CN108359167A - 一种耐磨微孔弹性体及其制备方法 - Google Patents
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Abstract
本发明涉及一种耐磨微孔弹性体及其制备方法,特征在于采用20质量份三元乙丙橡胶、30质量份顺丁橡胶、50质量份乙烯‑醋酸乙烯酯共聚物、40质量份动态硫化预分散胶、抗氧剂5‑7质量份,氧化锌5‑8质量份,硬脂酸0.5‑1质量份,促进剂2‑3质量份,硫黄0.5‑1质量份,2,5‑二甲基‑2,5‑二(叔丁基过氧基)己烷1‑2质量份,发泡剂3‑5质量份。本发明制备得到的微孔弹性体,其耐磨性能良好,兼具硬度小、弹性高、减振性能好、尺寸稳定、力学性能优异、柔软性佳和穿着舒适性良好等综合性能,可用于运动鞋的鞋底。
Description
技术领域
本发明属于橡胶类聚合物复合材料及其制备方法,特别是一种具有良好耐磨性能的微孔弹性体及其制备方法。
背景技术
微孔弹性体具有密度小,力学性能高,防滑、减振及良好的穿着舒适性,被大量应用做运动鞋底材料。目前市面上的微孔弹性体鞋材,主要是以乙烯醋酸乙烯酯共聚物(EVA)为基体,搭配一定的橡胶、填料、硫化剂和发泡剂等多种配合剂共混发泡而成。但是由于微孔材料的体积中含有大量的微孔,导致其耐磨性不足,影响鞋材的使用寿命。为了提高耐磨性,市面上存在几种措施:(1)在EVA鞋材底部贴一层耐磨橡胶大底,但是这种方法增加了工序和材料,严重提高的生产成本;(2)在填料中加入片层滑石粉,利用片层材料层与层之间滑移,降低外界与微孔材料的摩擦系数,但是摩擦系数的降低会增加滑倒的风险,特别是在湿路面的时候;(3)加入玻璃化转变温度较低的聚合物,聚合物的分子柔顺性,提高微孔材料的耐磨性,但是这些柔顺聚合物大多数为非极性,与极性的EVA基体相容性不好,导致微孔弹性体的综合性能降低。因此,如何在提高EVA基微孔弹性体耐磨性的同时,保持甚至是提高其他性能,是目前鞋类工业界的研究方向之一。
发明内容
本发明的目的在于提供了一种耐磨微孔弹性体及其制备方法。
实现本发明的技术解决方案:
一种耐磨微孔弹性体的制备方法,其特征在于包含以下步骤:
步骤一:将100 g的碳酸钙加入500 mL乙醇溶液中,500 W超声搅拌10 min,加入2-4 g硬脂酸,500 W超声搅拌5 min,离心,干燥,球磨,得到改性碳酸钙;
步骤二:将30质量份的顺丁橡胶加入开炼机,加入100质量份步骤一得到的改性碳酸钙,混炼8 min,加入20质量份三元乙丙橡胶和100质量份步骤一得到的改性碳酸钙,混炼3min,加入5质量份的顺丁烯二酸酐,混炼3 min,升高温度到80 ℃,加入50质量份乙烯-醋酸乙烯酯共聚物和100质量份步骤一得到的改性碳酸钙,混炼5 min,加入5质量份2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷, 80 ℃继续混炼10 min,得到动态硫化预分散胶;
步骤三:将30质量份顺丁橡胶和20质量份三元乙丙橡胶在开炼机上共混5 min,升温到80℃,加入50质量份的乙烯-醋酸乙烯酯共聚物和40质量份步骤二得到的动态硫化预分散胶,加入抗氧剂5-7质量份,氧化锌5-8质量份,硬脂酸0.5-1质量份,促进剂2-3质量份,硫黄0.5-1质量份,2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷1-2质量份,发泡剂3-5质量份;薄通,得到共混胶;
步骤四:将步骤三制得的共混胶停放24h后,用硫化仪测定正硫化时间和发泡时间,用平板硫化机模压发泡,硫化温度为160℃,得到耐磨微孔弹性体。
所述的碳酸钙的尺寸为10-20 μm。
所述的顺丁橡胶为BR9000,三元乙丙橡胶为含有3%乙叉降冰片烯第三单体的三元乙丙橡胶,乙烯-醋酸乙烯酯为含有20%醋酸乙烯酯单体的乙烯-醋酸乙烯酯共聚物。
所述的抗氧剂为抗氧剂264和抗氧剂2246中的任意一种,促进剂为TMTD和TMTM中的任意一种,发泡剂为偶氮二甲酰胺。
本发明还公开了利用上述方法制备得到的耐磨微孔弹性体。
