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CN104774313B - 一种阻燃剂和聚氨酯泡沫材料及其制备方法 - Google Patents

一种阻燃剂和聚氨酯泡沫材料及其制备方法 Download PDF

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CN104774313B
CN104774313B CN201410010510.7A CN201410010510A CN104774313B CN 104774313 B CN104774313 B CN 104774313B CN 201410010510 A CN201410010510 A CN 201410010510A CN 104774313 B CN104774313 B CN 104774313B
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flame retardant
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CN104774313A (zh
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胡源
袁海霞
卓锦德
董阳
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China Energy Investment Corp Ltd
National Institute of Clean and Low Carbon Energy
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National Institute of Clean and Low Carbon Energy
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Abstract

本发明涉及一种阻燃剂和聚氨酯泡沫材料及其制备方法。所述阻燃剂含有磷酸二氢铵和粉煤灰。所述聚氨酯泡沫材料含有聚氨酯和阻燃剂,其中,所述阻燃剂为上述阻燃剂。所述制备聚氨酯泡沫材料的方法包括将A组分和B组分进行反应,其中,所述A组分含有多元醇和阻燃剂,所述组分B含有异氰酸酯,所述阻燃剂为上述阻燃剂。在本发明提供的所述阻燃剂中,通过将磷酸二氢铵和粉煤灰配合使用,表现出优异的阻燃性能。

