CN112480351A - 一种有机/无机复配阻燃硬质聚氨酯泡沫及其制备方法 - Google Patents
一种有机/无机复配阻燃硬质聚氨酯泡沫及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种有机/无机复配阻燃硬质聚氨酯泡沫及其制备方法。本发明的有机/无机复配阻燃硬质聚氨酯泡沫由组分A、组分B和组分C组成,其中组分A由聚醚多元醇、含磷多元醇、正戊烷以及助剂组成,组分B为多异氰酸酯,组分C为有机金属骨架材料(MOF)。本发明还提供了所述有机/无机复配阻燃硬质聚氨酯泡沫的制备方法。本发明的有机/无机复配阻燃硬质聚氨酯泡沫材料能够显著提高管材阻燃性、延长阻燃时间、保证管材质量、降低施工难度,且原料绿色环保,不会对环境造成不良影响,具有良好的工业化生产前景。
Description
技术领域
本发明涉保温材料技术领域,尤其涉及一种有机/无机复配阻燃硬质聚氨酯泡沫。
背景技术
高密度聚乙烯外护管硬质聚氨酯泡沫塑料预制直埋保温管是城市集中供热系统中常用的主要材料。目前,在我国城市综合管廊的建设中,所采用的直埋保温管的材料必须要达到GB8624-2012《建筑材料及制品燃烧性能分级》中规定的B1级阻燃要求才能正式投入使用。
通常,提高硬质聚氨酯泡沫塑料保温层阻燃性能一般会采用在硬质聚氨酯泡沫塑料基体里添加阻燃剂的方法。然而,管材的施工工艺极大的限制了无机添加型阻燃剂的使用。少量无机添加型阻燃剂的添加不能达到提高集体阻燃性能的效果,而大量无机添加型阻燃剂的添加则会影响到管材的施工性能。同时,无机添加型阻燃剂的阻燃持久性差,易迁移对环境造成二次污染。而环保法规又对传统卤系阻燃剂的使用进行了严格的限定。因此,开发一种新型无卤阻燃聚氨酯直埋保温管已经成为企业、社会亟待解决的问题,有着广泛的应用前景。
含磷多元醇为液体,通过化学键与基体相连,在改善产品性质的同时对产品的生产工艺、结构和性能几乎无不良影响,具有明显的性能优势。但是,与传统的无机添加型阻燃剂和卤素系阻燃剂相比,含磷多元醇的阻燃效率较低,且生产成本较高,限制了其在工业生产中的大规模应用。而过渡金属离子,如Fe、Zr、Zn等,具有催化聚合物脱氢反应的作用,能够提高交联成炭效率,稳定高温下的残炭结构,少量添加,可以有效增强无卤阻燃剂效率,尤其是提高凝聚相的阻燃作用。通过将含磷多元醇与金属盐复配,有望开发出新型的阻燃硬质聚氨酯泡沫塑料。
发明内容
有鉴于此,本发明提供了一种有机/无机复配阻燃硬质聚氨酯泡沫。本发明提供的有机/无机复配阻燃硬质聚氨酯泡沫,采用含磷多元醇作为有机反应型阻燃剂,无机金属盐作为成炭催化剂,得到了具备B1级阻燃要求的高密度聚乙烯外护管硬质聚氨酯泡沫塑料预制直埋保温管聚氨酯保温层材料。
一种有机/无机复配阻燃硬质聚氨酯泡沫,包括以下重量份的原料组成:
进一步的,所述含磷多元醇为膦酸酯型含磷多元醇。
进一步的,所述含磷多元醇的制备方法包括以下步骤:
1)在配有搅拌、真空系统、温度计的三口烧瓶中,加入乙基膦酸二乙酯(DEEP)、二元醇和催化剂;
2)将反应体系温度缓慢升温至140-160℃进行酯交换反应3-3.5小时;
3)将步骤2)中的产物常压分馏出乙醇,然后减压并逐渐升温至165-180℃,进一步酯化缩合,得到含磷多元醇。
进一步的,步骤1)所述的催化剂为二丁基氧化锡,所述二元醇为乙二醇或丙二醇。
进一步的,步骤1)DEEP的添加量为166g,所述二元醇的添加量为68.2-87.4g,所述催化剂添加量为0.2-0.3g。
进一步的,步骤3)中含磷多元醇的羟值为55-60mgKOH/g,酸值不高于1mgKOH/g,25℃下的黏度为700-800mPaS。
进一步的,所述组分C为含Fe金属有机骨架材料、含Zr金属有机骨架材料、含Zn金属有机骨架材料中的一种或几种。
进一步的,所述组分C为MIL-53(Fe)、ZIF-8(Zn)、UiO-66(Zr)中的一种或几种。
本发明还提供了所述有机/无机复配阻燃硬质聚氨酯泡沫的制备方法,包括以下步骤:
(1)将配置好的组分A和组分C混合,置于聚氨酯发泡机的白料罐中,35-45℃保温;
