CN106832184B - 一种热塑性有机硅聚氨酯弹性体及其制备方法 - Google Patents

一种热塑性有机硅聚氨酯弹性体及其制备方法 Download PDF

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CN106832184B
CN106832184B CN201710073545.9A CN201710073545A CN106832184B CN 106832184 B CN106832184 B CN 106832184B CN 201710073545 A CN201710073545 A CN 201710073545A CN 106832184 B CN106832184 B CN 106832184B
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parts
polyol
polyurethane elastomer
organic silicon
thermoplastic
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CN106832184A (zh
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宋红玮
王黑龙
刘德富
张生
王仁鸿
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Miracll Chemicals Co Ltd
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Miracll Chemicals Co Ltd
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Priority to CN201710073545.9A priority Critical patent/CN106832184B/zh
Priority to MX2019009417A priority patent/MX2019009417A/es
Priority to EP17895997.9A priority patent/EP3581603A4/en
Priority to PCT/CN2017/074660 priority patent/WO2018145333A1/zh
Priority to KR1020197023764A priority patent/KR102224198B1/ko
Priority to US16/483,670 priority patent/US11643498B2/en
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Abstract

本发明涉及一种热塑性有机硅聚氨酯弹性体及其制备方法，弹性体的原料包括如下组分：大分子多元醇25‑80份；有机硅油或液态硅橡胶0‑60份；二异氰酸酯10‑50份；扩链剂小分子二元醇3‑20份；助剂0.1‑3份；所述大分子多元醇为分子量介于1000‑4000g/mol的无硅多元醇以及被有机硅通过共聚或接枝改性的多元醇；所述小分子二元醇小分子二元醇是指10个碳以下的小分子二元醇。本发明的热塑性有机硅聚氨酯弹性体具有如下优异的性能参数：硬度Shore A40‑D80；拉伸强度≥5MPa；手感爽滑；耐灰尘等脏污；耐液体渗透；对皮肤无刺激；对PC、ABS、TPU等包胶效果好，180°剥离强度>25N/25mm。

Description

一种热塑性有机硅聚氨酯弹性体及其制备方法
技术领域
本发明涉及一种热塑性聚氨酯弹性体，尤其涉及一种热塑性有机硅聚氨酯弹性体及其制备方法，属于高分子材料技术领域。
背景技术
热塑性聚氨酯弹性体(以下简称TPU)，是由大分子二元醇、二异氰酸酯和小分子二元醇或二元胺聚合而成的线性高分子材料。TPU是一种嵌段共聚物，由大分子二元醇形成软段，由二异氰酸酯和小分子二元醇反应形成硬段，软段和硬段交替的分子结构形成微相区并产生微观相分离；此外由于大量极性基团的存在，TPU的分子内和分子间可以形成氢键而产生物理交联点，因而在变形时，高分子链之间也不会发生滑动，而呈现弹性，而当加热时，交联点熔融后高分子链活动，便发生流动。TPU独特的结构特点使其兼具有塑料的加工工艺性能和橡胶的物理机械性能。TPU可溶可熔，不仅具有硬度范围宽、强度高、耐磨、耐油、低温柔韧性好等优良性能；而且通过调整原料及其配比可以大幅度的改变产品性能及用途。广泛应用于医疗卫生、电子电器、工业及体育等方面。
