CN109354669A - 一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料 - Google Patents

一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料 Download PDF

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CN109354669A
CN109354669A CN201811060515.5A CN201811060515A CN109354669A CN 109354669 A CN109354669 A CN 109354669A CN 201811060515 A CN201811060515 A CN 201811060515A CN 109354669 A CN109354669 A CN 109354669A
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钱立军
李林洁
许博
许健哲
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Abstract

本发明公开了一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其原料包括反应型阻燃剂2‑6质量份，添加型阻燃剂15‑40质量份，聚醚多元醇80‑100质量份，催化剂5‑10质量份，发泡剂10‑20质量份，泡沫稳定剂2‑6质量份，多异氰酸酯100‑150质量份。该材料由反应型阻燃剂TGIC‑DOPO和添加型阻燃剂甲基膦酸二甲酯、可膨胀石墨、氢氧化铝多元复配阻燃，其极限氧指数达到32％以上，热释放速率峰值降低到120kW/m2以下，平均有效燃烧热降低到9MJ/kg以下，总热释放量降低到9MJ/m2以下，并且具有自熄灭现象，熄灭时间降低到50秒以下，同时具有高强度，低密度和低导热系数。

Description

一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料
技术领域
本发明涉及一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，尤其是一种由添加型阻燃剂和反应型阻燃剂复配的具有高效阻燃特性的硬质聚氨酯泡沫，属于利用多种材料复配组合的方式制备阻燃性能材料的技术领域。
背景技术
硬质聚氨酯泡沫(RPUF)具有绝热效果好、重量轻、比强度大、施工方便等优良特性，广泛应用于冰箱、冰柜的箱体绝热层、冷库、冷藏车的绝热材料和建筑物、储罐及管道的保温材料。
硬质聚氨酯泡沫的极限氧指数只有19.4％，属于极易燃烧的一种材料，为了使RPUF更安全广泛的应用到生产生活中，需要对RPUF的阻燃改性进行研究，目前RPUF中常用的阻燃剂有添加型和反应型两种。
专利申请号CN201711443995.9公开了一种基于可膨胀石墨的含磷阻燃硬质聚氨酯泡沫及其制备方法：其特点在于在不改变聚氨酯结构的前提下提硬质聚氨酯泡沫的阻燃性,并且不存在长期服役的迁移现象，但其中可膨胀石墨添加量过多，密度过高，并且阻燃效果有限；专利申请号CN201710440608.X公开了一种聚氨酯硬质泡沫材料及其制备方法与应用，该专利采用的液体阻燃剂为含卤阻燃剂，所制造的材料受热会产生大量的烟雾和有毒的腐蚀性卤化氢气体，造成二次危害。
发明内容
本发明采用添加型阻燃剂与反应型阻燃剂复配，制备出一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，本发明通过在硬质聚氨酯泡沫中添加了多种阻燃剂，降低了每种阻燃剂的用量并且结合了各阻燃剂的作用，制得了高效阻燃硬质聚氨酯材料。
本发明所采用的阻燃剂包括反应型阻燃剂和添加型阻燃剂，其中反应型阻燃剂是三-(3-DOPO-2-羟基-丙基)-1,3,5-三嗪-2,4,6-三酮(TGIC-DOPO)，添加型阻燃剂包括甲基膦酸二甲酯(DMMP)、可膨胀石墨(EG)、氢氧化铝(ATH)，其中TGIC-DOPO结构式如下
本发明的接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料的制备方法，包括如下步骤：
第一步：取2-6质量份反应型阻燃剂，15-40质量份添加型阻燃剂，80-100质量份的聚醚多元醇，5-10质量份的催化剂，10-20质量份的发泡剂，2-6质量份的泡沫稳定剂，在室温下充分混合搅拌得到混合液A。
第二步：将充分搅拌的混合液A与100-150质量份的多异氰酸酯进行快速混合搅拌得到混合液B。
第三步：将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料。
上述方案中，聚醚多元醇选自DSU-450L、DSU-450M、DSU-450K中的一种或几种；多异氰酸酯选自MDI、TDI、PAPI中的一种或多种；催化剂包括五甲基二亚乙烯三胺、N,N-二甲基环己胺、质量浓度30％的醋酸钾溶液；发泡剂为水和HCFC-141b混合；泡沫稳定剂是SD-622。
本发明制得的聚氨酯泡沫，结构式如下
本发明通过反应型阻燃剂TGIC-DOPO和添加型阻燃剂DMMP、EG、ATH共同阻燃改性硬质聚氨酯泡沫材料，充分发挥了每种阻燃剂的阻燃作用，得到的聚氨酯材料极限氧指数达到32％以上，热释放速率峰值降低到120kW/m2以下，平均有效燃烧热降低到9MJ/kg以下，总热释放量降低到9MJ/m2以下，并且具有自熄灭现象，熄灭时间降低到50秒以下，在提高了阻燃效果的同时还维持了材料的压缩强度，较低的密度和导热系数，从而获得了高阻燃性，高强度，低导热系数和低密度的硬质聚氨酯泡沫材料，并且制备方法简单，有利于工业化生产。
在本发明构建的硬质聚氨酯复合阻燃体系中，与含有羟基的磷杂菲/三嗪三酮双基阻燃剂TGIC-DOPO相比，具有类似结构的不含羟基的磷杂菲/三嗪三酮双基阻燃剂TAIC-DOPO结构式如下，阻燃改性硬质聚氨酯泡沫时，得到的聚氨酯材料热释放速率峰值在150kW/m2以上,平均有效燃烧热在17MJ/kg以上，总热释放量在18MJ/m2以上，熄灭时间在100秒以上，其热释放速率峰值，平均有效燃烧热，总热释放量，熄灭时间都明显高于TGIC-DOPO阻燃体系，说明了TGIC-DOPO阻燃体系相比TAIC-DOPO阻燃体系能够赋予聚氨酯材料更加优异的阻燃性能。
具体实施方式
实施例1
将2质量份的反应型阻燃剂TGIC-DOPO，30质量份的添加型阻燃剂，DMMP:ATH:EG＝10:14:6，80质量份的聚醚多元醇DSU-450L，6质量份的催化剂,五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝1:4:1，10质量份的发泡剂,水：HCFC-141b＝1:9，2质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与100质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例2
将4质量份的反应型阻燃剂TGIC-DOPO，26质量份的添加型阻燃剂，DMMP:ATH:EG＝8:14:4，取90质量份的聚醚多元醇DSU-450M，7质量份的催化剂五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:4:1，15质量份的发泡剂，水：HCFC-141b＝2:13，4质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与110质量份的多异氰酸酯MDI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例3
将2质量份的反应型阻燃剂TGIC-DOPO，28质量份的添加型阻燃剂，DMMP:ATH:EG＝6:16:6，取100质量份的聚醚多元醇DSU-450M，8质量份的催化剂五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:4:2，14质量份的发泡剂，水：HCFC-141b＝1:13，3质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与140质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例4
将4质量份的反应型阻燃剂TGIC-DOPO，24质量份的添加型阻燃剂，DMMP:ATH:EG＝6:12:6，取90质量份的聚醚多元醇DSU-450L，8质量份的催化剂，五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:4:2，16质量份的发泡剂，水：HCFC-141b＝2:14，6质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与140质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例5
将6质量份的反应型阻燃剂TGIC-DOPO，20质量份的添加型阻燃剂，DMMP:ATH:EG＝6:10:4，100质量份的聚醚多元醇DSU-450L，9质量份的催化剂，五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:5:2，20质量份的发泡剂，水：HCFC-141b＝3:17，5质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与150质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例6
将20质量份的添加型阻燃剂，DMMP:ATH:EG＝6:10:4，100质量份的聚醚多元醇DSU-450L，9质量份的催化剂，五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:5:2，20质量份的发泡剂，水：HCFC-141b＝3:17，5质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与150质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
实施例7
将6质量份的阻燃剂TGIC-DOPO，20质量份的添加型阻燃剂，DMMP:ATH:EG＝6:10:4，100质量份的聚醚多元醇DSU-450L，9质量份的催化剂，五甲基二亚乙烯三胺：N,N-二甲基环己胺：30％的醋酸钾溶液＝2:5:2，20质量份的发泡剂，水：HCFC-141b＝3:17，5质量份的泡沫稳定剂SD-622，在室温下充分混合搅拌得到混合液A，将充分搅拌的混合液A与150质量份的多异氰酸酯PAPI进行快速混合搅拌得到混合液B，将混合完成的混合液B倒入模具当中进行固化24小时后，获得硬质聚氨酯泡沫材料，将制得的聚氨酯进行性能测试，结果见表1。
表1聚氨酯性能测试结果

