CN116640379A - 一种橡塑粒复合材料及其制备方法与应用 - Google Patents
一种橡塑粒复合材料及其制备方法与应用 Download PDFInfo
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- CN116640379A CN116640379A CN202310649983.0A CN202310649983A CN116640379A CN 116640379 A CN116640379 A CN 116640379A CN 202310649983 A CN202310649983 A CN 202310649983A CN 116640379 A CN116640379 A CN 116640379A
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- Prior art keywords
- rubber
- ethylene
- composite material
- vinyl acetate
- parts
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Abstract
本发明公开了一种橡胶粒复合材料及其制备方法与应用。所述橡胶粒复合材料是由高分子聚合物复合微球、载体以及助剂制备而成,所述的载体为热塑性弹性体、橡胶中的一种或两种,其中,所述的热塑性弹性体为乙烯‑醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、氢化苯乙烯‑丁二烯嵌段共聚物、烯烃嵌段共聚物中的一种或几种的混合物,所述的助剂为硬脂酸、聚乙烯蜡、润滑剂、流动剂中的一种或几种的组合。通过添加本发明的橡塑粒复合材料来制备全改性复合母粒,可大比例增加再生乙烯‑醋酸乙烯酯共聚物回料的使用量,可使添加了高比例再生回料的全改性复合母粒的各项物性指标性能得到显著地提升,提高了再生乙烯‑醋酸乙烯酯共聚物回料资源的循环再利用率。
Description
技术领域
本发明涉及高分子材料领域,尤其是应用于发泡材料(包含但不限于发泡鞋材、运动鞋中底、拖鞋、凉鞋、登山鞋、棉鞋、鞋垫、乙烯-醋酸乙烯酯共聚物(EVA)板材、EVA组合地板、瑜伽垫、冲浪板、防震垫、泡沫胶带等)、功能性棚膜、医用膜、包装膜、热熔胶、电线电缆、玩具、手机保护套、平板电脑保护套、隔音板、体操垫、密封材领域和EVA油墨、箱包、酒瓶垫盖等领域的功能性产品,具体涉及一种橡塑粒复合材料及其制备方法与应用。
背景技术
目前发泡鞋类行业实际使用经发泡交联后的乙烯-醋酸乙烯酯共聚物再生回料,在考核物性指标的情况下,添加量一般为5%~15%,不超过20%,这是一个行业“卡脖子”关键共性技术问题,使得经发泡交联后的乙烯-醋酸乙烯酯共聚物回料的资源循环再利用率不高。例如在发泡鞋材现有实际使用条件下,存在着标的产品中的乙烯-醋酸乙烯酯共聚物回料添加比例比较低,主要是因为随着回料添加量不断增加,特别是在添加量达到或超过20%的情况下,标的产品的物性指标下降比较大、性能不稳定,各物料间的相容性比较差,且须兼顾考虑经发泡交联后的乙烯-醋酸乙烯酯共聚物回料改性产业化利用的低成本和便利性的矛盾,是制约经发泡交联后的乙烯-醋酸乙烯酯共聚物回料资源产业化循环再利用的一个痛点。
发明内容
针对现有技术的不足,本发明的目的在于提供一种橡塑粒复合材料及其制备方法与应用。本发明通过科学研究攻关,反复试验,充分利用配伍的各组份材料的特性,并充分利用和结合现有产业化生产装备,解决了现有材料的部分痛点,破解了行业“卡脖子”关键共性,提供了一种大幅提高再生乙烯-醋酸乙烯酯共聚物回料使用比率的高分子复合材料,实现最大化资源再利用,助力下游制鞋行业在制程上实现废弃塑料资源的循环再使用和降低碳排放。
