CN106478915A - 聚氨酯硬泡外墙保温材料及其制备方法 - Google Patents

聚氨酯硬泡外墙保温材料及其制备方法 Download PDF

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CN106478915A
CN106478915A CN201610882665.9A CN201610882665A CN106478915A CN 106478915 A CN106478915 A CN 106478915A CN 201610882665 A CN201610882665 A CN 201610882665A CN 106478915 A CN106478915 A CN 106478915A
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刘涛
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Abstract

本发明提出了一种聚氨酯硬泡外墙保温材料及其制备方法，由A组分和B组分组成，按照重量份数计算，A组分由酚醛树脂1～4份、溴化环氧树脂4～16份、聚醚多元醇60～80份、氧化石墨烯5～10份、催化剂1～4份、阻燃剂15～30份、稳定剂1～3份以及发泡剂15～30份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷1～5份、五氟环戊烷6～12份与二氯乙烷2～6份组成。该保温材料提高阻燃性同时保持其优异的力学性能。

Description

聚氨酯硬泡外墙保温材料及其制备方法
技术领域
本发明属于外墙体保温材料技术领域，具体涉及一种聚氨酯硬泡外墙保温材料及其制备方法。
背景技术
我国正在制定一系列强制性的建筑节能措施，这无疑给PU泡沫塑料在建筑节能中大规模使用创造了一个发展机遇。然而聚氨酯硬泡是一种容易燃烧的有机材料，它在燃烧时释放出大量有毒烟雾，可使人在短时间内中毒和窒息。在我国PU泡沫塑料的实际使用中，火灾事故不断发生。因此如果不能有效、切实地解决其防火安全性的问题，找不到一个具有充分科学根据的途径来解决其使用过程中的防火安全性问题，那么PU泡沫塑料就无法在我国建筑节能中获得大规模推广应用。所以聚氨酯泡沫塑料的耐燃、防火等问题成为迫切需要解决的重要课题，这个问题是硬质聚氨酯泡沫塑料今后能否继续发展的关键因素之一。
公开号为CN 101435254A、CN 100363578C和CN 100443683C等文献都报道了聚氨酯硬质泡沫外墙保温系统，基本上都包括基体墙面、防潮层、聚氨酯硬质泡沫保温层、界面层和修饰层，其关键技术都是变换界面层材料，以增强修饰层在聚氨酯硬质泡沫外表面的附着力。
专利ZL200610043347.X、提出了一种聚氨酯硬泡外墙外保温系统材料，包括聚氨酯防潮底漆、聚氨酯硬体材料、界面剂、内含玻璃纤维网格布的抗裂聚合物水泥砂浆和饰面涂料。其特点是解决了外墙保温墙面裂缝的产生，提高了表面平整度和装饰性。但是该专利对材料的防火阻燃性没有提及，保温体系也没有防火阻燃的相关措施。另外的相关专利ZL200810204580.0提出了一种喷涂型聚氨酯外墙保温系统及其施工方法，聚氨酯直接喷涂于涂有防潮底漆的基层墙面上，聚氨酯硬泡外设有找平层，找平层和聚氨酯硬泡间设有界面砂浆，找平层外设有耐碱网格布，网格布外是抹面砂浆。此保温系统的特点是结构简单施工快捷，可有效的防止墙面空鼓、开裂、渗水等缺陷。该专利提出系统具有阻火功能，其阻火功能的实现是通过界面砂浆和抹面聚合物砂浆阻隔作用来实现的，对聚氨酯硬泡材料本身的防火阻燃没有提及，而聚氨酯硬泡本身的防火阻燃性不好，将影响了整个体系的防火阻燃效果。专利CN200810105000.2公开了一种聚氨酯/酚醛泡沫保温材料的制备方法，采用异氰酸酯与聚醚多元醇的预聚物对酚醛树脂进行改性，添加表面活性剂、发泡剂，在室温下自由发泡，制备聚氨酯/酚醛泡沫保温材料，所得泡沫保温材料具有表面粉化小、韧性好、耐火性能好等优点。然而该体系从本质上说是一种用聚氨酯增加柔韧性的酚醛树脂发泡体系，其力学性能和粘接性能同聚氨酯体系是无法相比的。
