CN113462009A - 一种磁性吸油聚烯烃泡沫材料及其制备方法 - Google Patents
一种磁性吸油聚烯烃泡沫材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及吸油材料技术领域,具体涉及一种磁性吸油聚烯烃泡沫材料及其制备方法。本发明制备方法主要包括以下步骤:首先将四氧化三铁置于共混机中,加入偶联剂进行共混表面改性;然后将改性好的四氧化三铁加入聚烯烃发泡组合物中共混,在挤出机中经超临界气体发泡,冷却造粒,即得该磁性吸油聚烯烃泡沫材料。本发明制备方法简单,成本低,可工业化生产,所制备的磁性吸油聚烯烃泡沫材料具有良好的亲油疏水和高回弹性能,吸油效果良好,可重复使用,铺覆于海面上,通过磁场作用,不扩散,易回收重复使用,并且回收的吸油泡沫材料通过离心可对油品进行回收。
Description
技术领域
本发明涉及吸油材料技术领域,具体涉及一种磁性吸油聚烯烃泡沫材料及其制备方法。
背景技术
随着世界经济的快速发展,全球工业化进程的加快和全球能源需求的快速增长,原油的开发力度越来越大,对石油资源及其衍生物的需求也在不断增加。石油泄露事件时有发生,油水混合处理不好,会对环境和生态***甚至人类的生存造成严重损害。因此,对油水混合物的有效分离成为近年的研究热点。目前,处理水体泄油的方法主要包括分散、燃烧和吸附几种方式。其中,吸附净化油污被认为是最经济、快速、最有效的方法之一。泡沫、海绵等多孔材料因其具有比表面积大、吸油率高、原料易得且制造简单等优点,成为进行油水分离处理的首选吸附材料。
公告号为CN104744819B的专利公开了一种发泡聚丙烯吸油材料及其制备方法,该吸油材料的亲油疏水性能较好,可以有效解决油品回收纯度和重复使用的问题,但是所制备的吸油材料超疏水,在水中具有良好的流动性和分散性,应用于油水分离处理时常出现吸油材料易分散、不容易聚集回收的情况,导致其在动态水面处理油污泄露的环境下难以进行大规模应用。公告号为CN104151600B的发明专利公开了一种超疏水磁性海绵的制备方法,通过浸润和利用黏合剂的方式将海胆状碳包覆四氧化三铁粒子附着在聚氨酯海绵的表面,使得海绵获得磁性和疏水性能,但是该方法所制备的超疏水磁性海绵在使用过程中,随着重复使用次数的增多,海绵中的磁性层会逐渐减少,疏水性能逐渐减弱,从而将会影响重复使用率和油水回收效果。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种磁性吸油聚烯烃泡沫材料及其制备方法。本发明所提供的磁性吸油聚烯烃泡沫材料不仅具有良好的亲油疏水和高回弹性能,可重复使用,吸油率和保油率优异,而且在外加磁场的作用下,可以在动态水面上对本发明的聚烯烃泡沫材料进行有效的定位收集,可以有效解决现有吸油材料存在的在动态水面应用时不容易回收,以及吸油材料重复利用率低、油水分离效果不佳、回收油品纯度不高等技术问题。
为了解决上述技术问题,本发明采取的技术方案是:
一种磁性吸油聚烯烃泡沫材料的制备方法,包括以下步骤:
S1,将经干燥处理的四氧化三铁置于共混机中,加入偶联剂,在常温下搅拌混合均匀后静置,制得改性四氧化三铁;
S2,将所述改性四氧化三铁与聚烯烃发泡组合物在共混机中共混均匀,得到磁性聚烯烃发泡组合物;
S3,将所述磁性聚烯烃发泡组合物加入单螺杆挤出机的料仓中进行挤出,同时在挤出机的压缩段通过注气***加入超临界气体,经过挤出机的模头挤出发泡,然后冷却切粒,即得所述磁性吸油聚烯烃泡沫材料。
上述步骤S1中的共混机搅拌速度为100~350rpm,搅拌时间为10min,静置时间为30min。
在某些实施方式中,按重量份数计:在所述步骤S1中,四氧化三铁为99~99.5份,偶联剂为0.5~1份;在所述步骤S2中,改性四氧化三铁为5~15份,聚烯烃发泡组合物为85~95份。
在某些实施方式中,在所述步骤S1中,所述偶联剂包括γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、三异硬脂酰基酞酸酯和二异硬脂酰基钛酸乙二酯中的任意一种或多种。
