CN109422927B - 一种具有形状记忆功能的软硬一体化复合材料、制备方法及应用 - Google Patents

一种具有形状记忆功能的软硬一体化复合材料、制备方法及应用 Download PDF

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CN109422927B
CN109422927B CN201710710742.7A CN201710710742A CN109422927B CN 109422927 B CN109422927 B CN 109422927B CN 201710710742 A CN201710710742 A CN 201710710742A CN 109422927 B CN109422927 B CN 109422927B
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layer
soft
rubber
composite material
protective layer
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CN109422927A (zh
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张继川
张立群
李亮亮
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Xi'an Zhonghai Machinery Manufacturing Co ltd
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Shandong Belong New Materials Technology Co ltd
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Priority to PCT/CN2018/097178 priority patent/WO2019033912A1/zh
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Abstract

本发明公开了一种具有形状记忆功能的软硬一体化复合材料、制备方法及应用。复合材料包括三层，由外及内分别为：表面装饰层、防护层和软衬层；防护层为塑胶或者硫化塑胶；塑胶在55℃以上受热软化，温度低于55℃之后结晶硬化；软衬层为发泡聚氨酯、橡胶或发泡橡胶；软衬层与防护层通过热帖合或共硫化成为一体结构；表面装饰层为涂料层。本发明利用材料形状记忆原理，以及升温60℃以上，杜仲胶等材料结晶融化变为无定形态，可随意塑型的原理，采用分别混炼，硫化的工艺制备出可随意塑型的个性护具或残疾人辅具。所制备的护具或辅具可以根据不同人群体型的不同，调整出最贴合人体形状的个性化器械。

Description

一种具有形状记忆功能的软硬一体化复合材料、制备方法及 应用
技术领域
本发明涉及高分子材料技术领域，进一步地说，是涉及一种具有形状记忆功能的软硬一体化复合材料、制备方法及应用。
背景技术
高分子材料在体育护具、残疾人辅具以及医疗器械方面有较为广泛的应用。比如，目前国内市场上销售的体育护具主要由高分子材料制成外壳，抵挡外力对人体的伤害，再由EVA、橡胶、聚氨酯等发泡材料做成内衬，耗散能量，保护人体不受伤害。但是这些护具都有两个共同的缺点无法克服：其一，是这些防护材料都是一次性成型，定型后外观形状不可改变，因而不能适应不同人群身体特征不同的特点；这点对于青少年运动员特别重要，因为青少年是人成长最快的阶段，随着青少年不断长高，身体特征也会发生显著改变，因此不得不多次更换护具，从而增加经济负担；其二，这些材料都是石油基化工原料制成，属于不可再生材料，不利于环保，并且由于运动员个体的体质不同，对部分化学成分刺激过敏，还有的可能产生不适。
