CN107459492A - 一种有机改性三聚氰胺聚磷酸盐及其制备方法 - Google Patents

一种有机改性三聚氰胺聚磷酸盐及其制备方法 Download PDF

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CN107459492A
CN107459492A CN201710619972.2A CN201710619972A CN107459492A CN 107459492 A CN107459492 A CN 107459492A CN 201710619972 A CN201710619972 A CN 201710619972A CN 107459492 A CN107459492 A CN 107459492A
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melamine polyphosphate
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modified melamine
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彭治汉
刘会阳
杜国毅
郭承鑫
何小春
彭治权
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Hunan Meilaipo Technology Development Co Ltd
Donghua University
National Dong Hwa University
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Donghua University
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Abstract

本发明涉及一种有机改性三聚氰胺聚磷酸盐及其制备方法,制备方法为:首先将有机胺与粒径D50小于5微米的三聚氰胺聚磷酸盐分散在溶剂中,然后在压力为0~0.6MPa、温度为80~180℃的条件下反应2~8h,最后在压力为‑0.01~‑0.09MPa或惰性气体保护下、温度为80~180℃的条件下反应2~6h得到有机改性三聚氰胺聚磷酸盐。最终制得产品的结构式为式中,m和n为聚合度,m≥1,n≥1;产品阻燃性能优异,并且对阻燃高分子材料的物理和化学性能影响小。本发明的制备方法,生产原料易得,合成工艺简单,成本低廉,易于工业化生产。

Description

一种有机改性三聚氰胺聚磷酸盐及其制备方法
技术领域
本发明属于阻燃剂领域,涉及一种有机改性三聚氰胺聚磷酸盐及其制备方法。
背景技术
目前,高分子材料由于其比强度高、来源广、价格低、品种多、功能全、易于加工等优势,被广泛应用于尖端技术、国防建设和国民经济等领域,成为现在社会生活不可缺少的材料。但其大多数是属于易燃或可燃的,这不仅仅限制其应用范围,频繁的火灾也给我们社会带来了严重的人员伤亡和经济损失。因此需要对高分子材料进行阻燃改性。目前应用较多、效果较好的阻燃剂属于卤系的阻燃剂,虽然较少的添加量可以达到很高的阻燃等级,但其燃烧会产生有毒和腐蚀性气体,部分卤系阻燃剂还会产生致癌的二噁英,对环境和人体都有很大的伤害。无卤阻燃剂是未来发展的重要方向,其中膨胀型阻燃剂高温受热时,表面产生一层均匀的炭质泡沫层,次层隔热、隔氧、抑烟,并能防止熔滴的产生,故其具有很好的阻燃效果。
三聚氰胺聚磷酸盐(MPP),属于典型的P-N协同膨胀型阻燃剂,集酸源、气源于一体,兼具磷系阻燃剂的凝聚相阻燃作用和氮系阻燃剂的气相阻燃作用,具有互补性,高聚物受强热或燃烧时,表面生成一层均匀的多孔炭质泡沫层,能起到隔氧、抑烟,防止产生熔滴的作用,具有良好的阻燃性能,同时能减少燃烧时释放的热量、烟量和毒气。因而应用较为广泛,可用于橡胶、环氧树脂、聚酯和尼龙等方面的阻燃。当然MPP也有其不足之处,如阻燃剂分子链上有一些未反应的羟基基团这会引发阻燃剂和基体的相容性差,还可能导致聚酯、聚酰胺和聚氨酯等树脂降解而使高分子材料力学强度大幅度下降,因此需要对MPP进行改性。由于MPP是大分子化合物所以很难溶解于溶剂中,用溶剂法来对其进行改性不仅成本高并且获得的效果欠佳;而且MPP分子链上的三聚氰胺基团位阻大,使得相邻的羟基基团因为位阻效应而反应活性降低。
