CN108456291B - 一种形状记忆型吸能防护透湿复合材料及其制备方法 - Google Patents

一种形状记忆型吸能防护透湿复合材料及其制备方法 Download PDF

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CN108456291B
CN108456291B CN201810066609.7A CN201810066609A CN108456291B CN 108456291 B CN108456291 B CN 108456291B CN 201810066609 A CN201810066609 A CN 201810066609A CN 108456291 B CN108456291 B CN 108456291B
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component
parts
composite material
shape memory
moisture
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CN108456291A (zh
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刘世勇
盖静
戴江臻
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Chengdu Dekeli Polymer Materials Co ltd
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Abstract

本发明公开了一种形状记忆型吸能防护透湿复合材料及其制备方法，所述形状记忆吸能防护透湿复合材料由A组分和B组分两种材料混炼制成，A组分和B组分的重量比为5‑500:100；其中，A组分为具有透湿和形状记忆功能的聚氨酯树脂，B组分为具有剪切增稠功能的硼改性有机硅树脂。本发明中，A组分可为复合材料提供支撑，帮助复合材料成型、透湿，并且在复合材料变形后通过加热恢复其初始形状，B组分在受到猛烈冲击时可以吸能***，提供复合材料优异的防护性能。

Description

一种形状记忆型吸能防护透湿复合材料及其制备方法
技术领域
本发明属于高分子复合材料领域，涉及一种形状记忆型吸能防护透湿复合材料及其制备方法。
背景技术
剪切增稠材料最大特点在于当外界应力的应变率大于临界剪切速率时，材料粘度或模量迅速变大，由柔软态迅速转变为坚硬固态，从而起到吸能防护的作用。剪切增稠材料主要包括两大类，一种是由纳米颗粒和液体分散介质组成的粒子胶体，另一种是以硼改性有机硅树脂为代表的分子胶体。公开号为CN 101871748 A的专利公开了一种软体防刺防弹材料，该材料即采用粒子胶体提供其吸能防护效果，但是粒子胶体无法塑型，通常需要密封使用，而且其中的纳米颗粒会逐渐团聚沉降，从而失去防护作用，而分子胶体无需密封，性能稳定，逐渐获得越来越多的关注，如公开号为CN 104862975B、CN 102037088A、CN102926211B等专利公开的剪切增稠材料均为此类。分子胶体虽然可以塑型，但其定型性差，较小应力即可导致其变形，所以前述专利均倾向将其用于浸渍织物，这解决了材料易变型的问题，但却限制了该材料的应用范围，而且硼改性有机硅树脂透湿性差，浸渍织物后用于人体穿戴时不利透湿，降低了穿着舒适性。此外，虽然剪切增稠材料和部分高性能织物防弹效果较好，但是其防刺效果较差，在防护性能上依然有不足之处。
发明内容
本发明的目的在于克服现有技术的不足，提供一种形状记忆型吸能防护透湿复合材料及其制备方法，将大量亲水基团引入聚氨酯树脂从而为复合材料提供良好的透湿性，通过分子设计使聚氨酯树脂具有温控形状记忆功能，从而即可帮助复合材料塑型定型，又可帮助复合材料在冲击变形后通过加热恢复初始形状，并且在不影响硼改性有机硅树脂吸能防护效果的前提下，为复合材料提供一定的防刺效果。
本发明的目的是通过以下技术方案来实现的：一种形状记忆型吸能防护透湿复合材料，包括A组分和B组分，所述A组分和B组分的重量比为5—500︰100；
