CN110711497A - 复合膜的干燥装置 - Google Patents
复合膜的干燥装置 Download PDFInfo
- Publication number
- CN110711497A CN110711497A CN201911126425.6A CN201911126425A CN110711497A CN 110711497 A CN110711497 A CN 110711497A CN 201911126425 A CN201911126425 A CN 201911126425A CN 110711497 A CN110711497 A CN 110711497A
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- Prior art keywords
- composite film
- coating
- drying
- composite
- hot air
- Prior art date
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Abstract
本发明提供复合膜的干燥装置,其是在多孔质基材的一面或两面上具有涂布层的复合膜的干燥装置,其具备具有接触式加热机构和热风送风机构的干燥机构,在对经水洗的所述复合膜进行传送的同时,使所述复合膜与所述接触式加热机构接触,并且使从所述热风送风机构送出的热风吹至所述复合膜,从而将水从所述复合膜中除去。
Description
本申请是申请日为2015年12月10日、申请号为201580078120.6(国际申请号为PCT/JP2015/084722)、发明名称为“复合膜的制造方法”的发明申请的分案申请。
技术领域
本发明涉及复合膜的制造方法。
背景技术
以往,作为电池隔膜、气体过滤器、液体过滤器等,在多孔质基材上具有多孔质层的复合膜是已知的。作为该复合膜的制造方法,已知有所谓的湿式制法,即,将含有树脂的涂布液涂布于多孔质基材上而形成涂布层,在凝固液中浸渍而使涂布层中的树脂凝固,经过水洗和干燥从而制作多孔质层的方法(例如,参见专利文献1)。湿式制法已作为可将包含树脂的多孔质层良好地多孔化的制法而为人们所知。
现有技术文献
专利文献
专利文献1:日本专利第5134526号公报
发明内容
发明要解决的课题
要利用湿式制法来批量生产在多孔质基材上具有多孔质层的复合膜时,将长尺寸的多孔质基材依次传送至涂布、凝固、水洗及干燥各工序并连续实施这些工序是理想的,从提高生产率的观点考虑,在各工序中提高多孔质基材的传送速度是理想的。然而,若提高多孔质基材的传送速度而实施干燥工序,则存在下述情况:设置于多孔质基材上的多孔质层发生剥离,或者在复合膜中产生收缩、变形、褶皱。迄今为止,尚未提出用于解决湿式制法的干燥工序中的上述课题的合适方法。
本发明的实施方式是鉴于上述情况而作成的。
本发明的实施方式的目的在于提供以高生产效率制造高品质的复合膜的复合膜制造方法。
用于解决课题的手段
用于解决上述课题的具体手段包括下述方式。
[1]复合膜的制造方法,其具有下述工序:
涂布工序,将含有树脂的涂布液涂布于多孔质基材的一面或两面上,从而形成涂布层;
凝固工序,使所述涂布层与凝固液接触从而使所述树脂凝固,得到在所述多孔质基材的一面或两面上具有包含所述树脂的多孔质层的复合膜;
水洗工序,对所述复合膜进行水洗;和
干燥工序,其是在以30m/min以上的传送速度传送所述复合膜的同时将水从所述复合膜中除去的干燥工序,其中,使用具备具有接触式加热机构和热风送风机构的干燥机构的干燥装置,使所述复合膜与所述接触式加热机构接触,并且使从所述热风送风机构送出的热风吹至所述复合膜,从而将水从所述复合膜中除去。
[2]如[1]所述的制造方法,其中,所述多孔质基材在105℃下放置30分钟时的机械方向(machine direction)的热收缩率为10%以下,且宽度方向的热收缩率为5%以下。
[3]如[1]或[2]所述的制造方法,其中,所述接触式加热机构的与所述复合膜接触的面的温度为105℃以下,所述热风在所述热风送风机构的送风口处的温度为105℃以下。
[4]如[1]~[3]中任一项所述的制造方法,其中,所述热风在所述热风送风机构的送风口处的风速为5m/sec以上且30m/sec以下。
[5]如[1]~[4]中任一项所述的制造方法,其中,所述干燥装置具备2个以上所述干燥机构,在所述干燥装置中存在2个以上的所述接触式加热机构根据与所述复合膜接触的面的温度的异同而被分为2个以上的组,与构成位于所述复合膜的传送方向的最上游侧的第一组的所述接触式加热机构的所述面的温度相比,构成作为在所述第一组下游侧邻接的组的第二组的所述接触式加热机构的所述面的温度更高。
[6]如[1]~[5]中任一项所述的制造方法,其中,所述接触式加热机构相对于所述复合膜的总接触长度为30m以下。
[7]如[1]~[6]中任一项所述的制造方法,其中,所述干燥装置具备具有传入口及传出口的外壳,所述干燥机构被配置于所述外壳的内部,从所述传入口至所述传出口为止的所述复合膜的传送长度为50m以下。
[8]如[1]~[7]中任一项所述的制造方法,其中,所述接触式加热机构的与所述复合膜接触的面含有氟系树脂。
发明的效果