本发明所述的一种橡塑粒复合材料,是一种橡塑粒,是一款基于提升运动鞋、拖鞋行业再生乙烯-醋酸乙烯酯共聚物回料(行业称“布料”、粉料)的高填充循环再利用的高性能聚合物改质母粒,是一种降低碳排放和促进废弃塑料资源循环再利用的绿色技术,为实现“双减”目标和促进绿色循环经济,提供行业科技创新支撑,主要用于提升循环再生的乙烯-醋酸乙烯酯共聚物回料物性和提高填充比例,主要应用于运动鞋乙烯-醋酸乙烯酯共聚物复合材料的发泡中底。
为了实现上述的技术目的,本发明采用的技术方案为:
一种橡塑粒复合材料(改质母粒),是由高分子聚合物复合微球、载体以及助剂制备而成。
所述的高分子聚合物复合微球为一种水溶性高聚物,主要由热塑性醋酸乙烯-羧酸(类)乙烯共聚物、纤维素、改性聚乙烯醇及其他助剂材料组成的,经喷雾干燥制备得到的堆积密度400~600g/L、细度(≥150μm)≤10.0%、灰分(1000℃)为12±2%、平均粒径为10~500μm的空心微球粉体。
所述的载体为热塑性弹性体、橡胶中的一种或两种,其中,所述的热塑性弹性体包括但不限于乙烯-醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、氢化苯乙烯-丁二烯嵌段共聚物、烯烃嵌段共聚物中的一种或几种的混合物;其中,所述的橡胶包括但不限于天然橡胶NR、二元乙丙橡胶EPR、三元乙丙橡胶EPDM、丁晴橡胶NBR、顺丁橡胶BR、丁基橡胶IIR、丁苯橡胶SBR、氯丁橡胶CR、硅橡胶SI、再制橡胶、再生橡胶,所述的橡胶外观为块状、颗粒状和粉末状。
所述助剂为硬脂酸、聚乙烯蜡、润滑剂、流动剂或其它高分子蜡中的一种或几种的组合。
进一步地,按重量计,所述橡塑粒复合材料是由5~35份高分子聚合物复合微球、3~80份载体以及以上两者总重量0.2-3%的助剂制备而成。
当所述载体组分中含有乙烯-醋酸乙烯酯共聚物时,其乙烯-醋酸乙烯酯共聚物添加量为30~80份。
当所述载体组分中含有橡胶时,其橡胶添加量为3~10份。
当所述载体组分中含有氢化苯乙烯-丁二烯嵌段共聚物时,其氢化苯乙烯-丁二烯嵌段共聚物添加量为1~20份。
当所述载体组分中含有聚烯烃热塑性弹性体时,其聚烯烃热塑性弹性体添加量为3~10份。
当所述载体组分中含有烯烃嵌段共聚物时,其烯烃嵌段共聚物添加量为3~10份。
作为本发明的一种实施方式,所述的橡塑粒复合材料由5~35份的高分子聚合物复合微球(泉州市云尚三维科技有限公司YSV07)与30~60份乙烯-醋酸乙烯酯共聚物、1~20份填充了0.5~2倍润滑油的氢化苯乙烯-丁二烯嵌段共聚物、3~10份的三元乙丙橡胶或二元乙丙橡胶、3~10份的聚烯烃热塑性弹性体、3~10份的烯烃嵌段共聚物的两种或两种以上混合物以及以上总重量0.2-3%的助剂制备而成。
进一步地,所述橡塑粒复合材料的制备方法为:将高分子聚合物复合微球、载体以及助剂通过加热型密炼机共混密炼,或经过加热型开炼机共混压片,然后造粒制得。造粒设备为单螺杆风切、水环切、水下造粒等造粒设备,或双螺杆造粒设备。
本发明还提供所述橡塑粒复合材料的应用,即将其用于制备全改性复合母粒。
取橡塑粒复合材料(5~15份),再生乙烯-醋酸乙烯酯共聚物回料(4~70份),三元乙丙橡胶、二元乙丙橡胶、乙烯-醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、烯烃嵌段共聚物中的一种或几种的混合物(共40~60份),以及助剂,经共混密炼后造粒冷却,得到全改性复合母粒。
作为本发明的一种实施方式,按重量计,取5~10份橡塑粒复合材料(改质母粒),4~70份经消泡并压成薄片处理或研磨成粉末状后的再生乙烯-醋酸乙烯酯共聚物回料,5~10份三元乙丙橡胶、二元乙丙橡胶中的一种或两种,5~10份聚烯烃热塑性弹性体,3~10份烯烃嵌段共聚物,40~60份乙烯-醋酸乙烯酯共聚物,视情况选择再添加若干发泡剂、交联剂、色粉、填充剂、热稳定剂及其他助剂后,经共混密炼后造粒冷却,得到高再生比例全改性复合母粒(全改料)。
