CN111763299A - 一种高强度单组份聚脲及其制备方法 - Google Patents

一种高强度单组份聚脲及其制备方法 Download PDF

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CN111763299A
CN111763299A CN202010701094.0A CN202010701094A CN111763299A CN 111763299 A CN111763299 A CN 111763299A CN 202010701094 A CN202010701094 A CN 202010701094A CN 111763299 A CN111763299 A CN 111763299A
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谢成
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Abstract

本发明涉及一种树脂，公开了一种高强度单组份聚脲及其制备方法，该树脂由下列质量份数的原料制备而成：63‑74份单组份聚脲预聚体、13‑22份醛亚胺树脂和9‑18份溶剂。高强度单组份聚脲经湿固化后，醛亚胺树脂的二环己烷基甲烷的结构被设计和分相调控分布于硬段区域之中，对于物理机械性能具有增强增韧作用。本发明的单组份聚脲，具有拉伸力学强度大于45MPa，断裂伸长率大于400％和撕裂强度大于130N/mm等优异的力学性能，明显超过双组分喷涂聚脲或单组份聚脲行业标准的物理化学性能，具有储存稳定性好，施工工艺简单方便等特点。

Description

一种高强度单组份聚脲及其制备方法
技术领域
本发明涉及一种树脂，具体涉及一种高强度单组份聚脲及其制备方法。
背景技术
聚脲由异氰酸酯组分与氨基化合物反应生成的一类化合物。异氰酸酯组分可以是单体、聚合物、异氰酸酯的衍生物、预聚物和半预聚物。聚脲为一种含有大量的高极性聚脲基团、氢键的致密弹性体物质，具有防腐、防水、耐磨等特性，因此在防水、防腐、防冲磨和表面装饰四大领域具有广泛的应用。聚脲根据包装和施工等特性不同，大体可分为双组分喷涂聚脲，双组分天冬聚脲和单组份聚脲。
双组分喷涂聚脲尽管具有诸多优点，但因需特殊设备进行喷涂施工、快干对基材润湿不足导致附着力偏弱，因此在实际应用过程中存在较多不足；双组分天冬聚脲尽管较好的克服双组分喷涂聚脲在很多实际应用过程存在的不足，但因需按照计量进行配比再搅拌均匀，存在因搅拌混合不均匀导致产品质量事故频发。单组份聚脲具有施工简便方便，不需要额外进行配比搅拌均匀，可直接施工，并且具有优异的物理化学性能。专利号CN109280469A报道通过合成单组份聚脲预聚体，与恶唑烷潜固化剂、色浆、催化剂和粉料填料以及溶剂混合制备，获得了性能优异的单组份聚脲，基本符合单组份聚脲JC/T2435-2018标准中的力学强度要求；专利号CN102676039B报道通过聚醚多元醇制得预聚体，与恶唑烷潜固化剂、色浆、催化剂、助剂、粉料填料和溶剂混合制得潜固化型单组份聚氨酯涂料，该法所得力学强度较低，只有6MPa以内；专利号CN108530593A公开了一种单组份聚氨酯潜固化剂及其制备方法，其潜固化剂为醛和二胺所制得的，并以该潜固化剂所得单组份聚氨酯具有12个月以上的储存稳定性和优异的力学性能。
本发明的高强度单组份聚脲，通过醛亚胺结构，经过潜固化在聚脲本体结构引入二环己烷基甲烷的结构，使其可分相调控分布于硬段区域之中，对于物理机械性能具有明显的增强增韧作用，所制得的单组份聚脲，具有拉伸力学强度大于45MPa，断裂伸长率大于400％和撕裂强度大于130N/mm等优异的力学性能，明显超过双组分喷涂聚脲或单组份聚脲JC/T2435-2018标准中的物理化学性能，具有储存稳定性好，施工工艺简单方便等优点。
发明内容
为了克服现有技术的缺点和不足，本发明的首要目的在于提供一种高强度单组份聚脲及其制备方法。
本发明的另一目的在于提供上述高强度单组分聚脲的制备方法。
本发明的目的通过以下技术方案实现：
一种高强度单组份聚脲，由下列质量份数的原料制备而成：63-74份单组份聚脲预聚体、13-22份醛亚胺树脂和9-18份溶剂；所述醛亚胺树脂结构式如式Ⅰ所示：
Figure BDA0002590873570000021
式Ⅰ中，R1、R2分别为异丙基或正丙基或正丁基或异丁基。
所述单组份聚脲预聚体由下列质量份数的原料制备而成：80-100份聚酯二元醇预聚体或聚醚二元醇预聚体、0-16份二环己基甲烷二异氰酸酯，0-6份六亚甲基二异氰酸酯三聚体。
所述聚酯二元醇预聚体由按质量分数计的69-86份聚酯二元醇和14-31份二异氰酸酯制备而成；所述聚醚二元醇预聚体由按质量分数计的69-86份醚二元醇和14-31份二异氰酸酯制备而成；所述聚酯二元醇为聚碳酸酯二元醇或聚己二酸己二醇二元醇，聚醚二元醇为聚四氢呋喃醚二元醇。
所述聚酯二元醇或聚醚二元醇的数均分子量为1000-2000g/mol。
优选的，所述聚酯二元醇或聚醚二元醇的数均分子量为1000g/mol。
所述二异氰酸酯为1,6-己二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷二异氰酸酯的一种以上。
所述溶剂为醋酸丁酯、二甲苯、丙二醇甲醚醋酸酯、二丙二醇甲醚醋酸酯和二价酸酯的一种以上。
所述高强度单组份聚脲的制备方法，包括以下步骤：
(1)在反应器中加入聚酯二元醇或聚醚二元醇，在真空度0.01-0.05MPa，反应温度90-120℃真空脱水2-4h，然后加入二异氰酸酯在70℃反应0.5-1h后，升温至100-120℃，继续反应6-10h，降温至30-50℃，得到聚酯二元醇预聚体或聚醚二元醇预聚体；
