CN106397738A - 一种延长环氧树脂固化时间的方法 - Google Patents
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Abstract
本发明属于材料技术领域，具体涉及一种延长环氧树脂固化时间的方法，具体的为，包括以下步骤：(1)将纳米介孔二氧化硅、固化剂和溶剂在容器内混合0.1‑12h，得混合料；(2)将混合料在0‑200℃下混合处理0.1‑24h；(3)向上述混合料中加入环氧树脂，混合均匀。本发明方法制备的环氧树脂可以使固化剂从环氧树脂孔道内部缓慢释放出来，从而实现延长固化时间的目的。
Description
技术领域
本发明属于材料技术领域，具体涉及一种延长环氧树脂固化时间的方法。
背景技术
环氧树脂(EP)广泛应用于机械、电器、电子、航空、航天、化工、交通运输、建筑等领域，是一种非常重要的高分子材料。目前环氧树脂与固化剂混合使用时，采取现用现配的方式，其原因在于，环氧树脂直接与固化剂混合时，需控制加料速度。加料过快，反应剧烈，热量集聚在环氧树脂内部，不易排出，造成局部糊化；若加料过慢，在使用前大部分环氧树脂已经固化，后期操作时间就会缩短，影响使用。综合以上情况，对环氧树脂的操作有很大要求，且对环氧树脂的使用造成了很大局限。ZL201110193050.2公开了一种二氧化硅改性环氧树脂固化剂及清漆制备方法，其是使用二氧化硅改性后的酯类化合物作为封端剂对固化剂进行封端，从而达到控制固化速度的目的，方法相对复杂。ZL201310563916.3公开了一种环氧树脂潜伏性固化剂及相应的环氧树脂涂料，其包括双氰胺、脲类衍生物、二氧化硅、石棉纤维、稀释剂等，脲类衍生物作为双氰胺的促进剂，其目的是使涂料的固化时间缩短。目前使用纳米介孔二氧化硅延长环氧树脂固化时间的研究还没有相关的报道。
发明内容
本发明主要提供了一种延长环氧树脂固化时间的方法，可以使固化剂从环氧树脂孔道内部缓慢释放出来，从而实现延长固化时间的目的。其技术方案如下：一种延长环氧树脂固化时间的方法，包括以下步骤：
(1)将纳米介孔二氧化硅、固化剂和溶剂在容器内混合0.1-12h，得混合料；
(2)将混合料在0-200℃下混合处理0.1-24h；
(3)向上述混合料中加入环氧树脂，混合均匀。
优选的，步骤(1)中纳米介孔二氧化硅、固化剂和溶剂的重量比为1:(0.1-100):(0.1100)。
优选的，纳米介孔二氧化硅、固化剂和溶剂的重量比为1:(0.1-20):(0.1-50)。
优选的，步骤(1)中所述溶剂选自水、甲醇、乙醇、正丁醇、三氯甲烷、二氯甲烷和石油醚中的一种或几种。
优选的，步骤(1)中所述固化剂为胺类固化剂。
优选的，步骤(2)中处理温度为20-80℃，时间为0.1-12h。
优选的，步骤(3)中混合料与环氧树脂的重量比为1:1-100。
优选的，步骤(3)中混合温度为0-100℃。
采用上述延长环氧树脂固化时间的方法，本发明具有以下优点：
本发明的方法利用介孔二氧化硅纳米粒子具有高比表面积、大孔容、吸附性好等特点，首先与固化剂进行混合，使其进入二氧化硅孔道内部，再将吸附了固化剂的二氧化硅与环氧树脂混合，使固化剂从环氧树脂孔道内部缓慢释放出来，从而实现延长固化时间的目的。
具体实施方式
实施例1
(1)将重量比1:3:3的纳米介孔二氧化硅、脂肪胺和乙醇在容器内混合0.5h，得混合料；(2)将混合料放于烘箱中70℃下混合干燥2h；(3)向上述混合料中加入12倍重量的环氧树脂，50℃混合均匀。所得环氧树脂的表干时间为360min。
实施例2
(1)将重量比1:100:70的纳米介孔二氧化硅、芳香胺和溶剂在容器内混合6h，得混合料；(2)将混合料放于烘箱中200℃下混合干燥0.1h；(3)向上述混合料中加入1倍重量的环氧树脂，100℃混合均匀。所得环氧树脂的表干时间为350min。
实施例3
(1)将重量比1:20:50的纳米介孔二氧化硅、固化剂和溶剂在容器内混合12h，得混合料；(2)将混合料放于烘箱中20℃下混合干燥24h；(3)向上述混合料中加入100倍重量的环氧树脂，20℃混合均匀。所得环氧树脂的表干时间为156min。
实施例4
(1)将重量比1:0.1:0.1的纳米介孔二氧化硅、固化剂和溶剂在容器内混合3h，得混合料；(2)将混合料放于烘箱中100℃下混合干燥12h；(3)向上述混合料中加入50倍重量的环氧树脂，0℃混合均匀。所得环氧树脂的表干时间为120min。
实施例5
(1)将重量比1:50:100的纳米介孔二氧化硅、固化剂和溶剂在容器内混合9h，得混合料；(2)将混合料放于烘箱中50℃下混合干燥3h；(3)向上述混合料中加入10倍重量的环氧树脂，0℃混合均匀。所得环氧树脂的表干时间为540min。
对比例1
将一定质量的固化剂直接加入到4倍质量的环氧树脂中，混合均匀。测其表干时间为68min。
对本领域的技术人员来说，可根据以上描述的技术方案以及构思，做出其它各种相应的改变以及形变，而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (8)
1.一种延长环氧树脂固化时间的方法，其特征在于：包括以下步骤：
(1)将纳米介孔二氧化硅、固化剂和溶剂在容器内混合0.1-12h，得混合料；
(2)将混合料在0-200℃下混合处理0.1-24h；
(3)向上述混合料中加入环氧树脂，混合均匀。
2.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(1)中纳米介孔二氧化硅、固化剂和溶剂的重量比为1:(0.1-100):(0.1100)。
3.根据权利要求2所述的延长环氧树脂固化时间的方法，其特征在于：纳米介孔二氧化硅、固化剂和溶剂的重量比为1:(0.1-20):(0.1-50)。
4.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(1)中所述溶剂选自水、甲醇、乙醇、正丁醇、三氯甲烷、二氯甲烷和石油醚中的一种或几种。
5.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(1)中所述固化剂为胺类固化剂。
6.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(2)中处理温度为20-80℃，时间为0.1-12h。
7.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(3)中混合料与环氧树脂的重量比为1:1-100。
8.根据权利要求1所述的延长环氧树脂固化时间的方法，其特征在于：步骤(3)中混合温度为0-100℃。
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| CN104292754A (zh) * | 2014-10-15 | 2015-01-21 | 中国航空工业集团公司基础技术研究院 | 一种环氧树脂的缓释固化方法 |
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| CN104292754A (zh) * | 2014-10-15 | 2015-01-21 | 中国航空工业集团公司基础技术研究院 | 一种环氧树脂的缓释固化方法 |
Non-Patent Citations (3)
| Title |
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| FEI XY, ET AL.: "Comparison of amino and epoxy functionalized SBA-15 used for carbonic", 《JOURNAL OF BIOSCIENCE AND BIOENGINEERING》 * |
| ROMANES M C, ET AL.: "Surface and subsurface characterization of epoxy-mesoporous silica composites to clarify tribological properties", 《WEAR》 * |
| 林晶晶: "聚合物/介孔硅功能复合材料的制备及性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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