CN104311790A - 用于合成ndi基聚氨酯微孔弹性体的配方 - Google Patents

用于合成ndi基聚氨酯微孔弹性体的配方 Download PDF

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CN104311790A
CN104311790A CN201410660086.0A CN201410660086A CN104311790A CN 104311790 A CN104311790 A CN 104311790A CN 201410660086 A CN201410660086 A CN 201410660086A CN 104311790 A CN104311790 A CN 104311790A
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顾晓军
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SHANGHAI NDI CHEMICAL TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种用于合成NDI基聚氨酯微孔弹性体的配方。该配方中的各成份重量配比如下：预聚体100份，扩链剂3～5.5份，复配催化剂1.9～2.4份。与现有技术相比，本发明方法通过采用复配催化剂提高反应速度，缩短了后期熟化所需时间；通过合理选择配方以及平衡各组分的配比，在动态和静态性能不受影响的前提下，保持了硬度低，塑性高和内生热较小等优点，扩大了制品的应用范围。

Description

用于合成NDI基聚氨酯微孔弹性体的配方
技术领域
本发明涉及聚氨酯微孔弹性体，特别是一种合成NDI基聚氨酯微孔弹性体的配方。
背景技术
聚氨酯是一种介于橡胶与塑料之间的高分子耐磨材料，具有卓越的耐磨性、耐油、耐低温、耐水解和耐腐蚀等特性。
聚氨酯微孔弹性体是一种由软段和硬段交替构成的嵌段聚合物，其优良的动态、静态力学性能和便宜、方便的加工方法都决定了其在我国工业应用领域的重要性，尤其适用于缓冲、减震和阻尼等领域。采用不同种类的原料或者同种原料采用不同配比可生产出机械性能和加工性能区别很大的产品。NDI基聚氨酯微孔弹性体具有优异的动态力学性能，压力形变性能，反复形变的内生热小，这是其他异氰酸酯基产品无法企及的。在其工艺配方中，选择合适的聚酯多元醇以及合理的配方是成功的关键。例如选用了聚(己二酸-1,4-丁二醇)酯或聚己二酸乙二醇酯等为主的多羟基聚合物组分，会导致后期熟化所需时间长(通常需15个小时以上)，成品硬度指标不稳定，甚至会由于硬度偏高而出现产品报废等缺点。虽然可以添加一定量的外增塑剂来改善成品硬度不稳定的问题，但此方法会降低制品的其他性能，例如降低成品的硬度，降低耐温性等；另外，在制品的使用过程中添加的外增塑剂会不可避免的发生迁移和抽出，从而在更大程度上影响制品的性能和使用寿命。
发明内容
本发明的目的在于克服上述现有技术的不足，提供一种合成NDI基聚氨酯微孔弹性体的配方，生产中所需的熟化时间短，所制备的聚氨酯微孔弹性体保持了硬度低，塑性高和内生热较小等优点。
本发明的技术解决方案如下。
一种用于合成NDI基聚氨酯微孔弹性体的配方，该配方中的各成份重量配比如下：
预聚体    100份
扩链剂        3～5.5份
复配催化剂    1.9～2.4份
其中：
所述扩链剂是具有内增塑作用的扩链剂，其选自小分子醇类或小分子胺类扩链剂中的一种或几种。
所述复配催化剂由以下重量份数的组分组成：一缩二丙二醇6份，1,4-二氮杂二环[2.2.2]辛烷3份，二醋酸二丁基锡4～7份，聚乙二醇单甲醚-聚丙交酯高分子表面活性剂11～20份。
本发明中，所述预聚体中，-NCO含量≤6％，由过量的1,5-萘二异氰酸酯基聚氨酯和聚合物多元醇在100-150℃下反应生成，其中所述聚酯多元醇的平均相对分子质量为1000-4000，官能度为2；优选的，所述聚合物多元醇选自聚己二酸-丁二醇酯，聚己二酸-乙二醇酯，聚己二酸-丁二醇-乙二醇酯，聚己内酯，聚碳酸酯，聚醚酯和含有侧甲基的聚酯多元醇中的一种或几种。
本发明中，所述扩链剂选自1,4-丁二醇，4,4’-双仲丁基氨基二苯基甲烷，二甲硫基甲苯二胺或N-N’二仲丁基对苯二胺中的一种或几种。
本发明中，所述复配催化剂中，聚乙二醇单甲醚-聚丙交酯高分子表面活性剂的聚乙二醇段平均相对分子质量为2000，聚丙交酯段平均相对分子质量为2000～4000。