发明内容
针对目前国内外结合聚氨酯硬泡保温系统的存在的主要问题，结合目前聚氨酯硬泡防火阻燃技术的研究进展，聚氨酯保温材料达到国标B1级或更高的防火等级，单一的添加阻燃剂技术不能解决问题，并且存在聚氨酯硬泡保温材料防火阻燃性能与力学性能相互矛盾的问题，本发明提出一种聚氨酯硬泡外墙保温材料，该保温材料提高阻燃性同时保持其优异的力学性能。
本发明的技术方案是这样实现的：
一种聚氨酯硬泡外墙保温材料，由A组分和B组分组成，按照重量份数计算，A组分由酚醛树脂1～4份、溴化环氧树脂4～16份、聚醚多元醇60～80份、氧化石墨烯5～10份、催化剂1～4份、阻燃剂15～30份、稳定剂1～3份以及发泡剂15～30份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷1～5份、五氟环戊烷6～12份与二氯乙烷2～6份组成。
进一步，溴化环氧树脂由四溴双酚与环氧氯丙烷为原料制备得到，其环氧当量为450～480g/eq，溴含量为48～52wt％。
进一步，所述催化剂为月桂酸二丁基锡、辛酸亚锡、醋酸锡、二乙酸二丁基锡或二乙酸二辛基锡。
进一步，所述阻燃剂为磷酸三(2-氯乙基)酯、甲基磷酸二甲酯、三(2，3-二溴丙基)聚异氰脲酸酯或三溴新戊醇。
进一步，稳定剂为聚醚改性有机硅氧烷。
本发明的另一个目的是提供一种聚氨酯硬泡外墙保温材料的制备方法，包括以下步骤：将酚醛树脂、溴化环氧树脂、聚醚多元醇、二氯乙烷与五氟环戊烷预混合，同时加入氧化石墨烯、稳定剂、催化剂、阻燃剂和环戊烷得到A组分，将多苯基多亚甲基多异氰酸酯作为B组分，将A组分与B组分混合发泡，异氰酸酯指数为1.05～1.15，得到聚氨酯硬泡外墙保温材料。
进一步，A组分与B组分的混合重量比为1∶1～1.8。
本发明中采用酚醛树脂最突出的特点是阻燃、低烟、抗高温歧变，具有质量轻、绝热性好、耐热性能好、尺寸稳定性好等特点，是唯一一种不用添加阻燃剂能够达到难燃级别(防火B1级)的有机材料，氧指数高达45。酚醛树脂阻燃性能好的根本原因是其高残炭率和酚羟基的自由基捕获作用，在本发明中将酚醛树脂和聚氨酯结合，优势互补，可以明显提高聚氨酯硬泡的阻燃性能。
本发明采用环氧树脂改性聚氨酯硬泡的主要目的为环氧基团与异氰酸酯反应生成高耐热的聚噁唑酮化合物，因此引入不同的环氧树脂可以得到不同耐热性的聚氨酯泡沫塑料；如果采用普通的环氧树脂会降低聚氨酯硬泡的阻燃性能，因此本发明采用已经市场化的阻燃性环氧树脂溴化环氧树脂，即提高聚氨酯硬泡的耐热性又提高其阻燃性。
本发明所述聚醚多元醇还包括含叔胺基聚醚多元醇，可以由多元伯或仲胺与环氧化合物开环反应制得，多元胺的碳原子数在2～18之间，具体包括乙二胺聚氧化丙烯四醇或二乙烯三胺聚氧化丙烯五醇。
在本发明中，所述的阻燃剂为磷酸三(2-氯乙基)酯、甲基磷酸二甲酯、三(2.3二溴丙基)聚异氰脲酸酯或三溴新戊醇，这些阻燃剂属于添加型或反应型阻燃剂，与聚氨酯体系相容性好，加入后体系能保持长时间的稳定性，并且对聚氨酯硬泡本身的力学性能影响较小，在聚氨酯硬泡系统中使用阻燃抑烟效果显著。
本发明采用氧化石墨烯增强了其与聚氨酯基体的界面结合力，制备的聚氨酯硬泡外墙保温材料更耐老化，通透性更好。根据DIN EN50147-1，在磁场，平面波和微波场类型的频率下测得该外墙保温材料屏蔽衰减效果显著
本发明的有益效果是产品同时具有较高的阻燃性能和优异的力学性能。
具体实施方式
实施例1
一种聚氨酯硬泡外墙保温材料，由A组分和B组分组成，按照重量份数计算，A组分由酚醛树脂1份、溴化环氧树脂4份、聚醚多元醇60份、氧化石墨烯7份、月桂酸二丁基锡1份、甲基磷酸二甲酯15份、聚醚改性有机硅氧烷1份以及发泡剂15份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷1份、五氟环戊烷6份与二氯乙烷4份组成。A组分与B组分的混合重量比为1∶1。
