CN117924879A - 一种稀土增强酚醛芯层 - Google Patents

一种稀土增强酚醛芯层 Download PDF

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CN117924879A
CN117924879A CN202410092284.5A CN202410092284A CN117924879A CN 117924879 A CN117924879 A CN 117924879A CN 202410092284 A CN202410092284 A CN 202410092284A CN 117924879 A CN117924879 A CN 117924879A
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rare earth
core layer
parts
reinforced phenolic
phenolic aldehyde
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黄金登
连惠山
池佩富
戢超
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Fujian Ten Lead Advanced Material Co ltd
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Abstract

本发明涉及防火材料技术领域，特别涉及一种稀土增强酚醛芯层。该稀土增强酚醛芯层由稀土改性醇溶性磷酸盐、氧化铝、酚醛树脂及聚乙二醇在助剂作用下固化而得，所述助剂包括乳化剂、发泡剂及固化剂。本发明提供的稀土增强酚醛芯层，其采用稀土改性醇溶性磷酸盐提高防火性能，且分散均匀，不会出现沉积的问题；同时，其采用复合的乳化剂配合，进一步防止分层现象的出现，最终制得的稀土增强酚醛芯层防火性能好，韧性及抗压强度高，可作为防火泡沫板芯层的材料使用，以为市场提供新型的具有良好阻燃效果的外墙保温材料，具有良好的应用价值。

