CN112724351A - 真空绝热板用高开孔阻燃型聚氨酯泡沫芯材及其制备方法 - Google Patents

真空绝热板用高开孔阻燃型聚氨酯泡沫芯材及其制备方法 Download PDF

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CN112724351A
CN112724351A CN202011563150.5A CN202011563150A CN112724351A CN 112724351 A CN112724351 A CN 112724351A CN 202011563150 A CN202011563150 A CN 202011563150A CN 112724351 A CN112724351 A CN 112724351A
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刘玄
马海晶
殷守相
魏光曦
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Shandong Inov New Material Co Ltd
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Abstract

本发明涉及聚氨酯硬泡技术领域，具体涉及一种真空绝热板用高开孔阻燃型聚氨酯泡沫芯材及其制备方法。所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，由A组分和B双组分组成，A组分包括聚醚多元醇35‑50份、聚酯多元醇10‑15份、阻燃剂13‑18份、去离子水0.5‑1.1份、发泡剂7‑17份、开孔剂2‑4.4份、泡沫稳定剂1‑2份、防沉剂1‑1.5份、催化剂1‑1.6份、沸石粉5‑15份；B组分为多亚甲基多苯基多异氰酸酯。本发明的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，泡沫强度高，开孔率高、阻燃性好，密度可调，可以切割制作曲面和有棱角的真空绝热制品，扩大真空绝热板的应用领域；本发明还提供其制备方法。