(2)将聚酯二元醇预聚体或聚醚二元醇预聚体加入二环己基甲烷二异氰酸酯和六亚甲基二异氰酸酯三聚体，混合均匀，得到单组份聚脲预聚体；
(3)在单组份聚脲预聚体中加入醛亚胺树脂和溶剂混合搅拌均匀，出料，密封包装，得到高强度单组份聚脲。
本发明相对于现有技术具有如下的优点及效果：
本发明通过聚脲预聚体以醛亚胺潜固化后，在聚脲本体结构引入二环己烷基甲烷的结构，使其可分相调控分布于硬段区域之中，对于物理机械性能具有明显的增强增韧作用，制得的单组份聚脲具有拉伸力学强度大于45MPa，断裂伸长率大于400％和撕裂强度大于130N/mm等优异的力学性能，明显超过双组分喷涂聚脲或单组份聚脲行业标准的物理化学性能，具有储存稳定性好，施工工艺简单方便等特点。
具体实施方法
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1
将63份单组份聚脲预聚体、19份醛亚胺树脂(其中R1和R2皆为正丙基)和18份溶剂的混合得到高强度单组份聚脲。具体步骤如下：在反应器中加入69份的数均分子量为1000的聚碳酸酯二元醇，在真空度0.01-0.05MPa，反应温度120℃真空脱水2h；加入31份的异佛尔酮二异氰酸酯在70℃反应0.5h后，升温至100℃，继续反应10h，降温至30-50℃，得到100份聚碳酸酯二元醇预聚体；取87.5份聚碳酸酯二元醇预聚体，加入6.5份二环己基甲烷二异氰酸酯，6份六亚甲基二异氰酸酯(HDI)三聚体，混合均匀得到100份单组份聚脲预聚体；取63份单组份聚脲预聚体，加入18份丙二醇甲醚醋酸酯和19份醛亚胺树脂混合搅拌均匀，出料，密封包装，即得所述的高强度单组份聚脲。其中，醛亚胺树脂的结构如式Ⅱ所示：
Figure BDA0002590873570000041
实施例2
将69份单组份聚脲预聚体、22份醛亚胺树脂(其中R1和R2皆为异丙基)和9份溶剂的混合得到高强度单组份聚脲。具体步骤如下：在反应器中加入86份的数均分子量为2000的聚己二酸己二醇二元醇，在真空度0.01-0.05MPa，反应温度90℃真空脱水4h；加入14份的1,6-己二异氰酸酯在70℃反应0.5h后，升温至120℃，继续反应6h，降温至30-50℃，得到100份聚己二酸己二醇二元醇预聚体；取80份聚己二酸己二醇二元醇预聚体，加入16份二环己基甲烷二异氰酸酯，4份六亚甲基二异氰酸酯(HDI)三聚体，混合均匀得到100份单组份聚脲预聚体；取69份单组份聚脲预聚体，加入9份二丙二醇甲醚醋酸酯和22份醛亚胺树脂混合搅拌均匀，出料，密封包装，即得所述的高强度单组份聚脲。其中，醛亚胺树脂的结构如式Ⅲ所示：
Figure BDA0002590873570000051
实施例3
将74份单组份聚脲预聚体、13份醛亚胺树脂(其中R1和R2皆为正丁基)和13份溶剂的混合所得。具体步骤如下：在反应器中加入74份的数均分子量为1500的聚四氢呋喃醚二元醇，在真空度0.01-0.05MPa，反应温度100℃真空脱水3h；加入26份的二环己基甲烷二异氰酸酯在70℃反应1h后，升温至110℃，保持温度继续反应8h，降温至30-50℃，得到100份聚四氢呋喃醚二元醇预聚体；取74份聚四氢呋喃醚二元醇预聚体直接作为74份单组份聚脲预聚体(二环己基甲烷二异氰酸酯和六亚甲基二异氰酸酯(HDI)三聚体无添加)，加入6份醋酸丁酯和4份二甲苯以及3份二价酸酯(DBE)共计13份溶剂和13份醛亚胺树脂混合搅拌均匀，出料，密封包装，即得所述的高强度单组份聚脲。其中，醛亚胺树脂结构如式Ⅳ所示：
Figure BDA0002590873570000052
实施例4
将65份单组份聚脲预聚体、19份醛亚胺树脂(其中R1和R2皆为异丁基)和16份溶剂的混合所得。具体步骤如下：在反应器中加入77份的数均分子量为1500的聚碳酸酯二元醇，在真空度0.01-0.05MPa，反应温度100℃真空脱水3h；加入23份的异佛尔酮二异氰酸酯在70℃反应1h后，升温至100℃，继续反应10h，降温至30-50℃，得到100份聚碳酸酯二元醇预聚体；将88份聚碳酸酯二元醇预聚体，加入10份二环己基甲烷二异氰酸酯，2份六亚甲基二异氰酸酯(HDI)三聚体，混合均匀得到100份单组份聚脲预聚体；将65份单组份聚脲预聚体，加入8份二甲苯和8份丙二醇甲醚醋酸酯，共计16份溶剂和和19份醛亚胺树脂IV混合搅拌均匀，出料，密封包装，即得所述的高强度单组份聚脲。其中，醛亚胺树脂Ⅴ的结构如下式所示：
Figure BDA0002590873570000061
效果实施例
将各实施例所述的单组份聚脲，根据JC/T2435-2018标准制样、测试其拉伸强度、断裂伸长率、撕裂强度，将单组份聚脲储存6个月，观察外观，测试其稳定性，结果见表1。
表1各实施例单组份聚脲性能检测结果
Figure BDA0002590873570000062
Figure BDA0002590873570000071
通过表1数据，本发明通过通过醛亚胺潜固化后，在聚脲本体结构引入二环己烷基甲烷的结构，使其可分相调控分布于硬段区域之中，对于物理机械性能具有明显的增强增韧作用，制得的单组份聚脲具有拉伸力学强度大于45MPa，断裂伸长率大于400％和撕裂强度大于130N/mm等优异的力学性能，具有储存稳定性好，施工工艺简单方便等特点。
为了使本发明的目的及优点更加简洁明了，本发明将用上述具体实施例进行阐明，但本发明绝非仅限于这些实施例。上述实施例仅为本发明较优选的实施例，且仅用于阐述本发明，不能理解为对本发明的范围的限制。应当指出的是，凡在本发明的实质和原则之内所做的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (8)