再比如传统的假肢接收腔是由丙烯酸树脂，经过测量、修形和制造三个步骤制备而成。具有许多缺点：1)制造周期较长、工艺繁杂；2)接收腔的制作属于个性化非标准作业，对假肢矫形师的经验和职业素质要求都比较高，所得产品对于残疾人的适应性差异较大；3)原材料都来源于化石资源，属于不可再生资源，显然不属于绿色产品；4)废弃之后，均会增加碳排放，在环保呼声日益高涨的今天，显然不具环保优势；5)接收腔制备一次定型，不能再次更改。因此，残疾人只能选择近似适合于自身残肢形状的接收腔，而不能得到完全适合于自身残肢形状的接收腔。6)残肢萎缩后，不得不反复制造接收腔，成本昂贵，增加残疾人的经济负担。并且生产过程耗费大量人力、物力。7)在成本方面，接收腔本身价格在3000元左右，再加上假肢关节、支撑杆、假肢等制件，整个假肢的售价往往在2—4万之间，造价昂贵。因此，由于上述原因，加之残障人士往往因为残疾而失去劳动能力，经济能力往往不高，根本无法负担昂贵的假肢费用。由于得不到优质假肢的支撑，残障人士无法获得重返社会工作的机会，生活质量也会变差，从而陷入致残—返贫—买不起假肢—不能重返社会—生活质量变差这样一个恶性循环。
同样高分子材料制备的医疗器械，特别是骨科固定以及矫形器材，也面临体育护具和残疾人假肢的诸多缺点，比如不能够标准化制作，制作工艺复杂，产品为石油基原料等。
发明内容
为解决现有技术中出现的问题，本发明提供了一种具有形状记忆功能的软硬一体化复合材料、制备方法及应用。本发明利用杜仲胶等塑胶材料形状记忆的特殊性能，制备出可反复塑形的个性化产品，可广泛应用于体育护具、残疾人辅具以及医疗器械，特别是骨科固定和矫形领域。比如个性化足球护腿板，这样足球运动员，特别是青少年足球运动员，就可以根据自己的腿型不同或者成长带来的腿型变化，很方便的调整护腿板的形状，使之完全贴合腿部，与腿部融为一体，从而最大限度起到防护作用。再比如个性化残疾人假肢接收腔，这样可以根据残疾人自身残肢的形状，由残疾人士亲自操作，制备出适应于残疾人自身残肢外形的个性化接收腔。同样医疗器械也可以标准化生产、个性化操作，满足医生和患者的需求。此外，本发明的复合材料的结晶熔点在60℃左右，并且是热的不良导体，因而不会在软化塑性的操作过程中烫伤人体。本发明利用的天然高分子材料，属于绿色、环保、可再生的材料，且制备过程基本没有三废排放，符合国家节能减排、发展绿色、低碳、循环经济的要求。
本发明的目的之一是提供一种具有形状记忆功能的软硬一体化复合材料。
所述复合材料包括三层，由外及内分别为：表面装饰层、防护层和软衬层；
所述防护层为塑胶或硫化塑胶；
所述生胶在55℃以上受热软化，温度低于55℃之后结晶硬化；
所述软衬层为发泡聚氨酯；或橡胶与助剂混炼而得；
所述软衬层与防护层通过热帖合或共硫化成为一体结构；
所述表面装饰层为涂料层。
其中，优选：软衬层与防护层共硫化成为一体结构。
所述塑胶为杜仲胶、古塔波胶、巴拉塔胶、桃叶卫矛胶、合成反式-1,4-聚异戊二烯、聚己内酯中的一种或组合；
所述橡胶为天然橡胶、丁苯橡胶、顺丁橡胶、三元乙丙橡胶、硅橡胶、氟橡胶、氯丁橡胶、丁腈橡胶、丁基橡胶、丙烯酸酯橡胶、氯磺化聚乙烯中的一种或组合；
所述表面装饰层为弹性涂料，更优选为聚氨酯类涂料。表面装饰层可以采用通常的涂覆手段，可刷可涂可喷等方式附着在防护层的表面，起到美化、装饰的作用。涂料必须满足两个条件：一是不溶于水，不水解、耐一定温度(60—100℃)不降解，二是可以随着防护层和软衬层反复塑性不破裂，本发明优选具有弹性的聚氨酯系列涂料。
防护层的塑胶优选经过硫化的塑胶，硫化方法可采用现有技术通常的硫化工艺，本发明中，可以优选：
