CN107652665A - 复合阻燃型环保聚氨酯弹性体的制备方法 - Google Patents

复合阻燃型环保聚氨酯弹性体的制备方法 Download PDF

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CN107652665A
CN107652665A CN201710802342.9A CN201710802342A CN107652665A CN 107652665 A CN107652665 A CN 107652665A CN 201710802342 A CN201710802342 A CN 201710802342A CN 107652665 A CN107652665 A CN 107652665A
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郑小明
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Abstract

本发明属于化工合成技术领域，具体涉及一种复合阻燃型环保聚氨酯弹性体的制备方法，先制备热塑性聚氨酯弹性体颗粒，再制备复合阻燃型环保聚氨酯弹性体。本发明制备的弹性体氧指数高，空气中燃烧试验无熔滴且仅具有少量的黑烟和自熄性；加工方便，阻燃剂可在粒子后加工过程中直接与粒子混合加入；制品机械性能损失少、保持了优良的耐低温性、柔韧性和耐水解性。由于使用了复合无卤阻燃剂，减少了加入单一阻燃剂的量，极大的保证了弹性体本身的优良性能。即使遇火燃烧也不产生对环境有害的气体，可广泛用于线缆护套、汽车部件和输油软管等领域。

Description

复合阻燃型环保聚氨酯弹性体的制备方法
技术领域
本发明属于化工合成技术领域，具体涉及一种复合阻燃型环保聚氨酯弹性体的制备方法。
背景技术
热塑性聚氨酯弹性体（TPU）具有独特的软硬段嵌段共聚物的结构，这种结构使得TPU具有强度高、弹性大、耐磨性好、耐油、低温柔软、高伸长率，耐腐蚀性好等优异性能。TPU同时兼具橡胶的高弹性和塑料的易加工性，已被广泛应用于鞋材、板材、管材、薄膜、线缆、汽车部件、医疗及运动休闲等领域。聚醚型TPU具有良好的韧性、回弹性、耐低温性和耐水解性等，其在电缆护套、汽车部件及消防救生等领域得到了广泛的关注。但是聚醚型TPU氧指数仅18%左右，属易燃材料。TPU自身没有阻燃性能，空气中燃烧时，火焰非常剧烈且伴有浓烈的黑烟，并具有严重的滴流现象。长期以来TPU的阻燃特性一直没有得到满意解决，制约了TPU在电缆护套、汽车部件及输油软管等领域的应用。
发明内容
本发明的目的是提供一种复合阻燃型环保聚氨酯弹性体的制备方法，科学合理、简单易行，制备的弹性体可以实现自熄灭，空气中燃烧时不产生对环境有毒害的卤化氢气体，降低对救援人员和民众的伤害。
本发明所述的复合阻燃型环保聚氨酯弹性体的制备方法，步骤如下：
（1）热塑性聚氨酯弹性体颗粒的制备：聚醚多元醇在90-110℃熔化，加入阻燃剂A混合均匀，真空脱除水分，二异氰酸酯和扩链剂分别在40-55℃和35-50℃熔化；以重量百分比计，将聚醚多元醇55-65%、二异氰酸酯28-35%、聚乙酰胺1-2%、扩链剂7-10%和阻燃剂A混合均匀，异氰酸酯指数控制在1.005-1.03，混合物料注入双螺杆反应器中，经连续反应制得热塑性聚氨酯弹性体颗粒；
（2）复合阻燃型环保聚氨酯弹性体的制备：将塑料开炼机升温至175-190℃，加入热塑性聚氨酯弹性体颗粒塑炼至熔融均匀，加入阻燃剂B，塑炼均匀后压成热塑性弹性体薄片。
步骤（1）中所述的聚醚多元醇是聚四氢呋喃二醇，分子量为1000-2000；
步骤（1）中所述的二异氰酸酯是二苯基甲烷二异氰酸酯。
步骤（1）中所述的扩链剂是含有2-10个碳原子的小分子二元醇。
步骤（1）中所述的扩链剂是乙二醇、丙二醇、二甘醇、1,4-丁二醇或1,6-己二醇中的一种或几种。
