~31之電容器之基準。
於電流密度20 mA/cm2
下測定電容器之電容及內部電阻。以比較例4之電容器之電容及內部電阻為基準,按照以下基準評價實施例26~31之電容器。顯示出電容越大,又,內部電阻越小,作為電容器之性能越良好。
A:電容較比較例4大20%以上。
B:電容較比較例4大10%以上且未達20%。
C:電容為比較例4之同等以下。
A:內部電阻較比較例4小20%以上。
B:內部電阻較比較例4小10%以上且未達20%。
C:內部電阻為比較例4之同等以下。
將各種親水性塗佈液之組成示於表5-1及5-2。再者,將膦醯基丁烷三羧酸簡稱為「PBTC」,將丁烷四羧酸簡稱為
「BTC,butane tetracarboxylic acid」,將聚丙烯酸簡稱為「PAA,polyacrylic acid」,將聚順丁烯二酸簡稱為「PMA,polymaleic acid」,將聚乙烯醇簡稱為「PVA,polyvinyl alcohol」,將聚乙二醇簡稱為「PEG,polyethylene glycol」,將聚環氧乙烷簡稱為「PEO,polyethylene oxide」。
使聚葡萄胺糖(脫乙醯化度85%,重量平均分子量10萬)5份分散於離子交換水79份中而獲得分散液。於所獲得之分散液中添加50%PBTC水溶液(Thermphos公司製造,Dequest 7000)16份後,於室溫下攪拌4小時而製備100份之親水性塗佈液。
使聚葡萄胺糖(脫乙醯化度85%,重量平均分子量6萬)6份分散於離子交換水64份中而獲得分散液。於所獲得之分散液中添加50%PBTC水溶液(Thermphos公司製造,Dequest 7000)20份後,於室溫下攪拌4小時。繼而,於攪拌下,添加聚丙烯酸水溶液(東亞合成公司製造,JURYMER AC-10L(固形份40%,MW25,000))10份後,於室溫下攪拌2小時而製備100份之親水性塗佈液。
設為表5-1及5-2所示之組成,除此以外,以與上述實施例32及33相同之方式製備親水性塗佈液。
將離子交換水90份與甘油化聚葡萄胺糖10份加以混合,於室溫下攪拌溶解4小時而製備親水性塗佈液。
於離子交換水37.5份中添加10%PVA水溶液(Kuraray公司製造,Kuraray Poval PVA117)50份後,於攪拌下,添加聚丙烯酸水溶液(束亞合成公司製造,JURYMER AC-10L(固形份40%,Mw25,000))12.5份。於室溫下攪拌2小時而製備100份之親水性塗佈液。
設為表5-1及5-2所示之組成,除此以外,以與上述實施例32相同之方式製備親水性塗佈液。
(1)親水性塗佈膜之形成
使用棒式塗佈機(No.3)將實施例32~47及比較例5~8之親水性塗佈液以成為1 g/m2
之乾燥膜量之方式塗佈於板厚1 nm之玻璃板(100×100 mm)表面。繼而,於表6所示之條件下加熱乾燥塗佈有親水性塗佈液之玻璃板,而獲得玻璃板上形成有約0.7μm之親水性塗佈膜之供試材。
(2)供試材之清洗
利用自來水對供試材進行1小時流水清洗(流量1 L/分鐘)後,於80℃下送風乾燥1小時。將該流水清洗與80℃乾燥之處理設為1循環,進行合計10循環之反覆清洗。
(3)接觸角之測定
於設置為水平狀態之供試材之表面滴加2 μl之純水。依據JIS K2396,使用接觸角計(協和界面科學公司製造,DropMaster100)測定水滴之接觸角。再者,接觸角之測定係於供試材之清洗前及10循環之反覆清洗後兩種情況下進行。
(4)親水性評價基準
根據所測定之接觸角,依據以下基準對親水性塗佈膜之清洗前後之親水性進行評價。將結果示於表6。
5:接觸角未達10°。
4:接觸角為10°以上且未達20°。
3:接觸角為20°以上且未達30°。
2:接觸角為30°以上且未達40°。
1:接觸角為40°以上且未達50°。
0:接觸角為50°以上。
若使用本發明之水性液狀組成物,則可形成具有對基材之優異之密接性、耐久性、耐溶劑性及耐水性,並且可發揮導電性、親水性、耐污染性、防黴/抗菌性、防臭性及加工性等功能之功能性塗佈膜。包含此種功能性塗佈膜之複合材料作為蓄電裝置用之集電體等較為有用。
10‧‧‧集電體
12‧‧‧導電性塗佈膜
14‧‧‧電極板用構件
16‧‧‧活性物質層
20‧‧‧電極板
圖1係說明本發明之電極板用構件及電極板之一實施形態之層構成之剖面圖。
Claims (24)
- 一種水性液狀組成物,其含有包含水之水系介質、具有羥基及/或胺基之聚合物、及膦醯基丁烷三羧酸;上述聚合物為選自由多糖、聚胺基酸、聚乙烯醇、聚烯丙胺、聚乙烯胺、聚脒、聚乙烯亞胺及該等之衍生物所組成之群組中之至少一種,但同時含有幾丁聚醣衍生物及改質聚乙烯醇者除外。
- 一種水性液狀組成物,其含有包含水之水系介質、具有羥基及/或胺基之聚合物、及膦醯基丁烷三羧酸;上述聚合物為選自由多糖、聚胺基酸、聚乙烯醇、聚烯丙胺、聚乙烯胺、聚脒、聚乙烯亞胺及該等之衍生物所組成之群組中之至少一種,但含有可溶化劑者除外。