所述防护层是由包括以下组份的原料混炼而得：
各组分按重量份数计：
Figure BDA0001382597820000031
软衬层的橡胶可优选按配方：
所述软衬层是由包括以下组份的原料混炼而得：
各组分按重量份数计：
Figure BDA0001382597820000041
如果软衬层采用发泡橡胶，则在配方中需要添加发泡剂，发泡工艺可以采用本领域通常的工艺条件，本发明中，优选采用以下配方：
所述软衬层是由包括以下组份的原料混炼而得：
各组分按重量份数计：
Figure BDA0001382597820000042
所述复合材料总厚度为1～10mm，软衬层厚度0.5～9mm。
以上所述的硫化剂、促进剂、发泡剂、防老剂、填料，可采用现有技术中通常的硫化剂、促进剂、发泡剂、防老剂、填料。本发明中，可以优选：
硫化剂包括：硫磺、过氧化物(DCP、双25、BPO)
促进剂包括：促TMTD、促M、促CZ、促DM、促TMTM、促TETD、促DPTT、促ZDC、促BZ、促PZ、促D、促CBS、促TBBS、促NOBS、促DZ
发泡剂包括：发泡剂AC，发泡剂H，发泡剂DPT
防老剂包括：防264、防AW、防BLE、防RD、防AH、防AP、防A、防D、防4010、防4010NA、防H、防DPD、防CMA、防2264。
填料优选钛白粉，碳酸钙，白炭黑；
防护层和软衬层的配方中还可根据实际情况添加不同的助剂，如：活化剂、调色剂、填充补强剂、增塑剂、增硬剂等，其用量也为常规用量，技术人员可根据实际情况确定。
本发明的目的之二是提供一种所述的具有形状记忆功能的软硬一体化复合材料的制备方法。
包括：
所述防护层和软衬层通过热帖合或共硫化成一体结构，防护层外面涂敷表面装饰层，制得所述具有形状记忆功能的复合材料。
其中，
共硫化压力>3.5Mpa，共硫化温度140～200℃，共硫化时间5～100分钟。
软衬层为发泡聚氨酯，是通过聚氨酯特有的热贴合工艺与防护层贴合；热帖合工艺采用现有技术中通常的热帖合工艺。
防护层和软衬层的共硫化工艺比较适合开炼机配合模压，或者挤出机配合模压生产工艺过程。首先要调节二者的正硫化时间趋于一致，然后将二者分别裁剪成设计好的形状和重量，将二者同时放入模具，采取共硫化工艺，硫化压力>3.5Mpa，硫化温度140～200℃，硫化时间5～100分钟，模压制备成为软硬同体个性化护具或夹具等。最后通过表面修饰层进行修饰、美化，得到软硬同体结构的个性化护具或夹具。
防护层和软衬层的共硫化也可采用辐照硫化，其工艺条件为常规工艺条件。
本发明的目的之三是提供一种所述的具有形状记忆功能的软硬一体化复合材料在体育护具、残疾人辅具以及医疗器械中的应用。
主要用于体育护具、残疾人辅具以及医疗器械中骨科固定、矫形、夹板等。
本发明克服了以往体育护具、残疾人辅具一次定型不可更改以及源自不可再生化石基原料，不利于环保的缺点。本发明利用材料形状记忆原理，以及升温60℃以上，杜仲胶等材料结晶融化变为无定形态，可随意塑型的原理，分别采用混炼，硫化等工艺制备出可随意塑型的个性护具或残疾人辅具。所制备的护具或辅具可以根据不同人群体型的不同，调整出最贴合人体形状的个性化器械器械。本发明体现在：①制作具有普适性，因而模具的制备简单，降低制造成本；②可随意塑型，同一款产品可以适用不同人群，适用面较宽；③随着青少年成长造成的体型变化，可随意塑型，重复使用，为用户节约成本；④原料来自于可再生高分子材料，有利于环保。
附图说明
图1为本发明的具有形状记忆功能的复合材料示意图
附图说明：
1表面装饰层；2防护层；3软衬层。
具体实施方式
下面结合实施例，进一步说明本发明。
实施例1
防护层具体配方为：
聚己内酯(塑胶) 100份
DCP 0.5份
钛白粉(填料) 5份
软衬层具体配方为：
Figure BDA0001382597820000061