但是TPU亲肤性较差，耐脏污、耐渗透能力不足；而硅橡胶产品具有较优异的亲肤性，光稳定性，耐脏耐渗透，但是其力学强度尤其是拉伸强度和撕裂强度较差。
因此存在如下需求，提供一种亲肤性良好，力学强度优良的热塑性聚氨酯弹性体，特别是提供高抗张强度和撕裂强度、无致敏性、耐黄变、加工性能好可重复加工使用的，同时保证生产工艺比较简单高效且便于自动化生产，并能广泛应用于智能穿戴设备、医疗、工业包胶、皮革等对手感和耐脏污性能要求较高领域的一种热塑性有机硅聚氨酯弹性体。
发明内容
本发明针对现有TPU材料在亲肤性、耐脏污、耐渗透能力方面存在的不足以及硅橡胶在力学强度方面存在的不足，提供一种热塑性有机硅聚氨酯弹性体及其制备方法。
本发明解决上述技术问题的技术方案如下：
一种热塑性有机硅聚氨酯弹性体，所述弹性体的原料包括如下组分：
大分子多元醇25-80份；
有机硅油或液态硅橡胶0-60份；
二异氰酸酯10-50份；
扩链剂小分子二元醇3-20份；
助剂0.1-3份；
其中，所述大分子多元醇为分子量介于1000-4000g/mol的无硅多元醇、被有机硅通过共聚或接枝改性的多元醇中的一种；所述小分子二元醇是指含有10个以下碳原子的二元醇。
进一步，所述大分子多元醇为聚醚多元醇、聚酯多元醇、聚己内酯多元醇、聚碳酸酯多元醇、端羟基聚烯烃多元醇中的一种或多种的复配，以及上述的聚醚多元醇、聚酯多元醇、聚己内酯多元醇、聚碳酸酯多元醇、端羟基聚烯烃多元醇被有机硅通过共聚或接枝改性的聚合物中的一种。
进一步，所述的有机硅油为含醇羟基的有机硅油，其中醇羟基的官能团数为1-3个。
进一步，所述的液态硅橡胶为工业化的室温固化硅橡胶，固化时间大于60分钟。
进一步，所述的二异氰酸酯为甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的一种或多种的复配。
进一步，所述的小分子二元醇为乙二醇、1,3-丙二醇、2-甲基-1,3-丙二醇，1,3-丁二醇、1,4-丁二醇、1,6-己二醇、1,4-环己烷二甲醇、二乙二醇、三乙二醇、新戊二醇、一缩二丙二醇、氢醌-双(β-羟乙基)醚中的一种或多种的复配。
进一步，所述的助剂是指抗氧剂、光稳定剂、润滑剂、催化剂和抗静电剂中的一种或多种。
本发明的有益效果是：
本发明的热塑性有机硅聚氨酯弹性体具有如下优异的性能参数：硬度Shore A40-D80；拉伸强度≥5MPa；手感爽滑；耐灰尘等脏污；耐液体渗透；对皮肤无刺激；对PC、ABS、TPU等包胶效果好，180°剥离强度>25N/25mm。
本发明还要求保护上述的热塑性有机硅聚氨酯弹性体在穿戴设备、医疗、工业包胶、电子注塑、皮革领域的应用。
本发明还提供了上述的热塑性有机硅聚氨酯弹性体的制备方法，包括如下步骤：
1)将称量好的助剂加入到大分子多元醇中，搅拌使助剂完全溶解；
2)后将步骤1)中所得的大分子多元醇与计量份的小分子多元醇、液体状态的二异氰酸酯以及液体状态的有机硅油或液态硅橡胶加入到双螺杆挤出机中，挤出后的物料经水下切割造粒；
3)将步骤2)所得的造粒后的产品干燥，即得。
进一步，步骤2)中所述双螺杆挤出机的温度设定为120-250℃，造粒水温控制在5-70℃，步骤3)中所述干燥的干燥温度控制在50-90℃，干燥时间控制在0.5-4h。
具体实施方式
以下结合实例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量2000g/mol的聚四氢呋喃醚二醇(PTMG)，57份；两端由PEG封端的有机硅油，羟值为38mg KOH/g，15份；二苯基甲烷二异氰酸酯(MDI)，23份；1,4-丁二醇，总体系中R＝nNCO/nOH＝1.01，15份；抗氧剂
Figure BDA0001223547210000045
1010，0.6份；光稳定剂
Figure BDA0001223547210000047
622，0.5份，
Figure BDA0001223547210000046
3280.8份；润滑剂EBO，0.3份，硅酮粉0.2份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂加入到聚四氢呋喃醚二醇(PTMG)中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚四氢呋喃醚二醇(PTMG)、1,4-丁二醇、45-50℃的二苯基甲烷二异氰酸酯(MDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得椭圆形粒料，水的温度控制为20-30℃；