根据本发明的实施方式,可提供以高生产效率制造高品质的复合膜的复合膜制造方法。
附图说明
[图1]为示出本公开文本的制造方法的一种实施方式的概念图。
[图2]为示出本公开文本的制造方法中使用的干燥装置的一例的示意图。
[图3A]为示出热风送风机构所具有的送风口的一例的示意图。
[图3B]为示出热风送风机构所具有的送风口的一例的示意图。
具体实施方式
本说明书中,使用“~”表示的数值范围,表示将“~”前后记载的数值分别作为最小值及最大值包含在内的范围。
本说明书中,术语“工序”不仅包含独立的工序,而且,即使在无法与其他工序明确区分的情况下,如果能达成该工序所期望的目的,则也包含在本术语中。
本说明书中,“机械方向”是指被制造成长条状的多孔质基材及复合膜中的长尺寸方向,“宽度方向”是指与“机械方向”正交的方向。将“机械方向”亦称为“MD方向”,将“宽度方向”亦称为“TD方向”。
以下,对本发明的实施方式进行说明。这些说明及实施例是对本发明进行例示,并不限制本发明的范围。
<复合膜的制造方法>
本公开文本的制造方法是制造具有多孔质基材和被设置在该多孔质基材的一面或两面的、含有树脂的多孔质层的复合膜的方法。本公开文本的制造方法是将含有树脂的涂布液涂布于多孔质基材的一面或两面上、从而在多孔质基材的一面或两面上设置多孔质层的制造方法。本公开文本的制造方法具有下述的工序。
·涂布工序:将含有树脂的涂布液涂布于多孔质基材的一面或两面上,从而形成涂布层。
·凝固工序:使涂布层与凝固液接触从而使树脂凝固,得到在多孔质基材的一面或两面上具有包含树脂的多孔质层的复合膜。
·水洗工序:对复合膜进行水洗。
·干燥工序:将水从复合膜中除去。
本公开文本的制造方法是被称作湿式制法的方法,是在多孔质基材上设置多孔质层的制造方法。
本公开文本的制造方法还可具有制备涂布工序中使用的涂布液的涂布液制备工序。
图1为示出本公开文本的制造方法的一种实施方式的概念图。图1中,在图中的左侧放置有供于复合膜的制造的多孔质基材的卷,在图中的右侧放置有将复合膜进行卷绕而得的卷。图1所示的实施方式具有涂布液制备工序、涂布工序、凝固工序、水洗工序、及干燥工序。本实施方式中,连续地依次进行涂布工序、凝固工序、水洗工序、及干燥工序。此外,本实施方式根据涂布工序的实施时期而进行涂布液制备工序。各工序的详情如后文所述。
对于本公开文本的制造方法而言,从复合膜的生产效率的观点考虑,干燥工序中的复合膜的传送速度为30m/min以上。传送速度越快,附着于复合膜的水分越难以除去,如何才能维持复合膜的高品质并充分地进行干燥成为重要的课题。因此,本公开文本的制造方法中,干燥工序为下述工序:使用具有接触式加热机构和热风送风机构的干燥机构,使复合膜与接触式加热机构接触,并且使从热风送风机构送出的热风吹至复合膜,从而将水从复合膜中除去。根据该干燥工序,与仅使用接触式加热机构作为干燥机构的干燥工序相比,多孔质层不易剥离,与仅使用热风送风机构作为干燥机构的干燥工序相比,复合膜中不易产生收缩、变形及褶皱。因此,根据本公开文本的制造方法,能够以高生产效率制造高品质的复合膜。若干燥工序中的复合膜的传送速度小于30m/min,则生产效率差,并存在下述情况:复合膜中产生收缩、变形或褶皱,或者产生多孔质层的剥离。
根据本公开文本的制造方法,由于干燥机构同时设置有接触式加热机构和热风送风机构,使用这两者将水从复合膜中除去,因此可缩短干燥工序所需的时间,此外,不需要将干燥工序的传送长度增长,可抑制制造设备的设置空间及设置成本。
以下,详细说明本公开文本的制造方法的各工序。
[涂布液制备工序]
本公开文本的制造方法可具有制备供于涂布工序的涂布液的涂布液制备工序。本公开文本的制造方法也可不具有涂布液制备工序,可将已经制造并被保存的涂布液供于涂布工序。
涂布液制备工序是制备含有树脂的涂布液的工序。涂布液是例如将树脂溶解于溶剂中并进一步根据需要使无机填料、有机填料分散而制备的。关于涂布液的制备中使用的树脂、填料等(即多孔质层中包含的树脂、填料等),在后述的[多孔质层]的项中进行详细说明。
作为涂布液的制备中使用的将树脂溶解的溶剂(以下,也称为“良溶剂”。),可举出N-甲基吡咯烷酮、二甲基乙酰胺、二甲基甲酰胺、二甲基甲酰胺等极性酰胺溶剂。从形成具有良好的多孔结构的多孔质层的观点考虑,优选将诱发相分离的相分离剂混合在良溶剂中。作为相分离剂,可举出水、甲醇、乙醇、丙醇、丁醇、丁二醇、乙二醇、丙二醇、三丙二醇等。对于相分离剂而言,优选将其以可确保适于进行涂布的涂布液的粘度的范围内的质量比与良溶剂混合。
作为涂布液的制备中使用的溶剂,从形成良好的多孔结构的观点考虑,含有60质量%以上的良溶剂、且含有5质量%~40质量%的相分离剂的混合溶剂是优选的。对于涂布液而言,从形成良好的多孔结构的观点考虑,优选的是,以3质量%~15质量%的浓度含有树脂。
[涂布工序]
涂布工序是将含有树脂的涂布液涂布于多孔质基材的一面或两面上从而形成涂布层的工序。涂布液向多孔质基材的涂布可利用迈耶棒、模涂机、逆转辊涂布机、凹版涂布机等涂布机构进行。对于涂布量而言,两面合计例如为10mL/m2~60mL/m2。
涂布工序的一种实施方式为下述方式:使用隔着多孔质基材相对地配置的第一涂布机构(涂布一侧的面)和第二涂布机构(涂布另一侧的面),将涂布液同时涂布于多孔质基材的两面。
