CN115028805B - 一种快速固化的环氧室温固化剂及制备方法 - Google Patents
一种快速固化的环氧室温固化剂及制备方法 Download PDFInfo
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- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
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Abstract
本发明为一种快速固化的环氧室温固化剂及制备方法,其克服了现有技术中存在的环氧树脂在室温下固化速度慢的问题。本发明可在室温环境下使环氧涂层快速固化。本发明包括以下步骤:(1)将2,4,6—三(二甲胺基甲基)苯酚、卤代烷、乙醇混合物加热至30‑60℃、20‑50分钟;然后添加氢氧化钠水溶液,反应在60‑90℃,持续2‑4H;过滤盐,使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1;(2)将产物1,基础胺、硫脲按照顺序加入后在110‑130℃反应1h,液体由黄色浑浊变为黄色澄清液体,再反应3‑15min;(3)降温出料后得到快速固化的环氧室温固化剂。
Description
技术领域:
本发明属于环氧固化剂制备技术领域,涉及一种快速固化的环氧室温固化剂及制备方法。
背景技术:
环氧树脂作为一种热固性塑料,由于其高机械性能,低收缩率,低密度,出色的附着力,优异的功能性,优异的耐候性和耐化学性以及高的热稳定性,这些良好的性能使得环氧树脂广泛地应用于多种领域,包装电子设备,绝缘,涂料,复合材料,地板和防水等。环氧树脂分子本身是一种含有多个环氧基的具有热塑性的低分子量化合物,室温下是固体或者液体,熔点不高,在室温或者普通加热条件下都不会固化,不能直接单独使用。
一个完整的环氧树脂组成体系应该由四个方面成分组成:(1)树脂成分(环氧树脂和固化剂);(2)改性成分(增塑剂、增韧剂和填充剂);(3)调节流动性成分(稀释剂和触变剂);(4)其他成分。在实际应用时,不一定四个方面的成分都要同时具备,但树脂成分中的固化剂确是必不可少,在加入固化剂后,使其交联形成高度交联的三维网络状体型结构,才能使其各种优异性能显现出来。
环氧树脂固化剂的种类很多,根据固化剂使用温度范围可将其分为4种:低温固化剂、室温固化剂、中温固化剂与高温固化剂。低温固化剂指固化温度在5℃以下,常见的低温固化剂有聚硫醇型、改性胺及多异氰酸酯型固化剂等。室温固化剂的使用温度区间在5~50℃,其中多元胺类固化剂是常见的室温型固化剂,占目前固化剂总用量的71%。除此以外,还有一些自身与环氧树脂不直接发生化学反应的催化型环氧固化剂也可用于室温固化。中温固化剂的固化温度为50~100℃。固化温度在100℃以上的为高温固化剂,常见的高温型固化剂有芳香族多胺、酸酐、酚醛树脂、氨基树脂、双氰胺等。
环氧涂料和黏接剂等应用在一些例如土木建筑中与地面的情况,由于在这些场所涂膜不易加热,因此只能采用室温固化。常见的环氧树脂室温型固化剂有脂肪族多胺、脂环族多胺、改性芳香胺以及低分子酰胺等。现有的硫脲改性多元胺固化剂在17℃时涂膜的固化时间为7h,严重影响了环氧树脂作业的效率以及适用范围,也给环氧使用带来极大不便和极高的能耗,因此合成一种快速固化的环氧室温固化剂是很有必要的。且现有的改性多元胺固化剂采用分步加料,这势必会使气体从烧瓶中溢出,对操作者产生较大危害。
发明内容:
本发明的目的在于提供一种快速固化的环氧室温固化剂及制备方法,其克服了现有技术中存在的环氧树脂在室温下固化速度慢的问题。本发明可在室温环境下使环氧涂层快速固化。
为实现上述目的,本发明采用的技术方案为:
一种快速固化的环氧室温固化剂,其特征在于:采用下述质量份原料制备:
卤代烷20-45份
2,4,6—三(二甲胺基甲基)苯酚70-140份
基础胺固化剂30-50份
硫脲20-45份
乙醇70-120份
20%wt氢氧化钠20-50份。
卤代烷为1-氯丁烷、1-氯丙烷、碘甲烷中的任意一种。
基础胺固化剂为二乙烯三胺、己二胺、乙二胺、三乙烯四胺中的任意一种。一种快速固化的环氧室温固化剂的制备方法,其特征在于:包括以下步骤:
(1)将2,4,6—三(二甲胺基甲基)苯酚、卤代烷、乙醇混合物加热至30-60℃ 20-50分钟;然后添加氢氧化钠水溶液,反应在60-90℃,持续2-4H;过滤盐,使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1;
(2)将产物1,基础胺、硫脲按照顺序加入后在110-130℃反应1h,液体由黄色浑浊变为黄色澄清液体,再反应3-15min;
(3)降温出料后得到快速固化的环氧室温固化剂。
与现有技术相比,本发明具有的优点和效果如下:
(1)本发明固化剂颜色较为稳定,使用卤代烷作为改性剂DMP-30中酚羟基反应,DMP-30中的酚不易被氧化成对醌或邻醌变为更深的颜色。
(2)本发明在第二步合成固化剂时采用一锅法,改善现有的改性多元胺固化剂采用分步加料导致气体从烧瓶中溢出,对操作者产生较大危害。
(2)本发明固化速度快,大多数环氧室温固化剂在室温下涂膜固化速度较慢,而本发明可在室温环境下使环氧涂层快速固化。
具体实施方式:
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
本发明为一种环氧用室温快速固化固化剂,该室温固化剂包括如下质量份:
卤代烷20-45份
2,4,6—三(二甲胺基甲基)苯酚(DMP-30)70-140份
