CN112625210B - 一种磺酸型自修复水性聚氨酯及制备方法 - Google Patents
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Abstract
本发明公开一种磺酸型自修复水性聚氨酯及制备方法,通过聚合物二元醇、二异氰酸酯、双硫键和酰腙键化合物和磺酸盐扩链剂合成含双硫键和酰腙键的磺酸型水性聚氨酯乳液;本发明利用双硫键和酰腙键的可逆化学键以及聚氨酯自身的氢键作用,实现聚氨酯的无限次自我修复,具有粘度小、无刺激性气味、耐热性好、固含量高,而且在弱酸和中性环境下可以稳定存在,具有良好的经济价值和市场前景。
Description
技术领域
本发明涉及水性聚氨酯技术领域,具体涉及一种磺酸型自修复水性聚氨酯及制备方法。
背景技术
聚氨酯材料具有耐磨、耐油、硬度范围宽、强度高、性能的可调节范围大等特点,应用领域涉及轻工、化工、电子、纺织、医疗、建筑、建材、汽车、国防、航天、航空等领域。在使用过程中,因摩擦、碰撞和弯曲造成的机械损伤,会破坏材料美观、影响材料性能,最终缩短材料使用寿命。
鉴于上述缺陷,本发明创作者经过长时间的研究和实践终于获得了本发明。
发明内容
为解决上述技术缺陷,本发明采用的技术方案在于,提供一种磺酸型自修复水性聚氨酯的制备方法,包括步骤:
S1,将聚合物多元醇加热至100℃~130℃,真空脱水1h~2h;
S2,对步骤S1中所得溶液进行氮气保护,并降温至60℃~90℃,加入多异氰酸酯和催化剂,反应1h~3h,加入30~60份有机溶剂调节黏度;
S3,向步骤S2中所得溶液加入磺酸盐单体,50℃~90℃下反应1h~3h;
S4,向步骤S3中所得溶液加入双硫键化合物和酰腙键化合物,40℃~90℃下反应1h~3h;
S5,将步骤S4中所得溶液降温至30℃~50℃,加入去离子水高速分散10min~30min;
S6,将步骤S5中所得溶液真空度脱溶剂制得磺酸型自修复水性聚氨酯乳液。
较佳的,所述磺酸型自修复水性聚氨酯的制备原料按重量计,其组份设置为:60~120份所述聚合物多元醇、30~60份所述多异氰酸酯、0.01~0.03份所述催化剂、30~60份所述有机溶剂、8~13份所述磺酸盐单体、5~10份所述双硫键化合物、5~10份所述酰腙键化合物、200~400份所述去离子水。
较佳的,所述聚合物多元醇为聚醚多元醇、聚酯多元醇中一种或两种。
较佳的,所述多异氰酸酯为芳香族多异氰酸酯、脂肪族多异氰酸酯、脂环族多异氰酸酯中的一种。
较佳的,所述磺酸盐单体为N-(2-氨基乙基)-2-氨基乙烷磺酸钠、N,N-二(2-羟乙基)-2-氨基乙磺酸钠、乙二氨基乙烷磺酸钠、1,4-丁二醇-2-磺酸钠及其衍生物中的一种或两种以上的混合物。
较佳的,所述双硫键化合物为4,4′-二氨基二苯硫醚、3,3′-二羟基二苯二硫醚、4,4′-二羟基二苯硫醚、2-氨基二苯硫醚、2,2′-二硫二乙醇、二羟乙基二乙基二硫化秋兰姆的一种或两种以上的混合物。
较佳的,所述酰腙键化合物为醌肟腙和氟吡草腙一种或两种。
较佳的,所述催化剂为有机锡类、叔胺类中的一种或两种以上的混合物。
较佳的,所述有机溶剂为丙酮、丁酮、甲乙酮、二氧六环、N,N-二甲基酰胺、N-甲基吡咯烷酮、乙酸乙酯中的一种或两种以上的混合物。
较佳的,一种磺酸型自修复水性聚氨酯,通过所述磺酸型自修复水性聚氨酯的制备方法制得。
与现有技术比较本发明的有益效果在于:本发明利用双硫键和酰腙键的可逆化学键以及聚氨酯自身的氢键作用,实现聚氨酯的无限次自我修复,具有粘度小、无刺激性气味、耐热性好、固含量高,而且在弱酸和中性环境下可以稳定存在,具有良好的经济价值和市场前景。
附图说明
图1为所述磺酸型自修复水性聚氨酯的制备方法的流程图。
具体实施方式
以下结合附图,对本发明上述的和另外的技术特征和优点作更详细的说明。
如图1所示,图1为所述磺酸型自修复水性聚氨酯的制备方法的流程图;本发明所述磺酸型自修复水性聚氨酯的制备方法,原料以质量份计,包括步骤:
S1,将60~120份聚合物多元醇加热至100℃~130℃,真空脱水1h~2h;
S2,对步骤S1中所得溶液进行氮气保护,并降温至60℃~90℃,加入30~60份多异氰酸酯和0.01~0.03份催化剂,反应1h~3h,加入30~60份的有机溶剂调节黏度;
S3,向步骤S2中所得溶液加入8~13份磺酸盐单体,50℃~90℃下反应1h~3h;
S4,向步骤S3中所得溶液加入5~10份双硫键化合物和5~10份酰腙键化合物,40℃~90℃下反应1h~3h;
S5,将步骤S4中所得溶液降温至30℃~50℃,加入200~400份去离子水高速分散10min~30min;
S6,将步骤S5中所得溶液真空度脱溶剂制得磺酸型自修复水性聚氨酯乳液。
所述聚合物多元醇为聚醚多元醇、聚酯多元醇中一种或两种。
所述多异氰酸酯为芳香族多异氰酸酯、脂肪族多异氰酸酯、脂环族多异氰酸酯中的一种。
所述磺酸盐单体为N-(2-氨基乙基)-2-氨基乙烷磺酸钠、N,N-二(2-羟乙基)-2-氨基乙磺酸钠、乙二氨基乙烷磺酸钠、1,4-丁二醇-2-磺酸钠及其衍生物中的一种或两种以上的混合物。
所述双硫键化合物为4,4′-二氨基二苯硫醚、3,3′-二羟基二苯二硫醚、4,4′-二羟基二苯硫醚、2-氨基二苯硫醚、2,2′-二硫二乙醇(HEDS)、二羟乙基二乙基二硫化秋兰姆(TDS二醇)的一种或两种以上的混合物。
所述酰腙键化合物为醌肟腙和氟吡草腙一种或两种。
所述催化剂为有机锡类、叔胺类中的一种或两种以上的混合物。
所述有机溶剂为丙酮、丁酮、甲乙酮、二氧六环、N,N-二甲基酰胺、N-甲基吡咯烷酮、乙酸乙酯中的一种或两种以上的混合物。
本发明利用双硫键和酰腙键的可逆化学键以及聚氨酯自身的氢键作用,实现聚氨酯的无限次自我修复,具有粘度小、无刺激性气味、耐热性好、固含量高,而且在弱酸和中性环境下可以稳定存在,具有良好的经济价值和市场前景。
实施例一
本发明所述磺酸型自修复水性聚氨酯的制备:
S1,将100份聚四氢呋喃二醇加入反应器,120℃真空脱水处理2h;
S2,在N2保护下,降温至80℃,加入44.5份异佛尔酮二异氰酸酯和0.03份二月桂酸二丁基锡,升温90℃下反应3h,40份N-甲基吡咯烷酮调节黏度;
S3,降温至70℃,加入12份N-(2-氨基乙基)-2-氨基乙烷磺酸钠反应3h
S4,降温至50℃,加入10份4,4′-二氨基二苯硫醚和8份醌肟腙反应2h;
S5,降温30℃,转移至乳化桶,加入300份去离子水高速分散30min;
S6,最后真空度脱溶剂制得磺酸型自修复水性聚氨酯乳液。
所得乳液平均粒径80nm,pH=8.0,固含量为36.5%,粘度60mPa·s。
实施例二
本发明所述磺酸型自修复水性聚氨酯的制备:
S1,将100份聚己内酯二醇加入反应器,120℃真空脱水处理2h;
S2,在N2保护下,降温至70℃,加入50份,4,4-二苯基甲烷二异氰酸酯(MDI)和0.02份辛酸亚锡,升温85℃下反应3h,40份20ml二氧六环调节黏度;
S3,降温至70℃,加入10份乙二氨基乙烷磺酸钠反应3h;
S4,升温至50℃,加入10份4,4′-二羟基二苯硫醚和7份氟吡草腙,反应3h;
S5,降温30℃,转移至乳化桶,加入300份去离子水高速分散30min;
S6,最后真空度脱溶剂制得磺酸型自修复水性聚氨酯乳液。
所得乳液平均粒径70nm,pH=9.0,固含量为36%,粘度80mPa·s。
实施例三
本发明所述磺酸型自修复水性聚氨酯的制备:
S1,将100份聚氧化丙烯二醇加入反应器,120℃真空脱水处理2h;
S2,在N2保护下,降温至70℃,加入35份甲苯二异氰酸酯(TDI)和滴加0.02份辛酸亚锡,升温85℃下反应3h,40份20ml丁酮调节黏度;
S3,降温至80℃,加入12份N,N-二(2-羟乙基)-2-氨基乙磺酸钠反应3h;