涂布工序的一种实施方式为下述方式:使用在多孔质基材的传送方向上隔开间隔地配置的第一涂布机构(涂布一侧的面)和第二涂布机构(涂布另一侧的面),逐面地依次将涂布液涂布于多孔质基材的两面。
[凝固工序]
凝固工序为下述工序:使涂布层与凝固液接触从而使涂布层中含有的树脂凝固,得到在多孔质基材的一面或两面上具有多孔质层的复合膜。作为使涂布层与凝固液接触的方法,优选使具有涂布层的多孔质基材浸渍于凝固液中,具体而言,优选使具有涂布层的多孔质基材从装有凝固液的槽(凝固槽)中通过。
凝固液通常为水与在涂布液的制备中使用的良溶剂及相分离剂的混合溶液。在生产方面,良溶剂与相分离剂的混合比同在涂布液的制备中使用的混合溶剂的混合比一致是优选的。从多孔结构的形成及生产率的观点考虑,凝固液的水的含量优选为40质量%~80质量%。凝固液的温度例如为10℃~50℃。
[水洗工序]
水洗工序是基于除去复合膜中含有的溶剂(涂布液的溶剂及凝固液的溶剂)的目的而对复合膜进行水洗的工序。水洗工序优选为在水浴中传送复合膜的工序。用于水洗的水的温度例如为0℃~70℃。
[干燥工序]
干燥工序是基于除去水洗后的复合膜中包含的水的目的而进行的工序。
从复合膜的生产效率的观点考虑,干燥工序中的复合膜的传送速度为30m/min以上。所述传送速度更优选为40m/min以上,进一步优选为50m/min以上。另一方面,从确保干燥时间的观点考虑,所述传送速度的上限优选为100m/min以下。
实施干燥工序的干燥装置具备具有接触式加热机构和热风送风机构的干燥机构。干燥装置具备1个或2个以上所述干燥机构,从干燥效率的观点考虑,优选具备2个以上所述干燥机构。
作为接触式加热机构,具体而言,可举出加热辊、加热带、热板等。接触式加热机构为加热辊或加热带的情况下,加热辊或加热带的外周面为与复合膜接触的面。
本公开文本的制造方法中,干燥装置可不具备外壳(housing),从控制复合膜的周围的温度及湿度的观点考虑,优选具备外壳。
以下,参照附图对干燥装置的实施方式例进行说明,但本公开文本的制造方法当然不限于这些例子。以下,举出加热辊作为接触式加热机构的一例,对干燥装置的实施方式例进行说明。以下说明的干燥装置的实施方式例对于接触式加热机构为除加热辊以外的机构(例如,加热带、热板)的干燥装置也适用。对于接触式加热机构为例如加热带或热板的实施方式例而言,可通过将以下说明中的加热辊31~34替换记载为加热带31~34或热板31~34而实施。
图2所示的干燥装置10具备外壳21、配置于外壳21的内部的干燥机构51~54、和用于传送复合膜70的驱动辊61。外壳21具有用于将复合膜70传入的传入口22、和用于将复合膜70传出的传出口23。外壳21例如为金属制的外壳。对于驱动辊61,利用未图示的马达及控制部来控制旋转速度。
基于控制外壳21内部的温度及湿度的目的,干燥装置10还可具备温度传感器、湿度传感器及排气管道(duct)。
干燥装置10中,从节省空间的观点考虑,从传入口22至传出口23为止的复合膜70的传送长度优选为50m以下,更优选为40m以下,进一步优选为30m以下。另一方面,从确保干燥时间的观点考虑,所述传送长度优选为5m以上,更优选为10m以上。
在外壳21内部,干燥机构51、52、53及54排列的方向没有限定。例如,如图2所示,可以以使复合膜70在外壳21的上面附近和下面附近之间往返的方式排列,除此之外,例如,可以以使复合膜70在外壳21的左侧面附近和右侧面附近之间往返的方式排列。
干燥机构51具有1个加热辊和1个热风送风机构。干燥机构51具有的加热辊31和热风送风机构41被配置于例如相对于位于其间的复合膜70而呈对置的位置。加热辊31与热风送风机构41的位置关系并不限定为相对于位于其间的复合膜70而呈对置的位置,只要为从热风送风机构41送出的热风能吹到与加热辊31接触的复合膜70上的位置关系即可。
除了加热辊31及热风送风机构41以外,干燥机构51也可进一步具有向复合膜70施予热的其他放热机构(例如,远红外线照射机构等)。
干燥机构52~54、加热辊32~34及热风送风机构42~44的实施方式也与干燥机构51、加热辊31及热风送风机构41的实施方式同样。
图2中示出了具有4个干燥机构的干燥装置的例子,但干燥机构的个数并不限定于此,可选择1个或2个以上。图2中例示了1个干燥机构中相对于1个接触式加热机构具有1个热风送风机构的实施方式例,但1个干燥机构中也可相对于1个接触式加热机构具有2个以上热风送风机构。
加热辊31~34的外径例如为10cm~200cm。加热辊31~34的宽度优选根据要制造的复合膜的宽度而进行选择,例如为10cm~300cm。
作为加热辊31~34的外周面的材质,例如,可举出不锈钢、镀覆金属、陶瓷、硅橡胶、氟系树脂等。从抑制复合膜对加热辊31~34的附着的观点考虑,加热辊31~34的外周面优选含有氟系树脂。作为氟系树脂,例如,可举出聚四氟乙烯(PTFE)、全氟烷氧基氟树脂(PFA)、四氟乙烯·六氟丙烯共聚物(FEP)等。
从抑制在复合膜70中产生收缩、变形、褶皱的观点考虑,加热辊31~34的外周面的温度优选为105℃以下,更优选为100℃以下,进一步优选为95℃以下。另一方面,从使复合膜70干燥的观点考虑,所述温度优选为65℃以上。
加热辊31~34优选可各自控制外周面的温度。加热辊31~34的外周面的温度可全部相同,也可一部分相同,还可互不相同。