所述A组分为具有透湿和形状记忆功能的聚氨酯树脂；
所述B组分为具有剪切增稠功能的硼改性有机硅树脂。
优选的，所述A组分和B组分的重量比为30—200:100。
一种形状记忆型吸能防护透湿复合材料的制备方法，所述吸能防护透湿复合材料由A组分和B组分混炼制得；
所述A组分和B组分的重量比为5—500︰100，所述A组分为具有透湿和形状记忆功能的聚氨酯树脂，所述B组分为具有剪切增稠功能的硼改性有机硅树脂。
优选的，所述A组分和B组分的重量比为30—200:100。
优选的，所述A组分的制备包括以下步骤，其中所用原料以质量份数计：
将相对分子质量为2000-6000的聚二元醇100份加入密封分散釜中，依次加入二异氰酸酯8-40份、催化剂0-0.1份、小分子扩链剂0.5-5份·、亲水扩链剂10-15份反应4-6小时，温度控制在70-90℃，然后降温至30℃，加入中和剂0-12份中和，加入去离子水搅拌乳化，然后加入0.5-5份后扩链剂，制得固含量为20%—30%的水性聚氨酯乳液；
将所述水性聚氨酯乳液喷雾干燥，即得A组分。
优选的，所述聚二元醇包括聚碳酸酯二元醇、聚己内酯二元醇和聚己二酸二元醇酯二元醇中的至少一种；
所述二异氰酸酯包括甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、氢化二苯基甲烷二异氰酸酯、异氟尔酮二异氰酸酯、六亚甲基二异氰酸酯中的至少一种；
所述催化剂包括有机铋催化剂和有机银催化剂中的至少一种；
所述小分子扩链剂包括1，4-丁二醇、1，4-环己基二甲醇、乙二醇、1，6-己二醇中的至少一种；
所述亲水扩链剂包括2，2-二羟甲基丙酸、2-(2-氨基乙基)氨基乙磺酸钠盐、α，ω-聚丙二醇-二胺-磺丙基钠盐中的至少一种；
所述中和剂包括三乙胺、二甲基乙醇胺、2-氨基-2-甲基-1-丙醇中的至少一种；
所述后扩链剂包括乙二胺、己二胺、甲基环己二胺、水合肼中的至少一种。
优选的，所述密封分散釜为带控温和分散装置的密封分散釜。
优选的，所述B组分的制备包括以下步骤，其中所用原料以质量份数计：
取聚硅氧烷100份，向其中加入硼化物5-20份，控制温度在120-300℃，反应2-6小时后即得B组分。
优选的，所述聚硅氧烷为至少带有两个硅烷醇官能团的聚二甲基硅氧烷。
优选的，所述硼化物为硼酸、氧化硼、焦硼酸中的至少一种。
本发明的有益效果是：
（1）本发明提供的具有形状记忆功能的吸能防护透湿复合材料以带有亲水基团的形状记忆聚氨酯树脂和硼改性有机硅树脂为主体原料，亲水基团的引入赋予复合材料一定的透湿性能，提高了其用于人体穿戴材料时的使用舒适性；
（2）本发明所用形状记忆聚氨酯材料具有良好的塑型和定型性，升温时该聚氨酯材料可随意塑型，冷却后即可定型，从而该复合材料适用性强，应用范围广，可用于骨折外固定材料、运动防护材料、车用防撞击材料等民用用途，也可配合高性能纤维等用于防弹衣、防弹头盔等军用用途；
（3）本发明所用形状记忆聚氨酯材料在常温时具有优异的强度和韧性，用于防护材料时可提供一定的防刺效果；
（4）本发明所用硼改性有机硅树脂材料具有优异的吸能效果，在受到快速冲击时即刻***，从而提供复合材料良好的防护效果；
（5）本发明提供的形状记忆聚氨酯在再次加热升温后可以恢复其原始形状，因此赋予复合材料在受损时一定的可修复性，并且该复合材料可以反复重复利用，在完全破损后仍可重新混炼成型，避免了资源的浪费和对环境的污染破坏。
具体实施方式
下面将结合实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域技术人员在没有付出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
本实施例提供了一种形状记忆型吸能防护透湿复合材料，所述的复合材料由A组分和B组分混炼而得，其中A组分为50份聚氨酯树脂，B组分为100份硼改性有机硅树脂材料。
上述的A组分聚氨酯树脂依次经过下述步骤制备：