步骤（1）中所述的阻燃剂A是甲基膦酸二甲酯（DMMP）或磷酸三苯酯中的一种或两种。
步骤（1）中所述的阻燃剂A的质量是聚醚多元醇、二异氰酸酯和扩链剂总质量的6-12%。
步骤（2）中所述的阻燃剂B是纳米氢氧化镁、纳米氢氧化铝、聚磷酸铵（APP）或三聚氰胺氰尿酸盐中的一种或几种。
步骤（2）中所述的阻燃剂B的质量是热塑性聚氨酯弹性体颗粒质量的10-25%。
本发明所述的复合阻燃型环保聚氨酯弹性体的制备方法，具体步骤如下：
（1）热塑性聚氨酯弹性体颗粒的制备：聚醚多元醇在90-110℃熔化，加入液态阻燃剂A混合均匀，真空脱除水分，二异氰酸酯和扩链剂分别在40-55℃和35-50℃熔化；以重量百分比计，以聚醚多元醇、二异氰酸酯和扩链剂的总质量为1，将聚醚多元醇55-65%、二异氰酸酯28-35%、聚乙酰胺1-2%、扩链剂7-10%和阻燃剂A混合均匀，异氰酸酯指数控制在1.005-1.03，混合物料注入双螺杆反应器中，经连续反应制得热塑性聚氨酯弹性体颗粒；
（2）复合阻燃型环保聚氨酯弹性体的制备：将塑料开炼机升温至175-190℃，加入热塑性聚氨酯弹性体颗粒塑炼至熔融均匀，加入固态阻燃剂B，塑炼均匀后压成1-3mm热塑性弹性体薄片。
本发明与现有技术相比，具有如下有益效果：
本发明制备的弹性体氧指数高，空气中燃烧试验无熔滴且仅具有少量的黑烟和自熄性；加工方便，阻燃剂可在粒子后加工过程中直接与粒子混合加入；制品机械性能损失少、保持了优良的耐低温性、柔韧性和耐水解性。由于使用了复合无卤阻燃剂，减少了加入单一阻燃剂的量，极大的保证了弹性体本身的优良性能。即使遇火燃烧也不产生对环境有害的气体，可广泛用于线缆护套、汽车部件和输油软管等领域。
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
复合阻燃型环保聚氨酯弹性体制备：聚四氢呋喃二醇（PTMG2M=2，加入甲基膦酸二甲酯（DMMP），在110℃真空脱除水分，二苯基甲烷二异氰酸酯（MDI）和1,4-丁二醇（BDO）分别在45℃和40℃保温。将PTMG22MDI：89.7g、BDO：22.8g、聚乙酰胺1.5g、DMMP：31.3g混合均匀，异氰酸酯指数为1.01。将上述物料剧烈搅拌，混合物料注入双螺杆反应器中，经连续反应制得TPU颗粒。
取2得的TPU颗粒加入塑料开炼机，升温至180℃塑炼1min至熔融均匀。向TPU熔融态中加入18.8g纳米氢氧化镁（MgOH）和25g聚磷酸铵（APP），继续塑炼1min下料至160℃平板硫化机，压成标准厚度的TPU薄片。
性能测试：垂直燃烧按GB/T2408-1996测试，样品尺寸125mm×12.5mm×1.6mm;氧指数按GB/T2406-1993测试，样品尺寸85mm×10mm×1.6mm;拉伸强度和断裂伸长率按GB/T528-1998测试;邵A硬度按GB/T531-1992测试。
实施例2
按照实施例1的制备方法。
复合阻燃型环保聚氨酯弹性体制备：PTMG22MDI：105g、BDO：28.3g、聚乙酰胺1.5g、DMMP：33.3g，纳米MgOH：20g、APP：26.7g。
其性能测试方法同实施例1。
实施例3
按照实施例1的制备方法。
复合阻燃型环保聚氨酯弹性体制备：PTMG22MDI：122.6g、BDO：34.6g、聚乙酰胺1.5g、DMMP：35.7g，纳米MgOH：21.4g、APP：28.6g。
其性能测试方法同实施例1。
实施例4
按照实施例1的制备方法。
复合阻燃型环保聚氨酯弹性体制备：PTMG-14MDI：123g、BDO：31g、聚乙酰胺1.5g、DMMP：35.4g，纳米MgOH：21.2g、APP：28.3g。
其性能测试方法同实施例1。
对比例1
按照实施例1的制备方法。
聚氨酯弹性体制备：PTMG22MDI：105g、BDO：28.3g。

