CN107286894B - 水工用低模量单组分聚氨酯密封胶及其生产方法 - Google Patents
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Abstract
本发明公开了一种水工用低模量单组分聚氨酯密封胶及其生产方法，由聚醚多元醇、二苯基甲烷二异氰酸酯、减四线油、硅烷偶联剂、T‑12催化剂、潜固化剂、环氧树脂、非活性稀释剂、粉状填料、白炭黑、炭黑、抗氧化剂制备而成；本发明的优点在于：克服了发泡的弱点，与混凝土粘结性优异，对环境更友好，同时降低了生产成本，延长了保质期，缩短了固化时间，固化成型与冰的粘结力低，能有效起到抗冰拔冰推的作用。此发明材料具有优异的性能并具备多个水工特性指标，可有效提高水工建筑的密封止水效果，增强其安全性、提高其使用寿命。
Description
技术领域
本发明涉及一种聚氨酯密封胶，具体地说是一种水工用低模量单组分聚氨酯密封胶及其生产方法，属于水工用密封材料领域。
背景技术
聚氨酯密封胶是用来填充空隙（孔洞、接头、接缝等）的材料，兼备粘接和密封两大功能。单组分主要是相对双组分而言的，只有一个组分，无需现场计量与调配，可以直接使用，施工简便。单组分聚氨酯胶是利用与空气中微量的水蒸气反应而固化，与基材表面的活性基团反应起到粘接作用。
根据行业标准JC/T482—2003《聚氨酯建筑密封胶》中25 LM型，聚氨酯建筑密封胶密度为规定值±0.1 g/cm3，表干时间 ≤ 24 h，适用期 ≥ 1 h，拉伸粘结性，最大抗拉强度 ≥ 0.2 MPa，最大延伸率 ≥ 200 %，定伸粘结性、浸水后定伸粘接性、冷拉-热压后的粘结性以及 -40 ℃低温柔性均无破坏，质量损失率 ≤ 7 %，弹性恢复率 ≥ 70 %。
查到相关硅烷化单组分聚氨酯密封材料方面的专利申请文献公开较少，如：申请号：201310119467.3一种单组份硅烷改性聚氨酯密封胶及其制备方法，以槽法炭黑、氧化锌和钛白粉中的一种或多种作为耐紫外线增强剂，所制备的硅烷改性聚氨酯密封胶具有较好的耐紫外线性能。
又如申请号：201110033123.1单组份硅烷改性聚氨酯密封胶及制备方法，以硅烷的固化机制代替异氰酸酯固化机制，含有硅氧键和极性的氨酯键，具有卓越的耐候性，粘接密封性能更为优异。
又如申请号：201410152614.1一种单组份硅烷改性聚氨酯密封胶及其制备方法，本发明制备的高强度单组份硅烷改性聚氨酯密封胶，不仅具有优异的机械性能，而且还可以免去传统聚氨酯密封胶施工工艺中底涂的使用。
现有的单组分聚氨酯密封胶均有发泡的的弱点，固化时间长，储存期短，与无机材料粘结不牢固，对环境不够友好，且价位较高。水工建筑连接缝密封止水至关重要，对密封止水材料的要求较高，开发综合性能优异的单组分聚氨酯密封胶，对密封胶的发展和水工建设都有重要意义。
发明内容
为了解决上述问题，本发明设计了一种水工用低模量单组分聚氨酯密封胶及其生产方法，利用硅酮密封胶不发泡、粘接强度高的优点，用硅烷偶联剂进行改性，既克服了发泡的弱点，又改善了与混凝土的粘结性，不添加任何可挥发性的有机溶剂，对环境友好，同时降低了生产成本，延长了储存期，缩短了固化时间，固化成型与冰的粘结力低，能有效起到抗冰拔冰推的作用。此发明材料具有优异的性能并具备多个水工特性指标，可有效提高水工建筑的密封止水效果，增强其安全性、提高其使用寿命。
本发明的技术方案为：
水工用低模量单组分聚氨酯密封胶，由以下重量份的原料制备而成：
聚醚多元醇（330N）50-70份，聚醚多元醇（DL-2000）180-200份，二苯基甲烷二异氰酸酯（MDI）60-70份，减四线油10-20份，硅烷偶联剂（KH-590）10-15份，催化剂（T-12）0.3-0.5份，潜固化剂3-5份，环氧树脂5-7份，非活性稀释剂30-40份，粉状填料300-350份，白炭黑20-30份，炭黑5-8份，抗氧化剂0.6份。