本发明与现有技术相比,其显著优点是:
(1)由于碳酸钙在发泡过程中能用作成核剂以及硬脂酸能促进发泡剂分解的效果,本发明采用了硬脂酸改性的碳酸钙,利用硬脂酸对发泡的促进作用,在碳酸钙的周围提高微孔的形成率,降低材料的密度,另一方面,利用碳酸钙的补强效果,对其周围形成的微孔进行补强,弥补由于微孔形成所造成的微孔弹性体力学强度下降的问题,实现了质轻高强的效果;
(2)在动态硫化预分散胶原材料的复配上,往乙烯-醋酸乙烯酯共聚物/三元乙丙橡胶体系中加入顺丁橡胶,搭配了顺丁烯二酸酐和硬脂酸改性碳酸钙,分别利用顺丁烯二酸酐的接枝改性、表面改性碳酸钙的界面活性和交联强制互溶技术,同时提高顺丁橡胶、三元乙丙橡胶与EVA基体的相容性,得到良好界面效果的动态硫化预分散胶;
(3)在微孔弹性体中采用了动态硫化预分散胶,一方面利用其预分散的效果,使得填料碳酸钙均匀分散在微孔弹性体中,另一方面利用其良好的界面效果,解决了微孔弹性体中三相的相容性,从而得到耐磨性能好、综合性能优良的微孔弹性体。
下面结合附图对本发明作进一步详细描述。
附图说明
图1 耐磨微孔弹性体的制备工艺流程。
具体实施方式
一种耐磨微孔弹性体,包括以下步骤:
步骤一:将100 g的碳酸钙加入500 mL乙醇溶液中,500 W超声搅拌10 min,加入2-4 g硬脂酸,500 W超声搅拌5 min,离心,干燥,球磨,得到改性碳酸钙;
步骤二:将30质量份的顺丁橡胶加入开炼机,加入100质量份步骤一得到的改性碳酸钙,混炼8 min,加入20质量份三元乙丙橡胶和100质量份步骤一得到的改性碳酸钙,混炼3min,加入5质量份的顺丁烯二酸酐,混炼3 min,升高温度到80 ℃,加入50质量份乙烯-醋酸乙烯酯共聚物和100质量份步骤一得到的改性碳酸钙,混炼5 min,加入5质量份2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷, 80 ℃继续混炼10 min,得到动态硫化预分散胶;
步骤三:将30质量份顺丁橡胶和20质量份三元乙丙橡胶在开炼机上共混5 min,升温到80℃,加入50质量份的乙烯-醋酸乙烯酯共聚物和40质量份步骤二得到的动态硫化预分散胶,加入抗氧剂5-7质量份,氧化锌5-8质量份,硬脂酸0.5-1质量份,促进剂2-3质量份,硫黄0.5-1质量份,2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷1-2质量份,发泡剂3-5质量份,薄通,得到共混胶;
步骤四:将步骤三制得的共混胶停放24h后,用硫化仪测定正硫化时间和发泡时间,用平板硫化机模压发泡,硫化温度为160℃,得到耐磨微孔弹性体。
所述的碳酸钙的尺寸为10-20μm。
所述的顺丁橡胶为BR9000,三元乙丙橡胶为含有3%乙叉降冰片烯第三单体的三元乙丙橡胶,乙烯-醋酸乙烯酯为含有20%醋酸乙烯酯单体的乙烯-醋酸乙烯酯共聚物。
所述的抗氧剂为抗氧剂264和抗氧剂2246中的任意一种,促进剂为TMTD和TMTM中的任意一种,发泡剂为偶氮二甲酰胺。
将制得的耐磨微孔弹性体进行以下性能测试。
(1)拉伸性能
根据GB/T528-2009标准对微孔弹性体进行测试,拉伸速度500mm/min。记录弹性体的定伸100%模量(M 100)、拉伸强度、断裂伸长率。具有越大拉伸强度的样品越好。
(2)撕裂性能
撕裂性能测试按照GB/T529-2008标准对微孔弹性体进行测试,速度为500mm/min,记录弹性体的撕裂强度。具有越大撕裂强度的样品越好。
(3)耐磨性能
耐磨性能按照GB/T9867-2001标准在中国台湾高铁GT-7912-D DIN摩耗试验机上测试,记录弹性体的磨耗体积。具有越小磨耗体积的样品越好。
(4)硬度测试
硬度采用GS-701N硬度计测试,按照GB/T 531-1999。
(5)冲击回弹性
冲击回弹性按照GB/T1681-1991标准冲击弹性试验机上测试,记录回弹值。具有越大回弹值的样品越好。
(6)变形率
压缩变形率按照标准HG/T 2876-2009在MZ-4020压缩永久变率试验器上进行测试,记录变形率。具有越小变形率的样品越好。