与现有技术相比，本发明方法通过采用复配催化剂提高反应速度，缩短了后期熟化所需时间；通过合理选择配方以及平衡各组分的配比，在动态和静态性能不受影响的前提下，降低了制品的内生热，扩大了制品的应用范围。
附图说明
图1是实施例1动态热分析曲线(DMA)。
图2是实施例2动态热分析曲线(DMA)。
具体实施方式
下面结合附图和实施例作进一步说明，但不应以此限制本发明的保护范围。
实施例1
1000g平均相对分子质量为2000的聚己二酸-丁二醇酯和286g NDI在130℃下反应1h得到-NCO％＝5.64％的预聚体；扩链剂组分为含有20g 1,4-丁二醇和51g 4,4’-双仲丁基氨基二苯基甲烷的混合物；复配催化剂25g。复配催化剂由6份一缩二丙二醇，3份1,4-二氮杂二环[2.2.2]辛烷，7份二醋酸二丁基锡，11份聚乙二醇单甲醚-聚丙交酯高分子表面活性剂混合而成。
首先将扩链剂和复配催化剂充分混合，将混合后的组分加入低压发泡机，按照异氰酸酯指数等于1的比例，将混合后的组分和预聚体充分混合，随后将反应料液注入80-110℃的模具中，20-40min后脱模，再放入110℃烘箱中后熟化9-10小时。
按照本实例制备获得的制品在室温下放置一周，然后测其机械性能和硬度。
测试静态机械性能从1557520mm的试片中取样，测试项目包括常态下的拉伸强度、断裂伸长率。
硬度测试采用邵C硬度计在制品表面平坦光滑处直接测试。结果如表1所示。
损耗因子测试采用动态热分析仪(DMA)。结果如图1。显示样品的损耗因子在25℃到200℃温度区间波动很小，有较好的耐热性。
实施例2
1000g平均相对分子质量为2000的聚己二酸-新戊二醇酯和234g NDI在130℃下反应1h得到-NCO％＝4.2％的预聚体；扩链剂组分为含有20g 1,4-丁二醇、10g二甲硫基甲苯二胺和9.25g N-N’二仲丁基对苯二胺的混合物；复配催化剂30g。复配催化剂由6份一缩二丙二醇，3份1,4-二氮杂二环[2.2.2]辛烷，4份二醋酸二丁基锡，20份聚乙二醇单甲醚-聚丙交酯高分子表面活性剂混合而成。
首先将扩链剂和复配催化剂充分混合，将混合后的组分加入低压发泡机，按照异氰酸酯指数等于1的比例，将混合后的组分和预聚体充分混合，随后将反应料液注入80-110℃的模具中，30-45min后脱模，再放入120℃烘箱中后熟化9-10小时。
按照本实例制备获得的制品在室温下放置一周，然后测其机械性能和硬度。
测试静态机械性能从1557520mm的试片中取样，测试项目包括常态下的拉伸强度、断裂伸长率。
硬度测试采用邵C硬度计在制品表面平坦光滑处直接测试。结果如表1所示。
损耗因子测试采用动态热分析仪(DMA)。结果如图2。显示样品的损耗因子在25℃到200℃温度区间波动很小，有较好的耐热性。
对比实施例1
1000g平均相对分子质量为2000的聚己二酸-丁二醇酯和286g NDI在130℃下反应1h得到-NCO％＝5.64％的预聚体；扩链剂组分为含有35g 1,4-丁二醇和9g水的混合物、市售TEGOAMIN 33催化剂10g、市售二甲基硅油表面活性剂15g；采用低压发泡机，按照异氰酸酯指数等于1的比例，将上述组分充分混合，将混合后的反应料液注入80-110℃的模具中，制造微孔弹性体制品，20-40min后脱模，再放入110℃烘箱中后熟化18小时。按照本实例制备获得的制品在室温下放置一周，然后测其机械性能和硬度。
测试静态机械性能从1557520mm的试片中取样，测试项目包括常态下的拉伸强度、断裂伸长率。
测试硬度采用邵C硬度计在制品表面平坦光滑处直接测试。
测试结果如表1所示。
对比实施例2
1000g平均相对分子质量为2000的聚己二酸-新戊二醇酯和234g NDI在130℃下反应1h得到-NCO％＝4.2％的预聚体；扩链剂组分为含有20g 1,4-丁二醇、19g二甲硫基甲苯二胺、和5.4g水的混合物、市售TEGOAMIN 33催化剂10g、辛酸亚锡催化剂5g；硅油表面活性剂15g。采用低压发泡机，按照异氰酸酯指数等于1的比例，将上述组分充分混合，将混合后的反应料液注入80-110℃的模具中，制造微孔弹性体制品，20-40min后脱模，再放入120℃烘箱中后熟化17小时。
按照本实例制备获得的制品在室温下放置一周，然后测其机械性能和硬度。
测试静态机械性能从1557520mm的试片中取样，测试项目包括常态下的拉伸强度、断裂伸长率。测试硬度采用邵C硬度计在制品表面平坦光滑处直接测试。测试结果如表1所示。
表1：对比实施例1-2和实施例1-2制品的机械性能和硬度