Description

一种稀土增强酚醛芯层
本申请是申请日为2022年08月05日、申请号为202210947742.X、发明名称为“一种稀土增强酚醛防火泡沫板”的申请的分案申请。
技术领域
本发明涉及防火材料技术领域，特别涉及一种稀土增强酚醛芯层。
背景技术
大量的无机或有机建筑保温材料广泛应用于建筑物的外墙结构。对人们所居住的建筑物而言，防火安全问题始终应该列于首位。
现有技术中，传统的保温材料，如聚苯乙烯(PS)和聚氨酯(PU)泡沫等，聚苯乙烯泡沫因其具有的价格较低、保温隔热性优良、吸水性小、水蒸气渗透性低、吸收冲击性好等优点而被大量用于建筑保温材料领域，但其自身的阻燃性较差，因此，近年来各行各业使用渐少；聚氨酯泡沫是隔热性能最好的保温材料之一，同时还具有不吸水的优点，但其价格较为昂贵、自身的阻燃性也较差，且燃烧时会释放出大量的有毒气体，这些因素很大程度上限制了其在建筑物外墙保温材料领域的应用。
鉴于此，公开号为CN111732814A，公告日为2020年10月02日，公开了《一种高性能防火阻燃酚醛泡沫及其制备方法》，所述高性能防火阻燃酚醛泡沫包括无机阻燃材料，与酚醛树脂、聚乙二醇、乳化剂以及发泡剂混合后加入固化剂，制备而得；其中，所述无机阻燃材料采用氢氧化铝、二氧化铈和二氧化硅按照10～25：5～10：8～25混合而得，通过特定比例的有机酸和无机酸进行混合(有机酸：无机酸的比例为1：3)作为固化剂，使得制备得到的酚醛泡沫测得火蔓延指数为0，烟指数降低到35，同时，测得导热系数≤0.023W/m·k，所述泡沫在具有良好保温性能的同时，达到更高要求的防火阻燃效果。
虽然，理论上该上述方案制备得到的高性能防火阻燃酚醛泡沫的导热系数高，可以提高防火阻燃效果；但是，其采用的无机填料固化过程中存在沉积、分布不均的问题，导致固化后的泡沫存在局部阻燃差的缺陷，导致其阻燃效果不佳。
发明内容
为解决上述现有技术中防火无机填料固化过程中存在沉积、分布不均的问题，本发明提供一种稀土增强酚醛芯层，其技术方案如下：
该稀土增强酚醛芯层，其由稀土改性醇溶性磷酸盐、氧化铝、酚醛树脂及聚乙二醇在助剂作用下固化而得；所述助剂包括乳化剂、发泡剂及固化剂。
在一些实施例中，所述乳化剂为EL-30与EL50中至少1种与硅油的组合；所述硅油占所述乳化剂总质量的40％～70％。
在一些实施例中，所述发泡剂为正戊烷、正己烷、环戊烷、环己烷中的一种或组合。
在一些实施例中，所述固化剂为有机酸和无机酸按照质量比1：3混合形成的混合酸。
在一些实施例中，所述有机酸为甲基磺酸、苯酚磺酸、对甲苯磺酸的一种或组合；所述无机酸为磷酸。
在一些实施例中，所述稀土改性醇溶性磷酸盐的制备过程为：在反应容器中加入85％磷酸溶液，升温至70℃后，恒温搅拌并缓慢加入氢氧化铝，然后将温度升高至90℃，逐滴加入氯化镧的乙醇溶液，恒温下冷凝回流5h，转移至旋转蒸发仪减压蒸馏2h，制得预聚物晶体，烘干后研磨，加入乙醇溶解，制得稀土改性醇溶性磷酸盐预聚物。
在一些实施例中，所述酚醛树脂为热固性酚醛树脂。
在一些实施例中，按质量份计，稀土增强酚醛芯层的组分中，所述稀土改性醇溶性磷酸盐10-15份，所述氧化铝10-25份，所述酚醛树脂100份，聚乙二醇5-18份，所述乳化剂10-15份，发泡剂8-16份，固化剂10-20份。
本发明还提供一种制备如上所述的稀土增强酚醛芯层的制备方法，步骤如下：
S100、在搅拌罐A料罐中加入酚醛树脂、聚乙二醇、发泡剂、乳化剂、稀土改性醇溶性磷酸盐及氧化铝搅拌均匀；
S200、将配置好的固化剂倒入固化剂罐B料罐中；
S300、在流水线前端部分先将下层水泥基卷材放置在下层放卷架上，上层水泥基卷材放置在上层放卷架上；
S400、烘房温度提前升至60～75℃；
S500、将A料罐和B料罐的料液抽至浇筑头快速搅拌后，将料液浇注在下层水泥基卷材、上层水泥基卷材这两块板之间，进入层压机起发、固化成型；其中，两块板之间料液浇注并固化形成的芯层，即为所述稀土增强酚醛芯层。
基于上述，与现有技术相比，本发明提供的稀土增强酚醛芯层，具有以下有益效果：
本发明提供的稀土增强酚醛芯层，其采用稀土改性醇溶性磷酸盐提高防火性能，且分散均匀，不会出现沉积的问题；同时，其采用复合的乳化剂配合，进一步防止分层现象的出现，最终制得的稀土增强酚醛芯层防火性能好，韧性及抗压强度高，可作为防火泡沫板芯层的材料使用，以为市场提供新型的具有良好阻燃效果的外墙保温材料，具有良好的应用价值。
本发明的其它特征和有益效果将在随后的说明书中阐述，并且，部分地从说明书中变得显而易见，或者通过实施本发明而了解。本发明的目的和其他有益效果可通过在说明书、权利要求书中所指出的结构和/或组分来实现和获得。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例；下面所描述的本发明不同实施方式中所设计的技术特征只要彼此之间未构成冲突就可以相互结合；基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
在本发明的描述中，需要说明的是，本发明所使用的所有术语(包括技术术语和科学术语)具有与本发明所属领域的普通技术人员通常所理解的含义相同的含义，不能理解为对本发明的限制；应进一步理解，本发明所使用的术语应被理解为具有与这些术语在本说明书的上下文和相关领域中的含义一致的含义，并且不应以理想化或过于正式的意义来理解，除本发明中明确如此定义之外。
本发明还提供以下实施例和对比例，以验证该稀土增强酚醛芯层的效果：
实施例1
S100、在搅拌罐(A料罐)中加入酚醛树脂、聚乙二醇、发泡剂、乳化剂、稀土改性醇溶性磷酸盐及氧化铝搅拌均匀。
S200、将配置好的固化剂倒入固化剂罐(B料罐)中。
S300、在流水线前端在流水线前端部分先将下层水泥基卷材放置在下层放卷架上，上层水泥基卷材放置在上层放卷架上。
S400、烘房温度提前升至70℃。
S500、将A\B料罐的料液抽至浇筑头快速搅拌后，将料液浇注在下层水泥基卷材、上层水泥基卷材这两块板之间，进入层压机起发、固化成型。其中，两块板之间料液浇注并固化形成的芯层，即为所述稀土增强酚醛芯层；下层水泥基卷材、稀土增强酚醛芯层、上层水泥基卷材由上之下层叠形成稀土增强酚醛防火泡沫板。
其中，以质量份数计，各组配比为：酚醛树脂100份，聚乙二醇5份，固化剂10份，氧化铝10份，稀土改性醇溶性磷酸盐10份，乳化剂10份，发泡剂8份。
发泡剂为正戊烷，乳化剂为质量比40％的硅油与60％EL-30的组合，固化剂为甲基磺酸与磷酸的组合，甲基磺酸与磷酸的质量比为1：3。所述稀土改性醇溶性磷酸盐的制备过程为：在反应容器中加入85％磷酸溶液，升温至70℃后，恒温搅拌并缓慢加入氢氧化铝，然后将温度升高至90℃，逐滴加入氯化镧的乙醇溶液，恒温下冷凝回流5h，转移至旋转蒸发仪减压蒸馏2h，制得预聚物晶体，烘干后研磨，加入乙醇溶解，制得稀土改性醇溶性磷酸盐预聚物。
实施例2
与实施例1相比，区别点在于：以质量份数计，各组配比为：酚醛树脂100份，聚乙二醇18份，固化剂20份，氧化铝25份，稀土改性醇溶性磷酸盐15份，乳化剂15份，发泡剂16份。
其余组分、配比及制备步骤与实施例1相同。
实施例3
与实施例1相比，区别点在于酚醛树脂100份，聚乙二醇12份，固化剂15份，氧化铝18份，稀土改性醇溶性磷酸盐12份，乳化剂12份，发泡剂12份。
其余组分、配比及制备步骤与实施例1相同。
对比例1
与实施例1相比，区别点在于酚醛树脂100份，聚乙二醇20份，固化剂25份，氧化铝30份，稀土改性醇溶性磷酸盐20份，乳化剂20份，发泡剂20份。
其余组分、配比及制备步骤与实施例1相同。
对比例2
与实施例1相比，区别点在于酚醛树脂100份，聚乙二醇3份，固化剂8份，氧化铝8份，稀土改性醇溶性磷酸盐5份，乳化剂8份，发泡剂5份。
其余组分、配比及制备步骤与实施例1相同。
对比例3
与实施例1相比，区别点在于乳化剂仅为硅油。
其余组分、配比及制备步骤与实施例1相同。对比例3在生产过程中出现分层现象，生产所得产品质量不合格。
对比例4
与实施例1相比，区别点在于稀土改性醇溶性磷酸盐替换为6份氧化镧及6份磷酸铝的组合。其余组分、配比及制备步骤与实施例1相同。
需要说明的是：
上述实施例中的具体参数或一些常用试剂，为本发明构思下的具体实施例或优选实施例，而非对其限制。本领域技术人员在本发明构思及保护范围内，可以进行适应性调整。
此外，若无特殊说明，所采用的原料也可以为本领域常规市售产品、或者由本领域常规方法制备得到。
对实施例及对比例的产物(中间层为稀土增强酚醛芯层、上下层为水泥基卷材的稀土增强酚醛防火泡沫板)进行性能测试，测试项目及方法见表1，测试结果见表2。
表1测试项目及方法
防火性能 GB8624
韧性(拉拔强度) GB20974
抗压强度 GB20974
表2测试结果
综上所述，与现有技术相比，本发明提供的稀土增强酚醛芯层，其采用稀土改性醇溶性磷酸盐提高防火性能，且分散均匀，不会出现沉积的问题；同时，其采用复合的乳化剂配合，进一步防止分层现象的出现，最终制得的稀土增强酚醛芯层防火性能好，韧性及抗压强度高，可作为防火泡沫板芯层的材料使用，以为市场提供新型的具有良好阻燃效果的外墙保温材料，具有良好的应用价值。
另外，本领域技术人员应当理解，尽管现有技术中存在许多问题，但是，本发明的每个实施例或技术方案可以仅在一个或几个方面进行改进，而不必同时解决现有技术中或者背景技术中列出的全部技术问题。本领域技术人员应当理解，对于一个权利要求中没有提到的内容不应当作为对于该权利要求的限制。
尽管本文中较多的使用了诸如稀土增强酚醛芯层、水泥基面层等术语，但并不排除使用其它术语的可能性。使用这些术语仅仅是为了更方便地描述和解释本发明的本质；把它们解释成任何一种附加的限制都是与本发明精神相违背的；本发明实施例的说明书和权利要求书中的术语“第一”、“第二”、等(如果存在)是用于区别类似的对象，而不必用于描述特定的顺序或先后次序。
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (8)

