CN102504182B - 刚性聚氨酯的制备方法 - Google Patents

刚性聚氨酯的制备方法 Download PDF

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CN102504182B
CN102504182B CN201110330929.7A CN201110330929A CN102504182B CN 102504182 B CN102504182 B CN 102504182B CN 201110330929 A CN201110330929 A CN 201110330929A CN 102504182 B CN102504182 B CN 102504182B
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陈海良
张芳
陈由亮
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Shandong Dongda Inov Polyurethane Co Ltd
Shandong Inov Polyurethane Co Ltd
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Abstract

本发明涉及一种聚氨酯的制备方法，具体涉及一种刚性聚氨酯的制备方法，是由预聚物组分和扩链剂两种组分配制而成。本发明的优点在于通过加入聚合物多元醇总质量10％～50％的官能度为3的聚合物多元醇，使刚性聚氨酯分子间产生一定的氨基甲酸酯化学交联，从弥补高温下分子间氢键断裂和分子间作用力的降低的影响，保证刚性聚氨酯制品在高温下使用。

Description

刚性聚氨酯的制备方法
技术领域
本发明涉及一种聚氨酯的制备方法，具体涉及一种刚性聚氨酯的制备方法。
背景技术
聚氨酯具有独特的软硬段嵌段共聚物的结构，这赋予了其制品具有优良的机械性能，同时制品的硬度可调节的范围宽，这些优异的综合性能是其他很多种商品化橡胶和塑料所不具备的。聚氨酯既可以生产具有优良的回弹性的聚氨酯弹性体，也可以用于生产硬度大于邵氏D60的刚性材料。这些刚性聚氨酯材料常用于承担载荷很重的工作场合和使用温度较高的工作环境，这就要求聚氨酯制品必须具有较高的硬度，通常要求硬度大于邵氏D60，并且在80℃高温下使用硬度大于邵氏D50。常规的聚氨酯高低温硬度变化很大，常温下容易达到硬度大于邵氏D60，但在80℃下由于高温分子间氢键断裂和分子间作用力的降低，制品硬度降低很快，通常只有不到邵氏D40的硬度，由于硬度的降低不能够承担更多的载荷，因此满足不了使用要求。
发明内容
本发明的目的是提供一种刚性聚氨酯的制备方法，能够解决刚性聚氨酯高温分子间氢键断裂和分子间作用力的降低，而使制品硬度降低的缺点，并借助此方法获得一种常温时硬度大于邵氏D60，在80℃下硬度仍然大于邵氏D50的刚性聚氨酯。
本发明所述的一种刚性聚氨酯的制备方法，由两种组分配制而成：
预聚物组分：按照如下制备方法得到：以重量百分数计，由二异氰酸酯24.5～50％与聚合物多元醇50～75.5％在80～85℃反应2～3小时，得到异氰酸根质量含量为7～10％的预聚物，所述二异氰酸酯为甲苯二异氰酸酯或二苯基甲烷二异氰酸酯中的一种或一种以上，所述聚合物多元醇采用官能度为2～3，数均分子量在300～3000范围内的聚环氧丙烷醚多元醇、聚四氢呋喃醚多元醇或聚己内酯多元醇中的一种或一种以上，其中，官能度为3的聚合物多元醇占聚合物多元醇总质量的10～50％；
扩链剂选用胺类扩链剂；
将扩链剂在100～110℃加热熔化后，与预聚物以质量比20～29.4∶100进行混合反应，混合温度为60～75℃，然后浇注到模具中在100～110℃条件下硫化30分钟脱模，最后在90～110℃条件下硫化8～10小时，得到刚性聚氨酯制品。
其中，官能度为3的聚合物多元醇优选占聚合物多元醇总质量的20～40％。
甲苯二异氰酸酯优选用TDI-80或TDI-100，二苯基甲烷二异氰酸酯优选用MDI-50或MDI-100。
胺类扩链剂优选用MOCA、E-300或M-CDEA。
本发明制备得到的刚性聚氨酯制品的硬度在邵氏D60～80之间，该刚性聚氨酯制品在使用温度80℃时，硬度能够保持在大于邵氏D50。
本发明的优点在于：通过加入聚合物多元醇总质量10％～50％的官能度为3的聚合物多元醇，使刚性聚氨酯分子间产生一定的氨基甲酸酯化学交联，从弥补高温下分子间氢键断裂和分子间作用力的降低的影响，保证刚性聚氨酯制品在高温下使用。
具体实施方式
以下结合实施例对本发明做进一步说明。
实施例所用材料如下：
PPG220：数均分子量2000的聚环氧丙烷醚二元醇
