CN111040249A - 一种橡塑阻燃添加剂及含有其的橡塑材料 - Google Patents
一种橡塑阻燃添加剂及含有其的橡塑材料 Download PDFInfo
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- CN111040249A CN111040249A CN201911373422.2A CN201911373422A CN111040249A CN 111040249 A CN111040249 A CN 111040249A CN 201911373422 A CN201911373422 A CN 201911373422A CN 111040249 A CN111040249 A CN 111040249A
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- rubber
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 67
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Abstract
本发明提出一种橡塑阻燃添加剂及含有其的橡塑材料,所述橡塑阻燃添加剂包括以下质量份的成分:三聚氰胺氰脲酸盐20~30份,铝化合物50~68份,合成助剂5~20份,界面助剂1~3份,气凝胶0~1份。本发明提出的橡塑阻燃剂,是高效环保的阻燃剂,阻燃性能好,在230‑650度脱水释放氮气,更耐高温。抑烟性能好,燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳且无滴落物,在高分子聚合物遇高温明火无软化、滴落物现象,自形成有孔封闭结构碳化层。防腐蚀,环保节能,无毒,无味,无任何有害气体。
Description
技术领域
本发明属于以有机高分子材料为基料的组合物领域,具体涉及一种阻燃剂及其应用。
背景技术
橡塑材料是塑料与橡胶的统称,都是含有碳链的高分子材料,因此橡塑材料普遍具有不耐火、易燃的性质。为了更安全、更广泛地应用橡塑材料,人们一直致力于提高橡塑材料的防火性能。
对于添加于橡塑材料中的阻燃剂,要求其与塑料或橡胶的相容性要好,不改变原有材料的优良性能,易于加工,毒性小,燃烧时不产生毒性气体。按其主要有效成分划分,现有的阻燃剂包括溴系阻燃剂、磷系阻燃剂、氮系阻燃剂等。有机氮系阻燃剂包括三嗪及其衍生物、三聚氰胺等,含有氮系阻燃剂的材料燃烧时不会释放有毒气体,对环境友好,且氮系阻燃剂与高分子物质相容性好;但氮系阻燃剂单独使用时,存在不耐高温、长期使用易分解、橡塑材料的耐冲击性会下降等不足,若与其他阻燃剂或助剂共同使用,可起到协同效应,提高阻燃性能,而且材料性能也有所改善。已有的研究提出在磷酸溶液中或用多聚磷酸参与反应合成氮系阻燃剂,以解决阻燃剂在橡塑材料中分配不均、材料机械性能差等问题(三聚氰胺系列阻燃剂的改性研究进展,池华春,广州化工,2015年8月);专利CN103224707A公开了一种硅树脂改性磷酸多元醇酯三聚氰胺盐阻燃剂及其制备方法和用途,是将原料多元醇与磷酸反应,获得磷酸多元醇酯;将三聚氰胺和含固化催化剂的硅树脂组成混合物;再将上述磷酸多元醇酯与三聚氰胺和含固化催化剂硅树脂的混合物按重量比投料,搅拌混合均匀,获得硅树脂改性磷酸多元醇酯三聚氰胺盐阻燃剂。
上述的磷酸和氮系复配的阻燃剂,在300度以下热损失很小,热分解温度在400℃以上。伴随着现代工业对阻燃材料的更高要求,需要进一步提升阻燃的橡塑材料的耐热温度。
发明内容
针对本领域存在的不足之处,本发明的目的是提出一种用铝化合物复配的橡塑阻燃添加剂。
本发明的第二个目的是提出含有所述橡塑阻燃添加剂的橡塑材料。
为实现本发明上述目的的技术方案为:
一种橡塑阻燃添加剂,所述橡塑阻燃添加剂包括以下质量份的成分:
三聚氰胺氰脲酸盐20~30份,铝化合物50~68份,合成助剂5~20份,界面助剂偶联剂1~3份,气凝胶0.1~1份;
所述铝化合物为氢氧化铝、铝酸锌、次磷酸铝中的一种或多种。
铝化合物是更耐高温的阻燃成分,在1400℃才开始分解。基于此,提出本发明三聚氰胺氰脲酸盐和铝化合物复配的技术方案。
本发明所述的质量份,可以是毫克、克、公斤、斤、吨,或为了操作方便自己定义的质量单位。在同一个配方中,“份”表示的单位质量相同。
其中,所述合成助剂为二聚氰胺和/或尿素。
其中,所述界面助剂为偶联剂为KH550、KH560、KH570、石蜡、氯化石蜡中的一种或多种。
其中,所述气凝胶为纳米气凝胶,密度每立方3.4~3.6千克。