从抑制在复合膜70中产生收缩、变形、褶皱的观点考虑,优选将加热辊31~34分为外周面的温度不同的多个组。作为根据外周面的温度的异同而进行分组的例子,例如,可举出下述(i)~(iii)。以下的说明中,T31、T32、T33、及T34分别表示加热辊31的外周面的温度、加热辊32的外周面的温度、加热辊33的外周面的温度、及加热辊34的外周面的温度。
(i)将加热辊31作为第一组,将加热辊32及33作为第二组,将加热辊34作为第三组。加热辊32的外周面的温度与加热辊33的外周面的温度相同。
上述(i)的情况下,优选地,第二组的外周面的温度比第一组的外周面的温度高,且第三组的外周面的温度比第二组的外周面的温度低。即,优选为T31<T32=T33>T34的关系。第一组的外周面的温度与第三组的外周面的温度可以相同也可以不同,不同的情况下,优选第三组的外周面的温度比第一组的外周面的温度高。
(ii)将加热辊31及32作为第一组,将加热辊33及34作为第二组。加热辊31的外周面的温度与加热辊32的外周面的温度相同。加热辊33的外周面的温度与加热辊34的外周面的温度相同。
上述(ii)的情况下,优选地,第二组的外周面的温度比第一组的外周面的温度高。即,优选为T31=T32<T33=T34的关系。
(iii)将加热辊31作为第一组,将加热辊32作为第二组,将加热辊33作为第三组,将加热辊34作为第四组。
上述(iii)的情况下,优选地,第二组的外周面的温度比第一组的外周面的温度高,且第三组的外周面的温度比第二组的外周面的温度高,且第四组的外周面的温度比第三组的外周面的温度低。即,优选为T31<T32<T33>T34的关系。第一组的外周面的温度与第四组的外周面的温度可以相同也可以不同,不同的情况下,优选第四组的外周面的温度比第一组的外周面的温度高。第二组的外周面的温度可与第四组的外周面的温度相同或不同,不同的情况下,优选第四组的外周面的温度比第二组的外周面的温度高。
在上述(i)~(iii)中的任一情况下均优选的是,与构成位于复合膜的传送方向的最上游侧的第一组的加热辊的外周面的温度相比,构成作为在第一组下游侧邻接的组的第二组的加热辊的外周面的温度更高。
上文中,以加热辊的数量是4个的情况为例进行了说明,但干燥装置具备的加热辊的数量并不限定于此。可以根据干燥装置具备的加热辊的总个数对上述(i)~(iii)的各组中包含的加热辊的个数进行增减。
从抑制在复合膜70中产生收缩、变形、褶皱的观点、及抑制多孔质层的剥离的观点考虑,加热辊31~34相对于复合膜70的总接触长度优选为30m以下,更优选为20m以下,进一步优选为10m以下。另一方面,从干燥效率的观点考虑,所述总接触长度优选为1m以上,更优选为3m以上。所述总接触长度与干燥装置具备的加热辊的个数无关,优选为上述范围。
加热辊31~34可以为利用马达而旋转的驱动辊,也可以为随着复合膜70的传送而旋转的从动辊。
加热辊31~34为驱动辊的情况下,优选可各自控制旋转速度。从抑制在复合膜70中产生收缩、变形、褶皱的观点、及抑制多孔质层的剥离的观点考虑,优选将加热辊31~34的旋转速度调节至以加热辊31为基准的±5%以下的范围内。作为对加热辊31~34的旋转速度加以调节的例子,例如,可举出下述(a)及(b)。当然,加热辊31~34的旋转速度也可以完全相同。
(a)相对于加热辊31的旋转速度而言,将加热辊32的旋转速度调节为101%,将加热辊33的旋转速度调节为102%,将加热辊34的旋转速度调节为103%。
(b)相对于加热辊31的旋转速度而言,将加热辊32的旋转速度调节为101%,将加热辊33的旋转速度调节为101%,将加热辊34的旋转速度调节为100%。
接着,对热风送风机构41~44进行说明。热风送风机构41~44例如在具有吸气口(其吸入空气)和送风口(其吹出热风)的壳体(casing)的内部具备电热器或蒸汽加热器或热媒加热器、和送风用风扇(fan)。所述壳体例如具有与加热辊相对的圆弧状的曲面,在该曲面上配置有1个或多个送风口。所述壳体例如为金属制的壳体。
优选地,热风送风机构41~44将包含从送风口吹出的热风的暖气从吸气口吸入,并进行温度调节、露点调节,从而循环使用空气。
作为热风送风机构41~44具有的送风口,例如,可举出图3A及图3B所示的实施方式例。图3A及图3B为示出热风送风机构41具有的送风口的一例的示意图,其示出了设置于壳体41a中的与加热辊31相对的面上的送风口41b。就图3A所示的送风口41b而言,开口部的形状为圆形,以多个送风口呈格子状周期性地排列的方式设置。就图3B所示的送风口41b而言,开口部的形状为长方形(其在与复合膜70的传送方向正交的方向上较长),以多个送风口沿复合膜70的传送方向以规定的间隔排列的方式设置。
送风口41b的开口部与加热辊之间的距离例如为2cm~15cm,优选为5cm~10cm。
从送风口41b的送风方向优选为热风到达复合膜70的距离最短的方向,即,优选为将开口部与加热辊连接的最短距离的方向。
从抑制在复合膜70中产生收缩、变形、褶皱的观点、及抑制多孔质层的剥离的观点考虑,从热风送风机构41~44送出的热风在送风口处的温度优选为105℃以下,更优选为100℃以下,进一步优选为95℃以下。另一方面,从使复合膜70干燥的观点考虑,所述温度优选为65℃以上。