Description

一种阻燃剂和聚氨酯泡沫材料及其制备方法
技术领域
本发明涉及一种阻燃剂,包含该阻燃剂的聚氨酯泡沫材料,以及该聚氨酯泡沫材料的制备方法。
背景技术
粉煤灰是燃料(主要是煤)在燃烧过程中形成的微小微粒,是一种硅铝质粉状工业废料。粉煤灰对大气污染危害极大,高价值地利用粉煤灰是降低其环境影响和增加其价值的有效方法。例如,Flame retardancy of polycarbonate enhanced by adding fly ash(通过添加粉煤灰提高聚碳酸酯的阻燃性)(Makoto Soyama,Kazuhiko Inoue和MasatoshiIji,Polym.Adv.Technol,2007(18):386-391)中报道了将40%的平均粒径为10微米的粉煤灰加到聚碳酸酯中,可以使聚碳酸酯的限氧指数从20提高至43,UL94试验等级由V-2级提高至V-0级;The Effects of Intumescent Flame Retardant Including AmmoniumPolyphosphate/Pentaerythritol and Fly Ash Fillers on the PhysicomechanicalProperties of Rigid Polyurethane Foams(含有聚磷酸铵/季戊四醇和粉煤灰填料的膨胀的阻燃剂对刚性的聚氨酯泡沫的物理机械性能的影响)(AliJournalof Applied Polymer Science.2011(120):2095-2102)中报道了聚磷酸铵/季戊四醇与5重量%的粉煤灰配合使用对刚性的聚氨酯泡沫具有协同的阻燃性能,具体地,能够显著降低火蔓延和提高自熄性。
发明内容
本发明的目的是提供一种含有低熔点磷酸盐和粉煤灰的阻燃剂以及包含该阻燃剂的聚氨酯泡沫材料及其制备方法。
作为阻燃剂方面的应用,通常低熔点磷酸盐和粉煤灰各自均没有阻燃性能。然而,本发明的发明人通过深入研究后发现,有一种低熔点磷酸盐和粉煤灰配合后能够表现出良好的阻燃性能。也就是将磷酸二氢铵和粉煤灰配合后能够表现出优异的阻燃性能,从而完成了本发明。
本发明提供了一种阻燃剂,其中,该阻燃剂含有磷酸二氢铵和粉煤灰。
本发明还提供了一种聚氨酯泡沫材料,该聚氨酯泡沫材料含有聚氨酯和阻燃剂,其中,所述阻燃剂为上述阻燃剂。
本发明还提供了一种制备聚氨酯泡沫材料的方法,该方法包括将A组分和B组分进行反应,其中,所述A组分含有多元醇和阻燃剂,所述组分B含有异氰酸酯,所述阻燃剂为上述阻燃剂。
在本发明提供的所述阻燃剂中,通过将磷酸二氢铵和粉煤灰配合使用,表现出优异的阻燃性能,具体地,包含本发明所述的阻燃剂的聚氨酯泡沫材料具有提高的限氧指数,并且UL-94试验等级可以达到V-0。
本发明的其他特征和优点将在随后的具体实施方式部分予以详细说明。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与下面的具体实施方式一起用于解释本发明,但并不构成对本发明的限制。
图1是实施例1和对比例4-6制备的聚氨酯泡沫材料在锥形量热仪燃烧试验过程中热释放速率(HRR)相对于燃烧时间的函数关系的图表。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是,此处所描述的具体实施方式仅用于说明和解释本发明,并不用于限制本发明。
本发明提供了一种阻燃剂,其中,该阻燃剂含有磷酸二氢铵和粉煤灰。
在所述阻燃剂中,以所述阻燃剂中磷酸二氢铵和粉煤灰的总重量为基准,所述磷酸二氢铵的含量可以为25-70重量%,优选为50-70重量%;所述粉煤灰的含量为30-75重量%,优选为30-50重量%。
在本发明中,所述粉煤灰可以为本领域常规使用的粉煤灰。然而,为了进一步改善所述阻燃剂的阻燃性能,优选地,所述粉煤灰的平均粒径为0.1-30微米,更优选为0.1-5微米。
所述粉煤灰的组成在本发明中没有特别的限定,优选情况下,在所述粉煤灰中,以所述粉煤灰的总重量为基准,SiO2的含量为30-65重量%,Al2O3的含量为15-55重量%,CaO的含量为1-12重量%,Fe2O3的含量为1-10重量%。当选用上述优选组成的所述粉煤灰时,所述阻燃剂具有较好的阻燃性能。
在本发明中,所述阻燃剂的制备方法很简单,只需要将各个组分均匀混合即可。
本发明还提供了一种聚氨酯泡沫材料,该聚氨酯泡沫材料含有聚氨酯和阻燃剂,其中,所述阻燃剂为本发明提供的上述阻燃剂。
在所述聚氨酯泡沫材料中,以所述聚氨酯泡沫材料的总重量为基准,所述聚氨酯的含量可以为70-80重量%,优选为70-75重量%;所述阻燃剂的含量可以为20-30重量%,优选为25-30重量%。
本发明还提供了一种制备聚氨酯泡沫材料的方法,该方法包括将A组分和B组分进行反应,其中,所述A组分含有多元醇和阻燃剂,所述组分B含有异氰酸酯,其中,所述阻燃剂为本发明提供的上述阻燃剂。
在上述制备聚氨酯泡沫材料的方法中,相对于100重量份的所述多元醇,所述阻燃剂的用量可以为75-140重量份,所述异氰酸酯的用量可以为100-200重量份。
在上述制备聚氨酯泡沫材料的方法中,所述组分A还可以含有锡类催化剂、胺类催化剂、泡沫稳定剂和发泡剂。优选情况下,相对于100重量份的所述多元醇,所述锡类催化剂的用量为0.05-1重量份,所述胺类催化剂的用量为1-5重量份,所述泡沫稳定剂的用量为1-9重量份,所述发泡剂的用量为1-9重量份。
在本发明中,所述多元醇可以为本领域常规使用的多元醇,例如可以为聚酯多元醇和聚醚多元醇中的至少一种,更优选为聚醚多元醇,如选自聚氧化丙烯醇和环氧丙烷封端的醇中的至少一种,最优选为聚氧化丙烯二醇、聚氧化丙烯三醇、聚氧化丙烯四醇、环氧丙烷封端的二醇、环氧丙烷封端的三醇和环氧丙烷封端的四醇中的至少一种。
在本发明中,所述锡类催化剂可以为本领域常规使用的锡类催化剂,优选地,所述锡类催化剂选自有机锡类催化剂,更优选为辛酸亚锡和/或二月桂酸二丁基锡。
在本发明中,所述胺类催化剂可以为本领域常规使用的胺类催化剂,优选地,所述胺类催化剂为三乙醇胺、二乙醇胺和三乙烯二胺中的至少一种。