根据上述防护层配方和软衬层配方，根据传统橡胶开炼、密炼、捏炼或者挤出混炼工艺，按照橡胶—活化剂—填料—软化剂—防老剂—硫化剂的加料顺序，分别对上述两个配方进行混炼，分别得到防护层混料胶半成品和软衬层混炼胶半成品，停放16小时以上待用。防护层的混炼温度为60℃±10℃；软衬层的混炼温度为常温加冷却水循环冷却。
按照50％的比例，称取等量的防护层混炼胶和软衬层混炼胶，先分别使用模具预压成型预定形状和厚度片材；防护层的预压成型温度为60℃±10℃；软衬层的预压成型温度为常温。
将形状和厚度几乎一样的防护层和软衬层的预压成型片材，依次放入到模具中进行模压共硫化成型反应，硫化压力10Mpa，硫化温度140℃，硫化时间200分钟。得到等厚度软硬一体化形状记忆复合材料，防护层厚度3mm，软衬层厚度3mm。
将得到的复合材料防护层进行表面处理，如砂纸打磨，使之粗糙，然后喷涂聚氨酯涂料。最终得到三层软硬一体化形状记忆复合材料。
实施例2
防护层具体配方为：
Figure BDA0001382597820000071
软衬层具体配方为：
Figure BDA0001382597820000081
根据上述防护层配方和软衬层配方，根据传统橡胶开炼、密炼、捏炼或者挤出混炼工艺，按照橡胶—活化剂—填料—软化剂—防老剂—硫化剂的加料顺序，分别对上述两个配方进行混炼，分别得到防护层混料胶半成品和软衬层混炼胶半成品，停放16小时以上待用。防护层的混炼温度为70℃±10℃；软衬层的混炼温度为常温加冷却水循环冷却。
按照1：9的体积比例，称取1体积份的防护层混炼胶和9体积份的软衬层混炼胶，先分别使用模具预压成型预定形状和厚度片材；防护层的预压成型温度为70℃±10℃；软衬层的预压成型温度为常温。
先将防护层预压成型片材，放入到模具中进行模压硫化成型反应，硫化压力3.5Mpa，硫化温度150℃，硫化时间100分钟。得到防护层硫化胶，厚度1mm。
将防护层和软衬层的预压成型片材，依次放入到另外的模具中进行模压共硫化成型反应，硫化温度150℃，硫化时间15分钟。得到发泡软硬一体化形状记忆复合材料，防护层厚度1mm，软衬层厚度9mm。
将得到的复合材料防护层进行表面处理，如砂纸打磨，使之粗糙，然后喷涂聚氨酯涂料。最终得到三层软硬一体化形状记忆复合材料。
实施例3
防护层具体配方为：
Figure BDA0001382597820000091
软衬层具体配方为：
Figure BDA0001382597820000092
根据上述防护层配方和软衬层配方，根据传统橡胶开炼、密炼、捏炼或者挤出混炼工艺，按照橡胶—活化剂—填料—软化剂—防老剂—硫化剂的加料顺序，分别对上述两个配方进行混炼，分别得到防护层混料胶半成品和软衬层混炼胶半成品，停放16小时以上待用。防护层的混炼温度为80℃±10℃；软衬层的混炼温度为常温加冷却水循环冷却。
按照3：7的体积比例，称取3体积份的防护层混炼胶和7体积份的软衬层混炼胶，先分别使用模具预压成型预定形状和厚度片材；防护层的预压成型温度为80℃±10℃；软衬层的预压成型温度为常温。
将形状和厚度几乎一样的防护层和软衬层的预压成型片材，依次放入到模具中进行模压共硫化成型反应，硫化压力7Mpa，硫化温度180℃，硫化时间50分钟。得到等厚度软硬一体化形状记忆复合材料，防护层厚度1.5mm，软衬层厚度3.5mm。
将得到的复合材料防护层进行表面处理，如砂纸打磨，使之粗糙，然后喷涂聚氨酯涂料。最终得到三层软硬一体化形状记忆复合材料。
实施例4
防护层具体配方为：
Figure BDA0001382597820000101
软衬层具体配方为：
Figure BDA0001382597820000102
根据上述防护层配方和软衬层配方，根据传统橡胶开炼、密炼、捏炼或者挤出混炼工艺，按照橡胶—活化剂—填料—软化剂—防老剂—硫化剂的加料顺序，分别对上述两个配方进行混炼，分别得到防护层混料胶半成品和软衬层混炼胶半成品，停放16小时以上待用。防护层的混炼温度为80℃±10℃；软衬层的混炼温度为常温加冷却水循环冷却。