全改性复合母粒(全改料)可应用于运动鞋发泡中底和拖鞋,发泡后的得到含有超高比例再生材料的再生运动鞋中底、再生拖鞋产品。
所述的橡塑粒复合材料(改质母粒)可分别与同非极性材料或与极性材料、弹性体材料、水凝胶材料、非牛顿流体材料,按一定比例混合或造粒使用,制成新的同非极性或极性材料或兼具了极性和非极性的相关改性复合材料。
所述的同非极性材料或与极性材料、弹性体材料、水凝胶材料、非牛顿流体材料,包括但不限于天然橡胶NR、二元乙丙橡胶EPR、三元乙丙橡胶EPDM、丁晴橡胶NBR、顺丁橡胶BR、丁基橡胶IIR、丁苯橡胶SBR、氯丁橡胶CR、硅橡胶SI、再制橡胶、再生橡胶、乙烯-醋酸乙烯酯共聚物EVA、茂金属聚烯烃、环烯烃共聚物COC/COP、氢化苯乙烯-丁二烯嵌段共聚物SEBS、SBS、POE、PE、TPU、ETPU、OBCs、聚醚酰胺嵌段共聚物TPAE、PEBAx、PA6、PA66、PA12、生物质材料、天然高分子材料等材料及其单一组分或多组分混合的再制、再生材料。
本发明采用上述的技术方案,其具有的有益效果为:
1、高分子聚合物复合微球,作为本发明的核心材料,其与再生乙烯-醋酸乙烯酯共聚物回料和其它组分形成互穿网络结构,在孔隙中形成连续的聚合物膜,加强了各组分材料之间的粘结,为最终的发泡产品提供了优异的抗压强度和抗折强度,提高了制成品的抗冲击韧性,也赋予了良好的应力分散作用,利用其一定的渗透性,与纤维素醚一起浸润材料表面,提高了大分子粘结/吸附性,降低原再生乙烯-醋酸乙烯酯共聚物回料中各添加物弹性模量,提高变形能力,从而提高了抗热撕裂能力,减少发泡制品生产过程中出现的热撕裂现象。
2、橡塑粒复合材料选用的乙烯-醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、橡胶、乙烯-醋酸乙烯酯共聚物、烯烃嵌段共聚物、氢化苯乙烯-丁二烯嵌段共聚物具可填充性,橡塑粒复合材料配方各组份间材料相容性好,不会出现分层现象。
3、本发明的橡塑粒复合材料与热塑性弹性体、橡胶的相容性好,应用于乙烯-醋酸乙烯酯共聚物及其再生回料的物性提升,适用于挤出和注塑加工,是一款可大比例提高乙烯-醋酸乙烯酯共聚物再生回料高填充比例的升级产品。通过添加本发明的橡塑粒复合材料,可大比例增加再生乙烯-醋酸乙烯酯共聚物回料的使用量,可使添加了高比例再生回料的全改性复合母粒的各项物性指标性能得到显著地提升,提高了再生乙烯-醋酸乙烯酯共聚物回料资源的循环再利用率,拓宽了应用领域。本发明的橡塑粒复合材料生产采用现有成熟的装备和生产工艺,大大降低了本发明的科研成果产业化转化复杂性,同时降低了最终标的产品(例如运动鞋中底、拖鞋)的综合材料成本,大幅降低了例如鞋制程中的碳排放量。
附图说明
图1是本发明的实施例制备的橡塑粒复合材料样品。
图2是添加50%再生EVA回料(布料)的运动鞋二次发泡中底样品。
图3是添加50%再生EVA回料(布料)的运动鞋一次射出发泡中底样品
图4是添加50%再生EVA回料(布料)的一次射出发泡拖鞋样品。
具体实施方式
本发明中热塑性弹性体,包含但不限于:苯乙烯系热塑性弹性体TPS、聚烯烃类热塑性弹性体TPO、热塑性聚氨酯弹性体TPU、聚酯热塑性弹性体TPEE、聚酰胺热塑性弹性体TPAE、热塑性硅弹性体(包括:嵌段共聚型含硅TPE和动态硫化型含硅TPV)、热塑性氟弹性体、嵌段共聚物型热塑性丙烯酸酯类弹性体、硫化热塑性弹性体。
部分化合物的英文缩写如下:
乙烯-醋酸乙烯酯共聚物EVA
乙烯和α-烯烃共聚物POE
氢化苯乙烯-丁二烯嵌段共聚物SEBS
烯烃嵌段共聚物OBCs
以下实施例中
(1)EVA 6110M购买于巴斯夫。
(2)EVA 02518购买于韩国韩华。
