CN112898533A - 一种多重固化聚氨酯潜伏型固化剂及其制备方法 - Google Patents
一种多重固化聚氨酯潜伏型固化剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种多重固化聚氨酯潜伏型固化剂，制备所述多重固化聚氨酯潜伏型固化剂的原料包括二异氰酸酯、聚合物多元醇、多元羟基单体、含羟基的丙烯酸酯；所述多羟基小分子选自三羟甲基丙烷、三羟甲基乙烷、三羟甲基甲烷、1,4‑丁二醇、1,3‑丙二醇、1,5‑戊二醇的一种或多种。本发明还包括上述多重固化聚氨酯潜伏型固化剂的制备方法。本发明的多重固化聚氨酯潜伏型固化剂，固化后具有较高的硬度和耐化学腐蚀的性能，兼有优异的耐水和耐溶剂腐蚀、以及耐擦拭的性能。
Description
技术领域
本发明属于固化剂领域，具体涉及一种多重固化聚氨酯潜伏型固化剂及其制备方法。
背景技术
目前市面上存在的聚氨酯潜伏型固化剂，其大多数的特性为，通过二异氰酸酯单体和含活泼氢的聚醚聚酯反应，再经小分子量多元醇扩链，在应用时通过异氰酸根和空气中的水反应生成脲键，从而赋予漆膜很好的柔韧性、抗划伤性以及强度。然而，这种结构的潜伏型固化剂缺陷在于：往往受环境的影响较大，低温度、低湿度时干燥较慢，消耗的时间成本太高；而高温度、高湿度时和空气中的水反应太快，所产生的CO2来不及释放，容易造成涂层缺陷。另外，完全固化后的涂层硬度往往不是太高，难以满足一些有特殊硬度要求的场所。
因此，基于上述缺陷，亟需找到一种多重固化聚氨酯潜伏型固化剂，可以克服上述缺陷。
发明内容
本发明公开了一种多重固化聚氨酯潜伏型固化剂，固化后具有较高的硬度和耐化学腐蚀的性能，可以较好地解决上述问题。本发明还提供了上述多重固化聚氨酯潜伏型固化剂的制备方法。
本发明的一个目的在于提供一种多重固化聚氨酯潜伏型固化剂，制备多重固化聚氨酯潜伏型固化剂的原料包括二异氰酸酯、聚合物多元醇、多元羟基单体、含羟基的丙烯酸酯；
所述多元羟基单体选自三羟甲基丙烷、三羟甲基乙烷、三羟甲基甲烷、1,4-丁二醇、1,3-丙二醇、1,5-戊二醇的一种或多种。
进一步地，所述二异氰酸酯选自甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、甲基环已基二异氰酸酯、氢化二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、对苯二异氰酸酯、亚二甲苯基二异氰酸酯中的一种或多种。
进一步地，所述聚合物多元醇选自聚醚多元醇、聚酯多元醇的一种或多种。
进一步地，所述含羟基的丙烯酸酯选自丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯的一种或多种。
本发明的另一个目的在于提供上述多重固化聚氨酯潜伏型固化剂的制备方法，包括如下步骤：
S1.将二异氰酸酯溶于溶剂，形成混合物；
S2.加热条件下，向所述混合物中加入所述聚合物多元醇反应，得到中间产物1；
S3.加热条件下，向所述中间产物1中加入所述多元羟基单体反应，得到中间产物2；
S4.加热条件下，向所述中间产物2中加入所述含羟基的丙烯酸酯反应，得到中间产物3；
S5.在40-50℃下，向所述中间产物3中加入光引发剂反应，得到产物。
进一步地，S2中，所述聚合物多元醇的加入是分批的。
进一步地，S3中，所述多元羟基单体的加入是分批的。
进一步地，S2-S4中，所述加热的温度为60-70℃。
进一步地，S2-S4中，所述加热的时间为1-2h。
本发明的有益效果在于：
本发明的多重固化聚氨酯潜伏型固化剂，固化后具有较高的硬度和耐化学腐蚀的性能，兼有优异的耐水和耐溶剂腐蚀、以及耐擦拭的性能。
具体实施方式
为了更清楚地说明本发明的技术方案，列举如下实施例。实施例中所出现的原料、反应和后处理手段，除非特别声明，均为市面上常见原料，以及本领域技术人员所熟知的技术手段。
本发明实施例所述的聚醚多元醇，采购自陶氏化学，牌号为2000LM；
本发明实施例所述的聚酯多元醇，采购自深圳光华伟业股份有限公司，牌号为PCL1000C。
实施例1
一种多重固化聚氨酯潜伏型固化剂，其原料包括甲苯二异氰酸酯、聚醚多元醇、聚酯多元醇、三羟甲基丙烷、丙烯酸羟乙酯。
上述多重固化聚氨酯潜伏型固化剂的制备方法，包括如下步骤：
S1.按质量份数计，将甲苯二异氰酸酯38份溶于乙酸丁酯25份中，形成混合物；
S2. 60℃的条件下，按质量份数计，向混合物中分批加入聚醚多元醇15份以及聚酯多元醇12份，反应2h，得到中间产物1；
S3. 60℃的条件下，按质量份数计，向所述中间产物1中分批加入三羟甲基丙烷7.7份，反应2h，得到中间产物2；
S4. 60℃的条件下，按质量份数计，向所述中间产物2中加入丙烯酸羟乙酯2.5份，反应2h，得到中间产物3；
S5.在40℃下，向中间产物3中加入催化量的光引发剂TPO(二苯基-(2,4,6-三甲基苯甲酰)氧磷)反应1h，得到产物多重固化聚氨酯潜伏型固化剂。