3)将步骤2)所得的粒料置于50℃下干燥2小时，后包装。
实施例2：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量1800g/mol的聚四氢呋喃醚二醇(PTMG)，59份；两端由PEG封端的有机硅油，羟值为55mg KOH/g，30份；二苯基甲烷二异氰酸酯(MDI)，32份；1,4-丁二醇，总体系中R＝nNCO/nOH＝1.01，20份；抗氧剂
Figure BDA0001223547210000041
1010，0.2份，
Figure BDA0001223547210000042
1076，0.3份；光稳定剂
Figure BDA0001223547210000043
770，1.0份，
Figure BDA0001223547210000044
P0.5份；润滑剂EBS，0.5份，油酸酰胺0.5份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂加入到聚四氢呋喃醚二醇(PTMG)中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚四氢呋喃醚二醇(PTMG)、1,4-丁二醇、45-50℃的二苯基甲烷二异氰酸酯(MDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为30-40℃；
3)将步骤2)所得的粒料置于60℃下干燥1.5小时，后包装。
实施例3：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量2500g/mol的聚氧化乙烯二醇(PEG)，45份；两端由PEG封端的有机硅油，羟值为40mg KOH/g，30份；甲苯二异氰酸酯(TDI)，50份；1,3-丙二醇，总体系中R＝nNCO/nOH＝1.01，10份；抗氧剂
Figure BDA0001223547210000051
1010，0.2份，
Figure BDA0001223547210000052
1076，0.2份，
Figure BDA0001223547210000053
1098，0.2份；光稳定剂
Figure BDA0001223547210000054
770，1.5份，
Figure BDA0001223547210000055
Figure BDA0001223547210000056
P0.5份；润滑剂芥酸酰胺，0.6份，硬脂酸酰胺0.6份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂加入到聚氧化乙烯二醇(PEG)中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚氧化乙烯二醇(PEG)、1,3-丙二醇、45-50℃的甲苯二异氰酸酯(TDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为5-15℃；
3)将步骤2)所得的粒料置于80℃下干燥0.5小时，后包装。
实施例4：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量3000g/mol的聚酯二元醇(己二酸、1，4-丁二醇、乙二醇聚合而成)，35份；两端由分子量500g/mol的聚酯二元醇(己二酸+1,4-丁二醇)封端的有机硅油，羟值为30mg KOH/g，45份；甲苯二异氰酸酯(TDI)，40份；1,6-己二醇，总体系中R＝nNCO/nOH＝1.01，8份；抗氧剂
Figure BDA0001223547210000061
1010，0.1份；光稳定剂
Figure BDA0001223547210000062
Figure BDA0001223547210000063
770，0.05份；润滑剂芥酸酰胺，0.05份，催化剂二月桂酸二丁基锡0.1份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂、催化剂加入到聚酯二元醇中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚酯二元醇、1,6-己二醇、45-50℃的甲苯二异氰酸酯(TDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为5-15℃；