Claims (6)

1.一种复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤如下：
（1）热塑性聚氨酯弹性体颗粒的制备：聚醚多元醇在90-110℃熔化，加入阻燃剂A混合均匀，真空脱除水分，二异氰酸酯和扩链剂分别在40-55℃和35-50℃熔化；以重量百分比计，以聚醚多元醇、二异氰酸酯和扩链剂的总质量为100%计，将聚醚多元醇55-65%、二异氰酸酯28-35%、聚乙酰胺1-2%、扩链剂7-10%和阻燃剂A混合均匀，异氰酸酯指数控制在1.005-1.03，混合物料注入双螺杆反应器中，经连续反应制得热塑性聚氨酯弹性体颗粒；
（2）复合阻燃型环保聚氨酯弹性体的制备：将塑料开炼机升温至175-190℃，加入热塑性聚氨酯弹性体颗粒塑炼至熔融均匀，加入阻燃剂B，塑炼均匀后压成热塑性弹性体薄片；
步骤（1）中所述的聚醚多元醇是聚四氢呋喃二醇，分子量为1000-2000；
步骤（1）中所述的阻燃剂A是甲基膦酸二甲酯或磷酸三苯酯中的一种或两种；
步骤（2）中所述的阻燃剂B是纳米氢氧化镁、纳米氢氧化铝、聚磷酸铵或三聚氰胺氰尿酸盐中的一种或几种。
2.根据权利要求1所述的复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤（1）中所述的二异氰酸酯是二苯基甲烷二异氰酸酯。
3.根据权利要求1所述的复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤（1）中所述的扩链剂是含有2-10个碳原子的小分子二元醇。
4.根据权利要求1所述的复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤（1）中所述的扩链剂是乙二醇、丙二醇、二甘醇、1,4-丁二醇或1,6-己二醇中的一种或几种。
5.根据权利要求1所述的复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤（1）中所述的阻燃剂A的质量是聚醚多元醇、二异氰酸酯和扩链剂总质量的6-12%。
6.根据权利要求1所述的复合阻燃型环保聚氨酯弹性体的制备方法，其特征在于步骤（2）中所述的阻燃剂B的质量是热塑性聚氨酯弹性体颗粒质量的10-25%。
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CN108484856A (zh) * 2018-04-13 2018-09-04 王强 储存罐底修复方法
CN109575212A (zh) * 2018-11-02 2019-04-05 江苏亨通电子线缆科技有限公司 一种储能装备电缆用弹性体
CN111205633A (zh) * 2020-03-25 2020-05-29 河北兴瑞铁路器材有限公司 一种铁路钢轨设备引接线高强高韧护套及其制备方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484856A (zh) * 2018-04-13 2018-09-04 王强 储存罐底修复方法
CN108484856B (zh) * 2018-04-13 2019-04-16 王强 储存罐底修复方法
CN109575212A (zh) * 2018-11-02 2019-04-05 江苏亨通电子线缆科技有限公司 一种储能装备电缆用弹性体
CN111218102A (zh) * 2020-02-24 2020-06-02 顺德职业技术学院 含“p-c-n共生”阻燃剂的聚氨酯弹性体及其制备方法
CN111205633A (zh) * 2020-03-25 2020-05-29 河北兴瑞铁路器材有限公司 一种铁路钢轨设备引接线高强高韧护套及其制备方法

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