在本发明中,所述异氰酸酯可以为本领域常规使用的异氰酸酯,例如可以为二苯基亚甲基二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)和多聚异氰酸酯中的至少一种。
在本发明中,所述发泡剂可以为水和/或戊烷。
在本发明中,所述泡沫稳定剂可以为有机硅表面活性剂,优选为聚二甲基硅氧烷和/或硅油。
在上述制备聚氨酯泡沫材料的方法中,所述反应的过程可以包括先进行发泡,然后进行交联。其中,所述发泡的条件可以包括:温度为20-25℃,时间为3-10分钟,发泡的过程可以在常压下进行;所述交联的条件可以包括:温度为60-80℃,时间为10-24小时,所述交联的过程可以在常压下进行。
以下通过实施例对本发明作进一步说明。
实施例1
本实施例用于说明本发明提供的阻燃剂和聚氨酯泡沫材料及其制备方法。
本实施例中使用的粉煤灰的平均粒径为2.3微米,其组成为:41.25重量%的SiO2,35.58重量%的Al2O3,10.14重量%的CaO,5.94重量%的Fe2O3,来自国华电力公司北京热电厂。
(1)配制阻燃剂
将50重量份的粉煤灰和50重量份的磷酸二氢铵均匀混合,得到阻燃剂S1。
(2)制备聚氨酯泡沫材料
将100重量份的聚醚多元醇4110(羟基值为430±10mgKOH/g)、100重量份的阻燃剂S1、0.5重量份的二月桂酸二丁基锡、2重量份的硅油、2重量份的水、1重量份的三乙烯二胺和3重量份的三乙醇胺均匀混合,得到混合组分A1。将所述混合组分A1与150重量份的二苯基亚甲基二异氰酸酯(MDI)混合,并在70℃、常压下反应24小时,得到聚氨酯泡沫材料PU1。
实施例2
本实施例用于说明本发明提供的阻燃剂和聚氨酯泡沫材料及其制备方法。
本实施例中使用的粉煤灰的平均粒径为2.3微米,其组成为:41.25重量%的SiO2,35.58重量%的Al2O3,10.14重量%的CaO,5.94重量%的Fe2O3,来自国华电力公司北京热电厂。
(1)配制阻燃剂
将75重量份的粉煤灰和25重量份的磷酸二氢铵均匀混合,得到阻燃剂S2。
(2)制备聚氨酯泡沫材料
将100重量份的聚醚多元醇4110(羟基值为430±10mgKOH/g)、100重量份的阻燃剂S2、0.5重量份的二月桂酸二丁基锡、2重量份的硅油、2重量份的水、1重量份的三乙烯二胺和3重量份的三乙醇胺均匀混合,得到混合组分A2。将所述混合组分A2与150重量份的二苯基亚甲基二异氰酸酯(MDI)混合,并在60℃、常压下反应24小时,得到聚氨酯泡沫材料PU2。
对比例1
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,以磷酸钠代替阻燃剂S1中的磷酸二氢铵,从而制得聚氨酯泡沫材料DPU1。
对比例2
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,以磷酸氢二钾代替阻燃剂S1中的磷酸二氢铵,从而制得聚氨酯泡沫材料DPU2。
对比例3
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,以磷酸二氢钾代替阻燃剂S1中的磷酸二氢铵,从而制得聚氨酯泡沫材料DPU3。
对比例4
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,不加入阻燃剂S1,从而制得聚氨酯泡沫材料DPU4。
对比例5
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,用粉煤灰(与实施例1相同)代替阻燃剂S1,从而制得聚氨酯泡沫材料DPU5。
对比例6
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,只用磷酸二氢铵代替阻燃剂S1,且相对于100重量份的所述多元醇,其添加量只有50重量份,从而制得聚氨酯泡沫材料DPU6。
对比例7
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,用粉煤灰(与实施例1相同)代替阻燃剂S1,且相对于100重量份的所述多元醇,其添加量只有75重量份,从而制得聚氨酯泡沫材料DPU7。
对比例8
根据实施例1的方法制备聚氨酯泡沫材料,所不同的是,只用磷酸二氢铵代替阻燃剂S1,且相对于100重量份的所述多元醇,其添加量只有25重量份,从而制得聚氨酯泡沫材料DPU8。
测试例
(1)根据ASTM D2863-97的方法检测上述实施例和对比例制备的聚氨酯泡沫材料的限氧指数,结果如下表2所示。
(2)根据UL-94的方法对上述实施例和对比例制备的聚氨酯泡沫材料进行燃烧试验,具体地,将聚氨酯泡沫材料形成厚度为1.6mm、宽度为13.0±0.5mm、长度为125±5mm的测试样品;燃烧器的火焰长度为20mm,
实施2×10s的样品测试,并且按照以下表1所示标准判定各个样品的UL-94试验等级,结果如下表2所示。
表1
注:F指火焰燃烧
表2
序号 聚氨酯泡沫材料 限氧指数(LOI) UL94等级
实施例1 PU1 24.0 V-0
实施例2 PU2 23.5 V-1
对比例1 DPU1 22.0 NR
对比例2 DPU2 22.0 NR
对比例3 DPU3 22.0 NR
对比例4 DPU4 20.0 NR
对比例5 DPU5 21.5 NR
对比例6 DPU6 21.5 V-1
对比例7 DPU7 21.5 NR
对比例8 DPU8 21.5 NR
在上述表2中,通过将实施例1与对比例1-6进行比较可以看出,粉煤灰与磷酸二氢铵配合用作阻燃剂可以表现出优异的阻燃效果。通过将实施例2与对比例7-8进行比较也可以看出,粉煤灰与磷酸二氢铵配合用作阻燃剂可以表现出优异的阻燃效果。
(3)采用锥形量热仪根据ASTM E1354的方法对实施例1和对比例4-6的聚氨酯泡沫材料进行燃烧试验,得到的热释放速率(HRR)相对于燃烧时间的函数关系的图表如图1所示。
由图1可以看出,实施例1中粉煤灰与磷酸二氢铵的配合使用,可抑制热释放速率,表现出优异的阻燃效果。