将相对分子质量为6000的聚己内酯二元醇100份加入带加热、控温和分散装置的密封分散釜中，加入六亚甲基二异氰酸酯8份,有机银催化剂0.1份，于90度反应2小时，然后加入1,4-环己基二甲醇0.5份反应1小时，加入亲水扩链剂α，ω-聚丙二醇-二胺-磺丙基钠盐10份反应1小时，降温至30℃，加入去离子水高速搅拌乳化，然后加入0.5份乙二胺，制得固含量为20%的水性聚氨酯乳液；
将上述水性聚氨酯乳液喷雾干燥，即得具有透湿和形状记忆功能的聚氨酯树脂。
上述的B组分硼改性有机硅树脂经过下述步骤制备：
取100份二羟基聚二甲基硅氧烷（纽玻利化工有限公司，牌号为NEWTECH-1381），加入硼酸5份，在300℃下反应2小时，即得B组分硼改性有机硅树脂。
本实施例提供的复合材料具有优异的吸能防护效果，而且具有一定的形状记忆功能，磺酸钠基团的引入也赋予复合材料良好的透湿性。
实施例2
本实施例提供了一种形状记忆型吸能防护透湿复合材料，所述的复合材料由A组分和B组分混炼而得，其中A组分为5份聚氨酯树脂，B组分为100份硼改性有机硅树脂材料。
上述的A组分聚氨酯树脂依次经过下述步骤制备：
将相对分子质量为2000的聚碳酸酯二元醇100份加入带加热、控温和分散装置的密封分散釜中，加入甲苯二异氰酸酯40份，于70度反应2小时，然后加入1,6-己二醇5份反应1小时，加入亲水扩链剂2，2-二羟甲基丙酸13份反应3小时，降温至30℃，加入三乙胺10份进行中和，中和完全后加入去离子水高速搅拌乳化，然后加入5份甲基环己二胺，制得固含量为30%的水性聚氨酯乳液；
将上述水性聚氨酯乳液喷雾干燥，即得具有透湿和形状记忆功能的聚氨酯树脂。
上述的B组分硼改性有机硅树脂经过下述步骤制备：
取100份二羟基聚二甲基硅氧烷（纽玻利化工有限公司，牌号为NEWTECH-1384），加入焦硼酸20份，在160℃下反应6小时，即得B组分硼改性有机硅树脂。
实施例3
本实施例提供了一种形状记忆型吸能防护透湿复合材料，所述的复合材料由A组分和B组分混炼而得，其中A组分为200份聚氨酯树脂，B组分为100份硼改性有机硅树脂材料。
上述的A组分聚氨酯树脂依次经过下述步骤制备：
将相对分子质量为3000的聚己二酸二元醇酯二元醇100份加入带加热、控温和分散装置的密封分散釜中，加入异氟尔酮二异氰酸酯38份，有机铋催化剂0.07份于85度反应2小时，然后加入1，4-丁二醇1份反应0.5小时，加入亲水扩链剂2，2-二羟甲基丙酸15份反应3小时，降温至30℃，加入三乙胺12份进行中和，中和完全后加入去离子水高速搅拌乳化，然后加入1份己二胺，制得固含量为30%的水性聚氨酯乳液；
将上述水性聚氨酯乳液喷雾干燥，即得具有透湿和形状记忆功能的聚氨酯树脂。
上述的B组分硼改性有机硅树脂经过下述步骤制备：
取100份二羟基聚二甲基硅氧烷（纽玻利化工有限公司，牌号为NEWTECH-1385），加入硼酸10份，在140℃下反应5小时，即得B组分硼改性有机硅树脂。
实施例4
本实施例提供了一种形状记忆型吸能防护透湿复合材料，所述的复合材料由A组分和B组分混炼而得，其中A组分为500份聚氨酯树脂，B组分为100份硼改性有机硅树脂材料。
上述的A组分聚氨酯树脂依次经过下述步骤制备：
将相对分子质量为4000的聚己内酯二元醇100份加入带加热、控温和分散装置的密封分散釜中，加入二苯基甲烷二异氰酸酯35份，有机铋催化剂0.03份于60度反应2小时，然后加入1，4-丁二醇0.6份反应0.5小时，加入亲水扩链剂2，2-二羟甲基丙酸11份反应3小时，降温至30℃，加入三乙胺9份进行中和，中和完全后加入去离子水高速搅拌乳化，然后加入1.2份水合肼（80%水溶液），制得固含量为25%的水性聚氨酯乳液；
将上述水性聚氨酯乳液喷雾干燥，即得具有透湿和形状记忆功能的聚氨酯树脂。
上述的B组分硼改性有机硅树脂经过下述步骤制备：
取100份二羟基聚二甲基硅氧烷（纽玻利化工有限公司，牌号为NEWTECH-1385），加入硼酸8份，在120℃下反应4小时，即得B组分硼改性有机硅树脂。
以上所述仅是本发明的优选实施方式，应当理解本发明并非局限于本文所披露的形式，不应看作是对其他实施例的排除，而可用于各种其他组合、修改和环境，并能够在本文所述构想范围内，通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围，则都应在本发明所附权利要求的保护范围内。

