CN111393697B - 一种层片式电容用离型膜及其制备方法 - Google Patents
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Abstract
本发明提供一种层片式电容用离型膜,制备原料包括:硅油8‑12份、溶剂70‑85份、催化剂0.5‑1.5份、锚固剂1‑2.5份、润滑剂5‑8份、有机胶1‑7份、有机胶固化剂0.2‑0.7份、无机胶1‑7份、无机胶固化剂0.2‑0.7份、延展剂3‑5份,有机胶选自烷基苯酚甲醛树脂、间苯二酚甲醛树脂、热固性烷基酚醛树脂中的至少一种,有机胶固化剂选自多聚甲醛或六亚甲基四胺的至少一种,无机胶选自纳米氧化铜‑磷酸无机胶或磷酸二氢铝无机胶,无机胶固化剂选自纳米氧化锆和纳米氧化锌的混合物。该离型膜具有优良的耐高温性能和平滑性,可避免其被擦花、划伤及受热而变形。本发明还提供上述层片式电容用离型膜的制备方法。
Description
技术领域
本发明涉及离型膜技术领域,尤其涉及一种层片式电容用离型膜及其制备方法。
背景技术
离型膜是与特定的材料在有限的条件下接触后不具有粘性,或轻微的粘性的膜材料。目前PET离型膜之所以具有离型效果,主要是因为表面涂布一层具有阻隔效果的硅油或者氟素硅油。
层片式电容(MLCC)所需的陶土层,是由液态陶土(即陶瓷浆)均匀流延涂布于离型膜表面,经高温干燥制得。离型膜主要作为流延涂布时承载陶土层用途,其离型面必须光滑和平滑,不能有擦花点和划伤的线等缺陷。其一,若离型膜在固化后因涂布局部不均,或因离型膜生产制备过程中与导辊接触时摩擦产生擦花点或直接划伤,导致MLCC在流延过程中,流延成型的表面出现细微的点缺陷或线缺陷、厚度不均等现象。因此,离型膜的涂层表面需具备较好的平滑性及低摩擦系数。其二,层片式电容(MLCC)的制备过程中,离型膜与陶瓷浆料进行烘干的过程中,温度升高,50um超薄的离型膜往往会受热而变形,会导致陶瓷浆料烘干后也固化变形,影响层片式电容(MLCC)的品质。
因此,非常有必要研发一种耐高温性能、低摩擦系数及平滑性优良的层片式电容用离型膜,以确保层片式电容(MLCC)的品质。
发明内容
本发明的目的之一是提供一种层片式电容用离型膜,该层片式电容用离型膜具有优良的耐高温性能和平滑性,避免该离型膜擦花、划伤及受热而变形。
本发明的目的之二是提供一种上述层片式电容用离型膜的制备方法。
为了实现上述目的,本发明提供了一种层片式电容用离型膜,按重量份数计,其制备原料包括:硅油8-12份、溶剂70-85份、催化剂0.5-1.5份、锚固剂1-2.5份、润滑剂5-8份、有机胶1-7份、有机胶固化剂0.2-0.7份、无机胶1-7份、无机胶固化剂0.2-0.7份、延展剂3-5份,其中,所述有机胶选自烷基苯酚甲醛树脂、间苯二酚甲醛树脂、热固性烷基酚醛树脂中的至少一种,所述有机胶固化剂选自多聚甲醛或六亚甲基四胺的至少一种,所述无机胶选自纳米氧化铜-磷酸无机胶或磷酸二氢铝无机胶,所述无机胶固化剂选自纳米氧化锆和纳米氧化锌的混合物。
本发明提供的层片式电容用离型膜的制备原料包括硅油、溶剂、催化剂、锚固剂、润滑剂、有机胶、有机胶固化剂、无机胶、无机胶固化剂、延展剂。有机胶选自烷基苯酚甲醛树脂、间苯二酚甲醛树脂、热固性烷基酚醛树脂中的至少一种,无机胶选自纳米氧化铜-磷酸无机胶或磷酸二氢铝无机胶,选用有机胶和无机胶的协同作用,并配合对应的有机胶固化剂和无机胶固化剂,使得膜层具有较大的剪切强度和较好的耐高温性能,避免离型膜受热变形。锚固剂的引用降低膜层表面张力,提高平滑性,延展剂的引入有助于降低摩擦系数,离型膜在受外力时,避免擦花和划伤。
较佳者,所述延展剂选自柔性环氧乙烯基树脂或聚氨酯树脂中的至少一种,优选采用柔性环氧乙烯基树脂,柔性乙烯基酯树脂与硅油形成膜层固化后具有延展性能好,受到应力后,会延长,韧性好。
较佳者,所述硅油选自聚(甲基苯基硅氧-二甲基硅氧)烷、聚甲基氢硅氧烷、二苯二氯硅烷、甲基三氯硅烷中的至少一种。
