CN106167541A - 连续式生产pir 大块泡用组合聚醚及其制备方法和应用 - Google Patents

连续式生产pir 大块泡用组合聚醚及其制备方法和应用 Download PDF

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CN106167541A
CN106167541A CN201610628638.9A CN201610628638A CN106167541A CN 106167541 A CN106167541 A CN 106167541A CN 201610628638 A CN201610628638 A CN 201610628638A CN 106167541 A CN106167541 A CN 106167541A
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徐业峰
朱文静
李明友
念以亭
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Shandong Inov New Material Co Ltd
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Abstract

本发明属于聚氨酯技术领域，具体涉及一种连续式生产PIR大块泡用组合聚醚及其制备方法和应用。所述组合聚醚由A组分和B组分构成，其中A组份由聚酯多元醇、聚醚多元醇、泡沫稳定剂、化学发泡剂、催化剂、阻燃剂和物理发泡剂组成；B组份为多亚甲基多苯基多异氰酸酯。使用时，将A、B组份料经高压发泡机混合即可连续式生产PIR高阻燃大块泡。本发明A组分料生产过程简单，无三废排放，由A、B组分料生产PIR型绝热材料操作工艺简单，易操作，无破坏大气层气体挥发，产品质量稳定，生产成本低，在达到环保目的的同时，实现了制品较好的低温尺寸稳定性、阻燃性，且密度分布均匀、热传导率低、抗压强度高、吸水率低。

