CN109593226A - 一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及其制备泡沫材料的方法 - Google Patents

一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及其制备泡沫材料的方法 Download PDF

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CN109593226A
CN109593226A CN201811367958.9A CN201811367958A CN109593226A CN 109593226 A CN109593226 A CN 109593226A CN 201811367958 A CN201811367958 A CN 201811367958A CN 109593226 A CN109593226 A CN 109593226A
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rigid foam
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刘树骏
冯伟
李善清
王善华
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SHANDONG PROV INST OF MARINE CHEMICAL SCIENCE
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Abstract

本发明公开了一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及制备泡沫材料的方法，配方的原料组成包括：聚醚多元醇、多亚甲基多苯基异氰酸酯、催化剂份、泡沫稳定剂、发泡剂、磷系阻燃剂、膨胀石墨、无机阻燃晶须。将上述原料混合均匀倒入模具中进行发泡，发泡完成后制得低收缩率阻燃聚氨酯硬质泡沫材料。用该配方可实现无氟无卤环保阻燃、收缩率低的制作泡沫材料。

Description

一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及其制备泡沫 材料的方法
技术领域
本发明涉及一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及用该配方制备泡沫材料的方法。
背景技术
硬质聚氨酯 (RPUR) 泡沫是一种耐化学试剂腐蚀，力学性能优异的泡沫材料，因其导热系数低，隔热性好，同时兼具的良好的耐老化性能和耐化学优势，更重要的是其具有很强的粘结力，与很多材料能够形成良好的粘结效果，因此聚氨酯泡沫材料在建筑建材、家居、交通运输等领域应用十分广泛。虽然聚氨酯泡沫材料具有良好的材料应用性能，但仍然需要相应完善的阻燃体系，以使其达到国家建筑材料所规定的阻燃标准并具有良好的经济技术性。
聚氨酯泡沫易燃，不添加阻燃剂的聚氨酯泡沫极限氧指数基本只有18%左右。而现今大量应用在聚氨酯泡沫的阻燃剂主要为卤系和无机金属氢氧化物阻燃剂。卤系阻燃剂燃烧毒性较大，而无机金属氢氧化物需要添加较大比例的量才能达到较好的阻燃效果，但大比例的使用无机金属氢氧化物，则容易导致阻燃材料力学性能降低，影响了阻燃材料的使用效果。
现今环保要求限制了卤素阻燃剂和氯氟发泡剂的应用，阻燃剂无卤化和发泡剂环境友好型的趋势使磷酸酯阻燃剂、无机纳米阻燃剂和环戊烷发泡剂得到很大应用。但是磷酸酯阻燃剂大部分为液体，阻燃的同时还有增塑作用，而环戊烷发泡剂沸点高（49.2℃），温度较低时易液化，导致泡沫内压力减小，两者都会导致泡沫材料成型收缩率大，严重影响泡沫材料的机械性能和实际使用。
近年来纳米无机材料填充阻燃聚氨酯泡沫研究较多，但是补强性能、耐热性能更好的无机晶须材料增强阻燃聚氨酯泡沫研究很少。且无机晶须材料补强塑料收缩率极低，同时具有良好的阻燃性能，与沸点（27.8℃）较低的异戊烷同时用于聚氨酯阻燃发泡可以达到更小的成型收缩率和更好的阻燃性能。
发明内容
本发明的目的之一是提供一种低收缩率阻燃聚氨酯硬质泡沫材料的配方。
为了实现上述发明目的，本发明所提供的低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计包括：聚醚多元醇25-30份、多亚甲基多苯基异氰酸酯35-45份、催化剂1-2份、泡沫稳定剂1-3份、发泡剂2-4份、磷系阻燃剂10-25份、膨胀石墨5-10份、无机阻燃晶须5-15份。