按照4：6的体积比例，称取4体积份的防护层混炼胶和6体积份的软衬层混炼胶，先分别使用模具预压成型预定形状和厚度片材；防护层的预压成型温度为80℃±10℃；软衬层的预压成型温度为常温。
将形状和厚度几乎一样的防护层和软衬层的预压成型片材，依次放入到模具中进行模压共硫化成型反应，共硫化压力12Mpa，硫化温度200℃，硫化时间5分钟。得到等厚度软硬一体化形状记忆复合材料，防护层厚度3mm，软衬层厚度4.5mm。
将得到的复合材料防护层进行表面处理，如砂纸打磨，使之粗糙，然后喷涂聚氨酯涂料。最终得到三层软硬一体化形状记忆复合材料。
实施例5
防护层具体配方为：
聚己内酯/杜仲胶(塑胶) 50/50份
防老剂264 2份
双25(硫化剂) 1.5份
软衬层具体配方为：
Figure BDA0001382597820000111
根据上述防护层配方以及传统橡胶开炼、密炼、捏炼或者挤出混炼工艺，按照橡胶—活化剂—填料—软化剂—防老剂—硫化剂的加料顺序，对防护层配方进行混炼，得到防护层混料胶半成品，停放16小时以上待用。防护层的混炼温度为80℃±10℃。
将防护层半成品放入到模具中进行模共硫化成型反应，硫化压力10Mpa，硫化温度150℃，硫化时间30分钟。得到防护层硫化胶，防护层厚度7mm。
按照软衬层的配方，依次放入聚醚多元醇---水---匀泡剂---MDI加入到搅拌釜中搅拌均匀。然后将防护层硫化胶放入到聚氨酯发泡模具中，再倒入搅拌均匀的聚氨酯预聚料，待其发泡完毕后，软硬一体化形状记忆复合材料，软衬层3mm。
将得到的复合材料防护层进行表面处理，如砂纸打磨，使之粗糙，然后喷涂聚氨酯涂料。最终得到三层软硬一体化形状记忆复合材料。

Claims (5)

1.一种具有形状记忆功能的软硬一体化复合材料，其特征在于：
所述复合材料包括三层，由外及内分别为：表面装饰层、防护层和软衬层；
所述防护层为塑胶或者硫化塑胶；
所述塑胶在55℃以上受热软化，温度低于55℃之后结晶硬化；
所述软衬层为发泡聚氨酯或发泡橡胶；
所述软衬层与防护层通过共硫化成为一体结构；
所述表面装饰层为弹性涂料；所述弹性涂料为聚氨酯类涂料；
所述塑胶为杜仲胶、古塔波胶、巴拉塔胶、桃叶卫矛胶、合成反式-1,4-聚异戊二烯中的一种或组合；
所述橡胶为天然橡胶、丁苯橡胶、顺丁橡胶、三元乙丙橡胶、硅橡胶、氟橡胶、氯丁橡胶、丁腈橡胶、丁基橡胶、丙烯酸酯橡胶、氯磺化聚乙烯中的一种或组合，
所述防护层是由包括以下组份的原料混炼而得：
各组分按重量份数计：
Figure FDF0000010177240000011
所述软衬层是由包括以下组份的原料混炼而得：
各组分按重量份数计：
Figure FDF0000010177240000012
Figure FDF0000010177240000021
2.如权利要求1所述的具有形状记忆功能的软硬一体化复合材料，其特征在于：
所述复合材料总厚度为1～10mm，软衬层厚度0.5～9mm。
3.一种如权利要求1～2之一所述的具有形状记忆功能的软硬一体化复合材料的制备方法，其特征在于所述方法包括：
所述防护层和软衬层通过共硫化成一体结构，防护层外面涂敷表面装饰层，制得所述具有形状记忆功能的复合材料。
4.如权利要求3所述的具有形状记忆功能的软硬一体化复合材料的制备方法，其特征在于：
共硫化压力>3.5Mpa，共硫化温度140～200℃，共硫化时间5～100分钟。
5.如权利要求1～2之一所述的具有形状记忆功能的软硬一体化复合材料在体育护具、残疾人辅具、以及医疗器械中的应用。
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