CN118906611B - 一种应用于mlcc离型膜的基膜及其制备方法 - Google Patents
一种应用于mlcc离型膜的基膜及其制备方法 Download PDFInfo
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Abstract
本案涉及一种应用于MLCC离型膜的基膜及其制备方法，PET膜采用ABA三层结构共挤，纵向拉伸后经在先涂布后横向拉伸，最后牵引收卷而成；其中，A层原料包括70～90份的PET切片、10～30份的特种母粒；B层原料为PET切片；所述特种母粒由KH550改性无机填料和半芳香族聚酰胺制得。本发明采用ABA三层结构来制备PET薄膜，首先在A层结构中以PET为基础材料添加了特种母粒使得薄膜材料具有较优异的力学性能和耐热性能，同时还具有较低的粗糙度，避免了无机粒子析出的风险；此外，在纵向拉伸片上涂覆一层抗静电涂布液，涂层结合牢固，改善了薄膜的抗静电性能，可作为MLCC离型膜基膜使用。
Description
技术领域
本发明涉及聚酯薄膜技术领域，具体为一种应用于MLCC离型膜的基膜及其制备方法。
背景技术
目前，市面上用到的聚酯薄膜通常为聚对苯二甲酸乙二醇酯材料(PET)，是一种无色透明、有光泽的薄膜，机械性能良好，且具有较高的硬度和韧性，耐穿刺、耐摩擦能力优良，因而在电工绝缘膜、电容膜、离型膜、复合集流体膜、偏光片保护膜、包装膜等诸多领域。
在被用作离型膜、保护膜时，需要PET膜具有较低的表面粗糙度，具有一定的抗粘性和表面光滑性。针对此类高性能的要求，目前针对聚酯薄膜的改性技术方案有在其表层加入纳米级或微米级的无机粒子，例如二氧化硅、碳酸钙等以降低表面粗糙度；亦或是在薄膜表面涂覆含有微米级粒子的涂层，已改善薄膜表面张力。然而，目前现有的解决聚酯薄膜的技术方案仍然存在不足，添加无机粒子需要控制其尺寸和添加量，且得到的表面粗糙度仍然不能满足Ra≤15nm，并且无机粒子易团聚导致加工性能下降；而通过涂覆形成涂层虽然能够改善表面张力，但涂覆液中通常含有小分子有机成分，在后续加工过程中也易存在析出的风险。
发明内容
针对现有技术中的不足之处，本发明通过将无机填料与半芳香族聚酰胺复合，并将其添加至表层PET中形成ABA三层复合结构的PET膜，薄膜表面无机粒子分散性好，稳定性高，表面粗糙度得到有效降低；在粗糙度得到有效降低的基础上，在基膜制备过程中在先涂布一层抗静电涂布液，可进一步改善表面粗糙度，同时起到抗静电作用。
为实现上述目的，本发明提供如下技术方案：
一种应用于MLCC离型膜的基膜的制备方法，包括如下步骤：
S1、将计量的PET切片和特种母粒混合送入辅挤出机；将纯净的PET切片投入与结晶器中，以120～140℃预结晶15min，之后送入干燥塔干燥，干燥后送入主挤出机内；
S2、调整辅挤出机的温度为265～290℃，主挤出机温度为255～270℃，熔融后，计量挤出过滤；
S3、以辅挤出机挤出的物料为上下表层，以主挤出机挤出的物料为中间芯层，经过多层共挤出工艺制成ABA三层复合铸片；
S4、将铸片在65～90℃下预热，在90～110℃条件下经纵向拉伸3～3.5倍得到纵向拉伸片；
S5、采用辊涂的方式在纵向拉伸片的上下表面上涂覆一层抗静电涂布液，随后在90～120℃下预热，并在100～130℃条件下经横向拉伸3.5～4倍；拉伸完成后进行热定型，之后冷却牵引收卷，即得；
其中，所述特种母粒由20～40wt％KH550改性无机填料和60～80wt％半芳香族聚酰胺制得，在反应瓶中将半芳香族聚酰胺采用甲苯和乙醇的混合溶剂溶解，加入催化剂LHMDS混合均匀；将KH550改性无机填料在乙醇中分散均匀之后加入到反应瓶中，室温下搅拌30～90min，之后采用碳酸氢钠进行淬灭并过滤，滤饼采用丙酮和水洗涤后干燥，通过挤出机挤出造粒即得。
进一步地，所述KH550改性无机填料是将一定量的无机粒子置于5wt％的氢氧化钾溶液中活化处理，随后将处理后的无机粒子重新分散到去离子水中并加入等质量的KH550，在50℃下搅拌24h，过滤、洗涤、干燥、研磨而得；所述无机粒子为二氧化硅。