3)将步骤2)所得的粒料置于90℃下干燥0.5小时，后包装。
实施例5：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量3500g/mol的聚酯二元醇(己二酸、1，4-丁二醇、1，6-己二醇聚合而成)，25份；两端由PEG封端的有机硅油，羟值为40mg KOH/g，15份；二环己基甲烷二异氰酸酯(H12MDI)，10份；乙二醇3份；抗氧剂
Figure BDA0001223547210000064
1010，0.05份；光稳定剂
Figure BDA0001223547210000065
770，0.05份；润滑剂芥酸酰胺，0.05份，催化剂二醋酸二丁基锡0.1份，抗静电剂0.05份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂、催化剂、抗静电剂加入到聚酯二元醇中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚酯二元醇、乙二醇、45-50℃的二环己基甲烷二异氰酸酯(H12MDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为15-25℃；
3)将步骤2)所得的粒料置于50℃下干燥4小时，后包装。
实施例6：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量3000g/mol的聚己内酯二元醇，35份；两端由PEG封端的有机硅油，羟值为40mg KOH/g，15份；二苯基甲烷二异氰酸酯(MDI)，15份；1，4-丁二醇6份；抗氧剂
Figure BDA0001223547210000071
1010，0.05份；光稳定剂
Figure BDA0001223547210000072
770，0.05份；润滑剂芥酸酰胺，0.05份，催化剂二醋酸二丁基锡0.05份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的润滑剂、催化剂加入到聚己酯二元醇中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的聚己酯二元醇、1，4-丁二醇、45-50℃的二苯基甲烷二异氰酸酯(MDI)、60-120℃的有机硅油按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为15-25℃；
3)将步骤2)所得的粒料置于50℃下干燥4小时，后包装。
实施例7：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量3000g/mol的有机硅共聚改性的聚酯多元醇(己二酸+1,4-丁二醇+1，6-己二醇+有机硅)，其中有机硅含量为10％，80份；二苯基甲烷二异氰酸酯(MDI)，20份；1，4-丁二醇，总体系中R＝nNCO/nOH＝1.01，10份；抗氧剂
Figure BDA0001223547210000073
1010，0.05份；催化剂二醋酸二丁基锡0.05份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、催化剂加入到有机硅改性的聚酯多元醇中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的有机硅改性的聚酯多元醇、1，4-丁二醇、45-50℃的二苯基甲烷二异氰酸酯(MDI)按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为15-25℃；
3)将步骤2)所得的粒料置于50℃下干燥4小时，后包装。
实施例8：
一种热塑性有机硅聚氨酯弹性体，其原料组成如下：分子量4000g/mol的有机硅接枝改性的聚酯多元醇(己二酸+1,4-丁二醇+乙二醇+有机硅)，其中有机硅含量为20％，80份；二苯基甲烷二异氰酸酯(MDI)，16份；1,4-环己烷二甲醇，总体系中R＝nNCO/nOH＝1.01，20份；抗氧剂
Figure BDA0001223547210000081
1010，0.05份；光稳定剂
Figure BDA0001223547210000082
770，0.05份；润滑剂芥酸酰胺，0.05份；催化剂二醋酸二丁基锡0.05份。
上述热塑性有机硅聚氨酯弹性体的制备方法如下：
1)将称量好的抗氧剂、光稳定剂、润滑剂、催化剂加入到有机硅改性的聚酯多元醇中，加热至100℃搅拌2小时使助剂彻底溶解；