PPG330：数均分子量3000的聚环氧丙烷醚三元醇
PPG210：数均分子量1000的聚环氧丙烷醚二元醇
PPG400：数均分子量400的聚环氧丙烷醚二元醇
PPG303：数均分子量300的聚环氧丙烷醚三元醇
PTMG2000：数均分子量2000的聚四氢呋喃醚二元醇
PTMG1000：数均分子量1000的聚四氢呋喃醚二元醇
PCL210：数均分子量1000的聚己内酯二元醇
PCL220：数均分子量2000的聚己内酯二元醇
MDI-50：4，4′-二苯基甲烷二异氰酸酯50％，2，4′-二苯基甲烷二异氰酸酯50％
MDI-100：4，4′-二苯基甲烷二异氰酸酯
TDI-100：2，4-甲苯二氰酸酯
TDI-80：2，4-甲苯二氰酸酯80％，2，6-甲苯二异氰酸酯20％
M-CDEA：4，4′-亚甲基-双-(3-氯-2，6-二乙二基苯胺)
MOCA：3，3′-二氯-4，4′-二氨基二苯基甲烷
E-300：二甲硫基甲苯二胺。
实施例1：
预聚物组分：按照重量百分数计，分子量1000的聚四氢呋喃醚多元醇(PTMG1000)37.75％，分子量3000的聚环氧丙烷醚多元醇(PPG330)37.75％，TDI-100 24.5％。在80℃反应3小时，然后真空(-0.095MPa)脱除气泡，得到异氰酸根质量含量为7.0％的预聚物。
预聚物和熔化后的M-CDEA以100∶29.4的质量比混合反应，混合温度为65℃，然后浇注到模具中在100℃条件下硫化30分钟脱模，最后在110℃条件下硫化8小时，得到25℃时硬度邵氏D60的刚性聚氨酯制品。
实施例2：
预聚物组分：按照重量百分数计，分子量2000的聚四氢呋喃醚多元醇(PTMG2000)53％，分子量300的聚环氧丙烷醚多元醇(PPG303)13％，TDI-80 34％。在85℃反应2小时，然后真空(-0.095MPa)脱除气泡，得到异氰酸根质量含量为8.5％的预聚物。
预聚物和熔化后的E-300以100∶20的质量比混合反应，混合温度为60℃，然后浇注到模具中在100℃条件下硫化30分钟脱模，最后在110℃条件下硫化8小时，得到25℃时硬度邵氏D70的刚性聚氨酯制品。
实施例3：
预聚物组分：按照重量百分数计，分子量1000的聚己内酯多元醇(PCL210)25％，分子量2000的聚己内酯多元醇(PCL220)15％，分子量300的聚环氧丙烷醚(PPG303)10％，MDI-50 40.3％，MDI-100 9.7％。在80℃反应3小时，然后真空(-0.095MPa)脱除气泡，得到异氰酸根质量含量为10％的预聚物。
预聚物和熔化后的MOCA以100∶28.5的质量比混合反应，混合温度为75℃，然后浇注到模具中在110℃条件下硫化30分钟脱模，最后在110℃条件下硫化8小时，得到25℃时硬度邵氏D80的刚性聚氨酯制品。
实施例4：
预聚物组分：按照重量百分数计，分子量1000的聚环氧丙烷醚多元醇(PPG210)25.5％，分子量2000的聚环氧丙烷醚多元醇(PPG220)25.5％，分子量300的聚环氧丙烷醚(PPG303)12.7％，TDI-100 30.3％，TDI-80 6％。在85℃反应3小时，然后真空(-0.095MPa)脱除气泡，得到异氰酸根质量含量为8.8％的预聚物。
预聚物和熔化后的MOCA以100∶25.5的质量比混合反应，混合温度为75℃，然后浇注到模具中在110℃条件下硫化30分钟脱模，最后在110℃条件下硫化8小时，得到25℃时硬度邵氏D75的刚性聚氨酯制品。
对比实施例1：
预聚物组分：按照重量百分数计，分子量1000的聚己内酯多元醇(PCL210)45.0％，分子量400的聚环氧丙烷醚多元醇(PPG400)19.7％，TDI-100 35.3％。在85℃反应3小时，然后真空(-0.095MPa)脱除气泡，得到异氰酸根质量含量为8.8％的预聚物。
预聚物和熔化后的MOCA以100∶25.5的质量比混合反应，混合温度为75℃，然后浇注到模具中在110℃条件下硫化30分钟脱模，最后在110℃条件下硫化8小时，得到25℃时硬度邵氏D75的刚性聚氨酯制品。
各实施例所制得刚性聚氨酯制品性能如下表：
  项目   实施例1   实施例2   实施例3   实施例4   对比实例1
  硬度25℃(邵氏)   D60   D70   D80   D75   D75
  硬度80℃(邵氏)   D54   D56   D67   D65   D38
  拉伸强度(Mpa)   57.4   59.3   61.1   51.6   49.7
  伸长率％   230   285   220   260   360
  撕裂强度(KN/m)   117.1   124.4   147.3   130.2   140.3

