CN112898535A - 一种环氧树脂用低温固化剂及其制备方法 - Google Patents
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- 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
- C08G59/40—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 characterised by the curing agents used
- C08G59/50—Amines
- C08G59/56—Amines together with other curing agents
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- 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
- C08G59/40—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 characterised by the curing agents used
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
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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
- C08G59/40—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 characterised by the curing agents used
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Abstract
本发明提供了一种环氧树脂用低温固化剂及其制备方法，属于低温固化剂领域，该低温固化剂包括基础胺固化剂、硫脲和促进剂。本发明可在低温环境下快速固化环氧树脂，能较快的固化并具有强度，便于施工提高效率，适用于混凝土、石板、陶瓷等粘接加固和建筑物防水修补加固工程等领域。
Description
技术领域
本发明属于低温固化剂技术领域，尤其涉及一种环氧树脂用低温固化剂及其制备方法。
背景技术
环氧树脂是一种高分子聚合物，分子式为(C11H12O3)n，是指分子中含有两个以上环氧基团的一类聚合物的总称。它是环氧氯丙烷与双酚A或多元醇的缩聚产物。由于环氧基的化学活性，可用多种含有活泼氢的化合物使其开环，固化交联生成网状结构，因此它是一种热固性树脂。在混凝土、石板、陶瓷等粘接加固和建筑物防水修补加固工程等领域施工时，常常处于低温环境，环氧树脂固化效果差，甚至不固化。
为此，提供一种环氧树脂用低温固化剂及其制备方法，以解决目前市场上的环氧树脂固化剂在低温环境中不易固化的问题。
发明内容
本发明实施例提供一种环氧树脂用低温固化剂及其制备方法，旨在解决背景技术中提出的问题。
本发明实施例是这样实现的，一种环氧树脂用低温固化剂，该低温固化剂包括如下以质量份数计的组分：
基础胺固化剂 68-80份；
硫脲 15-24份；
促进剂 5-9份。
优选的，所述基础胺固化剂包括乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中的任意一种或乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中至少两种组分的组合物。
优选的，所述硫脲为工业级硫脲。
优选的，所述促进剂包括DMP-30、壬基酚和苯甲醇中的任意一种或DMP-30、壬基酚和苯甲醇中至少两种组分的组合物。
一种环氧树脂用低温固化剂的制备方法，该方法用于制备上述的低温固化剂，包括如下步骤：
S1、将基础胺固化剂置于带搅拌器的三口烧瓶，升温至72-80℃进行搅拌；
S2、保持在72-80℃温度下，分3-4次向三口烧瓶内添加硫脲，时间控制在2.5-3h；
S3、硫脲加毕后，保持温度为85-88℃继续反应2h；
S4、反应完成后，调节温度至60-65℃，向三口烧瓶内加入促进剂，搅拌混合30min；
S5、降温后出料得到成品固化剂。
优选的，所述搅拌器的转速为85-95r/min。
优选的，所述出料的固化剂的温度为35-40℃。
本发明可在低温环境下快速固化环氧树脂，能较快的固化并具有强度，便于施工提高效率，适用于混凝土、石板、陶瓷等粘接加固和建筑物防水修补加固工程等领域。
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以解释本发明，并不用于限定本发明。
实施例1