(2)将组分B置于聚氨酯发泡机的黑料罐中,以0.25-0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
与现有技术相比,本发明具有以下有益效果:
本发明采用含磷多元醇作为有机反应型阻燃剂,无机金属盐作为成炭催化剂,得到了一种有机/无机复配阻燃硬质聚氨酯泡沫材料。本发明提供的有机/无机复配阻燃硬质聚氨酯泡沫材料能够应用于高密度聚乙烯外护管硬质聚氨酯泡沫塑料预制直埋保温管的生产中,在显著提高管材阻燃性、延长阻燃时间的同时,可以保证管材质量,降低施工难度。同时,本发明提供的有机/无机复配阻燃硬质聚氨酯泡沫材料采用的原料绿色环保,不会对环境造成不良影响,具有良好的工业化生产前景。
附图说明
下面结合附图说明对本发明作进一步说明。
图1为本发明实施例3、实施例4、对比例1、对比例2的热释放速率曲线。
具体实施方式
本发明提供了一种有机/无机复配阻燃硬质聚氨酯泡沫,由以下重量份的原料组成:
本发明所述含磷多元醇为膦酸酯型含磷多元醇。
本发明所述组分B为多异氰酸酯。
本发明所述组分C为含Fe金属有机骨架材料、含Zr金属有机骨架材料、含Zn金属有机骨架材料中的一种或几种。
本发明所述组分C为MIL-53(Fe)、ZIF-8(Zn)、UiO-66(Zr)中的一种或几种。
本发明还提供了所述有机/无机复配阻燃硬质聚氨酯泡沫的制备方法,包括以下步骤:
1)在配有搅拌、真空系统、温度计的三口烧瓶中,加入DEEP、二元醇、和催化剂;
2)将反应体系温度缓慢升温至140-160℃进行酯交换反应3-3.5小时;
3)将步骤2)中的产物常压分馏出乙醇,然后减压并逐渐升温至165-180℃,进一步酯化缩合,得到含磷多元醇;
4)将配置好的组分A和组分C混合,置于聚氨酯发泡机的白料罐中,35-45℃保温;
5)将组分B置于聚氨酯发泡机的黑料罐中,以0.25-0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
本发明步骤1)中DEEP加料量为166g,二元醇的加料量为68.2-87.4g。
本发明步骤1)中所述催化剂为二丁基氧化锡,催化剂添加量为0.2-0.3g。
本发明步骤3)中含磷多元醇的羟值为55-60mgKOH/g,酸值不高于1mgKOH/g,25℃下的黏度为700-800mPaS。
以下结合实施例对本发明提供的种植方法进行进一步说明。
实施例1
组分A中,含磷多元醇为膦酸酯型含磷多元醇,其制备方法如下:
1)在配有搅拌、真空系统、温度计的三口烧瓶中,加入DEEP166g、乙二醇70g,二丁基氧化锡0.25g;
2)将反应体系温度缓慢升温至150℃进行酯交换反应3小时;
3)将步骤2)中的产物常压分馏出乙醇,然后减压并逐渐升温至165℃,进一步酯化缩合,得到羟值控为58mgKOH/g,酸值为0.7mgKOH/g,25℃下的黏度为760mPa·S的含磷多元醇。
实施例2
一种有机/无机复配阻燃硬质聚氨酯泡沫,由以下重量份的原料组成:
将配置好的组分A和MIL-53(Fe)、混合,置于聚氨酯发泡机的白料罐中,45℃保温;再将组分B置于聚氨酯发泡机的黑料罐中,以0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
实施例3
一种阻燃硬质聚氨酯泡沫,由以下重量份的原料组成:
将配置好的组分A和MIL-53(Fe)混合,置于聚氨酯发泡机的白料罐中,45℃保温;再将组分B置于聚氨酯发泡机的黑料罐中,以0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
实施例4
一种阻燃硬质聚氨酯泡沫,由以下重量份的原料组成:
将配置好的组分A和UiO-66(Zr)混合,置于聚氨酯发泡机的白料罐中,45℃保温;再将组分B置于聚氨酯发泡机的黑料罐中,以0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
对比例1
一种硬质聚氨酯泡沫,由以下重量份的原料组成:
将配置好的组分A,置于聚氨酯发泡机的白料罐中,45℃保温;再将组分B置于聚氨酯发泡机的黑料罐中,以0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