实施例2
一种多重固化聚氨酯潜伏型固化剂，其原料包括二苯基甲烷二异氰酸酯、聚酯多元醇、三羟甲基丙烷、甲基丙烯酸羟乙酯。
上述多重固化聚氨酯潜伏型固化剂的制备方法，包括如下步骤：
S1.按质量份数计，将二苯基甲烷二异氰酸酯46份溶于乙酸丁酯30份中，形成混合物；
S2. 70℃的条件下，按质量份数计，向混合物中分批加入聚酯多元醇15份，反应2h，得到中间产物1；
S3. 70℃的条件下，按质量份数计，向所述中间产物1中分批加入三羟甲基丙烷6.2份，反应2h，得到中间产物2；
S4. 70℃的条件下，按质量份数计，向所述中间产物2中加入甲基丙烯酸羟乙酯1份，反应2h，得到中间产物3；
S5.在50℃下，向中间产物3中加入催化量的光引发剂TPO反应1h，得到产物多重固化聚氨酯潜伏型固化剂。
实施例3
一种多重固化聚氨酯潜伏型固化剂，其原料包括甲苯二异氰酸酯、聚醚多元醇、聚酯多元醇、三羟甲基丙烷、丙烯酸羟丙酯。
上述多重固化聚氨酯潜伏型固化剂的制备方法，包括如下步骤：
S1.按质量份数计，将甲苯二异氰酸酯40份溶于乙酸丁酯20份中，形成混合物；
S2. 65℃的条件下，按质量份数计，向混合物中加入分批聚醚多元醇13份以及聚酯多元醇15份，反应2h，得到中间产物1；
S3. 65℃的条件下，按质量份数计，向所述中间产物1中分批加入1,4-丁二醇2.3份，反应2h，得到中间产物2；
S4. 65℃的条件下，按质量份数计，向所述中间产物2中加入丙烯酸羟丙酯3份，反应2h，得到中间产物3；
S5.在45℃下，向中间产物3中加入催化量的光引发剂TPO反应1h，得到产物多重固化聚氨酯潜伏型固化剂。
对比例1
一种聚氨酯潜伏型固化剂，其原料包括甲苯二异氰酸酯、聚醚多元醇、三羟甲基丙烷。上述传统聚氨酯潜伏型固化剂的制备方法，包括如下步骤：
S1.按质量份数计，将甲苯二异氰酸酯45份溶于乙酸丁酯25份中，形成混合物；
S2. 65℃的条件下，按质量份数计，向混合物中分批加入聚醚多元醇21份，反应2h，得到中间产物1；
S3. 65℃的条件下，按质量份数计，向所述中间产物1中分批加入三羟甲基丙烷9份，反应2h，得到最终产物。
测试例
为了测试实施例1和对比例1中得到的产品的性能，设置以下测试例。产品各个性能指标的数据和相关执行标准，如表1所示。
表1实施例1和对比例1所得产品性能指标和相关测试标准
由此可见，本发明实施例1所公开的多重固化聚氨酯潜伏型固化剂，相比于对比例1，在各个性能指标上，均有明显的优势。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。
Claims (9)
1.一种多重固化聚氨酯潜伏型固化剂，其特征在于，制备所述多重固化聚氨酯潜伏型固化剂的原料包括二异氰酸酯、聚合物多元醇、多元羟基单体、含羟基的丙烯酸酯；
所述多元羟基单体选自三羟甲基丙烷、三羟甲基乙烷、三羟甲基甲烷、1,4-丁二醇、1,3-丙二醇、1,5-戊二醇的一种或多种。
2.根据权利要求1所述多重固化聚氨酯潜伏型固化剂，其特征在于，所述二异氰酸酯选自甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、甲基环已基二异氰酸酯、氢化二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、对苯二异氰酸酯、亚二甲苯基二异氰酸酯中的一种或多种。
3.根据权利要求1所述多重固化聚氨酯潜伏型固化剂，其特征在于，所述聚合物多元醇选自聚醚多元醇、聚酯多元醇的一种或多种。
4.根据权利要求1所述多重固化聚氨酯潜伏型固化剂，其特征在于，所述含羟基的丙烯酸酯选自丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯的一种或多种。
5.根据权利要求1-4任一项所述多重固化聚氨酯潜伏型固化剂的制备方法，其特征在于，包括如下步骤：
S1.将二异氰酸酯溶于溶剂，形成混合物；
S2.加热条件下，向所述混合物中加入所述聚合物多元醇反应，得到中间产物1；
S3.加热条件下，向所述中间产物1中加入所述多元羟基单体反应，得到中间产物2；
S4.加热条件下，向所述中间产物2中加入所述含羟基的丙烯酸酯反应，得到中间产物3；
S5.在40-50℃下，向所述中间产物3中加入光引发剂反应，得到产物。
6.根据权利要求5所述多重固化聚氨酯潜伏型固化剂的制备方法，其特征在于，S2中，所述聚合物多元醇的加入是分批的。
7.根据权利要求5所述多重固化聚氨酯潜伏型固化剂的制备方法，其特征在于，S3中，所述多元羟基单体的加入是分批的。
8.根据权利要求5所述多重固化聚氨酯潜伏型固化剂的制备方法，其特征在于，S2-S4中，所述加热的温度为60-70℃。
9.根据权利要求5所述多重固化聚氨酯潜伏型固化剂的制备方法，其特征在于，S2-S4中，所述加热的时间为1-2h。
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