将69克基础胺固化剂加入到带搅拌的三口烧瓶中，调节温度在72-80℃，开启搅拌，控制转速约85-95转/分；调节温度在72-80℃，分4次加入23克硫脲，时间在2.5-3小时，后调节温度在85-88℃，继续反应2小时；调节温度在60-65℃，一次性加入8克促进剂，搅拌混合30分钟，降温到35-40℃，出料即制得固化剂。
将该固化剂与环氧树脂配合在5℃环境下使用，90分钟固化，160分钟具有一定的粘结强度。
实施例2
将79克基础胺固化剂加入到带搅拌的三口烧瓶中，调节温度在72-80℃，开启搅拌，控制转速约85-95转/分；调节温度在72-80℃，分4次加入15克硫脲，时间在2.5-3小时，后调节温度在85-88℃，继续反应2小时；调节温度在60-65℃，一次性加入6克促进剂，搅拌混合30分钟，降温到35-40℃，出料即制得固化剂。
将该固化剂与环氧树脂配合在10℃环境下使用，76分钟固化，185分钟具有一定的粘结强度。
实施例3
将73克基础胺固化剂加入到带搅拌的三口烧瓶中，调节温度在72-80℃，开启搅拌，控制转速约85-95转/分；调节温度在72-80℃，分4次加入20克硫脲，时间在2.5-3小时，后调节温度在85-88℃，继续反应2小时；调节温度在60-65℃，一次性加入7克促进剂，搅拌混合30分钟，降温到35-40℃，出料即制得固化剂。
将该固化剂与环氧树脂配合在1℃环境下使用，115分钟固化,180分钟具有一定的粘接强度。
需要说明的是，在实施例1、实施例2和实施例3中，基础胺固化剂包括乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中的任意一种或乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中至少两种组分的组合物；硫脲为工业级硫脲；促进剂包括DMP-30、壬基酚和苯甲醇中的任意一种或DMP-30、壬基酚和苯甲醇中至少两种组分的组合物。
| 实施例1 | 实施例2 | 实施例3 | |
| 基础胺固化剂(g) | 69 | 79 | 73 |
| 硫脲(g) | 23 | 15 | 20 |
| 促进剂(g) | 8 | 6 | 7 |
| 使用环境温度(℃) | 5 | 10 | 1 |
| 固化时间(min) | 90 | 76 | 115 |
| 具有粘度时间(min) | 160 | 185 | 180 |
由上表可知，本发明与环氧树脂配合后，在低温环境下作业，能较快的固化并具有强度，便于施工提高效率。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.一种环氧树脂用低温固化剂，其特征在于，所述低温固化剂包括如下以质量份数计的组分：
基础胺固化剂68-80份；
硫脲15-24份；
促进剂5-9份。
2.如权利要求1所述的环氧树脂用低温固化剂，其特征在于，所述基础胺固化剂包括乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中的任意一种或乙二胺、二乙烯三胺、三乙烯四胺、聚醚胺220和异佛尔酮二胺中至少两种组分的组合物。
3.如权利要求1所述的环氧树脂用低温固化剂，其特征在于，所述硫脲为工业级硫脲。
4.如权利要求1所述的环氧树脂用低温固化剂，其特征在于，所述促进剂包括DMP-30、壬基酚和苯甲醇中的任意一种或DMP-30、壬基酚和苯甲醇中至少两种组分的组合物。
5.一种环氧树脂用低温固化剂的制备方法，其特征在于，所述方法用于制备权利要求1-5任意一项所述的低温固化剂，包括如下步骤：
S1、将基础胺固化剂置于带搅拌器的三口烧瓶，升温至72-80℃进行搅拌；
S2、保持在72-80℃温度下，分3-4次向三口烧瓶内添加硫脲，时间控制在2.5-3h；
S3、硫脲加毕后，保持温度为85-88℃继续反应2h；
S4、反应完成后，调节温度至60-65℃，向三口烧瓶内加入促进剂，搅拌混合30min；
S5、降温后出料得到成品固化剂。
6.如权利要求5所述的环氧树脂用低温固化剂的制备方法，其特征在于，所述搅拌器的转速为85-95r/min。
7.如权利要求5所述的环氧树脂用低温固化剂的制备方法，其特征在于，所述出料的固化剂的温度为35-40℃。
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| CN115028805A (zh) * | 2022-05-10 | 2022-09-09 | 西安工业大学 | 一种快速固化的环氧室温固化剂及制备方法 |
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| CN115028805B (zh) * | 2022-05-10 | 2023-12-22 | 西安工业大学 | 一种快速固化的环氧室温固化剂及制备方法 |
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