从抑制在复合膜70中产生收缩、变形、褶皱的观点、及抑制多孔质层的剥离的观点考虑,从热风送风机构41~44送出的热风在送风口处的风速优选为30m/sec以下,更优选为25m/sec以下。另一方面,从干燥效率的观点考虑,所述风速优选为5m/sec以上,更优选为10m/sec以上。
对于热风送风机构41~44而言,送风口处的热风的温度可以全部相同,也可以一部分相同,还可以互不相同。对于热风送风机构41~44而言,送风口处的热风的风速可以全部相同,也可以一部分相同,还可以互不相同。
在干燥装置10的下游侧的紧接着其的后方,可进一步设置有单独1个或多个加热辊,可使从干燥装置10传出的复合膜70与该加热辊接触,从而使其进一步干燥。
出于对复合膜70进行热缓和的目的,在干燥装置10的下游侧的紧接着其的后方,可设置有1个或多个加热辊。用于上述目的的加热辊优选外周面温度为60℃~130℃。
在干燥装置10的上游侧的紧接着其的前方,可设置有各自为1个或多个的上下一对夹持辊(其用于夹持复合膜70从而将水分从复合膜70中除去)、及/或空气喷嘴(其用于向复合膜70吹喷风从而将水分吹除)。
本公开文本的制造方法可采用下述的实施方式。
·作为涂布液制备工序的一部分,基于将异物从涂布液的制备用溶剂中除去的目的,在与树脂混合前进行使该溶剂通过过滤器的处理。该处理中使用的过滤器的保留粒径例如为0.1μm~100μm。
·在实施涂布液制备工序的箱体(tank)中设置搅拌机,利用搅拌机不断搅拌涂布液,抑制涂布液中的固态成分的沉降。
·使从涂布液制备工序向涂布工序输送涂布液的配管为循环式,使涂布液在配管内循环,从而抑制涂布液中的固态成分的凝集。该情况下,优选将配管内的涂布液的温度控制为恒定。
·在从涂布液制备工序向涂布工序输送涂布液的配管的中途设置过滤器,除去涂布液中的凝集物及/或异物。
·作为将涂布液从涂布液制备工序供给至涂布工序的泵,设置无脉动计量泵。
·在涂布工序的上游配置静电除去装置,将多孔质基材表面的静电除去。
·在涂布机构的周围设置外壳,保持涂布工序的环境清洁,另外,控制涂布工序的气氛的温度及湿度。
·在涂布机构的下游配置检测涂布量的传感器,校正涂布工序中的涂布量。
以下,对复合膜的多孔质基材及多孔质层进行详细说明。
[多孔质基材]
本公开文本中,多孔质基材是指在内部具有孔隙或空隙的基材。作为这样的基材,可举出:微多孔膜;由纤维状物形成的无纺布、纸等多孔性片材;在上述微多孔膜或多孔性片材上层叠1层以上的其他多孔性的层而成的复合多孔质片材;等等。本公开文本中,从复合膜的薄膜化及强度的观点考虑,优选为微多孔膜。微多孔膜是指下述膜:形成在内部具有大量微细孔并且这些微细孔被连接的结构,气体或液体可从一侧的面向另一侧的面通过的膜。
作为多孔质基材的材料,优选为具有电绝缘性的材料,有机材料及无机材料均可。
作为多孔质基材的材料,从向多孔质基材赋予关闭(shutdown)功能的观点考虑,优选为热塑性树脂。关闭功能是指下述功能:在将复合膜应用于电池隔膜的情况下,当电池温度升高时,构成材料熔化从而将多孔质基材的孔闭塞,由此阻断离子的移动,防止电池的热失控。作为热塑性树脂,熔点低于200℃的热塑性树脂是合适的,特别优选为聚烯烃。
作为多孔质基材,优选为包含聚烯烃的微多孔膜(称为“聚烯烃微多孔膜”。)。作为聚烯烃微多孔膜,例如,可举出现有的应用于电池隔膜的聚烯烃微多孔膜,优选从其中选择具有充分的力学特性和物质透过性的聚烯烃微多孔膜。
从呈现出关闭功能的观点考虑,聚烯烃微多孔膜优选包含聚乙烯,作为聚乙烯的含量,相对于聚烯烃微多孔膜的总质量而言,优选为95质量%以上。
对于聚烯烃微多孔膜而言,从赋予在暴露于高温时膜不容易发生破损的程度的耐热性的观点考虑,优选为包含聚乙烯和聚丙烯的聚烯烃微多孔膜。作为这样的聚烯烃微多孔膜,可举出聚乙烯和聚丙烯混合存在于1层中的微多孔膜。在这样的微多孔膜中,从同时实现关闭功能和耐热性这样的观点考虑,优选包含95质量%以上的聚乙烯和5质量%以下的聚丙烯。另外,从同时实现关闭功能和耐热性这样的观点考虑,还优选下述结构的聚烯烃微多孔膜:聚烯烃微多孔膜具有2层以上的层叠结构,至少1层包含聚乙烯,至少1层包含聚丙烯。
作为聚烯烃微多孔膜中包含的聚烯烃,重均分子量为10万~500万的聚烯烃是优选的。聚烯烃的重均分子量为10万以上时,可赋予微多孔膜充分的力学特性。另一方面,聚烯烃的重均分子量为500万以下时,微多孔膜的关闭特性良好,容易进行微多孔膜的成型。
作为聚烯烃微多孔膜的制造方法,可举出下述方法:将已熔融的聚烯烃树脂从T-模中挤出从而制成片材,对其进行结晶化处理,然后进行拉伸,接下来进行热处理,从而制成微多孔膜;将与液体石蜡等增塑剂一起熔融的聚烯烃树脂从T-模中挤出,将其冷却后制成片材,进行拉伸,然后提取增塑剂并进行热处理,从而制成微多孔膜;等等。
作为由纤维状物形成的多孔性片材,可举出由下述物质的纤维状物形成的无纺布、纸等多孔性片材,所述物质为:聚对苯二甲酸乙二醇酯等聚酯;聚乙烯、聚丙烯等聚烯烃;芳香族聚酰胺、聚酰亚胺、聚醚砜、聚砜、聚醚酮、聚醚酰亚胺等耐热性树脂;纤维素;等等。耐热性树脂是指熔点为200℃以上的树脂,或不具有熔点、分解温度为200℃以上的树脂。