较佳者,所述溶剂选自甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯中的至少一种。优选地,可采用甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的混合物,且丁酮的用量大于其余各溶剂的用量,丁酮沸点为79.6℃,作为低沸点溶剂,能降低指硅油的黏度,有快干性,有利于薄膜在涂布硅油混合液后在高温烘箱中快速烘干。其中,甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的用量比可为1:1:2:4:1或1:2:2:3:1。
较佳者,所述催化剂选自铂碳催化剂、铂-钯炭双金属催化剂或氯钯酸催化剂中的至少一种。进一步,铂碳催化剂的平均粒径(μm)为30-60μm,铂含量为3%-6%。铂-钯炭双金属催化剂的平均粒径(μm)为35-60μm,铂含量为5%-12%。氯钯酸催化剂中,甲苯含量为40%-75%。
较佳者,所述锚固剂选自聚醚改性聚二甲基硅氧烷。
较佳者,所述有机胶与所述无机胶的用量比为2:1。
较佳者,所述润滑剂选自丙三醇或道康宁硅油中的至少一种。道康宁硅油或丙三醇的加入可减少离型膜与导辊之间的摩擦,避免离型膜表面擦花或划伤。
较佳者,纳米氧化锆和纳米氧化锌的粒径为80-200nm。
本发明还提供了一种层片式电容用离型膜的制备方法,其步骤包括:
(1)将硅油和溶剂加入容器A中搅拌均匀,搅拌速度为500-700r/min,搅拌时间为2-3min;
(2)于所述容器A中加入锚固剂、催化剂和润滑剂并搅拌均匀,得到混合物A,控制搅拌速度上升至900-1100r/min,搅拌2-3min;
(3)于容器B中加入有机胶、无机胶、有机胶固化剂、无机胶固化剂、延展剂并搅拌均匀,得到混合物B,搅拌速度为1100-1400r/min,搅拌20-30min;
(4)采用过滤网对所述混合物A进行过滤,得到滤液;
(5)将所述滤液与所述混合物B混合并搅拌均匀,得到离型液,搅拌速度为1100-1400r/min;
(6)将所述离型液涂布在基材表面,经过烘烤固化,制得层片式电容用离型膜。
较佳地,步骤(4)中采用800-1000目的过滤网,可有效地将混合物A中选用的铂碳催化剂或铂-钯炭双金属催化剂颗粒过滤出来。
较佳地,基材选用PBT、PET、PCL或PBAT中的一种。
较佳地,烘箱采用悬浮式烘箱,悬浮式烘箱通过空气流速与张力让薄膜悬浮在空中,减少涂布后的薄膜与导辊的接触,减少摩擦,从而减少擦花与刮伤。
较佳地,所述烘烤固化采用5节烘箱进行,第一节烘箱的温度为70-90度,第二节烘箱的温度为90-100度,第三节烘箱的温度为110-130度,第四节烘箱的温度为140-150度,第五节烘箱的温度为80-100度。可让离型液固化更充分,避免因剧烈固化而导致溶剂锁在离型层内部,产生气泡,影响性能。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案,但不构成对本发明的任何限制。
实施例1
层片式电容用离型膜,按重量份数计,其制备原料包括:
其中,所述溶剂选自甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的混合物,且甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的用量比为1:1:3:3:1。铂碳催化剂的平均粒径为在40μm,铂含量3%-6%。纳米氧化锆和纳米氧化锌的混合物中,纳米氧化锆和纳米氧化锌颗粒的粒径为100nm。
采用上述组分和含量的原料制备离型膜的方法,其步骤包括:
(1)将聚甲基氢硅氧烷和甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯加入容器A(如不锈钢桶)中,采用搅拌机进行搅拌,搅拌速度为700r/min,搅拌时间为3min;
(2)然后于容器A中加入聚醚改性聚二甲基硅氧烷,控制搅拌速度上升至900r/min,搅拌2min后,加入铂碳催化剂和丙三醇,继续搅拌3min,得到混合物A;