所述系阻燃剂为甲基膦酸二甲酯、乙基膦酸二乙酯、磷酸三苯酯、季戊四醇磷酸酯、环磷酰胺、对苯二酚-双（磷酸二苯酯）和焦磷酸哌嗪中的一种或两种以上任意质量比的组合。
所述的膨胀石墨规格为80-120目，膨胀倍率为250-300。
所述无机阻燃晶须为硫酸镁晶须、氢氧化镁晶须、水合碱式硫酸镁晶须、硫酸钙晶须、硅酸钙晶须中的一种或两种以上任意质量比的组合。
所述的聚醚多元醇为聚醚多元醇4110，其羟基值为455±20 mgKOH/g、黏度为3500±1000 mPa·s /25℃。
所述催化剂为二月桂酸二丁基锡和胺类催化剂任意质量比的组合；所述泡沫稳定剂为水溶性硅油。
所述的发泡剂为水和异戊烷的组合，所述水和异戊烷的质量比为2:6或者1:12。
本发明的目的之二是提供一种利用上述配方生产低收缩率阻燃聚氨酯硬质泡沫材料的方法，该方法包括以下步骤：在20-30℃温度条件下，先将聚醚多元醇、催化剂、泡沫稳定剂和发泡剂混合并搅拌均匀，再加入磷系阻燃剂、膨胀石墨和无机晶须并搅拌均匀，最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，从而获得温度为20-30℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后再经熟化处理，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
所述聚醚多元醇、催化剂、泡沫稳定剂和发泡剂混合时的搅拌速度为800-1200r/min，搅拌时间为10-15秒；加入磷系阻燃剂、膨胀石墨和无机晶须后的搅拌速度为800-1200r/min，搅拌时间为15-20秒；加入多亚甲基多苯基异氰酸酯后的搅拌速度为1500-2000r/min，搅拌时间为8-12秒。
所述熟化处理的方式为：在温度40℃-50℃条件下熟化4-6小时后再常温熟化6-12小时。
本发明使用水与异戊烷作为发泡剂，替代全水发泡和环戊烷发泡，解决了全水发泡聚氨酯泡沫发脆和环戊烷发泡成型收缩率较大的问题，且无氟环保。阻燃复配试剂选择磷酸酯、膨胀石墨与无机阻燃晶须复配，将无机阻燃晶须作为阻燃补强剂用于硬质聚氨酯泡沫中，一方面利用晶须的耐高温性能、凝聚相阻燃性能和与树脂良好的相容性，另一方面还同时利用其高补强性和增强塑料时的低成型收缩率的特点，改善大量使用液体磷酸酯阻燃剂带来的泡沫成型收缩率大的普遍问题，实现无氟无卤环保阻燃，低成型收缩率的硬质聚氨酯泡沫材料的制备。
本发明所使用原料皆为市售，其中：甲基膦酸二甲酯的英文名称缩写为DMMP，乙基膦酸二乙酯的英文名称缩写为DEEP，磷酸三苯酯的英文名称缩写为TPP, 对苯二酚-双（磷酸二苯酯）的英文名称缩写为RDP。
具体实施方式
实施例1
低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计为：
聚醚多元醇 25份，
三乙烯二胺 0.6份，
二月桂酸二丁基锡 0.4份，
水溶性硅油 1.5份，
水 0.5份，
异戊烷 1.5份，
DMMP 12份，
膨胀石墨 8份，
硫酸镁晶须 10份，
多亚甲基多苯基异氰酸酯 37.5份。
制作低收缩率阻燃聚氨酯硬质泡沫材料的步骤如下：
按配方中各原料的配比关系取各原料；在25℃温度条件下，先将聚醚多元醇、三乙烯二胺、二月桂酸二丁基锡、水溶性硅油、水和异戊烷混合并搅拌均匀，搅拌速度为800r/min，搅拌时间为10秒；再加入DMMP、膨胀石墨和硫酸镁晶须并搅拌均匀，搅拌速度为1000r/min，搅拌时间为15秒；最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，搅拌时间10秒、搅拌速度为1800r/min，从而获得温度为25℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后在温度50℃的条件下经熟化处理5小时，出模后再常温熟化处理 6小时，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
实施例2
低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计为：
聚醚多元醇 25份，
三乙烯二胺 0.6份 ，
二月桂酸二丁基锡 0.4份 ，
水溶性硅油 1.5份 ，
水 0.25份 ，
异戊烷 3份，
DMMP 8份，
TPP 6份 ，
膨胀石墨 6份 ，
氢氧化镁晶须 6份，
多亚甲基多苯基异氰酸酯 39份。
制作低收缩率阻燃聚氨酯硬质泡沫材料的步骤如下：