其中，所述潜固化剂为亚胺类；所述非活性稀释剂为DBE ,又称二元酸酯；所述抗氧化剂为抗氧化剂THANOX1010；所述粉状填料为硅粉及超细粉煤灰混合物，加入表面活性剂改性后能够减少团聚，分散更均匀，粉体粒度大小为500～600目；所述白炭黑即气相二氧化硅，作为触变剂；所述炭黑要求表面积≥90m2/g，着色强度≥100%。
上述水工用低模量单组分聚氨酯密封胶的制备方法，包括以下步骤：
（1）将聚醚多元醇经升温脱水形成无水聚醚多元醇；
（2）然后加入MDI，再经过80℃恒温保持状态下加入一部分增韧剂，得到聚氨酯（PU）预聚体；
（3）降温至60℃后加入硅烷偶联剂进行封端，得到硅烷化聚氨酯（SPU）预聚体；
（4）最后加入粉状填料、催化剂、剩余增韧剂等，真空高速分散，制得SPU密封胶产品。
本发明的优点在于：以廉价易得的减四线油作为增韧剂，对硅粉与粉煤灰进行表面改性后作为粉状填料，环保型非活性溶剂作为稀释剂，对环境更友好，同时降低了生产成本；对预聚体硅烷封端改性，湿固化时只有醇类产生，不会有二氧化碳放出，克服了发泡的弱点；潜固化剂的加入延长了保质期，缩短了固化时间；湿固化形成Si-O-Si键为交联点的交联结构，加上环氧树脂的改性，增强了与混凝土的粘结性能；预聚体与粉状填料经真空高速分散，材料更均一，密封止水性能更好，施工更便捷，固化成型表面光洁，抗冰拔冰推效果良好。
下面结合附图和实施例对本发明作进一步说明。
附图说明
图1为本发明实施例的生产工艺流程图。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
除非另有说明，本发明中所采用的百分数均为重量百分数。
实施例1
水工用低模量单组分聚氨酯密封胶，
上述水工用低模量单组分聚氨酯密封胶的制备方法，包括以下步骤：
（1）按照上述重量配比称量各组分，将聚醚多元醇（330N）和聚醚多元醇（DL-2000）经升温至110℃，脱水2h，形成无水聚醚多元醇；
（2）然后加入二苯基甲烷二异氰酸酯（MDI），再经过80℃恒温保持3h状态下加入一部分增韧剂减四线油，得到PU预聚体；
（3）降温至60℃后加入硅烷偶联剂（KH-590）进行封端，30min，得到SPU预聚体；
（4）最后加入粉状填料，以及催化剂（T-12）、剩余增韧剂（与前面加的增韧剂种类一样，都是启到增塑作用,前面增塑剂的加入可以降低预聚体粘度，两步总量10-20份，第一步可以加30-50%），真空高速分散（真空度为0.08MPa，分散速度为1000～1500转/min）30min，制得SPU密封胶产品。
上述原料组分中在封端完成后加入潜固化剂、环氧树脂、非活性稀释剂；分散过程中加粉料时加白炭黑、炭黑、抗氧化剂，处理后，密封泵送。
本发明中，以廉价易得的减四线油作为增韧剂，环保型非活性溶剂作为稀释剂，对环境更友好，且材料性能好；
本发明中，对硅粉与粉煤灰进行表面改性后作为粉状填料，代替重钙、纳米钙、滑石粉等，对环境更友好，同时降低了生产成本；
本发明中，对预聚体硅烷封端，并加入潜固化剂，改善储存稳定性，缩短固化时间，解决发泡问题；
本发明中，湿固化形成Si-O-Si键为交联点的交联结构，加上环氧树脂的改性，增强与混凝土的粘接性能；
本发明中，预聚体与粉状填料经真空高速分散，材料更均一，性能更好，施工更便捷。
最终产品性能指标如下：
从上表可以看出：本发明产品表干时间与实干时间均比市场上同类材料短，有利于下一道工序的进行，更好服务于工程量大、工期紧的水利工程；弹性回复率高，很好的满足混凝土温差、沉降等位移变化；标准要求的浸水4天测试浸水后定伸粘结性，延长浸水时间为30天依然没有破坏；具有很好的抗渗性能，0.8MPa 120 min不透水，达到密封止水的目的；与冰的粘结强度低，可以抵抗冰推冰拔作用；故本发明产品综合性能优异，其中水工性能突出。
本发明使用方法：
①接缝中的杂物、浮灰清除干净；
②将用嵌缝机或油灰刀嵌入接缝，并将嵌入的嵌缝胶压密实，不得有断头或空洞，嵌缝后应及时修整，使其表面光滑、平整；
③施工完毕，及时清洗各种工具。
本发明运输与储存中应注意：
①本产品在使用过程中不得与水接触、施工时应避开雨天；