Description

真空绝热板用高开孔阻燃型聚氨酯泡沫芯材及其制备方法
技术领域
本发明涉及聚氨酯硬泡技术领域，具体涉及一种真空绝热板用高开孔阻燃型聚氨酯泡沫芯材及其制备方法。
背景技术
真空绝热板(VIP板)作为一种新型保温材隔热材料，具有优良的保温性能，在达到同等保温效果的情况下，真空绝热板的使用厚度仅为其他传统材料的十分之一。目前VIP板的设计制作已经趋于成熟，在冰箱、建筑、冷藏等领域得到广泛的应用。由于聚氨酯泡沫多孔结构和阻隔膜易吸收水分，在使用中会因老化分解而释放少量气体，从而大幅降低VIP板的保温性能，因此要加入吸气剂来吸收内部的气体。但吸气剂的导热系数大，过量添加会显著降低VIP绝热能力，同时吸气剂很难均匀分布在VIP板内部。
目前常见的VIP多为矩形平板，在管道、罐体和异形构件保温应用受限，常规聚氨酯开孔泡沫材料成本高、阻燃性差在VIP板中应用不多。
发明内容
本发明要解决的技术问题是提供一种真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，泡沫强度高，开孔率高、阻燃性好，密度可调，可以切割制作曲面和有棱角的真空绝热制品，扩大真空绝热板的应用领域；本发明还提供一种简单易行、节能环保的制备方法。
本发明所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，由A组分和B双组分组成，A组分包括以下重量份数的原料：
Figure BDA0002859878180000011
B组分为多亚甲基多苯基多异氰酸酯(粗MDI)；
A组分与B组分的混合质量比为1:0.9-1.3。
聚醚多元醇，选自下列聚醚多元醇中的一种或多种：
聚醚多元醇A，以丙二醇或者甘油为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为2-3，羟值为100-500mgKOH/g；优选山东一诺威新材料有限公司生产的C305、C310或C204；
聚醚多元醇B，以蔗糖或者山梨醇与甘油、丙二醇、乙二醇中的一种或者两种作为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为4.2-5.5，羟值为460-520mgKOH/g；优选山东一诺威新材料有限公司生产的R8345、R6350或R6207；
聚醚多元醇C，以三(2-羟乙基)异氰尿酸酯(赛克)为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为3，羟值为150-350mg KOH/g，粘度200-400mpa·s。
优选地，聚醚多元醇由以下质量份数的原料组成：
聚醚多元醇A 5-10份
聚醚多元醇B 20-25份
聚醚多元醇C 10-20份；
聚醚多元醇A、聚醚多元醇B和聚醚多元醇C的质量份数之和为35-50份。
聚酯多元醇为邻苯二甲酸酐系列多元醇，25℃黏度为10000-12000mpa·s，酸值≤1.0mgKOH/g；优选山东一诺威聚氨酯股份有限公司的PE-B175。
阻燃剂为磷酸三乙酯(TEP)。
发泡剂为245fa、异戊烷(IP)、环戊烷(CP)中的一种或两种。
泡沫稳定剂为南京美思德公司的M8855。
防尘剂为气相二氧化硅。
开孔剂为S25K、S1200或S1900，生产厂家均为山东一诺威新材料有限公司。
催化剂为三甲基羟乙基乙二胺、三甲基羟乙基丙二胺、二甲基乙醇胺、2,4,6-三(二甲氨基甲基)苯酚中的一种或多种。
沸石粉为高温除水处理后的沸石粉，粒径为50-100目。
本发明所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材的制备方法，包括以下步骤：
(1)将聚醚多元醇、聚酯多元醇、阻燃剂、去离子水、开孔剂、泡沫稳定剂、催化剂混合，降温后加入发泡剂，搅拌均匀后加入防沉剂和沸石粉，继续搅拌0.5-1.5h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)使用时，将A组分和B组分按照质量比A:B＝1:0.9-1.3混合，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
与现有技术相比，本发明具有以下有益效果：
(1)本发明在聚氨酯泡沫中加入沸石粉，在发泡过程沸石粉内部气体受热后膨胀，使沸石表面的气孔部分畅通，从而降低真空绝热板吸气剂的用量，减少热桥；另一方面沸石粉有增加泡沫力学性能，提高阻燃，降低泡沫内部反应温度，降低成本；
(2)本发明采用反应型催化剂和精制聚醚大大减少了后期泡沫内部小分子逸出对真空绝热板真空度的影响，同时催化剂有利于泡沫提高泡沫开孔率；
(3)本发明采用赛克起始剂聚醚、TEP和沸石粉使得聚氨酯泡沫具有较好的阻燃性能，泡沫不含卤素，绿色环保；
(4)本发明聚氨酯泡沫芯材开孔率高，密度可调，可以切割制作曲面和有棱角的真空绝热制品，提高真空绝热板的应用领域。
具体实施方式
为了便于理解本发明，本发明列举实施例如下。本领域技术人员应该明了，所述实施例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
实施例和对比例中提到的份数均为重量份数。
实施例1
(1)称取5份C305、20份R8345、10份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，15份PE-B175、18份TEP、1.1份去离子水、1份M8855、3份S25K、0.5份三甲基羟乙基乙二胺、0.5份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入17份245fa，搅拌后加入1份气相二氧化硅和7.9份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:1.2，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
实施例2
(1)称取10份C204、25份R6207、10份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，10份PE-B175、T13份EP、0.5份去离子水、2份M8855、2.4份S25K、2份S1200、0.7份三甲基羟乙基丙二胺、0.4份二甲基乙醇胺、0.5份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入7份异戊烷，搅拌后加入1.5份气相二氧化硅和15份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:1.3，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
实施例3
(1)称取5份C310、15份R6350、10份R6207、20份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，12份PE-B175、15份TEP、1.5份去离子水、1份M8855、2份S25K、0.6份三甲基羟乙基丙二胺、0.4份二甲基乙醇胺、0.4份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入3份环戊烷、8份245fa，搅拌后加入1.1份气相二氧化硅和5份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:0.9，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
实施例4
(1)称取6份C305、23.4份R6350、14份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，11份PE-B175、13份TEP、0.9份去离子水、2份M8855、2份S25K、2份S1900、0.5份三甲基羟乙基乙二胺、0.4份二甲基乙醇胺、0.4份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入13份245fa，搅拌后加入1.3份气相二氧化硅和10.1份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:1.1，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
对比例1
(1)称取5份C305、20份R8345、10份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，15份PE-B175、18份TEP、1.1份去离子水、1份M8855、3份S25K、0.5份N,N-二甲基环己胺、0.5份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入17份245fa，搅拌后加入1份气相二氧化硅和7.9份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:1.2，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
对比例2
(1)称取10份C204、40份R6207、10份聚醚多元醇C(起始剂为赛克，官能度为3，羟值为330mg KOH/g)，10份PE-B175、13份TEP、0.5份去离子水、2份M8855、2.4份S25K、2份S1200、0.7份三甲基羟乙基丙二胺、0.4份二甲基乙醇胺、0.5份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入7份异戊烷，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:1.3，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
对比例3
(1)称取5份C310、15份R6350、10份R6207、20份聚醚多元醇C305、12份PE-B175、15份TEP、1.5份去离子水、1份M8855、2份S25K、0.6份三甲基羟乙基丙二胺、0.4份二甲基乙醇胺、0.4份2,4,6-三(二甲氨基甲基)苯酚混合，降温后加入3份环戊烷、8份245fa，搅拌后加入1.1份气相二氧化硅和5份沸石粉，继续搅拌1h，取出进行检验，满足设定发泡参数，即可装桶，得到A组分；
(2)将A组分和B组分(粗MDI)按照质量比A:B＝1:0.9，通过发泡机混合在模具内发泡，经熟化后切割，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
将实施例1-4和对比例1-3制备的产品进行性能检测，其中泡沫密度参考GB/T6343进行检测，压缩强度参考GB/T8813进行检测，开孔率参考GB/T10799进行检测，导热系数参考GB/T3399进行检测，氧指数参考GB/T 2406.2进行检测。检测结果如表1所示。
表1 实施例1-4和对比例1-3制备的产品性能测试结果
Figure BDA0002859878180000051
从表1可以看出，本发明实施例1-4制得的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材具有密度可调、抗压强度高、开孔率高的的特点。结合实施例1-3和对比例1-3可以看出，当组合聚醚中更换催化剂后泡沫开孔率下降，导致真空绝热板导热系数高；当采用常规3官聚醚多元醇替换以赛克为起始剂的聚醚多元醇C后，泡沫的氧指数降低；当组合聚醚中不加沸石后，制作大块泡沫时出现烧心现象，抗压强度也有一定的影响，在添加相同吸气剂的条件下，没有添加沸石的真空绝热板三个月后导热系数明显增高，说明沸石在降低泡沫内部反应热有很大帮助，同时能够起到吸气剂的作用。