Claims (5)

1.一种刚性聚氨酯的制备方法，其特征在于由两种组分配置而成：
预聚物组分：按照如下制备方法得到：以重量百分数计，由二异氰酸酯24.5～50%与聚合物多元醇50～75.5%在80～85℃反应2～3小时，得到异氰酸根质量含量为7～10%的预聚物，所述二异氰酸酯为甲苯二异氰酸酯或二苯基甲烷二异氰酸酯中的一种或一种以上，所述聚合物多元醇采用官能度为2～3，数均分子量在300～3000范围内的聚环氧丙烷醚多元醇、聚四氢呋喃醚多元醇或聚己内酯多元醇中的一种或一种以上，其中，官能度为3的聚合物多元醇占聚合物多元醇总质量的10～50%；
扩链剂选用胺类扩链剂；
将扩链剂在100～110℃加热熔化后，与预聚物以质量比20～29.4:100进行混合反应，混合温度为60～75℃，然后浇注到模具中在100～110℃条件下硫化30分钟脱模，最后在90～110℃条件下硫化8～10小时，得到刚性聚氨酯制品；
所制备的刚性聚氨酯，常温下硬度为邵氏D60～80，80℃下硬度为邵氏D50～67。
2.根据权利要求1所述的刚性聚氨酯的制备方法，其特征在于官能度为3的聚合物多元醇占聚合物多元醇总质量的20～40%。
3.根据权利要求1所述的刚性聚氨酯的制备方法，其特征在于甲苯二异氰酸酯选用TDI-80或TDI-100。
4.根据权利要求1所述的刚性聚氨酯的制备方法，其特征在于二苯基甲烷二异氰酸酯选用MDI-50或MDI-100。
5.根据权利要求1所述的刚性聚氨酯的制备方法，其特征在于胺类扩链剂选用MOCA、E-300或M-CDEA。
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AU2012327770A AU2012327770B2 (en) 2011-10-27 2012-03-19 Preparation method of rigid polyurethane
BR112013026720-8A BR112013026720B1 (pt) 2011-10-27 2012-03-19 Método de preparação de poliuretano rígido
MYPI2013701710A MY163189A (en) 2011-10-27 2012-03-19 Preparation method of rigid polyurethane
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