(3)于容器B中加入烷基苯酚甲醛树脂和纳米氧化铜-磷酸无机胶,混合均匀,然后加入多聚甲醛、纳米氧化锆和纳米氧化锌的混合物、柔性环氧乙烯基树脂并搅拌均匀,反应时间30min,得到混合物B,搅拌速度为1400r/min;
(4)采用1000目的过滤网对所述混合物A进行过滤,得到滤液;
(5)将所述滤液与所述混合物B混合并搅拌均匀,得到离型液,搅拌速度为1300r/min;
(6)将所述离型液经过130#线型号的微凹辊涂布在PBAT基材表面,涂布后,经悬浮式烘箱进行烘烤固化,采用5节烘箱进行固化,第一节烘箱的温度为90度,第二节烘箱的温度为100度,第三节烘箱的温度为130度,第四节烘箱的温度为150度,第五节烘箱的温度为100度,固化时间为3min,收卷制得卷状的层片式电容用离型膜。
实施例2
层片式电容用离型膜,按重量份数计,其制备原料包括:
其中,所述溶剂选自甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的混合物,且甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的用量比为1:1:2:4:1。铂-钯炭双金属催化剂的平均粒径为在60μm,铂含量5%-12%。纳米氧化锆和纳米氧化锌的混合物中,纳米氧化锆和纳米氧化锌颗粒的粒径为150nm。
本实施例层片式电容用离型膜的制备方法与实施例1相同,故,在此不做详细说明。
实施例3
本实施例层片式电容用离型膜的制备方法与实施例1基本相同,不同点在于:实施例3中延展剂采用聚氨酯树脂,实施例1中延展剂采用柔性环氧乙烯基树脂。
实施例4
层片式电容用离型膜,按重量份数计,其制备原料包括:
其中,铂-钯炭双金属催化剂的平均粒径为在40μm,铂含量5%-12%。纳米氧化锆和纳米氧化锌的混合物中,纳米氧化锆和纳米氧化锌颗粒的粒径为200nm。
本实施例层片式电容用离型膜的制备方法与实施例1相同,故,在此不做详细说明。
实施例5
本实施例层片式电容用离型膜的制备方法与实施例1基本相同,不同点在于:实施例5中有机胶采用间苯二酚甲醛树脂,实施例1中有机胶采用烷基苯酚甲醛树脂。
对比例1
本对比例层片式电容用离型膜的制备方法与实施例1基本相同,不同点在于:实施例1中含有机胶(烷基苯酚甲醛树脂),而对比例1中不含有机胶。
对比例2
本对比例层片式电容用离型膜的制备方法与实施例1基本相同,不同点在于:实施例1中含无机胶(纳米氧化铜-磷酸无机胶),而对比例2中不含无机胶。
对比例3
本对比例层片式电容用离型膜的制备方法与实施例1基本相同,不同点在于:实施例1中含有机胶(烷基苯酚甲醛树脂)和无机胶(纳米氧化铜-磷酸无机胶),而对比例3中不含有机胶和无机胶。
对实施例1-5和对比例1-4获得的层片式电容用离型膜进行耐高温测试,耐高温测试的结果见表1。
耐高温测试的检测方法:
(1)将实施例1-5制备的离型膜常温静置24H后,取A4纸大小的该卷状的离型膜的首膜(标记为Ai1),与该卷状离型膜的底膜(标记为Ai2)。i代表实施例的序号,如实施例1,则计作A11、A12;实施例2,则计作A21、A22,以此类推。对应地,对比例1-4中,离型膜的首膜(标记为Bi1),与该卷状离型膜的底膜(标记为Bi2),i代表对比例的序号,如对比例1,则计作B11、B12;对比例2,则计作B21、B22,以此类推。
(2)采用表面平整度测试仪分别测试上述样品Ai1、Ai2、Bi1和Bi2的初始平整度L0。
(3)将上述样品Ai1、Ai2、Bi1和Bi2放置在电热鼓风干燥箱中,设置温度为160度,静置30min后,取出后采用表面平整度测试仪进行第一次高温测试的平整度L1。
(4)继续将上述样品Ai1、Ai2、Bi1和Bi2放置在电热鼓风干燥箱中,设置温度为160度,静置1h后,取出后采用表面平整度测试仪进行第二次高温测试的平整度L2。
(5)依次按上述的方法,将上述样品Ai1、Ai2、Bi1和Bi2放置在电热鼓风干燥箱中,静置2h、4h后,取出后采用表面平整度测试仪进行第三、四次高温测试的平整度分别为L3和L4。