1.一种稀土增强酚醛芯层，其特征在于：由稀土改性醇溶性磷酸盐、氧化铝、酚醛树脂及聚乙二醇在助剂作用下固化而得；
所述助剂包括乳化剂、发泡剂及固化剂。
2.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：所述酚醛树脂为热固性酚醛树脂。
3.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：所述稀土改性醇溶性磷酸盐的制备过程为：
在反应容器中加入85％磷酸溶液，升温至70℃后，恒温搅拌并缓慢加入氢氧化铝，然后将温度升高至90℃，逐滴加入氯化镧的乙醇溶液，恒温下冷凝回流5h，转移至旋转蒸发仪减压蒸馏2h，制得预聚物晶体，烘干后研磨，加入乙醇溶解，制得稀土改性醇溶性磷酸盐预聚物。
4.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：所述固化剂为有机酸和无机酸按照质量比1：3混合形成的混合酸。
5.根据权利要求4所述的稀土增强酚醛芯层，其特征在于：所述有机酸为甲基磺酸、苯酚磺酸、对甲苯磺酸的一种或组合；
所述无机酸为磷酸。
6.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：所述乳化剂为EL-30与EL50中至少1种与硅油的组合；所述硅油占所述乳化剂总质量的40％～70％。
7.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：所述发泡剂为正戊烷、正己烷、环戊烷、环己烷中的一种或组合。
8.根据权利要求1所述的稀土增强酚醛芯层，其特征在于：按质量份计，稀土增强酚醛芯层的组分中，所述稀土改性醇溶性磷酸盐10-15份，所述氧化铝10-25份，所述酚醛树脂100份，聚乙二醇5-18份，所述乳化剂10-15份，发泡剂8-16份，固化剂10-20份。
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