进一步地，所述半芳香族聚酰胺是由芳香族二元酸、脂肪族二元酸、含硅氧烷二胺单体、脂肪族二元胺以及含羟基的封端剂制备而成。
进一步地，所述脂肪族二元酸选自丁二酸、己二酸、庚二酸、戊二酸、丙二酸中的一种；所述芳香族二元酸选自2-溴对苯二甲酸或5-溴间苯二甲酸。
进一步地，所述含硅氧烷二胺单体为氨丙基封端聚二甲基硅氧烷，分子量400～1000；所述脂肪族二元胺选自1,2-二氨基-2-甲基丙烷、2,5-二甲基-2,5-己二胺、二甲基丙二胺、六亚甲基二胺、乙二胺中的一种。
进一步地，所述含羟基的封端剂为乙醇胺或邻羟基苯胺。
进一步地，所述芳香族二元酸、脂肪族二元酸、含硅氧烷二胺单体、脂肪族二元胺的摩尔比为3:2:1:4；所述含羟基的封端剂的用量为前述四类单体总质量的0.1～5wt％。
进一步地，所述ABA三层结构的原料用量比为A层：B层：A层＝10～20:60～80:10～20；A层中PET切片和特种母粒的质量之比为70～90:10～30。
进一步地，所述抗静电涂布液为包括如下重量份的组分：水性环氧树脂20～30份、2～6份聚噻吩、1～3份非离子型抗静电剂、1～3份相容剂、5～15份固化剂以及余量的水使总份数为100。
本发明提供一种如上所述的制备方法制得的应用于MLCC离型膜的基膜。
本申请制备了半芳香族聚酰胺作为功能性聚合物与无机填料复合形成特种母粒，无机填料是采用硅烷偶联剂改性的二氧化硅粒子，在无机粒子表面引入了氨基；半芳香族聚酰胺是由芳香族二元酸、脂肪族二元酸(2-溴对苯二甲酸或5-溴间苯二甲酸)、含硅氧烷二胺单体、脂肪族二元胺以及含羟基的封端剂为原料反应形成；通过聚合物中的溴与无机填料中的氨基反应将二氧化硅粒子接枝到聚合物链上形成刷状聚合物，末端羟基也能同氨基产生氢键效应，促进分子之间的相互作用和反应，进而改善了无机粒子的分散性，通过功能性聚合物与PET混合，具有良好地相容性，较好地解决了纳米材料在聚酯材料中团聚而难以分散的技术问题；同时与功能性聚合物复合后的无机粒子也很难从薄膜表面析出，提升了薄膜表面在加工使用过程中表面能的稳定性。
半芳香族聚酰胺具有优异的力学性能和耐热性能，将其引入到PET膜中可有效提升材料的耐热性；结合无机填料可有效提升膜的冲击强度，混合了特种母粒的PET作为纯净PET切片形成的中间芯层的外表层，与中间芯层协同作用，使薄膜的韧性得到提升；薄膜表面光滑，粗糙度低。在形成的三层复合结构的PET膜纵向拉伸片上再次涂覆一层涂布液，树脂材料选择环氧树脂与聚酰胺具有良好的相容性，表面附着力好，涂布液中添加有抗静电剂，起到抗静电作用。
与现有技术相比，本发明的有益效果是：本发明采用ABA三层结构来制备PET薄膜，首先在A层结构中以PET为基础材料添加了特种母粒使得薄膜材料具有较优异的力学性能和耐热性能，同时还具有较低的粗糙度，避免了无机粒子析出的风险；此外，在纵向拉伸片上涂覆一层抗静电涂布液，涂布液成分与PET膜表层中含有的半芳香族聚酰胺具有良好的相容性，涂层结合牢固，与表层配合，进一步降低了表面粗糙度，同时也改善了薄膜的抗静电性能，最终制得的PET基膜非常适合作为离型膜如MLCC离型膜基膜使用。
具体实施方式
下面将结合实施例对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
实施例：一种应用于MLCC离型膜的基膜的制备方法，包括如下步骤：
S1、将计量的PET切片和特种母粒混合送入辅挤出机；将纯净的PET切片投入与结晶器中，以120～140℃预结晶15min，之后送入干燥塔干燥，干燥后送入主挤出机内；
S2、调整辅挤出机的温度为265～290℃，主挤出机温度为255～270℃，熔融后，计量挤出过滤；
S3、以辅挤出机挤出的物料为上下表层，以主挤出机挤出的物料为中间芯层，经过多层共挤出工艺制成ABA三层复合铸片；
S4、将铸片在65～90℃下预热，在90～110℃条件下经纵向拉伸3～3.5倍得到纵向拉伸片；