本发明的一种优选技术方案为,所述铝化合物为铝酸锌,或铝酸锌和次磷酸铝质量比1:(1.8~2.2)的组合。
进一步优选地,所述橡塑阻燃添加剂包括以下质量份的成分:
次磷酸铝42~48份,三聚氰胺脲酸盐22~26份,铝酸锌20~25份,尿素5~8份,偶联剂1~3份,气凝胶0.1~0.6份。
优选地,本方法所述的橡塑阻燃添加剂通过以下方法制备而得:
将铝化合物、三聚氰胺氰脲酸盐、合成助剂按比例放入搅拌釜中进行搅拌,经过20~40分钟边搅拌边升温的操作,将温度升至30至125度,再搅拌10~20分钟;所述界面助剂在升温前或温度升至30至125度时加入。
更优选地,将温度升至30~50℃,再加入界面助剂搅拌10~20分钟后加入气凝胶。
含有本发明所述的橡塑阻燃添加剂的橡塑材料。
其中,在所述橡塑材料中所述的橡塑阻燃添加剂的质量为橡塑原料的20~30%。
所述橡塑原料,可以是聚乙烯、聚氯乙烯、聚氨酯、聚苯乙烯的树脂、或硅树脂、或异戊橡胶、氯丁橡胶、丁钠橡胶、乙丙橡胶、丁基橡胶的生胶料中的一种。
本发明的有益效果在于:
本发明提出的橡塑阻燃剂,是高效环保的阻燃剂,具备五大性能:①阻燃性能好:230-650度脱水释放氮气,1050-1100度部分分解,最高耐1400度高温。②抑烟性能好:燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳。③无滴落物:高分子聚合物材料遇高温明火无软化和滴落物现象,自形成有孔封闭结构碳化层。④防腐蚀:对高分子聚合物无任何腐蚀,不含酸、碱、氟卤。⑤环保节能,无毒,无味,无任何有害气体。
本技术用一种产品实现了添加多种阻燃剂效果复合的功效,降低了成本。
具体实施方式
以下实施例用于说明本发明,但不应用来限制本发明的范围。实施例中,如无特别说明,所用手段均为本领域常规技术手段。
实施例中的份数,如无特别说明,均指质量份。所用比例均为质量比。
原料中,所用气凝胶为纳米气凝胶购自浙江岩谷科技有限公司,密度每立方3.55千克。铝酸锌购自山东威海三友化工科技有限公司,为无毒无味、不溶于水的白色粉末。
实施例1:
本实施例提出一种橡塑阻燃添加剂,包括以下质量份的成分:
三聚氰胺氰脲酸盐(氰尿酸三聚氰胺盐)25份、二聚氰胺25份、铝酸锌50份、氯化石蜡10份,按比例加入到反应釜中,边搅拌边加热直到125度,再搅拌15分钟,把温度降到25度即可。
本橡塑阻燃添加剂环保,含卤素少,抑烟性能好,燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳。在橡塑材料中的用量少,用本橡塑阻燃添加剂按聚氨酯原料的25%添加制成的塑料样品耐热温度达到1000℃。
氯化石蜡是一种界面助剂,用以改进阻燃剂和塑料原料之间的相容性。常用的偶联剂如KH550,KH560,KH570等,也是改善树脂原料与无机填充剂的界面性能的一种塑料添加剂。发明人通过试验比较,发现偶联剂KH550,KH560,KH570等改善相容性的效果优于氯化石蜡,且制备的温度也不需达100度以上。因此后续实施例采用偶联剂KH550为界面助剂。
实施例2
本实施例橡塑阻燃添加剂的原料为:次磷酸铝34份,三聚氰胺氰脲酸盐25份,铝酸锌34份,尿素6.5份,偶联剂kH550 1.5份。
制备工艺:将次磷酸铝、三聚氰胺脲酸盐、铝酸锌、尿素按比例放入搅拌釜中进行搅拌30分钟,边搅拌边升温至温度升至50度,再加入偶联剂KH550搅拌15分钟。
本橡塑阻燃添加剂环保,含卤素少,制备条件温和;抑烟性能好,燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳。在橡塑材料中的用量少,用本橡塑阻燃添加剂按聚氨酯原料的25%添加制成的塑料样品耐热温度达到1100℃。
实施例3
本实施例橡塑阻燃添加剂原料为:次磷酸铝45份,三聚氰胺氰脲酸盐25份,铝酸锌23份,尿素6.5份,偶联剂kH550;1.5份。
制备方法同实施例2。本橡塑阻燃添加剂环保,含卤素少,制备条件温和;在橡塑材料中的用量少,用本橡塑阻燃添加剂按聚氨酯原料的25%添加制成的塑料样品耐热温度达到1200℃。抑烟性能好,燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳、且无滴落物,用本实施例橡塑阻燃添加剂制成的塑料样品遇高温明火无软化和滴落物现像,自形成有孔封闭结构碳化层。
纳米气凝胶的主要原料是二氧化硅,纳米气凝胶和铝酸锌混合后更耐髙温,在高分子聚合物中不挥发,耐热稳定性好。试验中发现,1400℃以下时气凝胶没有任何变化,温度超过1400℃材料也只是发红;而且发明人还发现,添加了气凝胶的塑料机械性能也有很大增强。以下为添加了气凝胶的阻燃剂实施例。