目前改性MPP主要是采用金属离子的改性,如Zn、Cu、Mg等金属离子,如专利CN200510010255.7中公开了金属离子改性聚磷酸三聚氰胺盐及其制备方法,将金属氧化物和三聚氰胺加入含稀磷酸溶液的反应釜中,温度设定90℃,反应3h冷却、离心、分离、干燥得到中间产物,将中间产物放入高温反应釜中,260℃-300℃,聚合反应5h,冷却,气流粉碎得到目标产物。虽然该发明制得的产品提高了阻燃性能,但这种方法只是提高了MPP的起始分解温度,其中比较好的Zn-MPP,起始分解温度从277.3℃提高到339.7℃,而其改善相容性和机械强度并不明显。再如专利CN 105924651 A中公开一种高聚合度的三聚氰胺聚磷酸盐的制备方法,其中提及用磷钨酸、硅钨酸、钨酸、氟锑酸、锡酸、钼酸和磷钼酸中的一种或几种,对MPP改性,提高了MPP高温热稳定性。上述两个专利都没有改善阻燃剂和基体的相容性以提高阻燃性能。
因此,开发一种通过提高MPP与聚合物基体相容性以进一步提高产品阻燃性能的制备方法极具有现实意义。
发明内容
本发明的目的是针对现有三聚氰胺聚磷酸盐的不足,提供一种有机改性三聚氰胺聚磷酸盐(MPP)及其制备方法,本发明选用有机胺改性MPP,使改性MPP分子中同时存在膨胀阻燃体系的三元要素(酸源、炭源和气源),使得三元要素之间的阻燃协同作用效率更高,因此具有优异的阻燃性能;同时有机胺与MPP分子链上的羟基反应后,改善了MPP与聚合物基体的相容性,以及所阻燃高分子材料的物理和化学性能。
为了达到上述目的,本发明采用如下技术方案:
一种有机改性三聚氰胺聚磷酸盐的制备方法,首先将有机胺与三聚氰胺聚磷酸盐(MPP)分散在溶剂中,使得有机胺均匀浸润到MPP的分子之间,然后在压力为0~0.6MPa、温度为80~180℃的条件下反应2~8h,最后在压力为-0.01~-0.09MPa或惰性气体保护下、温度为80~180℃的条件下反应2~6h得到有机改性三聚氰胺聚磷酸盐;
所述有机胺的结构式如下:
式中,R1和R2各自独立地选自氢、烷基醇、烷基、胺基、醇胺基、芳香基和杂环胺基,R3为烷基醇、烷基、芳香基或杂环胺基;
所述三聚氰胺聚磷酸盐的粒径D50小于5微米;
所述溶剂为水、有机溶剂或二者的混合物。
作为优选的技术方案:
如上所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,所述有机胺为乙二胺、二乙烯三胺、三乙烯四胺、乙醇胺、二乙醇胺、三乙醇胺、C1~C18的脂肪胺、苯胺或杂环胺。
如上所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,所述杂环胺为哌嗪、吡咯、四氢吡咯、吡唑、咪唑或以上物质的衍生物。
如上所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,哌嗪的衍生物为二苯基哌嗪、2-甲基哌嗪、2-哌嗪羧酸、N-氨乙基哌嗪、N-乙基哌嗪或N-甲基哌嗪;
吡咯的衍生物为2,2'-二吡咯基甲烷、N-甲基吡咯或2-甲基吡咯;
四氢吡咯的衍生物为1-乙基-2-氨甲基四氢吡咯、1-甲基四氢吡咯、2-甲基四氢吡咯、1-乙基-2-氨甲基四氢吡咯、N-乙基-2-乙酰基吡咯或1-甲基-2-(β-羟乙基)四氢吡咯;
吡唑的衍生物为1-甲基吡唑、1-丙基-1H-吡唑、4-碘吡唑或1-苯磺酰吡唑;
咪唑的衍生物为2-甲基吡唑、2-乙基吡唑或2-苯基咪唑。
如上所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,所述有机胺与三聚氰胺聚磷酸盐的质量比为100:50~500,所述溶剂的加入量为100-500mL/100克三聚氰胺聚磷酸盐。
如上所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,所述有机溶剂为甲醇、乙醇、丙醇、丁醇、环己醇、乙二醇、丙酮、环己酮、甲基异丁基酮、甲苯和二甲苯中的一种以上;所述惰性气体为氮气或氩气;反应结束后对产物进行洗涤、抽滤和烘干。
本发明还提供一种由如上所述的制备方法制得的有机改性三聚氰胺聚磷酸盐,结构式如下:
式中,m和n为聚合度,m≥1,n≥1;
在制备方法和测试条件完全相同的条件下(即两种阻燃复合材料仅仅存在阻燃剂种类的差异),添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高9.8%以上,拉伸强度提高5%以上,缺口冲击强度提高8%以上。当该改性MPP应用在玻纤增强的聚酰胺时,有机胺形成的炭层可以黏附在玻璃纤维表面,有力消除玻璃纤维带来的“烛芯效应”,从而有效提高了阻燃体系对聚酰胺的阻燃效率,两者相容性好,物理性能也得到了一定的提高。