S5、采用辊涂的方式在纵向拉伸片的上下表面上涂覆一层抗静电涂布液，随后在90～120℃下预热，并在100～130℃条件下经横向拉伸3.5～4倍；拉伸完成后进行热定型，之后冷却牵引收卷，即得；
其中，所述特种母粒由20～40wt％KH550改性无机填料和60～80wt％半芳香族聚酰胺制得，在反应瓶中将半芳香族聚酰胺采用甲苯和乙醇的混合溶剂溶解，加入催化剂LHMDS混合均匀；将KH550改性无机填料在乙醇中分散均匀之后加入到反应瓶中，室温下搅拌30～90min，之后采用碳酸氢钠进行淬灭并过滤，滤饼采用丙酮和水洗涤后干燥，通过挤出机挤出造粒即得。
实施例1：
按照上述工艺制备ABA三层结构PET膜，所述A层原料包括70份的PET切片、30份的特种母粒；所述B层原料为PET切片；原料用量比为A层：B层：A层＝10:80:10。
其中，所述特种母粒由20wt％KH550改性无机填料和80wt％半芳香族聚酰胺制得，在反应瓶中将半芳香族聚酰胺采用甲苯和乙醇的混合溶剂溶解，加入催化剂LHMDS混合均匀；将KH550改性无机填料在乙醇中分散均匀之后加入到反应瓶中，室温下搅拌30～90min，之后采用碳酸氢钠进行淬灭并过滤，滤饼采用丙酮和水洗涤后干燥，通过挤出机挤出造粒即得；
更进一步地，所述KH550改性无机填料是将一定量的无机粒子置于5wt％的氢氧化钾溶液中活化处理，随后将处理后的无机粒子重新分散到去离子水中并加入等质量的KH550，在50℃下搅拌24h，过滤、洗涤、干燥、研磨而得；所述无机粒子为二氧化硅。
所述半芳香族聚酰胺是由芳香族二元酸、脂肪族二元酸、含硅氧烷二胺单体、脂肪族二元胺以及封端剂制备而成的半芳香族聚酰胺。
在可供选择的实施例中，所述脂肪族二元酸选自丁二酸、己二酸、庚二酸、戊二酸、丙二酸中的一种；所述芳香族二元酸选自2-溴对苯二甲酸或5-溴间苯二甲酸。所述含硅氧烷二胺单体为氨丙基封端聚二甲基硅氧烷，分子量400～1000；所述脂肪族二元胺选自1,2-二氨基-2-甲基丙烷、2,5-二甲基-2,5-己二胺、二甲基丙二胺、六亚甲基二胺、乙二胺中的一种。
具体地，在本实施例中，以2-溴对苯二甲酸、丁二酸、氨丙基封端聚二甲基硅氧烷(1000)、乙二胺为原料，按照摩尔比为3:2:1:4称取各原料，将2-溴对苯二甲酸、丁二酸预先混合溶解在甲苯中，通入氮气，随后在机械搅拌下滴加己二胺，滴加完成后回流3h；之后再滴加含氨丙基封端聚二甲基硅氧烷的甲苯稀释液，滴加完成后继续回流2h；最后加入原料质量的1wt％的乙醇胺反应1-2h，将产生的混合物沉淀并用丙酮和水洗涤，烘干后即为功能性聚合物。
所述抗静电涂布液为包括如下重量份的组分：水性环氧树脂30份、5份聚噻吩、3份非离子型抗静电剂、2份相容剂、10份固化剂以及余量的水使总份数为100。
实施例2：
同实施例1，区别在于，原料用量比为A层：B层：A层＝20:60:20。
实施例3：
同实施例2，区别在于，所述A层原料包括80份的PET切片、20份的特种母粒。
实施例4：
同实施例2，区别在于，所述A层原料包括90份的PET切片、10份的特种母粒；所述B层原料为PET切片。
测试上述基膜的表面粗糙度、表面电阻以及涂层附着力。
将上述制得的基膜进行离线涂布离型剂，制备出MLCC用离型膜(GB/T25256-2010)。测试离型力，结果记录在表1中。
表1
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 纯PET膜 | |
| 表面粗糙度Ra(nm) | 10 | 7 | 8 | 12 | 27 |
| 表面电阻(Ω) | 7.1×1010 | 1.5×1010 | 3.4×1010 | 1.7×1011 | 1014 |
| 涂层附着力 | 1级 | 0级 | 0级 | 1级 | / |
| 残余接着率％ | 93.4 | 95.1 | 94.2 | 92.8 | 80.5 |