按配方中各原料的配比关系取各原料；在25℃温度条件下，先将聚醚多元醇、三乙烯二胺、二月桂酸二丁基锡、水溶性硅油、水和异戊烷混合并搅拌均匀，搅拌速度为800r/min，搅拌时间为10秒；再加入DMMP、TPP、膨胀石墨和氢氧化镁晶须并搅拌均匀，搅拌速度为 800r/min，搅拌时间为15s；最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，搅拌时间10秒、搅拌速度为1800r/min，从而获得温度为25℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后在温度 40℃的条件下经熟化处理6小时，出模后再常温熟化处理 10小时，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
实施例3
低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计为：
聚醚多元醇 24份，
三乙烯二胺 0.6份，
二月桂酸二丁基锡 0.4份，
水溶性硅油 1.5份，
水 0.5份，
异戊烷 1.5份，
RDP 10份，
膨胀石墨 10份，
硫酸铝晶须 5份，
硅酸钙晶须 5份，
多亚甲基多苯基异氰酸酯 37.5份。
制作低收缩率阻燃聚氨酯硬质泡沫材料的步骤如下：
按配方中各原料的配比关系取各原料；在25℃温度条件下，先将聚醚多元醇、三乙烯二胺、二月桂酸二丁基锡、水溶性硅油、水和异戊烷混合并搅拌均匀，搅拌速度为800r/min，搅拌时间为12秒；再加入RDP、膨胀石墨、硫酸铝晶须和硅酸钙晶须并搅拌均匀，搅拌速度为1000r/min，搅拌时间为15秒；最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，搅拌时间10秒、搅拌速度为1800r/min，从而获得温度为25℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后在温度40℃的条件下经熟化处理6小时，出模后再常温熟化处理6小时，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
实施例4
低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计为：
聚醚多元醇 26份，
三乙烯二胺 0.6份，
二月桂酸二丁基锡 0.4份，
水溶性硅油 1.5份，
水 0.5份，
异戊烷 1.5份，
DMMP 8份，
环磷酰胺 6份，
膨胀石墨 6份，
硫酸钙晶须 7份，
多亚甲基多苯基异氰酸酯 40份。
制作低收缩率阻燃聚氨酯硬质泡沫材料的步骤如下：
按配方中各原料的配比关系取各原料；在25℃温度条件下，先将聚醚多元醇、三乙烯二胺、二月桂酸二丁基锡、水溶性硅油、水和异戊烷混合并搅拌均匀，搅拌速度为 800r/min，搅拌时间为10秒；再加入DMMP、环磷酰胺、膨胀石墨和硫酸钙晶须并搅拌均匀，搅拌速度为800r/min，搅拌时间为10秒；最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，搅拌时间10秒、搅拌速度为1800r/min，从而获得温度为25℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后在温度60℃的条件下经熟化处理6小时，出模后再常温熟化处理10小时，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
实施例5
低收缩率阻燃聚氨酯硬质泡沫材料的配方的原料组成按重量配比关系计为：
聚醚多元醇 22份，
三乙烯二胺 0.6份，
二月桂酸二丁基锡 0.4份，
水溶性硅油 1.5份，
水 0.25份，
异戊烷 3份，
DEEP 6份，
焦磷酸哌嗪 6份，
膨胀石墨 6份，
水合碱式硫酸镁晶须 14份，
多亚甲基多苯基异氰酸酯 36份。
制作低收缩率阻燃聚氨酯硬质泡沫材料的步骤如下：
按配方中各原料的配比关系取各原料；在25℃温度条件下，先将聚醚多元醇、三乙烯二胺、二月桂酸二丁基锡、水溶性硅油、水和异戊烷混合并搅拌均匀，搅拌速度为800r/min，搅拌时间为12秒；再加入DEEP、焦磷酸哌嗪、膨胀石墨和水合碱式硫酸镁晶须并搅拌均匀，搅拌速度1000r/min，搅拌时间10秒；最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，搅拌时间10秒、搅拌速度为1800r/min，从而获得温度为25℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后在温度50℃的条件下经熟化6小时，出模后再常温熟化处理6小时，便制得低收缩率阻燃聚氨酯硬质泡沫材料。

