CN110218357B - 一种耐析出膨胀型阻燃剂及其制备方法 - Google Patents

一种耐析出膨胀型阻燃剂及其制备方法 Download PDF

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CN110218357B
CN110218357B CN201910574049.0A CN201910574049A CN110218357B CN 110218357 B CN110218357 B CN 110218357B CN 201910574049 A CN201910574049 A CN 201910574049A CN 110218357 B CN110218357 B CN 110218357B
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池哲明
申应军
高翔
刘荣亮
张丰
王伟
李德燊
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Jinyoung Xiamen Advanced Materials Technology Co Ltd
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Abstract

本发明公开了一种耐析出膨胀型阻燃剂及其制备方法。其组分按照重量百分比配比为:25‑45％蒸馏水；20‑35％磷酸酯类；14‑20％多羟基化合物；10‑20％含氮类化合物；5‑10％有机蒙脱土；1‑2％金属氧化物；1‑2％金属硼化物。所述耐析出膨胀型阻燃剂可用于聚乙烯、聚丙烯、聚苯乙烯及各种聚烯烃共聚物，尤其适用于聚丙烯，24％(w/w)添加量阻燃等级可达到UL94 V‑0，氧指数≥27，30％(w/w)添加量阻燃等级可达到UL94 V‑0，氧指数≥28。阻燃效率高，流动性好，耐析出，可满足建材、电器外壳、插座、波纹管和灯饰灯具等用阻燃材料的使用要求。

Description

一种耐析出膨胀型阻燃剂及其制备方法
技术领域
本发明涉及阻燃剂领域，尤其涉及一种耐析出膨胀型阻燃剂及其制备方法。
背景技术
高分子材料在国民生活生产形影不离，而作为消耗量仅次于增塑剂的阻燃剂也在不断推陈出新。目前应用于高分子材料的阻燃剂主要包括卤系、磷系、氮系、磷-氮系、无机化合物等，虽然卤系阻燃剂仍是使用量最大的阻燃剂，但是由于环保问题，随阻燃技术发展，终将退出历史舞台，取而代之则是无卤阻燃技术；磷系阻燃剂具有高效、环保、低毒、低烟等优点，但是与基体相容性较差，容易析出；无机阻燃剂要达到阻燃效果，往往需要添加大量阻燃剂，导致材料力学性能下降。
膨胀阻燃剂(IFR)是一种含有氮、磷、碳为主要成分，分别为阻燃过程中提供碳源、酸源和气源的新型环保复合阻燃剂，具有无卤、低烟、低毒、防滴等特点，作为未来阻燃剂发展重要方向之一，但目前膨胀阻燃剂与基体相容性较差，稳定性较低，易迁移、易吸潮等缺点限制了它的应用。
发明内容
本发明的目的在于针对现有的技术不足，提供一种耐析出的膨胀型阻燃剂。
为实现上述目的，本发明提供一种耐析出膨胀型阻燃剂，其特征在于：其组分按照重量
百分比配比为:
Figure BDA0002111594990000011
进一步，其组分按照重量百分比配比为:
Figure BDA0002111594990000012
Figure BDA0002111594990000021
进一步，所述的磷酸酯类是磷酸三苯酯、磷酸三甲苯、磷酸二苯辛酯、磷酸三丁酯、磷酸三(氯乙基)酯、磷酸三(二氯丙基)酯、异葵基二苯基磷酸酯、二乙基乙基二苯基磷酸酯、磷酸三异丙苯酯中的一种。
进一步，所述的多羟基化合物是糊精、季戊四醇、乙二醇、酚醛树脂中的一种。
进一步，所述的含氮类化合物是尿素、双氰胺、聚氨酯、三聚氰胺、聚磷酸胺、三聚氰胺磷酸酯、聚脲树脂中的一种。
进一步，所述的有机蒙脱土是钙基蒙脱土、钠基蒙脱土、镁基蒙脱土中的一种；优选的，平均晶片≤25nm，蒙脱土重量含量≥95％。
进一步，所述的金属氧化物是三氧化锑、氧化锌、氧化铁、氧化锡中的一种。
进一步，所述的金属硼化物是硼酸锌、硼酸钙、硼酸铝中的一种。
进一步，包括如下制备方法，
A.按配方比例添加蒸馏水、磷酸酯类、有机蒙脱土到反应釜中并通入氮气边加热边搅拌，温度70-110℃，搅拌2-5h，超声8-12h；
B.将A制备的混合物倒入到多羟基化合物和含氮类化合物中，40-50℃搅拌2-5h；
C.将金属氧化物和金属硼化物添加到B所得中，60-80℃充分搅拌2-5h后静置待沉降后，除去上清液得到沉淀；
D.将所得沉淀真空干燥即可。
本发明以磷酸酯类作为酸源进行脱水成碳，利用有机蒙脱土片层结构进行插层，磷酸酯类化合物与有机蒙脱土之间产生强的化学作用，提高了磷酸酯类迁移能力，也提高阻燃剂与基体相容性。同时，多羟基化合物燃烧成碳阻隔可燃气体产生和氧气进入，含氮类化合物产生难燃气体，再配和金属氧化物和金属硼化物协效阻燃，极大提高塑料阻燃能力。
同时本发明所述磷酸酯类化合物、多羟基化合物与蒙脱土形成化学结合，减少羟基，酯基、羧基等极性基团与水形成氢键，而降低吸潮发生。
所述耐析出的膨胀型阻燃剂，可用于聚乙烯、聚丙烯、聚苯乙烯及各种聚烯烃共聚物，尤其适用于聚丙烯，24％(w/w)添加量阻燃等级可达到UL94V-0，氧指数≥27，30％(w/w)添加量阻燃等级可达到UL94V-0，氧指数≥28。阻燃效率高，流动性好，耐析出，可满足建材、电器外壳、插座、波纹管和灯饰灯具等用阻燃材料的使用要求。
具体实施方式
下面详细描述本发明的实施例，所述实施例的示例旨在用于解释本发明，而不能理解为对本发明的限制。实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规产品。
实施例1：耐析出膨胀型阻燃剂的制备
原材料：见表1。
制备方法：
A.按配方比例添加蒸馏水、磷酸酯类、有机蒙脱土到反应釜中并通入氮气边加热边搅拌，温度70-110℃，搅拌2-5h，超声8-12h；
B.将A制备的混合物倒入到多羟基化合物和含氮类化合物中，40-50℃搅拌2-5h；
C.将金属氧化物和金属硼化物添加到B所得中，60-80℃充分搅拌2-5h后静置待沉降后，除去上清液得到沉淀；
D.将所得沉淀真空干燥即可。
效果验证：见表2。
其中熔体流动速率测定见ASTM D1238，单位为g/10min；LOI氧指数测定见GB/T2406.2-2009，单位为％；3.2mm阻燃测试测定见UL94，单位为级，析出测试测定见PV1306。
实施例2：耐析出膨胀型阻燃剂的制备
原材料：见表1。
制备方法：同实施例1。
效果验证：见表2。
实施例3：耐析出膨胀型阻燃剂的制备
原材料：见表1。
制备方法：同实施例1。
效果验证：见表2。
实施例4：耐析出膨胀型阻燃剂的制备
原材料：见表1。
制备方法：同实施例1。
效果验证：见表2。
对比例1：阻燃剂的制备
原材料：见表1。
制备方法：同实施例1。
效果验证：见表2。
对比例2：阻燃剂的制备
原材料：见表1。
制备方法：同实施例1。
效果验证：见表2。
表1实施例1-6和对比例1-2的原材料用量表
Figure BDA0002111594990000041
表2为实施例1-4和对比例1-2的性能表
Figure BDA0002111594990000042
Figure BDA0002111594990000051
从表1和表2的结果可以看出，24％(w/w)添加量时，实施例1-4的阻燃等级可达到UL94V-0，LOI氧指数≥27，熔体流动速率≥30；对比例1-2的阻燃等级为UL94V-1，LOI氧指数≤25，熔体流动速率≤27，析出测试的等级均为1级，即不析出发黏，同时稳定性好；而对比例为S，表明阻燃剂出现析出，不稳定。
30％(w/w)添加量时，实施例1-4的阻燃等级可达到UL94V-0，LOI氧指数≥28，熔体流动速率≥30；对比例1-2的阻燃等级为UL94V-1和UL94V-1，LOI氧指数≤26，熔体流动速率≤26，析出测试的等级均为1级，即不析出发黏，同时稳定性好；而对比例为S和2级，表明阻燃剂出现析出和轻微发黏，不稳定。
本发明的对比例所得到的阻燃剂阻燃效果较差、熔体流动速率更低、阻燃剂析出率更高，通过和实施例1-4比较可知，所述的磷酸酯类化合物、有机蒙脱土及含氮类化合物应具有合适的比例才能协效发挥膨胀型阻燃效果。从对比例1-2可以看出，磷酸酯化合物含量较多，有机蒙脱土含量较少时，磷酸酯化合物不能充分分散在蒙脱土层间，导致部分磷酸酯化合物仍然会析出，并且阻燃效果减弱。
通过比较可以看出，采用本发明技术方案的实施例1-4的耐析出膨胀型阻燃剂的阻燃效率高，流动性好，耐析出，可满足建材、电器外壳、插座、波纹管和灯饰灯具等阻燃材料的使用要求。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在不脱离本发明的原理和宗旨的情况下在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。