Claims (5)

1.一种用于合成NDI基聚氨酯微孔弹性体的配方，其特征在于，该配方中的各成份重量配比如下：
预聚体          100份
扩链剂          3～5.5份
复配催化剂      1.9～2.4份
其中：
所述扩链剂选自小分子醇类或小分子胺类扩链剂中的一种或几种；
所述复配催化剂由以下重量份数的组分组成：一缩二丙二醇6份，1,4-二氮杂二环[2.2.2]辛烷3份，二醋酸二丁基锡4～7份，聚乙二醇单甲醚-聚丙交酯高分子表面活性剂11～20份。
2.根据权利要求1所述的配方，其特征在于：所述预聚体中，-NCO含量≤6％，由过量的1,5-萘二异氰酸酯基聚氨酯和聚合物多元醇在100-150℃下反应生成；其中所述聚酯多元醇的平均相对分子质量为1000-4000，官能度为2。
3.根据权利要求2所述的配方，其特征在于：用于制备预聚体的聚合物多元醇选自聚己二酸-丁二醇酯，聚己二酸-乙二醇酯，聚己二酸-丁二醇-乙二醇酯，聚己内酯，聚碳酸酯，聚醚酯和含有侧甲基的聚酯多元醇中的一种或几种。
4.根据权利要求1所述的配方，其特征在于：所述扩链剂选自1,4-丁二醇，4,4’-双仲丁基氨基二苯基甲烷，二甲硫基甲苯二胺或N-N’二仲丁基对苯二胺中的一种或几种。
5.根据权利要求1所述的配方，其特征在于：所述复配催化剂中，聚乙二醇单甲醚-聚丙交酯高分子表面活性剂的聚乙二醇段平均相对分子质量为2000，聚丙交酯段平均相对分子质量为2000～4000。
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CN105482055A (zh) * 2015-12-31 2016-04-13 山东一诺威聚氨酯股份有限公司 耐低温聚氨酯弹性体及其制备方法
CN105482055B (zh) * 2015-12-31 2018-05-25 山东一诺威聚氨酯股份有限公司 耐低温聚氨酯弹性体及其制备方法
CN106008911A (zh) * 2016-05-20 2016-10-12 中国铁道科学研究院金属及化学研究所 钢轨扣件用垫板材料及其制备方法和用途
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CN108587118B (zh) * 2017-12-29 2020-12-04 东莞市雄林新材料科技股份有限公司 一种具有高尺寸稳定性的工装零部件用tpu材料及其制备方法
CN110105525A (zh) * 2019-05-21 2019-08-09 株洲时代新材料科技股份有限公司 一种耐湿热老化ndi基聚氨酯微孔弹性体及其制备方法
CN110105525B (zh) * 2019-05-21 2021-11-16 株洲时代新材料科技股份有限公司 一种耐湿热老化ndi基聚氨酯微孔弹性体及其制备方法
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