制备方法，包括以下步骤：将酚醛树脂、溴化环氧树脂、聚醚多元醇、二氯乙烷与五氟环戊烷预混合，同时加入氧化石墨烯、聚醚改性有机硅氧烷、月桂酸二丁基锡、甲基磷酸二甲酯和环戊烷得到A组分，将多苯基多亚甲基多异氰酸酯作为B组分，将A组分与B组分混合发泡，异氰酸酯指数为1.05，得到聚氨酯硬泡外墙保温材料。
实施例2
一种聚氨酯硬泡外墙保温材料，由A组分和B组分组成，按照重量份数计算，A组分由酚醛树脂2份、溴化环氧树脂10份、聚醚多元醇70份、氧化石墨烯5份、辛酸亚锡2份、磷酸三(2-氯乙基)酯24份、聚醚改性有机硅氧烷2份以及发泡剂24份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷3份、五氟环戊烷9份与二氯乙烷2份组成。A组分与B组分的混合重量比为1∶1.4。
制备方法，包括以下步骤：将酚醛树脂、溴化环氧树脂、聚醚多元醇、二氯乙烷与五氟环戊烷预混合，同时加入氧化石墨烯、聚醚改性有机硅氧烷、辛酸亚锡、磷酸三(2-氯乙基)酯和环戊烷得到A组分，将多苯基多亚甲基多异氰酸酯作为B组分，将A组分与B组分混合发泡，异氰酸酯指数为1.1，得到聚氨酯硬泡外墙保温材料。
实施例3
一种聚氨酯硬泡外墙保温材料，由A组分和B组分组成，按照重量份数计算，A组分由酚醛树脂4份、溴化环氧树脂16份、聚醚多元醇80份、氧化石墨烯10份、二乙酸二辛基锡4份、三溴新戊醇30份、聚醚改性有机硅氧烷3份以及发泡剂30份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷5份、五氟环戊烷12份与二氯乙烷6份组成。A组分与B组分的混合重量比为1∶1.8。
制备方法，包括以下步骤：将酚醛树脂、溴化环氧树脂、聚醚多元醇、二氯乙烷与五氟环戊烷预混合，同时加入氧化石墨烯、聚醚改性有机硅氧烷、二乙酸二辛基锡、三溴新戊醇和环戊烷得到A组分，将多苯基多亚甲基多异氰酸酯作为B组分，将A组分与B组分混合发泡，异氰酸酯指数为1.15，得到聚氨酯硬泡外墙保温材料。
实施例4
将实施例1-3制备得到的聚氨酯硬泡外墙保温材料进行抗压强度以及氧化指数等性能测定，结果见表1。
表1实施例1-3保温材料性能参数
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、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种聚氨酯硬泡外墙保温材料，由A组分和B组分组成，其特征在于，按照重量份数计算，A组分由酚醛树脂1～4份、溴化环氧树脂4～16份、聚醚多元醇60～80份、氧化石墨烯5～10份、催化剂1～4份、阻燃剂15～30份、稳定剂1～3份以及发泡剂15～30份组成，B组分为多苯基多亚甲基多异氰酸酯，所述发泡剂由环戊烷1～5份、五氟环戊烷6～12份与二氯乙烷2～6份组成。
2.根据权利要求1所述的聚氨酯硬泡外墙保温材料，其特征在于，溴化环氧树脂由四溴双酚与环氧氯丙烷为原料制备得到，其环氧当量为450～480g/eq，溴含量为48～52wt％。
3.根据权利要求1所述的聚氨酯硬泡外墙保温材料，其特征在于，所述催化剂为五甲基二乙烯三胺、双-二甲基胺基乙基醚或者N,N,N,N’,N”-四甲基乙二胺和四甲基己二胺。
4.根据权利要求1所述的聚氨酯硬泡外墙保温材料，其特征在于，所述阻燃剂为磷酸三(2-氯乙基)酯、甲基磷酸二甲酯、三(2，3-二溴丙基)聚异氰脲酸酯或三溴新戊醇。
5.根据权利要求1所述的聚氨酯硬泡外墙保温材料，其特征在于，稳定剂为聚醚改性有机硅氧烷。
6.制备如权利要求1至5任意一项所述的聚氨酯硬泡外墙保温材料的方法，其特征在于，包括以下步骤：将酚醛树脂、溴化环氧树脂、聚醚多元醇、二氯乙烷与五氟环戊烷预混合，同时加入氧化石墨烯、稳定剂、催化剂、阻燃剂和环戊烷得到A组分，将多苯基多亚甲基多异氰酸酯作为B组分，将A组分与B组分混合发泡，异氰酸酯指数为1.05～1.15，得到聚氨酯硬泡外墙保温材料。
7.根据权利要求6所述的聚氨酯硬泡外墙保温材料的制备方法，其特征在于，A组分与B组分的混合重量比为1∶1～1.8。
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