(6)可得到不同时间下的高温烘烤后的平整度及计算各自的平整度变化率(L4-L0)/(L0)×100%。
表1耐高温测试的结果
从表1的数据可知,通过本申请的原料及方法制备的离型膜具有优良的耐高温性能。对比实施例1-5与对比例1-3可知,实施例1-5的平整度变化率均远小于对比例1-3中的平整度变化率,本体系中有机胶和无机胶具有协同作用,可很好的提高离型膜的耐高温性能。从实施例1与实施例5的数据可知,有机胶采用间苯二酚甲醛树脂,其平整度变化率较小,可见,其耐温性能优于实施例1,原因可能是间苯二酚甲醛树脂中含有两个参与反应的酚基团,单分子中烷基苯酚甲醛树脂参与反应的基团只有一个,故间苯二酚甲醛树脂交联程度比烷基苯酚甲醛树脂大,形成三维网状结构越牢固,抵抗高温的能力越强。
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照最佳实施例对本发明做了详细的说明,但本发明并不局限于以上揭示的实施例,而应当涵盖各种根据本发明的本质进行的修改、等效组合。
Claims (10)
1.一种层片式电容用离型膜,其特征在于,按重量份数计,其制备原料包括:硅油8-12份、溶剂70-85份、催化剂0.5-1.5份、锚固剂1-2.5份、润滑剂5-8份、有机胶1-7份、有机胶固化剂0.2-0.7份、无机胶1-7份、无机胶固化剂0.2-0.7份、延展剂3-5份,其中,所述有机胶选自烷基苯酚甲醛树脂、间苯二酚甲醛树脂、热固性烷基酚醛树脂中的至少一种,所述有机胶固化剂选自多聚甲醛或六亚甲基四胺的至少一种,所述无机胶选自纳米氧化铜-磷酸无机胶或磷酸二氢铝无机胶,所述无机胶固化剂选自纳米氧化锆和纳米氧化锌的混合物。
2.如权利要求1所述的层片式电容用离型膜,其特征在于,所述延展剂选自柔性环氧乙烯基树脂或聚氨酯树脂中的至少一种。
3.如权利要求1所述的层片式电容用离型膜,其特征在于,所述硅油选自聚(甲基苯基硅氧-二甲基硅氧)烷、聚甲基氢硅氧烷中的至少一种。
4.如权利要求1所述的层片式电容用离型膜,其特征在于,所述溶剂选自甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯中的至少一种。
5.如权利要求4所述的层片式电容用离型膜,其特征在于,所述溶剂选自甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的混合物,且丁酮的用量大于其余各溶剂的用量,甲醇、乙二醇、正庚烷、丁酮、乙酸乙酯的用量比为1:1:2:4:1。
6.如权利要求1所述的层片式电容用离型膜,其特征在于,所述催化剂选自铂碳催化剂、铂-钯炭双金属催化剂或氯钯酸催化剂中的至少一种。
7.如权利要求1所述的层片式电容用离型膜,其特征在于,所述锚固剂选自聚醚改性聚二甲基硅氧烷。
8.如权利要求1所述的层片式电容用离型膜,其特征在于,所述有机胶与所述无机胶的用量比为2:1。
9.如权利要求1-8任一项所述的层片式电容用离型膜的制备方法,其特征在于,其步骤包括:
(1)将硅油和溶剂加入容器A中搅拌均匀,搅拌速度为500-700r/min;
(2)于所述容器A中加入锚固剂、催化剂和润滑剂并搅拌均匀,得到混合物A,控制搅拌速度上升至900-1100r/min;
(3)于容器B中加入有机胶、无机胶、有机胶固化剂、无机胶固化剂、延展剂并搅拌均匀,得到混合物B,搅拌速度为1100-1400r/min;
(4)采用过滤网对所述混合物A进行过滤,得到滤液;
(5)将所述滤液与所述混合物B混合并搅拌均匀,得到离型液,搅拌速度为1100-1400r/min;
(6)将所述离型液涂布在基材表面,经过烘烤固化,制得层片式电容用离型膜。
10.如权利要求9所述的层片式电容用离型膜的制备方法,其特征在于,所述烘烤固化采用5节烘箱进行,第一节烘箱的温度为70-90度,第二节烘箱的温度为90-100度,第三节烘箱的温度为110-130度,第四节烘箱的温度为140-150度,第五节烘箱的温度为80-100度。
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