Claims (10)

1.一种真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，由A组分和B双组分组成，其特征在于：A组分包括以下重量份数的原料：
Figure FDA0002859878170000011
B组分为多亚甲基多苯基多异氰酸酯；
A组分与B组分的混合质量比为1:0.9-1.3。
2.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：聚醚多元醇，选自下列聚醚多元醇中的一种或多种：
聚醚多元醇A，以丙二醇或者甘油为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为2-3，羟值为100-500mgKOH/g；
聚醚多元醇B，以蔗糖或者山梨醇与甘油、丙二醇、乙二醇中的一种或者两种作为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为4.2-5.5，羟值为460-520mgKOH/g；
聚醚多元醇C，以三(2-羟乙基)异氰尿酸酯为起始剂，以氧化丙烯作为聚合单体制备而成，官能度为3，羟值为150-350mg KOH/g，粘度200-400mpa·s。
3.根据权利要求2所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：聚醚多元醇由以下质量份数的原料组成：
聚醚多元醇A 5-10份
聚醚多元醇B 20-25份
聚醚多元醇C 10-20份；
聚醚多元醇A、聚醚多元醇B和聚醚多元醇C的质量份数之和为35-50份。
4.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：聚酯多元醇为邻苯二甲酸酐系列多元醇，25℃黏度为10000-12000mpa·s，酸值≤1.0mgKOH/g。
5.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：阻燃剂为磷酸三乙酯；发泡剂为245fa、异戊烷、环戊烷中的一种或两种。
6.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：泡沫稳定剂为M8855；防尘剂为气相二氧化硅。
7.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：开孔剂为S25K、S1200或S1900。
8.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：催化剂为三甲基羟乙基乙二胺、三甲基羟乙基丙二胺、二甲基乙醇胺、2,4,6-三(二甲氨基甲基)苯酚中的一种或多种。
9.根据权利要求1所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材，其特征在于：沸石粉为高温除水处理后的沸石粉，粒径为50-100目。
10.一种权利要求1-9任一项所述的真空绝热板用高开孔阻燃型聚氨酯泡沫芯材的制备方法，其特征在于：包括以下步骤：
(1)将聚醚多元醇、聚酯多元醇、阻燃剂、去离子水、开孔剂、泡沫稳定剂、催化剂混合，降温后加入发泡剂，搅拌均匀后加入防沉剂和沸石粉，继续搅拌0.5-1.5h，得到A组分；
(2)使用时，将A组分和B组分按照质量比A:B＝1:0.9-1.3混合发泡，即得真空绝热板用高开孔阻燃型聚氨酯泡沫芯材。
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