实施例4
次磷酸铝45份,三聚氰胺脲酸盐25份,铝酸锌23份,尿素6.5份,偶联剂kH550 1.5份,气凝胶0.5份。
工艺流程:将次磷酸铝,三聚氰胺脲酸盐,铝酸锌,尿素,按比例放入搅拌釜中进行搅拌30分钟温度升至40度,再加入偶联剂搅拌15分钟,再加入气凝胶搅拌均匀即可。
本阻燃剂阶段性受热的性质为:230-650度脱水释放氮气,1050-1100度部分熔融,发挥耐高温的作用直到1400度。本橡塑阻燃添加剂阻燃性能好,环保,含卤素少,制备条件温和;在橡塑材料中的用量少,且能提高塑料的机械性能。用本橡塑阻燃添加剂按聚氨酯原料的25%添加制成的塑料样品的耐热温度达到1400℃。
本实施例制成的塑料样品的燃烧等级B1级。本实施例橡塑阻燃添加剂抑烟性能好,燃烧时无黑色烟,遇明火高温时产生白色气雾,抑烟效果极佳、且无滴落物,制成的塑料样品遇高温明火无软化和滴落物现像,自形成有孔封闭结构碳化层。
实施例5
次磷酸铝42份,三聚氰胺脲酸盐23份,铝酸锌24份,尿素7份,偶联剂kH550;1.5份,气凝胶0.5份。
工艺流程同实施例4。
本阻燃剂阶段性耐热的性质为:230-650度脱水释放氮气,1050-1100度部分熔融,发挥耐高温的作用直到1400度。
试验例
将各实施例得到的橡塑阻燃剂按25%添加量加入到聚氨酯树脂原料中,按每100质量份塑料原料加25份所述橡塑添加剂;用常规方法制成样品,依据标准GB-T-6343-2009泡沫塑料表观密度的测定、标准GBT8813-2008硬质泡沫塑料压缩强度试验方法、标准GB8624-2012建筑材料及制品燃烧性能分级进行测试,结果见下表。
表1:塑料性能测试
表2:阻燃性能测试
虽然,上文中已经本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (10)
1.一种橡塑阻燃添加剂,其特征在于,所述橡塑阻燃添加剂包括以下质量份的成分:
三聚氰胺氰脲酸盐20~30份,铝化合物50~68份,合成助剂5~20份,界面助剂1~3份,气凝胶0~1份;
所述铝化合物为氢氧化铝、铝酸锌、次磷酸铝中的一种或多种。
2.根据权利要求1所述的橡塑阻燃添加剂,其特征在于,所述合成助剂为二聚氰胺和/或尿素。
3.根据权利要求1所述的橡塑阻燃添加剂,其特征在于,所述界面助剂为偶联剂为KH550、KH560、KH570、石蜡、氯化石蜡中的一种或多种。
4.根据权利要求1所述的橡塑阻燃添加剂,其特征在于,所述气凝胶为纳米气凝胶,密度为每立方3.4~3.6千克。
5.根据权利要求1所述的橡塑阻燃添加剂,其特征在于,所述铝化合物为铝酸锌,或为铝酸锌和次磷酸铝质量比1:(1.8~2.2)的组合。
6.根据权利要求1~5任一项所述的橡塑阻燃添加剂,其特征在于,所述橡塑阻燃添加剂包括以下质量份的成分:
次磷酸铝42~48份,三聚氰胺氰脲酸盐22~26份,铝酸锌20~25份,尿素5~8份,偶联剂1~3份,气凝胶0.1~0.6份。
7.根据权利要求1~5任一项所述的橡塑阻燃添加剂,其特征在于,所述的橡塑阻燃添加剂通过以下方法制备而得:
将铝化合物、三聚氰胺氰脲酸盐、合成助剂按比例放入搅拌釜中进行搅拌,经过20~40分钟边搅拌边升温的操作,将温度升至30至125度,再搅拌10~20分钟;所述界面助剂在升温前或温度升至30至125度时加入。
8.根据权利要求7所述的橡塑阻燃添加剂,其特征在于,将温度升至30~50℃,再加入界面助剂搅拌10~20分钟后加入气凝胶。
9.含有权利要求1~8任一项所述的橡塑阻燃添加剂的橡塑材料。
10.根据权利要求9所述的橡塑材料,其特征在于,在所述橡塑材料中所述的橡塑阻燃添加剂的质量为橡塑原料的20~30%。
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CN107266890A (zh) * | 2017-07-11 | 2017-10-20 | 济南泰星精细化工有限公司 | 一种不饱和聚酯树脂无卤阻燃剂及其制备方法和应用 |
CN110066435A (zh) * | 2019-04-29 | 2019-07-30 | 大连高科阻燃橡胶有限公司 | 用于丁苯橡胶的无卤阻燃剂组合物及丁苯橡胶的制备方法 |
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CN112159549A (zh) * | 2020-08-31 | 2021-01-01 | 浙江工业大学 | 一种阻燃剂及其应用 |
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