Claims (8)

1.一种聚氨酯泡沫材料,该聚氨酯泡沫材料含有聚氨酯和阻燃剂,其特征在于,所述阻燃剂由磷酸二氢铵和粉煤灰组成,且以所述阻燃剂中磷酸二氢铵和粉煤灰的总重量为基准,所述磷酸二氢铵的含量为50-70重量%,所述粉煤灰的含量为30-50重量%;其中,
该聚氨酯泡沫材料通过以下方法制得:
将A组分和B组分进行反应,其中,所述A组分含有多元醇和所述阻燃剂,所述组分B含有异氰酸酯;相对于100重量份的所述多元醇,所述阻燃剂的用量为75-140重量份。
2.根据权利要求1所述的聚氨酯泡沫材料,其中,以所述聚氨酯泡沫材料的总重量为基准,所述阻燃剂的含量为20-30重量%。
3.根据权利要求1所述的聚氨酯泡沫材料,其中,所述粉煤灰的平均粒径为0.1-30微米。
4.根据权利要求3所述的聚氨酯泡沫材料,其中,所述粉煤灰的平均粒径为0.1-5微米。
5.根据权利要求1-4中任意一项所述的聚氨酯泡沫材料,其中,在所述粉煤灰中,以所述粉煤灰的总重量为基准,SiO2的含量为30-65重量%,Al2O3的含量为15-55重量%,CaO的含量为1-12重量%,Fe2O3的含量为1-10重量%。
6.一种制备聚氨酯泡沫材料的方法,该方法包括将A组分和B组分进行反应,其中,所述A组分含有多元醇和阻燃剂,所述组分B含有异氰酸酯,其特征在于,所述阻燃剂由磷酸二氢铵和粉煤灰组成,且以所述阻燃剂中磷酸二氢铵和粉煤灰的总重量为基准,所述磷酸二氢铵的含量为50-70重量%,所述粉煤灰的含量为30-50重量%。
7.根据权利要求6所述的方法,其中,相对于100重量份的所述多元醇,所述阻燃剂的用量为75-140重量份,所述异氰酸酯的用量为100-200重量份。
8.根据权利要求6或7所述的方法,其中,所述A组分还含有锡类催化剂、胺类催化剂、泡沫稳定剂和发泡剂,且相对于100重量份的所述多元醇,所述锡类催化剂的用量为0.05-1重量份,所述胺类催化剂的用量为1-5重量份,所述泡沫稳定剂的用量为1-9重量份,所述发泡剂的用量为1-9重量份。
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CN1493754A (zh) * 2002-10-30 2004-05-05 毅 赵 膨胀防火包覆型(卷)材
CN102876178A (zh) * 2012-09-11 2013-01-16 南通博宇机电有限公司 一种防火涂料
CN102964693A (zh) * 2012-12-24 2013-03-13 胶州市富田化工有限公司 一种高效阻燃剂组合物

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Publication number Priority date Publication date Assignee Title
CN1493754A (zh) * 2002-10-30 2004-05-05 毅 赵 膨胀防火包覆型(卷)材
CN102876178A (zh) * 2012-09-11 2013-01-16 南通博宇机电有限公司 一种防火涂料
CN102964693A (zh) * 2012-12-24 2013-03-13 胶州市富田化工有限公司 一种高效阻燃剂组合物

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