作为优选的技术方案:
如上所述的有机改性三聚氰胺聚磷酸盐,所述有机改性三聚氰胺聚磷酸盐的熔点为300~400℃,所述有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为300~380℃,700℃的成炭量为30~40wt%。
发明原理:
本发明采用有机胺对三聚氰胺聚磷酸盐进行改性,是因为三聚氰胺聚磷酸盐分子分子中存在未反应的羟基,通过使用小分子的有机胺进行掺杂改性,一方面增加了MPP和高分子基体的相容性,另一方面也增加了MPP膨胀型阻燃剂的炭源,增加体系的残炭量,改善炭层质量,从而有利于形成更加致密的炭层,同时由于酸源、碳源和气源三元阻燃要素存在于同一分子中,因此协同阻燃效率更高。有益效果:
(1)本发明的一种有机改性三聚氰胺聚磷酸盐的制备方法,将有机胺引入到MPP分子中,大大将少了MPP分子中的羟基含量,有效提高了阻燃剂与高分子基体的相容性,减小了MPP对被阻燃高分子材料的化学作用,而且通过控制引入的有机胺分子结构和加入量能实现最终产物的性能的可设计性;
(2)本发明的一种有机改性三聚氰胺聚磷酸盐的制备方法,由于改性后的MPP其分子中同时存在膨胀阻燃体系的三元要素(酸源、炭源和气源),因此在燃烧或热裂解过程中三元要素的相互作用协同性更好,膨胀发泡和炭层的形成效率更高,使得材料分解时表面形成更加致密的保护层,提高了阻燃效率;
(3)本发明的一种有机改性三聚氰胺聚磷酸盐的制备方法,生产原料易得,合成工艺简单,成本低廉,易于工业化生产;
(4)本发明的一种有机改性三聚氰胺聚磷酸盐,阻燃性能优异,并且对阻燃高分子材料的物理和化学性能影响小。
附图说明
图1为未改性三聚氰胺聚磷酸盐阻燃聚丙烯的扫描电镜图;
图2为哌嗪改性三聚氰胺聚磷酸盐阻燃聚丙烯的扫描电镜图。
具体实施方式
下面结合具体实施方式,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺乙二胺与粒径D50为4.8微米的三聚氰胺聚磷酸盐(MPP)以100:50的质量比分散在溶剂中,然后在压力为0MPa、温度为80℃的条件下反应8h,最后在压力为-0.01MPa、温度为180℃的条件下反应2h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为水,溶剂加入量为100mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为1,n为2,
为离子态的乙二胺;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为320℃,700℃的成炭量为30wt%,熔点为300℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高10.0%,拉伸强度提高5.0%,缺口冲击强度提高8.2%。
实施例2
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺二乙烯三胺与粒径D50为4.9微米的三聚氰胺聚磷酸盐(MPP)以100:500的质量比分散在溶剂中,然后在压力为0.6MPa、温度为180℃的条件下反应2h,最后在压力为-0.09MPa、温度为80℃的条件下反应6h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为甲醇,溶剂加入量为500mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为2,n为3,
为离子态的二乙烯三胺;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为300℃,700℃的成炭量为35wt%,熔点为320℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高9.8%,拉伸强度提高5.2%,缺口冲击强度提高8.1%。
实施例3
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺哌嗪与粒径D50为4.3微米的三聚氰胺聚磷酸盐(MPP)以100:275的质量比分散在溶剂中,然后在压力为0.3MPa、温度为130℃的条件下反应5h,最后在压力为-0.05MPa、温度为130℃的条件下反应4h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为甲醇水溶液(体积比为1:1),溶剂加入量为300mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为1,n为1,