(7)尺寸收缩率
按照标准GB/T3903.13测试,具有越小收缩率的样品越好。
下面通过实施例和对比例对本发明作进一步说明。
实施例1
步骤一:将100 g 20μm的碳酸钙加入500 mL乙醇溶液中,500 W超声搅拌10 min,加入2g硬脂酸,500 W超声搅拌5 min,离心,干燥,球磨,得到改性碳酸钙;
步骤二:将30质量份的BR9000顺丁橡胶加入开炼机,加入100质量份步骤一得到的改性碳酸钙,混炼8 min,加入20质量份含3%乙叉降冰片烯第三单体的三元乙丙橡胶和100质量份步骤一得到的改性碳酸钙,混炼3 min,加入5质量份的顺丁烯二酸酐,混炼3 min,升高温度到80 ℃,加入50质量份20%醋酸乙烯酯单体乙烯-醋酸乙烯酯共聚物和100质量份步骤一得到的改性碳酸钙,混炼5 min,加入5质量份2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷,80 ℃继续混炼10 min,得到动态硫化预分散胶;
步骤三:将30质量份BR9000顺丁橡胶和20质量份含3%乙叉降冰片烯第三单体的三元乙丙橡胶在开炼机上共混5 min,升温到80℃,加入50质量份含20%醋酸乙烯酯单体的乙烯-醋酸乙烯酯共聚物和40质量份步骤二得到的动态硫化预分散胶,加入抗氧剂264 7质量份,氧化锌5质量份,硬脂酸1质量份,促进剂TMTM 2质量份,硫黄1质量份,2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷2质量份,发泡剂偶氮二甲酰胺5质量份;薄通,得到共混胶;
步骤四:将步骤三制得的共混胶停放24h后,用硫化仪测定正硫化时间和发泡时间,用平板硫化机模压发泡,硫化温度为160℃,得到耐磨微孔弹性体,微孔弹性体的制备流程如图1,详细性能如表1。
实施例2
按指定的各组分含量重复实施例1的方法,但在步骤一中采用了10 μm的碳酸钙,硬脂酸4 g,步骤三中采用了抗氧剂2246 5 质量份,氧化锌8质量份,硬脂酸0.5质量份,促进剂TMTD 3质量份,硫黄0.5质量份,2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷1质量份,发泡剂偶氮二甲酰胺3质量份,得到的微孔弹性体详细性能如表1。
对比例1
按指定的各组分含量重复实施例2的方法,但在配方中采用30 μm碳酸钙,得到的微孔弹性体详细性能如表1。
对比例2
按指定的各组分含量重复实施例2的方法,但在配方中采用5 μm碳酸钙,得到的微孔弹性体详细性能如表1。
对比例3
按指定的各组分含量重复实施例2的方法,但在配方步骤一中加入6 g 硬脂酸,得到的微孔弹性体详细性能如表1。
对比例4
按指定的各组分含量重复实施例2的方法,但在配方步骤一中不加入硬脂酸,得到的微孔弹性体详细性能如表1。
对比例5
按指定的各组分含量重复实施例2的方法,但在配方中直接将步骤二中的所有原料按比例与步骤三中原料混合,得到的微孔弹性体详细性能如表1。
对比例6
按指定的各组分含量重复实施例2的方法,但在配方步骤二中不添加2, 5-二甲基-2,5-二(叔丁基过氧基)己烷,得到的微孔弹性体详细性能如表1。
对比例7
按指定的各组分含量重复实施例2的方法,但在配方步骤二中,不加入顺丁烯二酸酐,得到的微孔弹性体详细性能如表1。
对比例8
按指定的各组分含量重复实施例2的方法,但在配方步骤二中,所有原料一次性加入,得到的微孔弹性体详细性能如表1。
对比例9
按指定的各组分含量重复实施例2的方法,但在配方步骤三中,不添加2, 5-二甲基-2,5-二(叔丁基过氧基)己烷,得到的微孔弹性体详细性能如表1。
对比例10
按指定的各组分含量重复实施例2的方法,但在配方步骤三中,不添加硬脂酸、氧化锌、促进剂和硫黄,得到的微孔弹性体详细性能如表1。
表1
硬度C | 密度(g/cm3) | 拉伸强度 (MPa) | 撕裂强度 (kN/m) | 尺寸收缩率(%) | 回弹性(%) | 压缩变形率(%) | DIN磨耗(mm3) | |