Claims (6)

1.一种形状记忆型吸能防护透湿复合材料，其特征在于，包括A组分和B组分，所述A组分和B组分的重量比为30—200︰100；
所述A组分为具有透湿和形状记忆功能的聚氨酯树脂；
所述B组分为具有剪切增稠功能的硼改性有机硅树脂；
所述A组分的制备包括以下步骤，其中所用原料以质量份数计：
将相对分子质量为2000-6000的聚二元醇100份加入密封分散釜中，依次加入二异氰酸酯8-40份、催化剂0-0.1份、小分子扩链剂0.5-5份、亲水扩链剂10-15份反应4-6小时，温度控制在70-90℃，然后降温至30℃，加入中和剂0-12份中和，加入去离子水搅拌乳化，然后加入0.5-5份后扩链剂，制得固含量为20%—30%的水性聚氨酯乳液；
将所述水性聚氨酯乳液喷雾干燥，即得A组分；
所述聚二元醇包括聚碳酸酯二元醇、聚己内酯二元醇和聚己二酸二元醇酯二元醇中的至少一种；
所述B组分的制备包括以下步骤，其中所用原料以质量份数计：
取聚硅氧烷100份，向其中加入硼化物5-20份，控制温度在120-300℃，反应2-6小时后即得B组分。
2.一种形状记忆型吸能防护透湿复合材料的制备方法，其特征在于，所述吸能防护透湿复合材料由A组分和B组分混炼制得；
所述A组分和B组分的重量比为30—200︰100，所述A组分为具有透湿和形状记忆功能的聚氨酯树脂，所述B组分为具有剪切增稠功能的硼改性有机硅树脂；
所述A组分的制备包括以下步骤，其中所用原料以质量份数计：
将相对分子质量为2000-6000的聚二元醇100份加入密封分散釜中，依次加入二异氰酸酯8-40份、催化剂0-0 .1份、小分子扩链剂0.5-5份、亲水扩链剂10-15份反应4-6小时，温度控制在70-90℃，然后降温至30℃，加入中和剂0-12份中和，加入去离子水搅拌乳化，然后加入0 .5-5份后扩链剂，制得固含量为20%—30%的水性聚氨酯乳液；
将所述水性聚氨酯乳液喷雾干燥，即得A组分；
所述聚二元醇包括聚碳酸酯二元醇、聚己内酯二元醇和聚己二酸二元醇酯二元醇中的至少一种；
所述B组分的制备包括以下步骤，其中所用原料以质量份数计：
取聚硅氧烷100份，向其中加入硼化物5-20份，控制温度在120-300℃，反应2-6小时后即得B组分。
3.根据权利要求2所述的一种形状记忆型吸能防护透湿复合材料的制备方法，其特征在于，所述二异氰酸酯包括甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、氢化二苯基甲烷二异氰酸酯、异氟尔酮二异氰酸酯、六亚甲基二异氰酸酯中的至少一种；
所述催化剂包括有机铋催化剂和有机银催化剂中的至少一种；
所述小分子扩链剂包括1，4-丁二醇、1，4-环己基二甲醇、乙二醇、1，6-己二醇中的至少一种；
所述亲水扩链剂包括2，2-二羟甲基丙酸、2-(2-氨基乙基)氨基乙磺酸钠盐、α，ω-聚丙二醇-二胺-磺丙基钠盐中的至少一种；
所述中和剂包括三乙胺、二甲基乙醇胺、2-氨基-2-甲基-1-丙醇中的至少一种；
所述后扩链剂包括乙二胺、己二胺、甲基环己二胺、水合肼中的至少一种。
4.根据权利要求2所述的一种形状记忆型吸能防护透湿复合材料的制备方法，其特征在于，所述密封分散釜为带控温和分散装置的密封分散釜。
5.根据权利要求2所述的一种形状记忆型吸能防护透湿复合材料的制备方法，其特征在于，所述聚硅氧烷为至少带有两个硅烷醇官能团的聚二甲基硅氧烷。
6.根据权利要求2所述的一种形状记忆型吸能防护透湿复合材料的制备方法，其特征在于，所述硼化物为硼酸、氧化硼、焦硼酸中的至少一种。
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