为离子态的哌嗪;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为380℃,700℃的成炭量为40wt%,熔点为400℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高11.2%,拉伸强度提高5.2%,缺口冲击强度提高8.8%,其与聚丙烯的复合材料扫描电镜图如图2所示,图1为未改性三聚氰胺聚磷酸盐阻燃聚丙烯的扫描电镜图,对比图1和图2可以看出有机胺改性后相容性明显改善。
实施例4
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺乙醇胺与粒径D50为4.0微米的三聚氰胺聚磷酸盐(MPP)以100:400的质量比分散在溶剂中,然后在压力为0.2MPa、温度为140℃的条件下反应5h,最后在压力为-0.04MPa、温度为100℃的条件下反应5h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为乙醇,溶剂加入量为200mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为3,n为1,
为离子态的乙醇胺;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为360℃,700℃的成炭量为38wt%,熔点为360℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高10.6%,拉伸强度提高5.4%,缺口冲击强度提高8.3%。
实施例5
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺二乙醇胺与粒径D50为4.5微米的三聚氰胺聚磷酸盐(MPP)以100:300的质量比分散在溶剂中,然后在压力为0.5MPa、温度为160℃的条件下反应6h,最后在氮气保护下、温度为100℃的条件下反应3h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为甲醇/乙醇混合溶液(体积比为1:1),溶剂加入量为400mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为2,n为3,
为离子态的二乙醇胺;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为365℃,700℃的成炭量为34wt%,熔点为380℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高10.3%,拉伸强度提高5.6%,缺口冲击强度提高8.5%。
实施例6
一种有机改性三聚氰胺聚磷酸盐的制备方法,其步骤如下:
首先将有机胺三乙醇胺与粒径D50为4.6微米的三聚氰胺聚磷酸盐(MPP)以100:100的质量比分散在溶剂中,然后在压力为0.1MPa、温度为90℃的条件下反应6h,最后在氩气保护下、温度为90℃的条件下反应2.5h,反应结束后对产物进行洗涤、抽滤和烘干得到有机改性三聚氰胺聚磷酸盐,其中溶剂为甲醇/乙醇/丙醇混合溶液(体积比为1:1:2),溶剂加入量为250mL/100克三聚氰胺聚磷酸盐。
最终制得的有机改性三聚氰胺聚磷酸盐的结构式为
式中,m和n为聚合度,m为2,n为2,
为离子态的三乙醇胺;
该有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为375℃,700℃的成炭量为39wt%,熔点为390℃。在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高10.8%,拉伸强度提高5.4%,缺口冲击强度提高8.4%。
实施例7~16
实施例7~16制备步骤及各实验条件同实施例1,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率1、2、3分别是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数、拉伸强度与缺口冲击强度的提高百分率)。
实施例17~26
实施例17~26制备步骤及各实验条件同实施例2,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高的百分率)。