1.一种高强度单组份聚脲，其特征在于，由下列质量份数的原料制备而成：63-74份单组份聚脲预聚体、13-22份醛亚胺树脂和9-18份溶剂；所述醛亚胺树脂结构式如式Ⅰ所示：
Figure FDA0002590873560000011
式Ⅰ中，R1和R2分别为异丙基或正丙基或正丁基或异丁基。
2.根据权利要求1所述高强度单组份聚脲，其特征在于，所述单组份聚脲预聚体由下列质量份数的原料制备而成：80-100份聚酯二元醇预聚体或聚醚二元醇预聚体、0-16份二环己基甲烷二异氰酸酯，0-6份六亚甲基二异氰酸酯三聚体。
3.根据权利要求2所述高强度单组份聚脲，其特征在于，所述聚酯二元醇预聚体由按质量分数计的69-86份聚酯二元醇和14-31份二异氰酸酯制备而成；所述聚醚二元醇预聚体由按质量份数计的69-86份醚二元醇和14-31份二异氰酸酯制备而成；所述聚酯二元醇为聚碳酸酯二元醇或聚己二酸己二醇二元醇，聚醚二元醇为聚四氢呋喃醚二元醇。
4.根据权利要求3所述高强度单组份聚脲，其特征在于，所述聚酯二元醇或聚醚二元醇的数均分子量为1000-2000g/mol。
5.根据权利要求4所述高强度单组份聚脲，其特征在于，所述聚酯二元醇或聚醚二元醇的数均分子量为1000g/mol。
6.根据权利要求3～5任一项所述的高强度单组份聚脲，其特征在于，所述二异氰酸酯为1,6-己二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷二异氰酸酯的一种以上。
7.根据权利要求1所述高强度单组份聚脲，其特征在于，所述溶剂为醋酸丁酯、二甲苯、丙二醇甲醚醋酸酯、二丙二醇甲醚醋酸酯和二价酸酯的一种以上。
8.根据权利要求1～7任一项所述高强度单组份聚脲的制备方法，其特征在于，包括以下步骤：
(1)在反应器中加入聚酯二元醇或聚醚二元醇，在真空度0.01-0.05MPa，反应温度90-120℃真空脱水2-4h，然后加入二异氰酸酯在70℃反应0.5-1h后，升温至100-120℃，继续反应6-10h，降温至30-50℃，得到聚酯二元醇预聚体或聚醚二元醇预聚体；
(2)将聚酯二元醇预聚体或聚醚二元醇预聚体加入二环己基甲烷二异氰酸酯和六亚甲基二异氰酸酯三聚体，混合均匀，得到单组份聚脲预聚体；
(3)在单组份聚脲预聚体中加入醛亚胺树脂和溶剂混合搅拌均匀，出料，密封包装，得到高强度单组份聚脲。
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