S4,升温至90℃,加入10份2,2′-二硫二乙醇和5份氟吡草腙反应3h;
S5,降温30℃,转移至乳化桶,加入300份去离子水高速分散30min;;
S6,最后真空度脱溶剂制得磺酸型自修复水性聚氨酯乳液。
所得乳液平均粒径90nm,pH=9.0,固含量为35%,粘度90mPa·s。
对实施例一、实施例二、实施例三磺酸型自修复水性聚氨酯倒到PTFE模板中,室温下待水分挥发成膜后,在2.66kPa下50℃真空干燥2天,得薄膜,供样自修复性能进行检测。
采用拉伸性能来表征聚氨酯的自修复性能。拉伸应力应变性能测试试样的制备按照标准GB/T528-1988,每组数据为5根样条测试结果的平均值。
将制得的聚氨酯按规格裁剪成哑铃状(100mm×10mm×1mm)待测试样条,均分为两部分,一部分作为原样,进行拉伸强度测试;
另一部分用医用剪刀,从试样颈部中间位置横刀剪断,随后立即拼合,置于模具中;
根据实验条件,将试样分别置于不同的时间以及温度下进行自愈合,随后取出并进行拉伸强度测试,记录最大拉伸强度(σ)。将自愈合样条强度与原始样条强度进行比较计算得到自修复效率。自修复效率(H)通常定义为:
表一磺酸型自修复水性聚氨酯自修复性能测试结果
以上所述仅为本发明的较佳实施例,对本发明而言仅仅是说明性的,而非限制性的。本专业技术人员理解,在本发明权利要求所限定的精神和范围内可对其进行许多改变,修改,甚至等效,但都将落入本发明的保护范围内。
Claims (7)
1.一种磺酸型自修复水性聚氨酯的制备方法,其特征在于,包括步骤:
S1,将聚合物多元醇加热至100℃~130℃,真空脱水1h~2h;
S2,对步骤S1中所得溶液进行氮气保护,并降温至60℃~90℃,加入多异氰酸酯和催化剂,反应1h~3h,加入30~60份有机溶剂调节黏度;
S3,向步骤S2中所得溶液加入磺酸盐单体,50℃~90℃下反应1h~3h;
S4,向步骤S3中所得溶液加入双硫键化合物和酰腙键化合物,40℃~90℃下反应1h~3h;
S5,将步骤S4中所得溶液降温至30℃~50℃,加入去离子水高速分散10min~30min;
S6,将步骤S5中所得溶液真空脱溶剂制得磺酸型自修复水性聚氨酯乳液;
所述磺酸型自修复水性聚氨酯的制备原料按重量计,其组份设置为:60~120份所述聚合物多元醇、30~60份所述多异氰酸酯、0.01~0.03份所述催化剂、30~60份所述有机溶剂、8~13份所述磺酸盐单体、5~10份所述双硫键化合物、5~10份所述酰腙键化合物、200~400份所述去离子水;
所述双硫键化合物为3,3′-二羟基二苯二硫醚、2,2′-二硫二乙醇、二羟乙基二乙基二硫化秋兰姆的一种或两种以上的混合物;
所述酰腙键化合物为醌肟腙和氟吡草腙一种或两种。
2.如权利要求1所述的磺酸型自修复水性聚氨酯的制备方法,其特征在于,所述聚合物多元醇为聚醚多元醇、聚酯多元醇中一种或两种。
3.如权利要求1所述的磺酸型自修复水性聚氨酯的制备方法,其特征在于,所述多异氰酸酯为芳香族多异氰酸酯、脂肪族多异氰酸酯、脂环族多异氰酸酯中的一种。
4.如权利要求1所述的磺酸型自修复水性聚氨酯的制备方法,其特征在于,所述磺酸盐单体为N-(2-氨基乙基)-2-氨基乙烷磺酸钠、N,N-二(2-羟乙基)-2-氨基乙磺酸钠、乙二氨基乙烷磺酸钠、1,4-丁二醇-2-磺酸钠及其衍生物中的一种或两种以上的混合物。
5.如权利要求1所述的磺酸型自修复水性聚氨酯的制备方法,其特征在于,所述催化剂为有机锡类、叔胺类中的一种或两种以上的混合物。
6.如权利要求1所述的磺酸型自修复水性聚氨酯的制备方法,其特征在于,所述有机溶剂为丙酮、甲乙酮、二氧六环、N-甲基吡咯烷酮、乙酸乙酯中的一种或两种以上的混合物。
7.一种磺酸型自修复水性聚氨酯,其特征在于,通过如权利要求1-6中任一项所述的磺酸型自修复水性聚氨酯的制备方法制得。
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