Claims (9)

1.一种耐析出膨胀型阻燃剂，其特征在于：其组分按照重量百分比配比为:
Figure FDA0002796954760000011
制备方法如下，
A.按配方比例添加蒸馏水、磷酸酯类、有机蒙脱土到反应釜中并通入氮气边加热边搅拌，温度70-110℃，搅拌2-5h，超声8-12h；
B.将A制备的混合物倒入到多羟基化合物和含氮类化合物中，40-50℃搅拌2-5h；
C.将金属氧化物和金属硼化物添加到B所得中，60-80℃充分搅拌2-5h后静置待沉降后，除去上清液得到沉淀；
D.将所得沉淀真空干燥即可。
2.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：其组分按照重量百分比配比为:
Figure FDA0002796954760000012
3.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的磷酸酯类是磷酸三苯酯、磷酸三甲苯、磷酸二苯辛酯、磷酸三丁酯、磷酸三(氯乙基)酯、磷酸三(二氯丙基)酯、异葵基二苯基磷酸酯、二乙基乙基二苯基磷酸酯、磷酸三异丙苯酯中的一种。
4.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于:所述的多羟基化合物是糊精、季戊四醇、乙二醇、酚醛树脂中的一种。
5.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的含氮类化合物是尿素、双氰胺、聚氨酯、三聚氰胺、聚磷酸胺、三聚氰胺磷酸酯、聚脲树脂中的一种。
6.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的有机蒙脱土是钙基蒙脱土、钠基蒙脱土、镁基蒙脱土中的一种。
7.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的有机蒙脱土的平均晶片≤25nm，蒙脱土重量含量≥95％。
8.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的金属氧化物是三氧化锑、氧化锌、氧化铁、氧化锡中的一种。
9.根据权利要求1所述的一种耐析出膨胀型阻燃剂，其特征在于：所述的金属硼化物是硼酸锌、硼酸钙、硼酸铝中的一种。
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