CN106320098B - 树脂复合云母纸及其制备方法 - Google Patents

树脂复合云母纸及其制备方法 Download PDF

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CN106320098B
CN106320098B CN201610805815.6A CN201610805815A CN106320098B CN 106320098 B CN106320098 B CN 106320098B CN 201610805815 A CN201610805815 A CN 201610805815A CN 106320098 B CN106320098 B CN 106320098B
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马西健
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Wuhu Saunaking Electronic Technology Co Ltd
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Abstract

本发明公开了一种树脂复合云母纸，包括云母层的制备、树脂层的制备以及云母层与树脂层的树脂复合；其中，树脂层的制备包括：先将酚醛环氧树脂、聚酰亚胺树脂、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水混合，接着进行热处理，最后挤出成型制得树脂层；树脂复合包括：将云母纸置于所述树脂层上方，先进行热压树脂复合，再进行自然冷却，得到树脂复合云母纸。该树脂复合云母纸除了具有云母纸绝缘、耐高温等优良特性外还具有很高的机械强度和韧性。

Description

树脂复合云母纸及其制备方法
技术领域
本发明涉及云母纸，具体涉及树脂复合云母纸及其制备方法。
背景技术
云母是一类含水铝硅酸盐类的总称，云母具有绝缘、耐高温等优良特性，在涂料、油漆、消防以及电气行业具有很广泛的应用。其中将云母制成云母纸是目前云母最广泛的应用途径之一。
目前，云母纸已具备片云母制品相对应的全部品种。工业上主要利用云母纸的绝缘性和耐热性，以及抗酸碱性用做作电气设备和电工器材的绝缘材料。但是，直接由云母片制得的云母纸的机械强度以及韧性都不好，不能满足多领域行业应用。
发明内容
本发明的目的是提供一种树脂复合云母纸，该树脂复合云母纸除了具有云母纸绝缘、耐高温等优良特性外还具有很高的机械强度和韧性。
为了实现上述目的，本发明提供了一种树脂复合云母纸，包括云母层的制备、树脂层的制备以及云母层与树脂层的树脂复合；
其中，云母层的制备包括：先将云母片水洗、烘干得到干云母片；接着将干云母片进行煅烧得到云母粉；再将云母粉、聚丙烯酰胺、乙二胺四乙酸与水进行搅拌混合制得云母纸浆；最后将云母纸浆抄造制得云母纸，云母纸为云母层；
树脂层的制备包括：先将酚醛环氧树脂、聚酰亚胺树脂、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水混合，接着进行热处理，最后挤出成型制得树脂层；
所述树脂复合包括：将云母纸置于所述树脂层上方，先进行热压树脂复合，再进行自然冷却，得到树脂复合云母纸。
本发明中，为了提高所制得树脂复合云母纸机械强度和韧性，优选地，相对于100重量份的水，云母片的用量为251-300重量份，聚丙烯酰胺的用量为5-10重量份，乙二胺四乙酸的重量份为4-10重量份。
为了提高所制得树脂层得性能，优选地，相对于100重量份的酚醛环氧树脂，聚酰亚胺树脂的用量为50-100重量份，乙二醇乙醚的用量为10-15重量份，醇脂十二的用量为1-5重量份，邻苯二甲酸二丁酯的用量为1-5重量份，水的用量为100-150重量份。
为了保证云母纸和树脂层的复合效果，优选地，热压复合的温度为170-175℃，热压复合的时间为3-4h；热压复合的压力为13-14MPa。
本发明中，为了提高云母纸的成型效果，将所用的云母片先进行水洗，优选地，水洗工序直至水的浊度≤12°为止，所述水洗工序中的液固比为4-6，水洗次数为2-3次。
本发明中，为了提高云母纸的成型效果，优选地，所用云母粉的规格为100-200目。
所用树脂的重均分子量可以在宽的范围内选择，但是为了使制得树脂复合云母纸具有更好地韧性，优选地，聚丙烯酰胺的重均分子量为0.5万-2.5万，所述酚醛环氧树脂的重均分子量为2万-4万、聚酰亚胺树脂的重均分子量为3万-5万。
在树脂层的制备过程中，为了提高树脂层的制备效果，优选地，热处理的温度为180-200℃，热处理的时间为0.5-1.5h。
本发明还提供了一种上述制备方法制得的树脂复合云母纸。
通过上述技术方案，本发明通过将云母纸与树脂层进行热压复合得到树脂复合云母纸。在云母纸的制备过程中，以云母片为主要的原料，加入了聚丙烯酰胺、乙二胺四乙酸作为助剂，增加了原料的成浆效果进而促进了云母纸的成型。而在树脂层的制备过程中以酚醛环氧树脂、聚酰亚胺树脂作为主要的树脂原料，而酚醛环氧树脂具有很强的耐高温性能并且具有很强的粘结性能有利于树脂层与云母纸层的复合。
本发明的其他特征和优点将在随后的具体实施方式部分予以详细说明。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
以下将通过实施例对本发明进行详细描述。
实施例1
1)云母粉(120目)、聚丙烯酰胺(重均分子量为0.5万)、乙二胺四乙酸与水按照重量配比为255：5：5：100进行搅拌混合制得云母纸浆；最后将所述的云母纸浆抄造制得云母纸，所述云母纸为云母层；在1)之前，将液固比为4的水清洗云母片直至水的浊度为11°，水洗3遍。
2)先将酚醛环氧树脂(重均分子量为2万)、聚酰亚胺树脂(重均分子量为3万)、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水按照重量配比为100：50：10：1：1：100进行混合，接着在180℃进行热处理1.5h，最后挤出成型制得树脂层。
3)将制得的云母纸置于制得的树脂层上方，在170℃下，压力选择13MPa进行热压复合4h，接着进行自然冷却，即得到所述树脂复合云母纸记作A1。
实施例2
1)云母粉(180目)、聚丙烯酰胺(重均分子量为2.0万)、乙二胺四乙酸与水按照重量配比为280：8：8：100进行搅拌混合制得云母纸浆；最后将所述的云母纸浆抄造制得云母纸，所述云母纸为云母层；在1)之前，将液固比为5的水清洗云母片直至水的浊度为10°，水洗3遍。
2)先将酚醛环氧树脂(重均分子量为3万)、聚酰亚胺树脂(重均分子量为4万)、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水按照重量配比为100：80：13：3：3：130进行混合，接着在190℃进行热处理1.0h，最后挤出成型制得树脂层。
3)将制得的云母纸置于制得的树脂层上方，在172℃下，压力选择13MPa进行热压复合4h，接着进行自然冷却，即得到所述树脂复合云母纸记作A2。
实施例3
1)云母粉(200目)、聚丙烯酰胺(重均分子量为2.5万)、乙二胺四乙酸与水按照重量配比为300：10：10：100进行搅拌混合制得云母纸浆；最后将所述的云母纸浆抄造制得云母纸，所述云母纸为云母层；在1)之前，将液固比为5的水清洗云母片直至水的浊度为12°，水洗3遍。
2)先将酚醛环氧树脂(重均分子量为4万)、聚酰亚胺树脂(重均分子量为5万)、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水按照重量配比为100：95：15：5：5：150进行混合，接着在200℃进行热处理0.5h，最后挤出成型制得树脂层。
3)将制得的云母纸置于制得的树脂层上方，在175℃下，压力选择14MPa进行热压复合3h，接着进行自然冷却，即得到所述树脂复合云母纸记作A3。
对比例1
按照实施例1的方法制得树脂复合云母纸B1，所不同的是云母粉(120目)、聚丙烯酰胺(重均分子量为0.5万)、乙二胺四乙酸与水按照重量配比为255：0：5：100。
对比例2
按照实施例1中步骤1)的方法制得云母纸B2，不同的是没有与树脂层复合。
对比例3
按照实施例2中步骤1)的方法制得云母纸B3，不同的是没有与树脂层复合。
对比例4
按照实施例3中步骤1)的方法制得云母纸B4，不同的是没有与树脂层复合。
检测例1
将复合云母纸A1-A3以及B1-B3先在150℃下处理2h，然后再于-15℃下处理2h，最后按照国标GB/T13022-91的方法进行抗拉强度(Rm/MPa)和收缩率(δ/％)的参数测试，具体结果见表1。
Rm/Mpa δ/％
A1 61.2 2.1
A2 59.5 2.3
A3 60.1 2.0
B1 55.6 3.3
B2 53.1 3.2
B3 42.5 4.5
B4 43.5 4.3
本发明提供的高强度云母纸在经过高温150℃和低温-15℃处理后其抗拉强度仍达到60MPa左右，表明本发明提供的高强度云母纸具有很高的机械强度。弥补了云母纸在应用过程中的机械强度差的缺陷。另外，经测试本发明提供的高强度云母纸在弯曲弧度大于45度小于80度时无断裂出现，弯折时无异响，表明其具有很好的韧性。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明的思想，其同样应当视为本发明所公开的内容。