2)后将加热的有机硅改性的聚酯多元醇、1,4-环己烷二甲醇、45-50℃的二苯基甲烷二异氰酸酯(MDI)按计量份数加入到双螺杆挤出机中，双螺杆挤出机的温度控制为120-250℃，模头排出的聚合物经水下切割造粒制得圆形粒料，水的温度控制为15-25℃；
3)将步骤2)所得的粒料置于50℃下干燥4小时，后包装。
对比例1：
原料组成为：分子量为2000g/mol的聚四氢呋喃醚二醇(PTMG)，57份；二苯基甲烷二异氰酸酯(MDI)，23份；1,4-丁二醇，总体系中R＝nNCO/nOH＝1.01，23份；抗氧剂
Figure BDA0001223547210000091
1010，0.6份；光稳定剂
Figure BDA0001223547210000092
Figure BDA0001223547210000093
622，0.5份，
Figure BDA0001223547210000094
3280.8份；润滑剂EBO，0.3份，硅酮粉0.2份。对比例2：
原料组成为：分子量3000g/mol的聚酯二元醇(己二酸、1，4-丁二醇、乙二醇聚合而成)，35份；甲苯二异氰酸酯(TDI)，40份；1,6-己二醇，总体系中R＝nNCO/nOH＝1.01，8份；抗氧剂
Figure BDA0001223547210000095
1010，0.1份；光稳定剂
Figure BDA0001223547210000096
770，0.05份；润滑剂芥酸酰胺，0.05份，催化剂二月桂酸二丁基锡0.1份。
为了验证本发明所得热塑性有机硅聚氨酯弹性体的性能，我们对具体实施例1～8和对比例1-2进行性能测试，其中：
硬度按ASTM D2240标准进行测试；
撕裂强度按ASTM D624标准进行测试；
耐黄等级按ASTM D1148测试48h，对比灰卡来进行判定；
致敏测试按ISO10993标准进行测试；
拉伸强度按ASTM D412标准进行测试；
手感爽滑按本公司规定标准进行测试；具体测试方法为：依照本公司制作的磨具，磨具有磨砂不同目数的3个试片模腔，1个平面试片模腔，使用同一磨具制作标样，分为5个等级，由观察者分别触摸试片，与标样进行比较，当4个试片都最接近某一等级试片标样时，确定其为此等级；
评价标准如下：手感爽滑度分为1、2、3、4、5五级，1为最差，5为最好。
1级：手感滞涩，试片完全粘于模腔；
2级：手感滞涩，试片有2/3粘于模腔；
3级：手感一般，试片1/2以下粘于模腔；
4级：手感爽滑，试片不粘于磨腔；
5级：手感爽滑，试片在开模时自然脱落；
耐渗透测试按照企业标准进行测试；将试片分别用记号笔、中性笔、圆珠笔、墨水等涂抹试片表面或者将试片浸泡于果汁、茶水等中，静止放置96h，然后取出，观察试片渗透情况，痕迹清理情况；
评价标准如下：耐渗透分为1、2、3三级，1为最差，3为最好。
1级：痕迹完全渗透，擦拭痕迹无变化，完全残留；
2级：痕迹部分渗透，擦拭痕迹减轻，但不能完全擦掉；
3级：痕迹无渗透，擦拭痕迹去除，无痕迹残留；
结果如表1所示：
表1实施例1-8和对比例1-2所得产品的主要理化性能
Figure BDA0001223547210000101
表1中的数据表明，本发明所提供的热塑性有机硅聚氨酯弹性体相对普通TPU来说在手感和亲肤性上提高了几个层级，从而使得本发明的含有机硅的TPU能够适用于在穿戴设备、医疗、工业包胶、电子注塑、皮革等对手感和耐脏污性能要求较高的领域。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种热塑性有机硅聚氨酯弹性体，其特征在于，所述弹性体的原料包括如下组分：
无硅多元醇25-80份；有机硅油15-45份；二异氰酸酯10-50份；扩链剂小分子二元醇3-20份；助剂0.1-3份；
其中，
所述无硅多元醇的分子量为1000-4000g/mol，选自聚醚多元醇、聚酯多元醇或聚己内酯多元醇之一；
所述有机硅油选自羟值为38mg KOH/g、40mg KOH/g或55mg KOH/g的两端由PEG封端的有机硅油之一或者选自羟值为30mg KOH/g的聚己二酸+1,4-丁二醇封端的有机硅油；
所述二异氰酸酯选自甲苯二异氰酸酯或二苯基甲烷二异氰酸酯；
所述小分子二元醇选自乙二醇、1,3-丙二醇或1,4-丁二醇之一。
2.根据权利要求1所述的热塑性有机硅聚氨酯弹性体，其特征在于，所述的助剂包括抗氧剂、光稳定剂、润滑剂、催化剂和抗静电剂中的一种或多种。
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