基础胺固化剂30-50份
硫脲20-45份
乙醇70-120份
20%wt氢氧化钠20份-50份
所述基础胺固化剂包括二乙烯三胺,己二胺,乙二胺,三乙烯四胺中的任意一种。
所述卤代烷包括1-氯丁烷,1-氯丙烷,碘甲烷中的任意一种
本发明还提供了一种环氧用室温快速固化固化剂的制备方法,该方法用于制备上述环氧用室温快速固化固化剂,包括如下步骤:
1.将DMP-30、1-氯丁烷,乙醇混合物加热至30-60℃20-50分钟。然后加入氢氧化钠水溶液,反应在60-90℃持续2-4H。过滤盐使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1。
2.将产物1,基础胺,硫脲按照顺序加入后在110-130℃反应1h,液体由黄色浑浊变为黄色澄清液体,再反应3-15min;
3.降温出料后得到环氧室温快速固化固化剂。
实施例1:
(1)将DMP-30 70g,1-氯丁烷24.64g和乙醇装入有磁力搅拌器,回流冷凝器和温度计的烧瓶中加热至40℃30分钟。然后添加32g氢氧化钠水溶液。反应在75℃持续2H。过滤盐使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1。
(2)将产物1,基础胺40克,硫脲35克按顺序加入三口烧瓶中,加入磁子,在可磁力搅拌的油浴锅中升温至115℃;保持在115℃反应1h,液体由浅黄色浑浊变为浅黄色澄清液体,继续反应7min;降温出料后得到环氧室温快速固化剂。
(3)降温出料后得到环氧室温快速固化固化剂。
实施例1实验例:
(1)称取10g E-51与固化剂于纸杯中,搅拌30s后,均匀涂抹于铁板上。
(2)记录杯中固化时间与铁板上固化时间。
实施例2:
(1)将DMP-30 115g,1-氯丁烷40g和乙醇装入有磁力搅拌器,回流冷凝器和温度计的烧瓶中加热至40℃30分钟。然后添加32g氢氧化钠水溶液。反应在75℃持续2H。过滤盐使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1。
(2)将产物1,基础胺40克,硫脲35克按顺序加入三口烧瓶中,加入磁子,在可磁力搅拌的油浴锅中升温至115℃;保持在115℃反应1h,液体由浅黄色浑浊变为浅黄色澄清液体,继续反应7min;
(3)降温出料后得到环氧室温快速固化剂。
实施例2实验例:
(1)称取10g E-51与固化剂于纸杯中,搅拌30s后,均匀涂抹于铁板上。
(2)记录杯中固化时间与铁板上固化时间。
实施例3:
(1)将DMP-30 140g,1-氯丁烷43.19g和乙醇装入有磁力搅拌器,回流冷凝器和温度计的烧瓶中加热至40℃30分钟。然后添加32g氢氧化钠水溶液。反应在75℃持续2H。过滤盐使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1。
(2)将产物1,基础胺40克,硫脲35克按顺序加入三口烧瓶中,加入磁子,在可磁力搅拌的油浴锅中升温至115℃;保持在115℃反应1h,液体由浅黄色浑浊变为浅黄色澄清液体,继续反应7min;
(3)降温出料后得到环氧室温快速固化剂。
实施例3实验例:
(1)称取10g E-51与固化剂于纸杯中,搅拌30s后,均匀涂抹于铁板上。
(2)记录杯中固化时间与铁板上固化时间。
以上所述,仅为本发明的较佳实施例而已,并非用于限定本发明的保护范围,凡是利用本发明的说明书内容所做的等同结构变化,均应包含在发明的专利保护范围内。
Claims (1)
1.一种快速固化的环氧室温固化剂的制备方法,其特征在于:采用下述质量份原料制备:
卤代烷20-45份
2,4,6—三(二甲胺基甲基)苯酚70-140份
基础胺固化剂30-50份
硫脲20-45份
乙醇70-120份
20%wt氢氧化钠20-50份;
卤代烷为1-氯丁烷;
基础胺固化剂为二乙烯三胺、己二胺、乙二胺、三乙烯四胺中的任意一种;
包括以下步骤:
(1)将2,4,6—三(二甲胺基甲基)苯酚、卤代烷、乙醇混合物加热至30-60℃20-50分钟;然后添加氢氧化钠水溶液,反应在60-90℃,持续2-4H;过滤盐,使用旋转蒸发仪在真空下除去乙醇,然后获得浅黄色液体产物1;
(2)将产物1,基础胺、硫脲按照顺序加入后在110-130℃反应1h,液体由黄色浑浊变为黄色澄清液体,再反应3-15min;
(3)降温出料后得到快速固化的环氧室温固化剂。
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US5321062A (en) * | 1992-10-20 | 1994-06-14 | Halliburton Company | Substituted alkoxy benzene and use thereof as wetting aid for polyepoxide resins |
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CN112898535A (zh) * | 2021-01-22 | 2021-06-04 | 上海众彦生物科技有限公司 | 一种环氧树脂用低温固化剂及其制备方法 |
CN114213648A (zh) * | 2021-12-27 | 2022-03-22 | 安徽壹石通材料科学研究院有限公司 | 一种可水解聚合物以及包含该聚合物的环氧树脂导热材料组合物 |
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