实施例27~31
实施例27~31制备步骤及各实验条件同实施例3,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高的百分率)。
实施例32~36
实施例32~36制备步骤及各实验条件同实施例4,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高的百分率)。
实施例37~46
实施例37~46制备步骤及各实验条件同实施例5,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高的百分率)。
实施例47~51
实施例47~51制备步骤及各实验条件同实施例6,仅原料乙二胺的种类和溶剂不同,其原料及产品参数如下所示(注:m和n为聚合度,X是指产品结构式中为离子态的X,温度是指产品热失重5wt%的温度,成炭量是指产品700℃时的成炭量,提高率是指在制备方法和测试条件完全相同的条件下,添加本产品的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料极限氧指数提高的百分率)。

Claims (8)

1.一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征是:首先将有机胺与三聚氰胺聚磷酸盐分散在溶剂中,然后在压力为0~0.6MPa、温度为80~180℃的条件下反应2~8h,最后在压力为-0.01~-0.09MPa或惰性气体保护下、温度为80~180℃的条件下反应2~6h得到有机改性三聚氰胺聚磷酸盐;
所述有机胺的结构式如下:
式中,R1和R2各自独立地选自氢、烷基醇、烷基、胺基、醇胺基、芳香基和杂环胺基,R3为烷基醇、烷基、芳香基或杂环胺基;
所述三聚氰胺聚磷酸盐的粒径D50小于5微米;
所述溶剂为水、有机溶剂或二者的混合物。
2.根据权利要求1所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征在于,所述有机胺为乙二胺、二乙烯三胺、三乙烯四胺、乙醇胺、二乙醇胺、三乙醇胺、C1~C18的脂肪胺、苯胺或杂环胺。
3.根据权利要求2所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征在于,所述杂环胺为哌嗪、吡咯、四氢吡咯、吡唑、咪唑或以上物质的衍生物。
4.根据权利要求3所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征在于,哌嗪的衍生物为二苯基哌嗪、2-甲基哌嗪、2-哌嗪羧酸、N-氨乙基哌嗪、N-乙基哌嗪或N-甲基哌嗪;
吡咯的衍生物为2,2'-二吡咯基甲烷、N-甲基吡咯或2-甲基吡咯;
四氢吡咯的衍生物为1-乙基-2-氨甲基四氢吡咯、1-甲基四氢吡咯、2-甲基四氢吡咯、1-乙基-2-氨甲基四氢吡咯、N-乙基-2-乙酰基吡咯或1-甲基-2-(β-羟乙基)四氢吡咯;
吡唑的衍生物为1-甲基吡唑、1-丙基-1H-吡唑、4-碘吡唑或1-苯磺酰吡唑;
咪唑的衍生物为2-甲基吡唑、2-乙基吡唑或2-苯基咪唑。
5.根据权利要求1所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征在于,所述有机胺与三聚氰胺聚磷酸盐的质量比为100:50~500,所述溶剂的加入量为100~500mL/100克三聚氰胺聚磷酸盐。
6.根据权利要求1所述的一种有机改性三聚氰胺聚磷酸盐的制备方法,其特征在于,所述有机溶剂为甲醇、乙醇、丙醇、丁醇、环己醇、乙二醇、丙酮、环己酮、甲基异丁基酮、甲苯和二甲苯中的一种以上;所述惰性气体为氮气或氩气;反应结束后对产物进行洗涤、抽滤和烘干。
7.采用如权利要求1~6任一项所述的制备方法制得的有机改性三聚氰胺聚磷酸盐,其特征是,结构式如下:
式中,m和n为聚合度,m≥1,n≥1;
在制备方法和测试条件完全相同的条件下,添加有机改性三聚氰胺聚磷酸盐的阻燃复合材料相对于添加未改性三聚氰胺聚磷酸盐的阻燃复合材料,极限氧指数提高9.8%以上,拉伸强度提高5%以上,缺口冲击强度提高8%以上。
8.根据权利要求7所述的有机改性三聚氰胺聚磷酸盐,其特征在于,所述有机改性三聚氰胺聚磷酸盐的熔点为300~400℃,所述有机改性三聚氰胺聚磷酸盐的热失重5wt%的温度为300~380℃,700℃的成炭量为30~40wt%。
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