②打开的材料尽量用完，剩余材料应密闭保存；
在本发明中：MDI是4,4'二苯基甲烷二异氰酸酯（纯MDI）、含有一定比例纯MDI与多苯基多亚甲基多异氰酸酯的混合物（聚合MDI）以及纯MDI与聚合MDI的改性物的总称，是生产聚氨酯最重要的原料，少量MDI应用于除聚氨酯外的其它方面。聚氨酯既有橡胶的弹性，又有塑料的强度和优异的加工性能，成为经济发展和人民生活不可缺少的新兴材料。 MDI和TDI互为替代品，都是生产聚氨酯的原料。目前MDI的价格略低一些，且毒性比TDI低，MDI形成的聚氨酯产品的模塑性相对较好。
在本发明中：硅烷偶联剂KH-590是一种具有反应性和可交联的硅烷偶联剂，在酸性或碱性条件下可水解，广泛应用于天然和合成橡胶的填料处理，另外作为补强剂和交联促进剂可用于复合材料（如树脂玻璃纤维复合材料）、涂层、油墨、胶水和密封材料等，还可用作树脂改性添加剂和酶固定剂。对于二氧化硅、碳黑等无机填料的处理，具有很好的作用。 它还可以在聚氨酯密封胶与基材之间发挥“分子桥”的作用，增加聚氨酯密封胶与基材的粘结性。
在本发明中：减四线油是减线油中的一种。减线油是指原油减压蒸馏塔产出的油，依据沸点的不同主要分为一线到四线，沸点越来越高。其中，减四线油沸点较高，常温下不挥发，可以作为聚氨酯密封胶的增韧剂。
在本发明中：填充料选择，以减四线油为液体填料；以硅粉及超细粉煤灰的混合物为产品的粉状填充料，并对该混合物进行了细度调整、表面改性、高温干燥等一系列处理，对其有关指标进行严格控制，使其完全满足产品性能和工业化生产的要求。
在本发明中：选择液体填充物减四线油为增韧剂。
在本发明中：助剂有抗氧化剂、潜固化剂和催化剂等，潜固化剂和催化剂主要是调整材料的固化干燥时间，利于产品在不同温度下施工。
本发明的优点较多，产品环保、性能稳定；固化后无接缝、抗渗能力强；常温下冷作业，操作简便，施工快速；具有优异的粘结力，与混凝土粘结性好，具有高塑性，回弹性优良；具有优异的低温柔性、高温稳定性、力学性能和耐久性能。
本发明中所用原料均为本领域生产中常用原料（本发明中用到的硅粉、粉煤灰、减四线油等在本领域不常用，这些原材料在新疆比较丰富、价格便宜、其中粉煤灰也是废物再利用。直接购买的硅粉和粉煤灰一般不符合要求，需经处理，以最优配比掺加，材料性能优异）其余均可从市场中得到，且对于生产结果不会产生影响；本发明中所采用的各种设备，均为本领域生产工艺中使用的常规设备，且各设备的操作、参数等均按照常规操作进行，仅需密封连接，并无特别之处。
Claims (1)
1.一种水工用低模量单组分聚氨酯密封胶的制备方法，其特征在于，包括以下步骤：
(1)将330N聚醚多元醇和DL-2000聚醚多元醇经升温脱水形成无水聚醚多元醇；
(2)然后加入二苯基甲烷二异氰酸酯，再经过80℃恒温保持状态下加入一部分增韧剂，得到PU预聚体；
(3)降温至60℃后加入硅烷偶联剂进行封端，得到SPU预聚体；
(4)最后加入粉状填料、催化剂、剩余增韧剂，真空高速分散，制得SPU密封胶产品；
所述增韧剂为减四线油；
在封端完成后加入潜固化剂、环氧树脂、非活性稀释剂；分散过程中加粉料时加白炭黑、炭黑、抗氧化剂；
所述潜固化剂为亚胺类；所述非活性稀释剂为DBE,又称二元酸酯；所述抗氧化剂为抗氧化剂THANOX1010；所述粉状填料为硅粉及超细粉煤灰混合物，加入表面活性剂改性，粉体粒度大小为500～600目；所述白炭黑即气相二氧化硅，作为触变剂；所述炭黑要求表面积≥90m2/g，着色强度≥100％；
其中，所述催化剂为T-12催化剂；
各组分的用量为：330N聚醚多元醇50-70份，DL-2000聚醚多元醇180-200份，二苯基甲烷二异氰酸酯60-70份，减四线油10-20份，硅烷偶联剂10-15份，T-12催化剂0.3-0.5份，潜固化剂3-5份，环氧树脂5-7份，非活性稀释剂30-40份，粉状填料300-350份，白炭黑20-30份，炭黑5-8份，抗氧化剂0.6份。
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