CN112759736A - 耐高温聚氨酯弹性体及其制备方法 - Google Patents
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Abstract
本发明属于聚氨酯技术领域,具体涉及一种耐高温聚氨酯弹性体及其制备方法。所述的耐高温聚氨酯弹性体,包括以异氰酸酯、聚合物多元醇和扩链剂合成的聚氨酯预聚体组分以及固化剂组分和/或聚酯多元醇组分。本发明制备的耐高温聚氨酯弹性体材料,其耐高温性能佳,克服了传统聚氨酯弹性体高温性能不好的问题,同时本发明将HQEE以扩链剂的形式加入预聚体中,在90℃‑95℃就可以将HQEE熔化反应,解决了扩链剂HQEE熔程短,工艺性能差的问题。
Description
技术领域
本发明属于聚氨酯技术领域,具体涉及一种耐高温聚氨酯弹性体及其制备方法。
背景技术
聚氨酯弹性体是一种主链上含有大量的氨基甲酸酯基高分子材料,由异氰酸酯与多元醇反应的一类硬段和软段交替的嵌段聚合物。他是一种介于橡胶与塑料的材料,其原材料种类多,配方多种多样,应用领域广泛。普通聚氨酯弹性体在80℃一下可以长期使用,温度上升到100℃后使用时间仅数小时,如何使常温环境下聚氨酯弹性体的优良性能在高温下得到保持,是目前的技术难题。
聚氨酯预聚体扩链剂的不同会使聚氨酯弹性体的性能有较大差别,1,4-二(2-羟基乙氧基)苯(HQEE)是一种常见的扩链剂,其为刚性对称结构,熔点为120℃,结晶性强,所以使用HQEE作为扩链剂制得的弹性体具有模量高、弹性好、和耐高温的优点。但是HQEE作为传统扩链剂使用有一个很大的缺点,温度必须升至120℃以上才能熔化,相应的预聚体的温度也应升温至110℃以上,并且HQEE熔程短,温度降低会快速结晶,工艺性能很差。
发明内容
本发明要解决的技术问题是:克服现有技术的不足,提供一种耐高温聚氨酯弹性体及其制备方法,制备的聚氨酯弹性体具有优异的耐高温性能,同时能够解决HQEE熔程短,工艺性能差的问题。
本发明所述的耐高温聚氨酯弹性体,包括以异氰酸酯、聚合物多元醇和扩链剂合成的聚氨酯预聚体组分以及固化剂组分和/或聚酯多元醇组分。
所述的聚氨酯预聚体包括如下重量份数的组分:
异氰酸酯15-60份,聚合物多元醇38-83份,扩链剂2-5份。
所述的异氰酸酯为2,4-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、50%2,4’-二苯基甲烷二异氰酸酯与50%4,4'-二苯基甲烷二异氰酸酯混合物、25%2,2’二苯基甲烷二异氰酸酯与75%4,4’二苯基甲烷二异氰酸酯液化MDI的混合物、1,6-六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷-4,4'-二异氰酸酯中的一种或多种。
所述的聚合物多元醇为官能度为2的聚己内酯多元醇(PCL-1000、PCL-2000或PCL-3000)、数均分子量为800-3200官能度为2的聚酯多元醇(PE-2020或PE-4020)或数均分子量在1800-2200官能度为2.01的聚酯多元醇(PE-4020-01)中的一种或多种。
所述的扩链剂为1,4-二(2-羟基乙氧基)苯(HQEE)。
所述的聚酯多元醇为官能度为2的聚酯多元醇(PE-2020,PE-2420或PE-4020)或官能度为2.01的聚酯多元醇(PE-4020-01)中的一种或多种。
所述的固化剂为3,3'-二氯-4,4'-二氨基二苯基甲烷(MOCA)、二乙基甲苯二胺(E-100)、二甲硫基甲苯二胺(E-300)、4,4'-亚甲基双(3-氯-2,6-二乙基苯胺)(MCDEA)、1,3-丙二醇-双(4-氨基苯甲酸)酯(XYlink 740M)或1,4-丁二醇(BDO)中的一种或多种。
所述的固化剂组分、聚酯多元醇组分与聚氨酯预聚体组分的质量比为10-30:0-120:100。
所述的聚氨酯预聚体的硬度为邵尔硬度75A-98A。
本发明所述的耐高温聚氨酯弹性体的制备方法,包括以下步骤:
(1)将聚合物多元醇升温至100℃-120℃,真空脱水至水分小于0.05%;
(2)将脱完水的聚合物多元醇降温至50-70℃后加入异氰酸酯,同时打开搅拌;
(3)在75℃-80℃反应0.5-2小时,然后加入扩链剂,半个小时内升温至90℃,反应0.5-2.5小时,得到异氰酸根含量为2%-18%的聚氨酯预聚体;