- 一種水性液狀組成物,其含有包含水之水系介質、具有羥基及/或胺基之聚合物、膦醯基丁烷三羧酸、及導電性材料;上述聚合物為選自由多糖、聚胺基酸、聚乙烯醇、聚烯丙胺、聚乙烯胺、聚脒、聚乙烯亞胺及該等之衍生物所組成之群組中之至少一種。
- 如申請專利範圍第3項之水性液狀組成物,其中,上述導電性材料為選自由乙炔黑、科琴黑、石墨、爐黑、單層或多層碳奈米纖維、及單層或多層碳奈米管所組成之群組中之至少一種。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,進一步含有聚合物酸;上述聚合物酸為含有羧基之乙烯系單體之均聚合體及/或含有羧基之乙烯系單體與不含羧基之乙烯系單體之共聚合體。
- 如申請專利範圍第5項之水性液狀組成物,其中,上述聚合物酸為選自由聚丙烯酸、聚順丁烯二酸、及聚衣康酸所組成之群組中之至少一種。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,進一步含有聚烷二醇及/或聚環氧烷。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,上述多糖為選自由海藻酸、澱粉、纖維素、幾丁質、幾丁聚醣、果膠及該等之衍生物所組成之群組中之至少一種。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,上述聚胺基酸為選自由聚離胺酸、聚鳥胺酸、聚精胺酸、聚組胺酸、魚精蛋白、明膠及膠原蛋白所組成之群組中之至少一種。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,上述聚合物(A)與上述膦醯基丁烷三羧酸(B)之質量比為A/B=1/5~5/1。
- 如申請專利範圍第1至4項中任一項之水性液狀組成 物,其中,上述聚合物之重量平均分子量為5,000~200萬。
- 如申請專利範圍第1至4項中任一項之水性液狀組成物,其中,上述聚合物與上述膦醯基丁烷三羧酸之合計之固形份濃度為0.1~40質量%。
- 一種水性塗佈液,其含有申請專利範圍第1至4項中任一項之水性液狀組成物。
- 一種功能性塗佈膜,其係藉由申請專利範圍第13項之水性塗佈液而形成。
- 如申請專利範圍第14項之功能性塗佈膜,其中,利用JIS K7194測定之表面電阻率為3,000Ω/□以下。
- 一種功能性塗佈膜之形成方法,其包括將申請專利範圍第13項之水性塗佈液加熱至80℃以上之步驟。
- 一種複合材料,其包含基材、及一體地配設於上述基材上之申請專利範圍第14項之功能性塗佈膜。
- 如申請專利範圍第17項之複合材料,其中,上述基材為選自由金屬、玻璃、天然樹脂、合成樹脂、陶瓷、木材、紙、纖維、不織布、織布及皮革所組成之群組中之至少一種。
- 如申請專利範圍第17項之複合材料,其中,上述基材為選自由鋁、銅、鎳及不鏽鋼所組成之群組中之至少一種。
- 一種電極板用構件,其包含集電體、及配設於上述集電體之表面之導電性塗佈膜;上述導電性塗佈膜係對塗佈於上述集電體之表面之申請 專利範圍第3或4項之水性液狀組成物進行加熱處理而形成者。
- 如申請專利範圍第20項之電極板用構件,其中,上述集電體為非水電解液二次電池用、電雙層電容器用、或鋰離子電容器用之集電體。
- 一種電極板,其包含申請專利範圍第20項之電極板用構件、及配設於上述導電性塗佈膜之表面之活性物質層。
- 一種蓄電裝置,其包含申請專利範圍第22項之電極板。
- 如申請專利範圍第23項之蓄電裝置,其係非水電解液二次電池、電雙層電容器、或鋰離子電容器。
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CN103403109B (zh) | 2015-12-23 |
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US20130316231A1 (en) | 2013-11-28 |
EP2679637B1 (en) | 2017-05-10 |
CN103403109A (zh) | 2013-11-20 |
JP5134739B2 (ja) | 2013-01-30 |
KR101521036B1 (ko) | 2015-05-15 |
EP2679637A4 (en) | 2015-08-05 |
US10400115B2 (en) | 2019-09-03 |
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EP2679637A1 (en) | 2014-01-01 |
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