Claims (6)

1.一种树脂复合云母纸的制备方法，其特征在于，包括云母层的制备、树脂层的制备以及云母层与树脂层的树脂复合；
其中，所述云母层的制备包括：先将云母片水洗、烘干得到干云母片；接着将所述干云母片进行煅烧得到云母粉；再将所述云母粉、聚丙烯酰胺、乙二胺四乙酸与水进行搅拌混合制得云母纸浆；最后将所述的云母纸浆抄造制得云母纸，所述云母纸为云母层；
所述树脂层的制备包括：先将酚醛环氧树脂、聚酰亚胺树脂、乙二醇乙醚、醇脂十二、邻苯二甲酸二丁酯和水混合，接着进行热处理，最后挤出成型制得树脂层；
所述树脂复合包括：将所述云母纸置于所述树脂层上方，先进行热压树脂复合，再进行自然冷却，得到所述树脂复合云母纸；
所述热压树脂复合的温度为170-175℃，热压树脂复合的时间为3-4h，
所述热压树脂复合的压力为13-14MPa；
相对于100重量份的水，所述云母片的用量为251-300重量份，所述聚丙烯酰胺的用量为5-10重量份，所述乙二胺四乙酸的重量份为4-10重量份，相对于100重量份的酚醛环氧树脂，所述聚酰亚胺树脂的用量为50-100重量份，所述乙二醇乙醚的用量为10-15重量份，所述醇脂十二的用量为1-5重量份，所述邻苯二甲酸二丁酯的用量为1-5重量份，所述水的用量为100-150重量份。
2.根据权利要求1所述的制备方法，其中，所述水洗工序直至水的浊度≤12°为止，所述水洗工序中的液固比为4-6，水洗次数为2-3次。
3.根据权利要求1所述的制备方法，其中，所述云母粉的规格为100-200目。
4.根据权利要求3所述的制备方法，其中，所述聚丙烯酰胺的重均分子量为0.5-2.5万，所述酚醛环氧树脂的重均分子量为2-4万、聚酰亚胺树脂的重均分子量为3-5万。
5.根据权利要求4所述的制备方法，其中，所述热处理的温度为180-200℃，热处理的时间为0.5-1.5h。
6.一种树脂复合云母纸，其特征在于，所述树脂复合云母纸由权利要求1-5中任意一项所述的制备方法制备而得。
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