CN110951100A - 一种树脂性能差异分布的自粘性阻燃预浸料的制备方法 - Google Patents
一种树脂性能差异分布的自粘性阻燃预浸料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，涉及复合材料技术领域，其步骤为：将环氧阻燃体系和环氧胶膜树脂体系的胶液置于涂膜设备上，分别涂膜，获得两种不同性能的树脂膜，作为预浸料的上、下胶膜；将上胶膜和下胶膜与纤维增强体复合，经加热板、热压辊、冷却板热处理后，覆PE膜得到具有自粘性的阻燃预浸料。本发明的有益效果为：通过采用性能差异的树脂体系制备获得同时具有自粘性和阻燃性的预浸料，在制备要求有阻燃性能的蜂窝夹层结构中无需加入额外的胶膜，而获得高滚筒剥离强度的夹层结构，提高了铺贴效率，同时满足多功能要求。该预浸料特别适合于制备要求有阻燃性能的夹层结构。
Description
技术领域
本发明涉及复合材料技术领域，具体涉及一种树脂性能差异分布的自粘性阻燃预浸料的制备方法。
背景技术
纤维增强树脂基复合材料具有高比强度、高比模量、耐腐蚀、耐烧蚀、抗疲劳和尺寸稳定等一系列优异性能，已在轨道交通、体育休闲领域及航空航天结构件中得到广泛的应用。预浸料是基体树脂与增强材料结合形成的复合材料中间状态产品，通过一定的铺层工艺和固化工艺形成一定结构形状、力学性能的复合材料。
阻燃环氧树脂预浸料由于其固化后具有良好的自熄性、低烟雾、低毒性，被广泛应用在轨道交通、航空内饰材料领域，如天花板、地板、墙板等，为减轻重量，内饰材料结构会采用蜂窝夹层结构。通常制备夹层结构时，对于无自粘性的预浸料，一般会在预浸料和蜂窝之间加入胶膜，来增加面板和蜂窝间的剥离强度。
常规阻燃体系预浸料由于其较高阻燃剂含量，且韧性不高，而不具有自粘性，直接与蜂窝复合剥离强度较低。制备夹层结构时胶膜的引入，一方面在生产工艺增加了成型工艺步骤，降低了生产效率，另一方面不具有阻燃性能的胶膜的引入会带来燃烧性能的增加。
发明内容
本发明的目的在于：提供一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，解决常规阻燃体系预浸料由于其较高阻燃剂含量，且韧性不高，而不具有自粘性，直接与蜂窝复合剥离强度较低，制备夹层结构时胶膜的引入，一方面在生产工艺增加了成型工艺步骤，降低了生产效率，另一方面不具有阻燃性能的胶膜的引入会带来燃烧性能的增加的问题。
本发明采用的技术方案如下：
一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，经以下步骤制备得到：
a)将环氧阻燃树脂体系胶液置于涂膜设备上，涂膜至离型纸上，冷却、覆PE膜，获得树脂膜一，作为预浸料的上胶膜；
b)将环氧胶膜树脂体系的胶液置于涂膜设备上，进行涂膜，冷却，获得树脂膜二，作为预浸料下胶膜；
c)将步骤a)中制备得到的上胶膜从预浸机的上胶辊中牵引出来，将步骤b)中制备得到的下胶膜从预浸机的下胶辊中牵引出来，然后上胶膜与纤维增强体的上表面复合，下胶膜与纤维增强体的下表面复合(所述预浸料的自粘性来自于环氧树脂胶膜体系，与纤维增强体复合后，要保证胶膜体系的树脂留在预浸料表面，即含浸程度相对低一些，故将下胶膜置于下表面。)；
d)复合后的整体经过加热板、热压辊、冷却板热处理后，将上层离型纸剥离，覆PE膜，即获得自粘性阻燃预浸料。
进一步地，所述环氧阻燃树脂体系包括阻燃剂，所述阻燃剂含量为15～50％，所述阻燃剂为磷环氧、磷腈、磷酸酯、聚磷酸铵、氢氧化铝、氢氧化镁、硼酸锌、三聚氰胺聚磷酸盐中的一种或多种的混合物。
进一步地，所述环氧胶膜树脂体系包括增韧剂，所述增韧剂的含量为20～35％，所述增韧剂为橡胶类增韧剂、纳米核壳橡胶树脂、热塑性树脂中的一种或多种的混合物，所述橡胶类增韧剂可以是端羧基丁腈橡胶、端氨基丁腈橡胶、端环氧基丁腈橡胶等，所述纳米核壳橡胶树脂可以是MX154、MX217、MX257等，所述热塑性树脂可以是聚醚砜、聚醚酮、苯氧树脂等。
进一步地，所述环氧阻燃树脂体系胶液70℃的粘度为20000cp～30000cp，所述环氧胶膜树脂体系胶液70℃的粘度为40000～60000cp。
进一步地，所述环氧阻燃树脂体系胶液120℃的凝胶时间为10～15min，所述环氧胶膜树脂体系胶液120℃的凝胶时间为10～15min，两种树脂体系功能性有差异，但反应活性要接近，利于固化过程增加界面结合强度。
进一步地，所述上胶膜和下胶膜的克重相同，且面密度均为70～110gsm，当树脂膜面密度低于此范围时，自粘性效果和阻燃性效果会降低。
进一步地，所述步骤d)中加热板和热压辊的温度在60～90℃，所述预浸料的自粘性来自于环氧树脂胶膜体系，与纤维增强体复合后，要保证胶膜体系的树脂留在预浸料表面，即含浸程度相对低一些，故含浸温度不能过高。