作为复合多孔质片材,可举出在微多孔膜或由纤维状物形成的多孔性片材上层叠功能层而得到的片材。从可利用功能层进一步附加功能的观点考虑,这样的复合多孔质片材是优选的。作为功能层,例如,从赋予耐热性这样的观点考虑,可举出由耐热性树脂形成的多孔性的层、由耐热性树脂及无机填料形成的多孔性的层。作为耐热性树脂,可举出选自芳香族聚酰胺、聚酰亚胺、聚醚砜、聚砜、聚醚酮及聚醚酰亚胺中的1种或2种以上的耐热性树脂。作为无机填料,可举出:氧化铝等金属氧化物;氢氧化镁等金属氢氧化物;等等。作为复合化的方法,可举出:在微多孔膜或多孔性片材上涂布功能层的方法;利用粘接剂将微多孔膜或多孔性片材与功能层接合的方法;将微多孔膜或多孔性片材与功能层热压接的方法;等等。
从适于本公开文本的制造方法的适合性的观点考虑,多孔质基材的宽度优选为0.1m~3.0m。
从机械强度的观点考虑,多孔质基材的厚度优选为5μm~50μm。
对于多孔质基材在105℃下放置30分钟时的热收缩率而言,在MD方向上优选为10%以下,更优选为5%以下,在TD方向上优选为5%以下,更优选为3%以下。
从机械强度的观点考虑,多孔质基材的断裂伸长率在MD方向上优选为10%以上,更优选为20%以上,在TD方向上优选为10%以上,更优选为20%以上。多孔质基材的断裂伸长率通过在温度为20℃的气氛中、使用拉伸试验机以100mm/min的拉伸速度进行拉伸试验而求出。
从机械强度和物质透过性的观点考虑,多孔质基材的Gurley值(JIS P8117:2009)优选为50秒/100cc~800秒/100cc。
从机械强度、操作性及物质透过性的观点考虑,多孔质基材的孔隙率优选为20%~60%。
从物质透过性的观点考虑,多孔质基材的平均孔径优选为20nm~100nm。多孔质基材的平均孔径是按照ASTM E1294-89、使用Perm-Porometer测得的值。
[多孔质层]
本公开文本中,多孔质层是指下述层:形成在内部具有大量微细孔并且这些微细孔被连接的结构,气体或液体可从一侧的面向另一侧的面通过的层。
在将复合膜应用于电池隔膜时,多孔质层优选为可与电极粘接的粘接性多孔质层。与粘接性多孔质层仅存在于多孔质基材的一面相比,粘接性多孔质层存在于多孔质基材的两面是优选的。
多孔质层是涂布含有树脂的涂布液而形成的。因此,多孔质层含有树脂。从多孔化的观点考虑,多孔质层优选通过涂布含有树脂及填料的涂布液而形成。因此,多孔质层优选含有树脂及填料。填料可以是无机填料及有机填料中的任何。作为填料,从多孔质层的多孔化及耐热性的观点考虑,优选为无机粒子。以下,对涂布液及多孔质层中含有的树脂等成分进行说明。
[树脂]
对多孔质层中包含的树脂的种类没有限制。作为多孔质层中包含的树脂,优选为具有将填料固定化的功能的树脂(所谓的粘结剂树脂)。从适于湿式制法的适合性的观点考虑,多孔质层中包含的树脂优选为疏水性树脂。在将复合膜应用于电池隔膜的情况下,多孔质层中包含的树脂优选为在电解液中稳定、电化学稳定、具有将无机粒子固定化的功能并且能与电极粘接的树脂。多孔质层可包含1种树脂,也可包含2种以上的树脂。
作为多孔质层中包含的树脂,例如,可举出聚偏氟乙烯、聚偏氟乙烯共聚物、苯乙烯-丁二烯共聚物、丙烯腈、甲基丙烯腈等乙烯基腈类的均聚物或共聚物、聚环氧乙烷、聚环氧丙烷等聚醚类。其中,优选聚偏氟乙烯及聚偏氟乙烯共聚物(将它们称为“聚偏氟乙烯系树脂”。)。
作为聚偏氟乙烯系树脂,可举出:偏氟乙烯的均聚物(即聚偏氟乙烯);偏氟乙烯与其他可共聚的单体形成的共聚物(聚偏氟乙烯共聚物);它们的混合物。作为可与偏氟乙烯共聚的单体,例如,可举出四氟乙烯、六氟丙烯、三氟乙烯、三氯乙烯、氟乙烯等,可使用1种或2种以上。聚偏氟乙烯系树脂可通过乳液聚合或悬浮聚合来进行制造。
作为多孔质层中包含的树脂,从耐热性的观点考虑,优选为耐热性树脂(熔点为200℃以上的树脂,或不具有熔点、分解温度为200℃以上的树脂)。作为耐热性树脂,例如,可举出聚酰胺(尼龙)、全芳香族聚酰胺(芳族聚酰胺,aramid)、聚酰亚胺、聚酰胺酰亚胺、聚砜、聚酮、聚醚酮、聚醚砜、聚醚酰亚胺、纤维素、及它们的混合物。其中,从形成多孔结构的容易性、与无机粒子的粘结性、耐氧化性等观点考虑,优选为全芳香族聚酰胺。全芳香族聚酰胺中,从容易成型的观点考虑,优选为间位型全芳香族聚酰胺,特别优选为聚间苯二甲酰间苯二胺(poly(m-phenylene isophthalamide))。
[无机粒子]
多孔质层优选包含无机粒子作为填料。多孔质层中包含的无机粒子优选为在电解液中稳定、并且电化学稳定的无机粒子。多孔质层可包含1种无机粒子,也可包含2种以上的无机粒子。
作为多孔质层中包含的无机粒子,例如,可举出氢氧化铝、氢氧化镁、氢氧化钙、氢氧化铬、氢氧化锆、氢氧化铈、氢氧化镍、氢氧化硼等金属氢氧化物;二氧化硅、氧化铝、氧化锆、氧化镁等金属氧化物;碳酸钙、碳酸镁等碳酸盐;硫酸钡、硫酸钙等硫酸盐;硅酸钙、滑石等粘土矿物;等等。其中,从赋予阻燃性、除电效果的观点考虑,优选为金属氢氧化物及金属氧化物。无机粒子可以是经硅烷偶联剂等进行了表面修饰的无机粒子。
多孔质层中包含的无机粒子的粒子形状是任意的,可以是球形、椭圆形、板状、针状、无定形中的任何。从多孔质层的成型性、复合膜的物质透过性、及复合膜的滑动性的观点考虑,无机粒子的一次粒子的体积平均粒径优选为0.01μm~10μm,更优选为0.1μm~10μm。
多孔质层含有无机粒子时,无机粒子在树脂和无机粒子的总量中所占的比例例如为30体积%~90体积%。