(3)再生乙烯-醋酸乙烯酯共聚物回料是指:将生产乙烯-醋酸乙烯酯共聚物运动鞋中底、拖鞋的边角料、次品、消费后乙烯-醋酸乙烯酯共聚物回收料,经过破碎、混炼、开炼机开练压膜制得到再生乙烯-醋酸乙烯酯共聚物回料的布料。
将生产乙烯-醋酸乙烯酯共聚物运动鞋中底、拖鞋的边角料、次品、消费后乙烯-醋酸乙烯酯共聚物回收料,经过破碎、研磨成一定目数的粉末状,为再生乙烯-醋酸乙烯酯共聚物回料的粉料。
再生乙烯-醋酸乙烯酯共聚物回料之布料、粉料,购自福建地区的再生乙烯-醋酸乙烯酯共聚物回料(布料、粉料)加工厂。
(4)高分子聚合物微球YSV07购买于泉州市云尚三维科技有限公司,主要由热塑性醋酸乙烯-羧酸(类)乙烯共聚物、纤维素、改性聚乙烯醇及其他助剂材料组成的,以改性聚乙烯醇为壳体保护层,经喷雾干燥制备得到的堆积密度400~600g/L、细度(≥150μm)≤10.0%、灰分(1000℃)为12±2%、平均粒径为10~500μm的空心微球粉体。
实施例1
一种橡塑粒复合材料(以下简称“改质母粒”)的制备方法:
取如下重量份的组分:
二元乙丙橡胶 50公斤;
高分子聚合物复合微球 25公斤;
硬脂酸 2公斤。
将上述各组分共混于75L加热型密炼机内,设定加工温度为105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水环切挤出造粒装备中,进行水冷造粒,得到橡胶复合材料,以下简称“改质母粒”。
将上述改质母粒连同经过消泡处理后的再生乙烯-醋酸乙烯酯共聚物回料,以及制备发泡鞋材的添加剂(包括但不仅限于:发泡剂、交联剂、氧化锌、硬脂酸、硬脂酸锌、滑石粉、色粉、填充剂、碳酸钙粉、稳定剂、流动剂、快熟剂、白矿油、硅胶)一起共混造粒,制备用于运动鞋中底和拖鞋发泡用的全改性复合母粒,以下简称“全改料”,具体如下:
取如下重量份的组分:
将上述各组分通过生产运动鞋中底和拖鞋的射出发泡装备,按1.5~1.9倍的发泡倍率,制备成品运动鞋中底或拖鞋;
或者,将上述各组分通过生产运动鞋中底的二次发泡装备,按1.7~1.8倍的发泡倍率,制备成品运动鞋中底。
实施例2
本实施例制备的改质母粒组分与实施例1相同,不同之处在于:①造粒设备改用风切挤出造粒,②全改料使用不同VA含量的乙烯-醋酸乙烯酯共聚物EVA,发泡后的成品软硬度有差异。
本实施例的橡塑粒复合材料(改质母粒),包括如下重量份的组分:
三元乙丙橡胶 50公斤;
高分子聚合物复合微球 25公斤;
硬脂酸 2公斤。
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆风切挤出造粒装备中,进行风冷造粒后备用。
全改性复合母粒(全改料)包括如下重量份的组分:
本实施例全改性复合母粒的制备方法同实施例1。
实施例3
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水环切挤出造粒装备中,进行水冷造粒。
实施例4
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
乙烯-醋酸乙烯酯共聚物EVA 50Kg;
高分子聚合物复合微球 25Kg;
硬脂酸 2.2Kg。
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水中造粒挤出装备中,造粒后备用。
实施例5
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃条件下,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水中造粒挤出装备中,进行造粒。
实施例6
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水中造粒挤出装备中,进行造粒。