对比例2
一种普通硬质聚氨酯泡沫,由以下重量份的原料组成:
将配置好的组分A,置于聚氨酯发泡机的白料罐中,45℃保温;再将组分B置于聚氨酯发泡机的黑料罐中,以0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
测试例1
分别测定实施例2、3、4,对比例1、2中所制备材料的物理性能,结果如下:
通过上述结果可以看出,含磷多元醇的加入可以提高硬质聚氨酯泡沫的阻燃性能和强度,并且对导热系数影响不大;但是,只加入含磷多元醇时,燃烧时仍然存在熔体滴落,不能通过垂直燃烧V-0级。控制少量添加MOF后,可以提高燃烧时凝聚相阻燃效果,避免滴落,燃烧热释放率下降,提高阻燃等级,并且,对力学性能和导热系数几乎没有影响。
与现有技术相比,采用本发明技术方案所制备的有机/无机复配阻燃硬质聚氨酯泡沫具有优良的导热系数、压缩强度以及燃烧性能。本发明显著提高了管材的阻燃性、延长阻燃时间、保证管材质量、降低施工难度,且原料绿色环保,不会对环境造成不良影响,具有良好的工业化生产前景。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
2.根据权利要求1所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,所述含磷多元醇为膦酸酯型含磷多元醇。
3.根据权利要求1所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,所述含磷多元醇的制备方法包括以下步骤:
1)在配有搅拌、真空系统、温度计的三口烧瓶中,加入乙基膦酸二乙酯(DEEP)、二元醇和催化剂;
2)将反应体系温度缓慢升温至140-160℃进行酯交换反应3-3.5小时;
3)将步骤2)中的产物常压分馏出乙醇,然后减压并逐渐升温至165-180℃,进一步酯化缩合,得到含磷多元醇。
4.根据权利要求3所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,步骤1)所述的催化剂为二丁基氧化锡,所述二元醇为乙二醇或丙二醇。
5.根据权利要求3所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,步骤1)DEEP的添加量为166g,所述二元醇的添加量为68.2-87.4g,所述催化剂添加量为0.2-0.3g。
6.根据权利要求3所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,其特征在于,步骤3)中含磷多元醇的羟值为55-60mgKOH/g,酸值不高于1mgKOH/g,25℃下的黏度为700-800mPaS。
7.根据权利要求1所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,所述组分C为含Fe金属有机骨架材料、含Zr金属有机骨架材料、含Zn金属有机骨架材料中的一种或几种。
8.根据权利要求1所述的有机/无机复配阻燃硬质聚氨酯泡沫,其特征在于,所述组分C为MIL-53(Fe)、ZIF-8(Zn)、UiO-66(Zr)中的一种或几种。
9.根据权利要求1-8任意一项所述有机/无机复配阻燃硬质聚氨酯泡沫的制备方法,其特征在于,包括以下步骤:
(1)将配置好的组分A和组分C混合,置于聚氨酯发泡机的白料罐中,35-45℃保温;
(2)将组分B置于聚氨酯发泡机的黑料罐中,以0.25-0.3Mpa的压力注入高密度聚乙烯外护管的夹层中,发泡成型,得到成品有机/无机复配阻燃硬质聚氨酯泡沫。
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CN115465852A (zh) * | 2022-07-15 | 2022-12-13 | 华中科技大学 | 一种抑烟剂、阻燃和抑烟硬质聚氨酯泡沫的制备 |
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