多孔质层可含有有机填料、其他成分。作为有机填料,例如,可举出由交联聚(甲基)丙烯酸、交联聚(甲基)丙烯酸酯、交联聚硅氧烷、交联聚苯乙烯、交联聚二乙烯基苯、苯乙烯-二乙烯基苯共聚物交联物、聚酰亚胺、三聚氰胺树脂、酚醛树脂、苯基胍胺(benzoguanamine)-甲醛缩合物等交联高分子形成的粒子;由聚砜、聚丙烯腈、芳族聚酰胺、聚缩醛、热塑性聚酰亚胺等耐热性树脂形成的粒子;等等。
从机械强度的观点考虑,多孔质层的厚度在多孔质基材的一面上优选为0.5μm~5μm。
从机械强度、操作性及物质透过性的观点考虑,多孔质层的孔隙率优选为30%~80%。
从物质透过性的观点考虑,多孔质层的平均孔径优选为20nm~100nm。多孔质层的平均孔径是按照ASTM E1294-89、使用Perm-Porometer测得的值。
[复合膜的特性]
复合膜的厚度例如为5μm~100μm,在用于电池隔膜的情况下,例如为5μm~50μm。
从机械强度和物质透过性的观点考虑,复合膜的Gurley值(JIS P8117:2009)优选为50秒/100cc~800秒/100cc。
从机械强度、操作性及物质透过性的观点考虑,复合膜的孔隙率优选为30%~60%。
本公开文本中,复合膜的孔隙率利用下式求出。多孔质基材的孔隙率及多孔质层的孔隙率也同样利用下式求出。
孔隙率(%)={1-(Wa/da+Wb/db+Wc/dc+...+Wn/dn)/t}×100
Wa、Wb、Wc、...、Wn为构成材料a、b、c、...、n的质量(g/cm2),da、db、dc、...、dn为构成材料a、b、c、...、n的真密度(g/cm3),t为膜厚(cm)。
[复合膜的用途]
作为复合膜的用途,例如,可举出电池隔膜、电容器用膜、气体过滤器、液体过滤器等,作为特别合适的用途,可举出非水系二次电池用隔膜。
实施例
以下举出实施例来进一步具体地说明本发明的实施方式。以下的实施例中所示的材料、使用量、比例、处理步骤等可进行适当变更,只要不超出本公开文本的主旨即可。因此,本发明的实施方式的范围不应被以下所示的具体例进行限定性解释。
<测定方法、评价方法>
实施例及比较例中应用的测定方法及评价方法如下所述。
[膜厚]
多孔质基材的膜厚(μm)通过下述方式求出:使用接触式的厚度计(Mitutoyo公司的LITEMATIC),对10cm×30cm内的任意20处进行测定,取其平均值。测定端子使用直径为5mm的圆柱状端子,以测定中施加7g的载荷的方式进行调节。
[105℃下的热收缩率]
将多孔质基材以MD方向19cm×TD方向6cm的大小切出3片,将其作为试样。用夹具把持试样的一端,以MD方向成为重力方向的方式将试样悬挂于烘箱(将箱内温度保持在105℃)中,在无张力状态下放置30分钟。在30分钟的热处理之前和之后,分别测定试样的MD方向及TD方向上的长度,根据下述式,算出MD方向及TD方向的热收缩率(%),并算出3片试样的平均值。
热收缩率(%)=(热处理前的长度-热处理后的长度)÷热处理前的长度×100
[复合膜的干燥状态]
用红外线水分率测定仪测定复合膜的水分率,如下所述地对干燥状态进行分类。
A:水分率小于1%。
B:水分率为1%以上且小于3%。
C:水分率为3%以上且小于5%。
D:水分率为5%以上。
[复合膜的收缩]
在干燥工序的前后,测定复合膜的宽度,计算收缩率(%),并如下所述地进行分类。
A:收缩率小于3%。
B:收缩率为3%以上且小于5%。
C:收缩率为5%以上。
[复合膜的褶皱]
在刚刚实施干燥工序之后及卷绕之后,通过目视观察复合膜的外观,如下所述地对褶皱的产生进行分类。
A:没有褶皱。
B:在刚刚实施干燥工序之后有轻微的褶皱。褶皱通过卷绕被消除。
C:在刚刚实施干燥工序之后有褶皱。褶皱未通过卷绕被消除。
[多孔质层的剥离]
用缺陷检查机对复合膜进行检查,检出亮缺陷(比周边部分亮的部分)和暗缺陷(比周边部分暗的部分),根据其大小(最大直径)及每100m2复合膜中的个数,如下所述地对多孔质层的剥离进行分类。若多孔质层发生剥离,则剥离后的部分作为亮缺陷被检出。若剥离后的多孔质层附着于复合膜表面,则附着的部分作为暗缺陷被检出。
A:500μm以下的缺陷少于10个,5mm以下的缺陷少于1个。
B:500μm以下的缺陷为10个以上且少于50个,5mm以下的缺陷少于1个。
C:500μm以下的缺陷为50个以上,5mm以下的缺陷为1个以上。
<复合膜的制造>
[实施例1]
-干燥装置-
准备图2所示的干燥装置作为用于实施干燥工序的干燥装置。干燥装置的形态如下所述。
干燥装置在具有传入口及传出口的金属制外壳的内部具有4个干燥机构。4个干燥机构分别具有1个加热辊和1个热风送风机构,该加热辊和该热风送风机构被配置于相对于位于其间的复合膜而呈对置的位置。4个加热辊的外周面包含聚四氟乙烯。
4个热风送风机构在具有吸气口(其吸入空气)和送风口(其吹出热风)的壳体的内部具备电热器和送风用风扇。壳体的与加热辊相对的面为圆弧状的曲面,在该曲面上配置有送风口。热风送风机构具有的送风口以像图3A所示的实施方式例那样排列的方式配置。
加热辊的外周面的温度、从热风送风机构送出的热风在送风口处的温度及风速、加热辊相对于复合膜的总接触长度、以及干燥装置的传送长度及传送速度如表1所示。
-多孔质基材-