(4)将步骤(3)中得到的聚氨酯预聚体加入固化剂和/或聚酯多元醇,混合均匀后,于100-120℃高温模具上浇筑试片,压模后得到样品,样品在90-110℃环境中后硫化10-40小时后达到使用强度,即得。
与现有技术相比,本发明的有益效果如下:
(1)本发明制备的耐高温聚氨酯弹性体材料,其耐高温性能佳,克服了传统聚氨酯弹性体高温性能不好的问题。
(2)本发明将HQEE以扩链剂的形式加入预聚体中,在90℃-95℃就可以将HQEE熔化反应,解决了扩链剂HQEE熔程短,工艺性能差的问题。
具体实施方式
下面结合实施例对本发明作进一步的说明,但其并不限制本发明的实施。
所用材料如下:
PCL-1000,官能度为2,数均分子量为1000的聚己内酯多元醇
PCL-2000,官能度为2,数均分子量为2000的聚己内酯多元醇
PE-2020,官能度为2,数均分子量为2000的聚酯多元醇
PE-2030,官能度为2,数均分子量为2000的聚酯多元醇
PE-4020-01,官能度为2.01,数均分子量为2000的聚酯多元醇
MB,25%2,2’二苯基甲烷二异氰酸酯,75%4,4’二苯基甲烷二异氰酸酯
MDI-100,4,4’二本基甲烷二异氰酸酯
XYlink 740M,1,3—丙二醇—双(4—氨基苯甲酸)酯
HQEE,1,4-二(2-羟基乙氧基)苯
MCDEA,4,4'-亚甲基双(3-氯-2,6-二乙基苯胺)
MOCA,3,3'-二氯-4,4'-二氨基二苯基甲烷
BDO,1,4-丁二醇
实施例中各原料分别按照质量百分比计算。
实施例1
预聚体组分:72份PCL-2000,3份HQEE,25份MB在80℃-90℃反应4小时,得到异氰酸根含量为4.1%的预聚物。
固化剂组分为MCDEA。
预聚体与固化剂温度为80℃,按照比例预聚体:固化剂=100:16.7混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
实施例2
预聚体组分:27.9份PE-4020-01,39份PCL-2000,2.1份HQEE,31份MB在80℃到90℃反应4小时,得到异氰酸根含量为6.0%的预聚物。
固化剂组分为MCDEA。
预聚体与固化剂温度为80℃,按照比例预聚体:固化剂=100:24.4混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
实施例3
预聚体组分:31份PE-4020-01,39份PCL-2000,3.7份HQEE,26.3份MB在80℃到90℃反应4小时,得到异氰酸根含量为4.1%的预聚物。
固化剂组分为XYlink 740M。
预聚体与固化剂温度为80℃,按照比例预聚体:固化剂=100:27.6混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
实施例4
预聚体组分:43.4份PCL-2000,25.3份PCL-1000,3.6份HQEE,27.7份MB在80℃到90℃反应4小时,得到异氰酸根含量为3.8%的预聚物。
固化剂组分为MOCA。
预聚体与固化剂温度为80℃,按照比例预聚体:固化剂=100:10.9混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
实施例5
预聚体组分:21.2份PE-2030,21.2份PE-4020-01,2份HQEE,55.6份MDI-100在80℃到90℃反应2小时,得到异氰酸根含量为16.3%的预聚物。
聚酯多元醇组分为PE-2020。
固化剂组分为BDO。
预聚体组分和固化剂组分温度为常温,聚酯多元醇组分温度为60℃,按照比例固化剂:聚酯多元醇:预聚体=13.6:80:100混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
实施例6
预聚体组分:21.2份PE-2030,21.2份PE-4020-01,2份HQEE,55.6份MDI-100在80℃到90℃反应2小时,得到异氰酸根含量为16.3%的预聚物。
聚酯多元醇组分为PE-2020。
固化剂组分为BDO。
预聚体组分和固化剂组分温度为常温,聚酯多元醇组分温度为60℃,按照比例固化剂:聚酯多元醇:预聚体=11.8:120:100混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
对比例1
预聚体组分:37.5份PCL-2000,11份PE-4020-01,26.2份PCL-1000,25.3份MB在80℃到90℃反应4小时,得到异氰酸根含量为4.1%含量的预聚物。