由表1可知，本申请制得的PET基膜具有较低的表面粗糙度，基膜与离型剂之间的粘结力好，离型层残余接着率高，适合作为MLCC离型膜的基膜使用。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。
Claims (9)
1.一种应用于MLCC离型膜的基膜的制备方法，其特征在于，包括如下步骤：
S1、将计量的PET切片和特种母粒混合送入辅挤出机；将纯净的PET切片投入与结晶器中，以120~140 ℃预结晶15 min，之后送入干燥塔干燥，干燥后送入主挤出机内；
S2、调整辅挤出机的温度为265~290 ℃，主挤出机温度为255~270 ℃，熔融后，计量挤出过滤；
S3、以辅挤出机挤出的物料为上下表层，以主挤出机挤出的物料为中间芯层，经过多层共挤出工艺制成ABA三层复合铸片；
S4、将铸片在65~90 ℃下预热，在90~110 ℃条件下经纵向拉伸3~3.5倍得到纵向拉伸片；
S5、采用辊涂的方式在纵向拉伸片的上下表面上涂覆一层抗静电涂布液，随后在90~120 ℃下预热，并在100~130 ℃条件下经横向拉伸3.5~4倍；拉伸完成后进行热定型，之后冷却牵引收卷，即得；
其中，所述特种母粒由20～40wt%KH550改性无机填料和60～80wt%半芳香族聚酰胺制得，在反应瓶中将半芳香族聚酰胺采用甲苯和乙醇的混合溶剂溶解，加入催化剂LHMDS混合均匀；将KH550改性无机填料在乙醇中分散均匀之后加入到反应瓶中，室温下搅拌30~90min，之后采用碳酸氢钠进行淬灭并过滤，滤饼采用丙酮和水洗涤后干燥，通过挤出机挤出造粒即得；
所述半芳香族聚酰胺的原料包括芳香族二元酸、脂肪族二元酸、含硅氧烷二胺单体、脂肪族二元胺以及含羟基的封端剂；
所述芳香族二元酸选自2-溴对苯二甲酸或5-溴间苯二甲酸。
2.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述KH550改性无机填料是将一定量的无机粒子置于5wt%的氢氧化钾溶液中活化处理，随后将处理后的无机粒子重新分散到去离子水中并加入等质量的KH550，在50℃下搅拌24h，过滤、洗涤、干燥、研磨而得；所述无机粒子为二氧化硅。
3.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述脂肪族二元酸选自丁二酸、己二酸、庚二酸、戊二酸、丙二酸中的一种。
4.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述含硅氧烷二胺单体为氨丙基封端聚二甲基硅氧烷，分子量400~1000；所述脂肪族二元胺选自1,2-二氨基-2-甲基丙烷、2,5-二甲基-2,5-己二胺、二甲基丙二胺、六亚甲基二胺、乙二胺中的一种。
5.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述含羟基的封端剂为乙醇胺或邻羟基苯胺。
6.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述芳香族二元酸、脂肪族二元酸、含硅氧烷二胺单体、脂肪族二元胺的摩尔比为3:2:1:4；所述含羟基的封端剂的用量为前述四类单体总质量的0.1~5wt%。
7.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述ABA三层结构的原料用量比为A层：B层：A层=10~20:60~80:10~20；A层中PET切片和特种母粒的质量之比为70~90:10~30。
8.根据权利要求1所述的应用于MLCC离型膜的基膜的制备方法，其特征在于，所述抗静电涂布液为包括如下重量份的组分：水性环氧树脂20~30份、2~6份聚噻吩、1~3份非离子型抗静电剂、1~3份相容剂、5~15份固化剂以及余量的水使总份数为100。
9.一种如权利要求1-8中任一项所述的制备方法制得的应用于MLCC离型膜的基膜。
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