实施例1 | 40 | 0.18 | 5.2 | 8.1 | 0.3 | 65 | 17 | 180 |
实施例2 | 40 | 0.19 | 5.8 | 8.6 | 0.2 | 68 | 18 | 170 |
对比例1 | 43 | 0.22 | 2.7 | 4.7 | 1.2 | 40 | 31 | 310 |
对比例2 | 43 | 0.23 | 2.5 | 4.8 | 1.1 | 42 | 29 | 305 |
对比例3 | 40 | 0.26 | 1.8 | 2.3 | 2.5 | 45 | 40 | 380 |
对比例4 | 44 | 0.24 | 2.8 | 5.2 | 0.9 | 48 | 35 | 285 |
对比例5 | 45 | 0.25 | 1.6 | 2.0 | 2.3 | 39 | 45 | 410 |
对比例6 | 44 | 0.26 | 2.8 | 4.6 | 1.9 | 43 | 37 | 365 |
对比例7 | 43 | 0.25 | 2.7 | 4.9 | 2.1 | 45 | 35 | 355 |
对比例8 | 45 | 0.24 | 2.5 | 4.8 | 1.8 | 45 | 36 | 360 |
对比例9 | 41 | 0.18 | 3.4 | 6.1 | 3.1 | 50 | 48 | 420 |
对比例10 | 44 | 0.17 | 4.1 | 4.4 | 1.6 | 38 | 28 | 350 |
本发明提供了一种具有耐磨微孔弹性体及其制备方法。制备得到的微孔弹性体,具有耐磨性能好,并且兼具硬度小、弹性高、减振性能好、尺寸稳定、力学性能优异、柔软性佳和穿着舒适性良好等综合性能,可用于制作运动鞋的鞋底。
Claims (5)
1.一种耐磨微孔弹性体的制备方法,其特征在于包含以下步骤:
步骤一:将100 g的碳酸钙加入500 mL乙醇溶液中,500 W超声搅拌10 min,加入2-4 g硬脂酸,500 W超声搅拌5 min,离心,干燥,球磨,得到改性碳酸钙;
步骤二:将30质量份的顺丁橡胶加入开炼机,加入100质量份步骤一得到的改性碳酸钙,混炼8 min,加入20质量份三元乙丙橡胶和100质量份步骤一得到的改性碳酸钙,混炼3min,加入5质量份的顺丁烯二酸酐,混炼3 min,升高温度到80 ℃,加入50质量份乙烯-醋酸乙烯酯共聚物和100质量份步骤一得到的改性碳酸钙,混炼5 min,加入5质量份2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷,80 ℃继续混炼10 min,得到动态硫化预分散胶;
步骤三:将30质量份顺丁橡胶和20质量份三元乙丙橡胶在开炼机上共混5 min,升温到80℃,加入50质量份的乙烯-醋酸乙烯酯共聚物和40质量份步骤二得到的动态硫化预分散胶,加入抗氧剂5-7质量份,氧化锌5-8质量份,硬脂酸0.5-1质量份,促进剂2-3质量份,硫黄0.5-1质量份,2, 5-二甲基-2, 5-二(叔丁基过氧基)己烷1-2质量份,发泡剂3-5质量份;薄通,得到共混胶;
步骤四:将步骤三制得的共混胶停放24h后,用硫化仪测定正硫化时间和发泡时间,用平板硫化机模压发泡,硫化温度为160℃,得到耐磨微孔弹性体。
2.根据权利要求1所述的一种耐磨微孔弹性体的制备方法,其特征在于,步骤一中的碳酸钙的尺寸为10-20 μm。
3.根据权利要求1所述的一种耐磨微孔弹性体的制备方法,其特征在于,步骤二和步骤三中的顺丁橡胶为BR9000,三元乙丙橡胶为含有3%乙叉降冰片烯第三单体的三元乙丙橡胶,乙烯-醋酸乙烯酯为含有20%醋酸乙烯酯单体的乙烯-醋酸乙烯酯共聚物。
4.根据权利要求1所述的一种耐磨微孔弹性体的制备方法,其特征在于,步骤四中的抗氧剂为抗氧剂264和抗氧剂2246中的任意一种,促进剂为TMTD和TMTM中的任意一种,发泡剂为偶氮二甲酰胺。
5.一种根据权利要求1-4任一项所述方法制备得到的耐磨微孔弹性体。
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