Claims (10)

1.一种低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于该配方的原料组成按重量配比关系计包括：聚醚多元醇20-30份、多亚甲基多苯基异氰酸酯35-45份、催化剂1-2份、泡沫稳定剂1-3份、发泡剂2-4份、磷系阻燃剂10-25份、膨胀石墨5-10份、无机阻燃晶须5-15份。
2.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述系阻燃剂为甲基膦酸二甲酯、乙基膦酸二乙酯、磷酸三苯酯、季戊四醇磷酸酯、环磷酰胺、对苯二酚-双（磷酸二苯酯）和焦磷酸哌嗪中的一种或两种以上任意质量比的组合。
3.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述的膨胀石墨规格为80-120目，膨胀倍率为250-300。
4.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述无机阻燃晶须为硫酸镁晶须、氢氧化镁晶须、水合碱式硫酸镁晶须、硫酸钙晶须、硅酸钙晶须中的一种或两种以上任意质量比的组合。
5.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述的聚醚多元醇为聚醚多元醇4110，其羟基值为455±20 mgKOH/g、黏度为3500±1000 mPa·s/25℃。
6.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述催化剂为二月桂酸二丁基锡和胺类催化剂任意质量比的组合；所述泡沫稳定剂为水溶性硅油。
7.如权利要求1所述的低收缩率阻燃聚氨酯硬质泡沫材料的配方，其特征在于所述的发泡剂为水和异戊烷的组合，所述水和异戊烷的质量比为2:6或者1:12。
8.一种用权利要求1-7中任一权利要求所述的配方制备低收缩率阻燃聚氨酯硬质泡沫材料方法，其特征在于包括以下步骤：在20-30℃温度条件下，先将聚醚多元醇、催化剂、泡沫稳定剂和发泡剂混合并搅拌均匀，再加入磷系阻燃剂、膨胀石墨和无机晶须并搅拌均匀，最后加入多亚甲基多苯基异氰酸酯并搅拌均匀，从而获得温度为20-30℃的混合物料；将混合物料倒入发泡模具中进行发泡，物料发泡成型后再经熟化处理，便制得低收缩率阻燃聚氨酯硬质泡沫材料。
9.如权利要求8所述的制备低收缩率阻燃聚氨酯硬质泡沫材料方法，其特征在于所述聚醚多元醇、催化剂、泡沫稳定剂和发泡剂混合时的搅拌速度为800-1200r/min，搅拌时间为10-15秒；加入磷系阻燃剂、膨胀石墨和无机晶须后的搅拌速度为800-1200r/min，搅拌时间为15-20秒；加入多亚甲基多苯基异氰酸酯后的搅拌速度为1500-2000r/min，搅拌时间为8-12秒。
10.如权利要求8所述的制备低收缩率阻燃聚氨酯硬质泡沫材料方法，其特征在于所述熟化处理的方式为：在温度40℃-50℃条件下熟化4-6小时后再常温熟化6-12小时。
CN201811367958.9A 2018-11-16 2018-11-16 一种低收缩率阻燃聚氨酯硬质泡沫材料的配方及其制备泡沫材料的方法 Withdrawn CN109593226A (zh)

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