进一步地，所述步骤d)中热压辊间的间隙为0.06～0.30mm，较优的为0.08～0.25mm，压辊间隙过低，会使预浸料的含浸程度增加，自粘性降低；压辊间隙过大，可能会存在干纱，影响制品质量。
一种阻燃蜂窝夹层结构，所述夹层结构从上至下包括预浸料层、夹芯层、预浸料层，所述预浸料层的材质为按照权利要求1-8任一项所述制备方法制得的自粘性阻燃预浸料，两所述预浸料层覆有环氧胶膜一面与夹芯层贴合，覆有阻燃树脂膜的一面远离夹芯层朝外，使得具有自粘性一面与蜂窝夹心贴合，保证面板与蜂窝间的剥离强度。
综上所述，由于采用了上述技术方案，本发明的有益效果是：
本发明将环氧阻燃树脂体系和环氧胶膜树脂体系结合起来，利用各自的性能特性，在预浸料制备方法上进行改进，而获得具有自粘性的阻燃预浸料，在制备蜂窝夹层结构时将该预浸料直接与蜂窝复合，无需加入额外胶膜，获得高滚筒剥离强度的夹层结构，同时具备阻燃性，提高了夹层结构的制备效率，提高了铺贴效率，同时满足多功能要求，特别适用于制备要求有阻燃性能的夹层结构。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚完整地描述，显然，所描述的实施例仅仅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。
实施例1
(1)预浸料制备
环氧阻燃树脂和环氧胶膜树脂的粘度、凝胶时间数据见表1。
将环氧阻燃树脂FR201(自制)，体系内含有的阻燃剂为聚磷酸铵、硼酸锌、氢氧化铝，总含量为30％,在烘箱中烘烤至可流动状态，倒入涂膜设备中，制备克重为80gsm的树脂膜，调整涂膜间隙，通过红外线检测树脂膜面密度，冷却后覆PE膜，收卷，作为上胶膜备用。
环氧胶膜树脂体系树脂FA301(自制)，体系内含有增韧剂为端羧基丁腈橡胶，核壳橡胶树脂MX154、MX157，总含量为35％,在烘箱中烘烤至可倒入涂膜设备中，制备克重为80gsm的树脂膜，调整涂膜间隙，通过红外线检测树脂膜面密度，冷却后覆PE膜，收卷，作为下胶膜备用。
分别设定41热板80℃、43#热压辊85℃、45#热压辊70℃，43#压辊间隙为0.15mm，45#热压辊间隙为0.18mm，将上述步骤中制备得到的上胶膜从预浸机的上胶辊中牵引出来，下胶膜从预浸机的下胶辊中牵引出来，待温度达到设定温度后，将上下胶膜与300gsm的7781玻纤织物复合，经过加热板、热压辊热处理后，冷却，将上层离型纸剥离，覆PE膜，得到自粘性阻燃预浸料。
(2)夹层结构制备
制备面板为2层预浸料的夹层结构。将预浸料含有环氧胶膜树脂体系的一面与Nomex蜂窝贴合，含环氧阻燃树脂预浸料面向外。将此夹层结构置于压机上固化，在135℃、压力0.3MPa条件下保温60min，降温至50℃以下脱模。将上述夹层结构按滚筒剥离测试和航空阻燃测试标准要求切割，测试。
测试结果见表1。
实施例2
(1)预浸料制备
环氧阻燃树脂和环氧胶膜树脂的粘度、凝胶时间数据见表1。
将环氧阻燃树脂FR201(自制)，体系内含有的阻燃剂为聚磷酸铵、硼酸锌、氢氧化铝，总含量为30％，在烘箱中烘烤至可流动状态，倒入涂膜设备中，制备克重为100gsm的树脂膜，调整涂膜间隙，通过红外线检测树脂膜面密度，冷却后覆PE膜，收卷，作为上胶膜备用。
环氧胶膜树脂体系树脂FA301(自制)，体系内含有的增韧剂为端羧基丁腈橡胶，核壳橡胶树脂MX154、MX157，总含量为35％，在烘箱中烘烤至可倒入涂膜设备中，制备克重为100gsm的树脂膜，调整涂膜间隙，通过红外线检测树脂膜面密度，冷却后覆PE膜，收卷，作为下胶膜备用。
分别设定41热板80℃、43#热压辊85℃、45#热压辊70℃，3#压辊间隙为0.17mm，45#热压辊间隙为0.20mm，将上述步骤中制备得到的上胶膜从预浸机的上胶辊中牵引出来，下胶膜从预浸机的下胶辊中牵引出来，待温度达到设定温度后，将上下胶膜与300gsm的7781玻纤织物复合，经过加热板、热压辊热处理后，冷却，将上层离型纸剥离，覆PE膜，得到自粘性阻燃预浸料。
(2)夹层结构制备
制备面板为2层预浸料的夹层结构。将预浸料含有环氧胶膜树脂体系的一面与Nomex蜂窝贴合，含环氧阻燃树脂预浸料面向外。将此夹层结构置于压机上固化，在135℃、压力0.3MPa条件下保温60min，降温至50℃以下脱模。将上述夹层结构按滚筒剥离测试和航空阻燃60s垂直燃烧测试标准要求切割，测试。
测试结果见表1。
表1：树脂及阶层结构性能测试结果
备注：
(1)对比例中，含浸时预浸料的上、下胶膜均为环氧阻燃树脂体系。
(2)60s垂直燃烧标准要求：燃烧长度不超过152mm，自熄时间不超过15s，滴落物熄灭时间不超过3s。
对比以上表1数据，采用本发明中方法制备的预浸料，可提高夹层结构的滚筒剥离强度，同时阻燃性能能满足60s垂直燃烧要求。
尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，经以下步骤制备得到：
a)将环氧阻燃树脂体系胶液置于涂膜设备上，涂膜至离型纸上，冷却、覆PE膜，获得树脂膜一，作为预浸料的上胶膜；
b)将环氧胶膜树脂体系的胶液置于涂膜设备上，进行涂膜，冷却，获得树脂膜二，作为预浸料下胶膜；
c)将步骤a)中制备得到的上胶膜从预浸机的上胶辊中牵引出来，将步骤b)中制备得到的下胶膜从预浸机的下胶辊中牵引出来，然后上胶膜与纤维增强体的上表面复合，下胶膜与纤维增强体的下表面复合；
d)复合后的整体经过加热板、热压辊、冷却板热处理后，将上层离型纸剥离，覆PE膜，即获得自粘性阻燃预浸料。
2.根据权利要求1所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述环氧阻燃树脂体系包括阻燃剂，所述阻燃剂含量为15～50％，所述阻燃剂为磷环氧、磷腈、磷酸酯、聚磷酸铵、氢氧化铝、氢氧化镁、硼酸锌、三聚氰胺聚磷酸盐中的一种或多种的混合物。
3.根据权利要求1所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述环氧胶膜树脂体系包括增韧剂，所述增韧剂的含量为20～35％，所述增韧剂为橡胶类增韧剂、纳米核壳橡胶树脂、热塑性树脂中的一种或多种的混合物。
4.根据权利要求1或2所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述环氧阻燃树脂体系胶液70℃的粘度为20000cp～30000cp，所述环氧胶膜树脂体系胶液70℃的粘度为40000～60000cp。
5.根据权利要求4所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述环氧阻燃树脂体系胶液120℃的凝胶时间为10～15min，所述环氧胶膜树脂体系胶液120℃的凝胶时间为10～15min。
6.根据权利要求1所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述上胶膜和下胶膜的克重相同，且面密度均为70～110gsm。
7.根据权利要求1所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述步骤d)中加热板和热压辊的温度在60～90℃。
8.根据权利要求1所述的一种树脂性能差异分布的自粘性阻燃预浸料的制备方法，其特征在于，所述步骤d)中热压辊间的间隙为0.06～0.30mm。
9.一种阻燃蜂窝夹层结构，其特征在于，所述夹层结构从上至下包括预浸料层、夹芯层、预浸料层，所述预浸料层的材质为按照权利要求1-8任一项所述制备方法制得的自粘性阻燃预浸料，两所述预浸料层覆有环氧胶膜一面与夹芯层贴合，覆有阻燃树脂膜的一面远离夹芯层朝外。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0439335A (ja) * | 1990-06-06 | 1992-02-10 | Ube Nitto Kasei Co Ltd | 繊維強化熱可塑性樹脂複合材料 |
| CN104842619A (zh) * | 2015-05-06 | 2015-08-19 | 江苏恒神股份有限公司 | 高韧性多层结构预浸料制造工艺 |
| CN106893126A (zh) * | 2017-03-22 | 2017-06-27 | 江苏恒神股份有限公司 | 一种树脂差异分布的预浸料制备方法 |
-
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0439335A (ja) * | 1990-06-06 | 1992-02-10 | Ube Nitto Kasei Co Ltd | 繊維強化熱可塑性樹脂複合材料 |
| CN104842619A (zh) * | 2015-05-06 | 2015-08-19 | 江苏恒神股份有限公司 | 高韧性多层结构预浸料制造工艺 |
| CN106893126A (zh) * | 2017-03-22 | 2017-06-27 | 江苏恒神股份有限公司 | 一种树脂差异分布的预浸料制备方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112677580A (zh) * | 2021-01-06 | 2021-04-20 | 成都希瑞方晓科技有限公司 | 一种防火隔热板及其制备方法 |
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