固化剂组分为MCDEA。
预聚体与固化剂温度为80℃,按照比例预聚体:固化剂=100:12混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
对比例2
预聚体组分:23.4份PE-2030,23.4份PE-4020-01,53.2份MDI-100在80℃到90℃反应2小时,得到异氰酸根含量为16.3%的预聚物。
聚酯多元醇组分为PE-2020。
固化剂组分为BDO。
预聚体组分和固化剂组分温度为常温,聚酯多元醇组分温度为60℃,按照比例固化剂:聚酯多元醇:预聚体=11.8:120:100混合,搅拌均匀后浇筑到110℃模具中,10分钟开模得到制品。结果见表1。
表1 实施例1-6与对比例1性能指标参数数据表
当然,上述内容仅为本发明的较佳实施例,不能被认为用于限定对本发明的实施例范围。本发明也并不仅限于上述举例,本技术领域的普通技术人员在本发明的实质范围内所做出的均等变化与改进等,均应归属于本发明的专利涵盖范围内。
Claims (10)
1.一种耐高温聚氨酯弹性体,其特征在于:包括以异氰酸酯、聚合物多元醇和扩链剂合成的聚氨酯预聚体组分以及固化剂组分和/或聚酯多元醇组分。
2.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的聚氨酯预聚体包括如下重量份数的组分:
异氰酸酯15-60份,聚合物多元醇38-83份,扩链剂2-5份。
3.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的异氰酸酯为2,4-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、50%2,4’-二苯基甲烷二异氰酸酯与50%4,4'-二苯基甲烷二异氰酸酯混合物、25%2,2’二苯基甲烷二异氰酸酯与75%4,4’二苯基甲烷二异氰酸酯液化MDI的混合物、1,6-六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷-4,4'-二异氰酸酯中的一种或多种。
4.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的聚合物多元醇为官能度为2的聚己内酯多元醇、数均分子量为800-3200官能度为2的聚酯多元醇或数均分子量在1800-2200官能度为2.01的聚酯多元醇中的一种或多种。
5.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的扩链剂为1,4-二(2-羟基乙氧基)苯。
6.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的聚酯多元醇为官能度为2的聚酯多元醇或官能度为2.01的聚酯多元醇中的一种或多种。
7.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的固化剂为3,3'-二氯-4,4'-二氨基二苯基甲烷、二乙基甲苯二胺、二甲硫基甲苯二胺、4,4'-亚甲基双(3-氯-2,6-二乙基苯胺)、1,3-丙二醇-双(4-氨基苯甲酸)酯或1,4-丁二醇中的一种或多种。
8.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的固化剂组分、聚酯多元醇组分与聚氨酯预聚体组分的质量比为10-30:0-120:100。
9.根据权利要求1所述的耐高温聚氨酯弹性体,其特征在于:所述的聚氨酯预聚体的硬度为邵尔硬度75A-98A。
10.一种权利要求1-9任一所述的耐高温聚氨酯弹性体的制备方法,其特征在于:包括以下步骤:
(1)将聚合物多元醇升温至100℃-120℃,真空脱水至水分小于0.05%;
(2)将脱完水的聚合物多元醇降温至50-70℃后加入异氰酸酯,同时打开搅拌;
(3)在75℃-80℃反应0.5-2小时,然后加入扩链剂,半个小时内升温至90℃,反应0.5-2.5小时,得到异氰酸根含量为2%-18%的聚氨酯预聚体;
(4)将步骤(3)中得到的聚氨酯预聚体加入固化剂和/或聚酯多元醇,混合均匀后,于100-120℃高温模具上浇筑试片,压模后得到样品,样品在90-110℃环境中后硫化10-40小时后,即得。
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