Description

连续式生产PIR大块泡用组合聚醚及其制备方法和应用
技术领域
本发明属于聚氨酯技术领域，具体涉及一种连续式生产PIR大块泡用组合聚醚及其制备方法和应用。
背景技术
聚异氰脲酸酯泡沫(PIR泡沫)是由聚醚多元醇或聚酯多元醇与异氰酸酯反应而成。在三聚催化剂作用下，过量的异氰酸酯反应生成六元环，给泡沫提供交联的同时还通过自身的六元环分子结构促使燃烧结焦成炭，提高了泡沫体系的防火性能。与聚氨酯PUR泡沫相比，聚异氰脲酸酯泡沫具有更好的尺寸稳定性，更低的热分解率，更高的机械强度。通过调整聚异氰酸酯浓度及其配方，防火性能可达B1级。
参照国际的先进技术与设备，采用连续式发泡生产线生产PIR块泡技术与国内普遍存在的非连续式生产方式相比具有泡沫品质稳定、密度均匀，保温性能突出；产能更大且可靠；泡沫块大、成品管壳尺寸长，可节省施工时间的显著特点。连续式生产以其优异的性能，被广泛应用于建筑节能、工业保温、冷链系统、新能源、军工领域等行业。
随着141b替代工作的逐步完成，戊烷已经成为聚氨酯行业的主流发泡剂，聚氨酯硬质泡沫的新技术、新工艺以及新材料的应用也进入一个崭新的连续化生产的新时代，其高质、高效、快速大量生产是连续化生产的显著特点。使用戊烷的泡沫阻燃性能有所下降、泡沫尺寸稳定性比其他发泡剂要差、导热系数较141b要高。
目前亟需开发一种密度分布更均匀、导热系数更低、尺寸稳定性更高、阻燃性能更优秀的PIR大块泡用组合聚醚。
发明内容
本发明的目的是提供一种连续式生产PIR大块泡用组合聚醚，提高了三聚转化效率及流动性，制得的PIR大块泡密度分布均匀、热传导率低、抗压强度高、吸水率低、稳定性好；本发明同时提供其制备方法和应用。
本发明所述的连续式生产PIR大块泡用组合聚醚，由A组分和B组分构成，A组分和B组分的重量百分比为100:170-175，其中：
A组份为，以重量百分数计：
聚酯多元醇：40-60％
聚醚多元醇：10-30％
泡沫稳定剂：1.5-2.5％
化学发泡剂：1.0-2.5％
催化剂：3.0-6.0％
阻燃剂：5.0-20％
物理发泡剂：5.0-15％；
B组份为：
多亚甲基多苯基多异氰酸酯；
其中：
聚酯多元醇为芳香族二元酸多元醇，粘度为8000-13000mpa.s/25℃，酸值≤1.0mgKOH/g，羟值为170-180mgKOH/g。优选山东一诺威聚氨酯股份有限公司PE-B175，是苯酐及其他芳香族二元酸系列多元醇。
聚醚多元醇为甲苯二胺聚醚多元醇，粘度为8000-12000mpa.s/25℃，羟值为310-370mgKOH/g。优选句容宁武新材料发展有限公司NJ-410HN。
本发明选用苯酐及其他芳香族二元酸系列多元醇PE-B175与甲苯二胺系列多元醇NJ-410HN搭配，利用PE-B175结构型阻燃和NJ-410HN高活性、高强度、低导热、互溶性好的特点，有效解决戊烷体系互溶性差、导热高、阻燃差的劣势。
所述的泡沫稳定剂为PIR体系用非水解硅碳类表面活性剂。优选迈图高新材料L-5568。
所述的化学发泡剂为去离子水。
所述的催化剂为凝胶/三聚催化剂和有机金属盐类催化剂。优选N,N-二甲基环己胺(PC8)、Dabco JXP508、Dabco JXP509和Dabco TMR-35的组合物。Dabco JXP508、DabcoJXP509、Dabco TMR-35均为空气化工市售产品。
所述的阻燃剂为脂肪族磷酸酯类阻燃剂，优选青岛联美化工有限公司FR-606。本发明选用FR606作为添加性阻燃剂，所得泡沫的自熄性、耐低温性、抗高温性能、可塑性、紫外线稳定性及抗静电性均优于其它阻燃剂泡沫，在有效降低体系粘度、改善操作性能的同时，在三聚催化剂体系的作用下搭配结构型阻燃聚酯PE-B175，可使大块泡氧指数达到26％以上。
所述的物理发泡剂为环戊烷，含量≥99％，优选湖北巨胜科技有限公司的环戊烷。
所述的连续式生产PIR大块泡用组合聚醚的制备方法，包括以下步骤：
制备A组分：先将聚酯多元醇、聚醚多元醇装入反应釜中；加入泡沫稳定剂、化学发泡剂、催化剂、阻燃剂、物理发泡剂，常温下搅拌0.5-1.5小时，即可装桶。
制备B组分：B组分为多亚甲基多苯基多异氰酸酯，直接装桶。
使用时，将A组份、B组份按A:B＝100:170-175的重量配比，经高压发泡机混合发泡成型即可连续式生产PIR大块泡。
本发明的有益效果如下：
本发明通过使用芳香族二元酸多元醇与甲苯二胺系列多元醇搭配高效阻燃剂，在凝胶/三聚催化剂与有机金属盐类催化剂的共同作用下，进一步提高三聚转化效率及流动性，在使用环保型物理发泡剂环戊烷的条件下，使PIR大块泡达到性能要求，实现了制品在超低温及高温条件下的长期稳定性。本发明组合聚醚生产的PIR大块泡适用性高、密度分布均匀、热传导率低、抗压强度高、吸水率低，有普通PU材料难以比拟的优良性质，是一种永不变形的高效节能、绿色低碳全功能型保温材料。
本发明A组分料是在常温下进行生产，既节约能源又减少设备能耗及繁琐的操作。由A、B组分料采用连续式发泡生产线生产PIR块泡技术与国内普遍存在的非连续式生产方式相比，具有泡沫品质稳定、密度均匀，保温性能突出、产能更大且可靠、泡沫块大、成品管壳尺寸长、可节省施工时间的显著特点。经检测，连续式生产PIR大块泡用组合聚醚产品可以达到以下指标，完全达到相关标准的规定。
整体密度：45±5kg/cm3
导热系数：≤0.025W/(m.k)
压缩强度：≥250KPa
吸水率：≤2％
闭孔率：≥92％
低温尺寸稳定性(-80℃)：≤1.0％
氧指数：≥26％。
具体实施方式
以下结合实施例对本发明做进一步描述。
实施例1
制备100公斤A组份料，称量以下原料：
聚酯多元醇PE-B175：50公斤，聚醚多元醇NJ-410HN：20公斤，泡沫稳定剂L-5568：2公斤，去离子水：1.4公斤，PC8(N,N-二甲基环己胺)：1公斤，JXP508：1.4公斤，JXP509：0.8公斤，TMR-35：1.4公斤，FR606：11公斤，CP：11公斤。
将PE-B175、NJ-410HN装入反应釜中，加入L-5568、去离子水、PC8、JXP508、JXP509、TMR-35、FR606、CP，常温下搅拌1小时，取出进行检验，满足设定发泡参数，即得A组份合格产品，从反应釜中取出装桶入库。
将A、B组份料按A:B＝100:170重量配比，经发泡设备混合均匀，制成高密度保冷管托用PIR材料，测试制品指标如下：
整体密度：43kg/cm3
导热系数：0.0231W/(m.k)
压缩强度：255KPa
吸水率：1.1％
闭孔率：94.5％
低温尺寸稳定性(-80℃)：0.65％
氧指数：27.5％
性能完全达到标准规定的性能要求。
实施例2
制备100公斤A组份料，称量以下原料：
聚酯多元醇PE-B175：60公斤，聚醚多元醇NJ-410HN：10公斤，泡沫稳定剂L-5568：2.0公斤，去离子水：1.5公斤，PC8(N,N-二甲基环己胺)：1.5公斤，JXP508：1.4公斤，JXP509：0.8公斤，TMR-35：1.4公斤，FR606：11公斤，CP：10.4公斤。
将PE-B175、NJ-410HN装入反应釜中，加入L-5568、去离子水、PC8、JXP508、JXP509、TMR-35、FR606、CP，常温下搅拌1小时，取出进行检验，满足设定发泡参数，即得A组份合格产品，从反应釜中取出装桶入库。
将A、B组份料按A:B＝100:170重量配比，经发泡设备混合均匀，制成深冷用PIR型绝热材料，测试制品指标如下：
整体密度：42.8kg/cm3
导热系数：0.0227W/(m.k)
压缩强度：267KPa
吸水率：0.98％
闭孔率：94.3％
低温尺寸稳定性(-80℃)：0.66％
氧指数：27.9％
性能完全达到标准规定的性能要求。
实施例3
制备100公斤A组份料，称量以下原料：
聚酯多元醇PE-B175：45公斤，聚醚多元醇NJ-410HN：20公斤，泡沫稳定剂L-5568：2.0公斤，去离子水：1.5公斤，PC8(N,N-二甲基环己胺)：1.2公斤，JXP508：1.5公斤，JXP509：0.8公斤，TMR-35：1.5公斤，FR606：14.5公斤，CP：12公斤。
将PE-B175、NJ-410HN装入反应釜中，加入L-5568、去离子水、PC8、JXP508、JXP509、TMR-35、FR606、CP，常温下搅拌1小时，取出进行检验，满足设定发泡参数，即得A组份合格产品，从反应釜中取出装桶入库。
将A、B组份料按A:B＝100:175重量配比，经发泡设备混合均匀，制成深冷用PIR型绝热材料，测试制品指标如下：
整体密度：42.6kg/cm3
导热系数：0.0221W/(m.k)
压缩强度：288KPa
吸水率：0.67％
闭孔率：94.2％
低温尺寸稳定性(-80℃)：0.64％
氧指数：28.3％
性能完全达到标准规定的性能要求。