实施例7
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水中造粒挤出装备中,进行造粒。
实施例8
一种橡塑粒复合材料(改质母粒),包括如下重量份的组分:
将上述各组分共混于75L加热型密炼机内,设定加工温度105℃,使上述组分材料充分分散、混匀、发生相关物理和化学变化,并熟成,取出经过密炼后的材料放置于单螺杆水中造粒挤出装备中,进行造粒。
表1添加5%橡塑粒复合材料(R系列改质母粒)和50%再生乙烯-醋酸乙烯酯共聚物回料的运动鞋全改料1.7发泡倍率的发泡片材测试结果
以上描述了本发明的具体实施方式,但是本领域的技术人员应当理解,这仅是举例说明,本领域的技术人员在不背离本发明的原理和实质的前提下,可以对此实施方式做出多种变更或修改,但这些变更和修改均落入本发明的保护范围。
Claims (9)
1.一种橡塑粒复合材料,其特征在于,其是由高分子聚合物复合微球、载体以及助剂制备而成,所述的载体为热塑性弹性体、橡胶中的一种或两种,其中,所述的热塑性弹性体包括但不限于乙烯-醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、氢化苯乙烯-丁二烯嵌段共聚物、烯烃嵌段共聚物中的一种或几种的混合物,所述的助剂为硬脂酸、聚乙烯蜡、润滑剂、流动剂的一种或几种的组合。
2.根据权利要求1所述的一种橡塑粒复合材料,其特征在于,所述的高分子聚合物复合微球是由热塑性醋酸乙烯-羧酸(类)乙烯共聚物、纤维素、改性聚乙烯醇及助剂,经喷雾干燥制备得到的堆积密度400~600g/L、平均粒径为10~500μm的空心微球粉体。
3.根据权利要求1所述的一种橡塑粒复合材料,其特征在于,所述的橡胶为天然橡胶、二元乙丙橡胶、三元乙丙橡胶、丁晴橡胶、顺丁橡胶、丁基橡胶、丁苯橡胶、氯丁橡胶、硅橡胶、再制橡胶、再生橡胶中的一种或一种以上的混合物。
4.根据权利要求1所述的一种橡塑复合材料,其特征在于,按重量计,所述橡塑粒复合材料是由5~35份高分子聚合物复合微球、3~80份载体以及以上两者总重量0.2-3%的助剂制备而成。
5.根据权利要求4所述的一种橡塑粒复合材料,其特征在于,当所述载体组分中含有乙烯-醋酸乙烯酯共聚物时,其乙烯-醋酸乙烯酯共聚物添加量为30~80份,当所述载体组分中含有橡胶时,其橡胶添加量为3~10份,当所述载体组分中含有氢化苯乙烯-丁二烯嵌段共聚物时,其氢化苯乙烯-丁二烯嵌段共聚物添加量为1~20份,当所述载体组分中含有聚烯烃热塑性弹性体时,其聚烯烃热塑性弹性体添加量为3~10份,当所述载体组分中含有烯烃嵌段共聚物时,其烯烃嵌段共聚物添加量为3~10份。
6.一种如权利要求1~5任一项所述的橡塑粒复合材料的制备方法,其特征在于,将高分子聚合物复合微球、载体以及助剂通过加热型密炼机共混密炼,或经过加热型开炼机共混压片,然后经过造粒机造粒制得。
7.一种如权利要求1~5任一项所述的橡塑粒复合材料的应用,其特征在于,将其用于制备全改性复合母粒,制备方法如下:取橡塑粒复合材料,再生乙烯-醋酸乙烯酯共聚物回料,三元乙丙橡胶、二元乙丙橡胶,乙烯-醋酸乙烯酯共聚物、聚烯烃热塑性弹性体、烯烃嵌段共聚物中的一种或几种的混合物,以及助剂,经共混密炼后造粒冷却,得到全改性复合母粒。
8.根据权利要求7所述的橡塑粒复合材料的应用,其特征在于,各组分重量份如下:
橡塑粒复合材料:5~15份;再生乙烯-醋酸乙烯酯共聚物回料:4~70份;乙烯-醋酸乙烯酯共聚物、三元乙丙橡胶、二元乙丙橡胶、聚烯烃热塑性弹性体、烯烃嵌段共聚物中的一种或几种的混合物:40~60份。
9.根据权利要求7所述的橡塑粒复合材料的应用,其特征在于,所制备的全改性复合母粒用于生产运动鞋中底或拖鞋。
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