准备长条状的宽1m的聚乙烯微多孔膜(PE膜)作为多孔质基材。将该聚乙烯微多孔膜的物性示于表1。
-涂布液制备工序-
将聚间苯二甲酰间苯二胺(PMIA)溶解于溶剂(二甲基乙酰胺和三丙二醇的混合溶剂)中,并使氢氧化镁分散于其中,从而制备粘度为3000cP(厘泊)的涂布液。涂布液的组成(质量比)为聚间苯二甲酰间苯二胺∶氢氧化镁∶二甲基乙酰胺∶三丙二醇=4∶16∶48∶32。
-涂布工序、凝固工序-
将上文中得到的涂布液(液温为20℃)等量涂布于多孔质基材的两面,在多孔质基材的两面形成涂布层。将形成涂布层后的多孔质基材传送至凝固槽并浸渍于凝固液(水:二甲基乙酰胺:三丙二醇=40:36:24[质量比],液温为30℃)中,从而使涂布层中包含的树脂凝固,得到复合膜。
-水洗工序、干燥工序-
将复合膜在水温被控制为30℃的水浴中传送,进行水洗,使水洗后的复合膜通过干燥装置从而进行干燥。
连续地实施上述各工序,得到在聚乙烯微多孔膜的表里两面上具有多孔质层的复合膜。将制得的复合膜的品质评价的结果示于表1。此外,将其他实施例及比较例的结果也同样地示于表1。
[比较例1~4]
如表1所记载的那样变更干燥工序的各条件,除此之外,与实施例1同样地操作,制作复合膜。
[实施例2~7]
如表1所记载的那样变更干燥工序的各条件,除此之外,与实施例1同样地操作,制作复合膜。
[实施例8~10]
将多孔质基材变更为具有表1所记载的物性的聚乙烯微多孔膜(PE膜),并如表1所记载的那样变更干燥工序的各条件,除此之外,与实施例1同样地操作,制作复合膜。
[实施例11]
在涂布液制备工序中,将聚间苯二甲酰间苯二胺变更为聚偏氟乙烯(PVDF),除此之外,与实施例1同样地操作,制作复合膜。
[实施例12]
将多孔质基材变更为聚对苯二甲酸乙二醇酯无纺布(PET无纺布),除此之外,与实施例1同样地操作,制作复合膜。
将于2015年3月27日提出申请的日本申请号2015-67607的全部公开内容通过参照并入本说明书中。
本说明书中记载的所有文献、专利申请及技术标准通过参照被并入本说明书中,各文献、专利申请及技术标准通过参照被并入的程度与具体且分别地记载的情况的程度相同。
Claims (14)
1.复合膜的干燥装置,其是在多孔质基材的一面或两面上具有涂布层的复合膜的干燥装置,其具备具有接触式加热机构和热风送风机构的干燥机构,在对经水洗的所述复合膜进行传送的同时,使所述复合膜与所述接触式加热机构接触,并且使从所述热风送风机构送出的热风吹至所述复合膜,从而将水从所述复合膜中除去。
2.如权利要求1所述的复合膜的干燥装置,其中,所述复合膜的传送速度为30m/min以上。
3.如权利要求1或2所述的复合膜的干燥装置,所述干燥装置具备2个以上所述干燥机构,
在所述干燥装置中存在2个以上的所述接触式加热机构根据与所述复合膜接触的面的温度的异同而被分为2个以上的组。
4.如权利要求1或2所述的复合膜的干燥装置,其中,所述接触式加热机构从加热辊、加热带或热板中选择。
5.如权利要求1或2所述的复合膜的干燥装置,其中,所述接触式加热机构相对于所述复合膜的总接触长度为30m以下。
6.如权利要求1或2所述的复合膜的干燥装置,所述干燥装置具备具有传入口及传出口的外壳,所述干燥机构被配置于所述外壳的内部,从所述传入口至所述传出口为止的所述复合膜的传送长度为50m以下。
7.如权利要求1或2所述的复合膜的干燥装置,其中,所述接触式加热机构的与所述复合膜接触的面含有氟系树脂。
8.如权利要求1或2所述的复合膜的干燥装置,其中,所述热风送风机构具备电热器或蒸汽加热器或热媒加热器、和送风用风扇。
9.复合膜的制造装置,其具有:
涂布机构,其在多孔质基材的一面或两面上涂布含有树脂的涂布液而形成涂布层;
凝固机构,其包含凝固液;
水洗机构,其对使所述涂布层与所述凝固液接触而使所述树脂凝固而得到的复合膜进行水洗;和
权利要求1~8中任一项所述的干燥装置。
10.如权利要求9所述的复合膜的制造装置,其中,所述涂布机构从迈耶棒、模涂机、逆转辊涂布机或凹版涂布机中选择。
11.如权利要求9所述的复合膜的制造装置,其中,所述涂布机构包含隔着所述多孔质基材相对地配置的第一涂布机构和第二涂布机构,所述第一涂布机构对一侧的面进行涂布,所述第二涂布机构对另一侧的面进行涂布。
12.如权利要求9所述的复合膜的制造装置,其中,所述涂布机构包含在所述多孔质基材的传送方向上隔开间隔地配置的第一涂布机构和第二涂布机构,所述第一涂布机构对一侧的面进行涂布,所述第二涂布机构对另一侧的面进行涂布。
13.如权利要求9所述的复合膜的制造装置,其中,所述凝固机构为凝固槽。
14.如权利要求9所述的复合膜的制造装置,其中,所述水洗机构为水浴。
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KR20220052375A (ko) | 2022-04-27 |
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US20180111158A1 (en) | 2018-04-26 |
CN107405580A (zh) | 2017-11-28 |
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