Claims (10)

1.一种连续式生产PIR大块泡用组合聚醚，其特征在于：由A组分和B组分构成，A组分和B组分的重量百分比为100:170-175，其中：
A组份为，以重量百分数计：
B组份为：
多亚甲基多苯基多异氰酸酯；
其中：
聚酯多元醇为芳香族二元酸多元醇，粘度为8000-13000mpa.s/25℃，酸值≤1.0mgKOH/g，羟值为170-180mgKOH/g；
聚醚多元醇为甲苯二胺聚醚多元醇，粘度为8000-12000mpa.s/25℃，羟值为310-370mgKOH/g。
2.根据权利要求1所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的泡沫稳定剂为PIR体系用非水解硅碳类表面活性剂。
3.根据权利要求2所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的泡沫稳定剂为L-5568。
4.根据权利要求1所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的化学发泡剂为去离子水。
5.根据权利要求1所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的催化剂为N,N-二甲基环己胺、Dabco JXP508、Dabco JXP509和Dabco TMR-35的组合物。
6.根据权利要求1所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的阻燃剂为脂肪族磷酸酯类阻燃剂。
7.根据权利要求6所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述的阻燃剂为FR-606。
8.根据权利要求1所述的连续式生产PIR大块泡用组合聚醚，其特征在于：所述物理发泡剂为环戊烷。
9.一种权利要求1-8任一所述的连续式生产PIR大块泡用组合聚醚的制备方法，其特征在于包括以下步骤：
制备A组分：将聚酯多元醇、聚醚多元醇装入反应釜中，加入泡沫稳定剂、化学发泡剂、催化剂、阻燃剂、物理发泡剂，常温下搅拌0.5-1.5小时即可。
10.一种权利要求1-8任一所述的连续式生产PIR大块泡用组合聚醚的应用，其特征在于：使用时，将A组份、B组份按A:B＝100:170-175的重量配比，经高压发泡机混合发泡成型即可连续式生产PIR大块泡。
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