Claims (8)

1.一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，是在聚氨酯泡沫组合物中加入了反应型阻燃剂和添加型阻燃剂制备而成，其中反应型阻燃剂是三-(3-DOPO-2-羟基-丙基)-1,3,5-三嗪-2,4,6-三酮(TGIC-DOPO)，添加型阻燃剂包括甲基膦酸二甲酯(DMMP)、可膨胀石墨(EG)和氢氧化铝(ATH)，其中TGIC-DOPO结构式如下
2.根据权利要求1所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，结构式如下
3.根据权利要求1所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，该材料采用如下方法制得：
将2-6质量份反应型阻燃剂，15-40质量份添加型阻燃剂，80-100质量份聚醚多元醇，5-10质量份催化剂，10-20质量份发泡剂，2-6质量份泡沫稳定剂在室温下充分混合搅拌得到混合液A；
将充分搅拌的混合液A与100-150质量份多异氰酸酯混合获得混合液B，倒入模具中固化获得接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料。
4.根据权利要求3所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，所述的聚醚多元醇为DSU-450L、DSU-450M、DSU-450K中的一种或几种。
5.根据权利要求3所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，所述的催化剂选自五甲基二亚乙烯三胺、N,N-二甲基环己胺、质量浓度为30％的醋酸钾溶液的一种或多种。
6.根据权利要求3所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，所述的发泡剂为水和HCFC-141b的混合。
7.根据权利要求3所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，所述的泡沫稳定剂为SD-622。
8.根据权利要求3所述的一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料，其特征在于，所述的多异氰酸酯为MDI、TDI、PAPI中的一种或几种。
CN201811060515.5A 2018-09-12 2018-09-12 一种接入磷杂菲基团的高效阻燃硬质聚氨酯泡沫材料 Pending CN109354669A (zh)

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