在某些实施方式中,在所述步骤S2中,按质量百分比计,所述聚烯烃发泡组合物由98.5~99.5%的聚烯烃和0.5~1.5%的成核剂组成。
在某些实施方式中,所述聚烯烃包括PP、PE和POE中的任意一种或多种。
上述PP采用HMSPP、共聚PP和均聚PP中的一种或多种。
在某些实施方式中,所述成核剂包括碳酸钙、氧化钙、云母、滑石粉、纳米粘土和高岭土中的任意一种或多种。
在某些实施方式中,在所述步骤S3中,所述单螺杆挤出机的挤出工艺为:挤出机的前半区温度为190~220℃,后半区温度为140~190℃,挤出机转速为9~55rpm。
在某些实施方式中,在所述步骤S3中,所述注气***的气体流量控制在3~15L/min。
在某些实施方式中,在所述步骤S3中,所述超临界气体为超临界二氧化碳或者超临界氮气。
本发明上述四氧化三铁的粒径小于300nm,聚烯烃的熔融指数为0.5~6g/10min,成核剂的粒径不超过0.01mm。
本发明还提供了采用上述方法制备的磁性吸油聚烯烃泡沫材料,所述磁性吸油聚烯烃泡沫材料的开孔率大于95%,堆密度为0.03~0.08g/cm3,粒子粒径为3mm。
与现有吸油材料相比,本发明提供的磁性吸油聚烯烃泡沫材料及其制备方法具有以下有益效果:
(1)本发明提供的磁性吸油聚烯烃泡沫材料具有良好的亲油疏水性和优异的回弹性能,可多次重复使用,吸油率高,保油性能优异。本发明的聚烯烃泡沫材料铺覆在动态水面上,能快速吸附油水混合物中的油类物质,并且在外加磁场的作用下,不容易扩散,方便进行有效的定位收集,并且回收的吸油泡沫材料通过离心可对油品进行回收重复利用。
(2)本发明采用纳米级别的四氧化三铁,因其具有较高的比表面积且有较强的聚集倾向,故通过偶联剂与四氧化三铁表面的羟基之间发生偶联反应,对其进行表面改性,降低四氧化三铁纳米颗粒的表面能,减小颗粒之间的相互作用,避免其出现团聚,还可以增强四氧化三铁与聚合物之间的界面作用,改善四氧化三铁在聚合物中的分散效果。然后再将表面改性后的四氧化三铁与聚烯烃发泡组合物共混进行超临界气体发泡,能够显著提高四氧化三铁与聚烯烃泡沫之间的结合强度,保证磁性吸油聚烯烃泡沫材料具有良好的磁性以及疏水稳定性。
(3)本发明在吸油泡沫的制备过程中,在挤出机的压缩段注入超临界气体对环境无污染,并且可以显著提高聚烯烃泡沫材料中微孔发泡的成核数量,降低泡孔尺寸,有助于提高吸油泡沫成品的吸油率和保油性能。
具体实施方式
以下结合具体实施方式对本发明作进一步详细说明,应当理解,以下所述的实施例,仅是本发明的较佳实施例,显示和描述了本发明的基本原理、主要特征以及有益效果,仅用于说明和解释本发明,并非用于限定本发明。
实施例1
本实施例提供的磁性吸油聚烯烃泡沫材料的制备方法,具体步骤如下:
S1,将经干燥处理的99份四氧化三铁(粒径为200nm)置于共混机中,加入1份偶联剂KH-550(γ-氨丙基三乙氧基硅烷),在常温下以350rpm的搅拌速度混合搅拌10min,然后静置30min,制得改性四氧化三铁;
S2,取5份上述改性四氧化三铁与95份聚烯烃发泡组合物在共混机中共混均匀,得到磁性聚烯烃发泡组合物,其中聚烯烃发泡组合物由99份均聚PP(熔融指数为1g/10min)和1份成核剂滑石粉(粒径为10μm)组成;
S3,将上述磁性聚烯烃发泡组合物加入单螺杆挤出机的料仓中,设定挤出机的前半区温度为200℃,后半区温度为150℃,挤出机转速为35rpm,进行挤出,同时在挤出机的压缩段通过注气***加入超临界二氧化碳气体,气体流量控制在5L/min,经过挤出机的模头挤出发泡并冷却切粒,即得磁性吸油聚烯烃泡沫材料。
实施例2
本实施例提供的磁性吸油聚烯烃泡沫材料的制备方法,具体步骤如下:
S1,将经干燥处理的99.5份四氧化三铁(粒径为30nm)置于共混机中,加入0.5份偶联剂KH-560(γ-(2,3-环氧丙氧)丙基三甲氧基硅烷),在常温下以100rpm的搅拌速度混合搅拌10min,然后静置30min,制得改性四氧化三铁;
S2,取15份上述改性四氧化三铁与85份聚烯烃发泡组合物在共混机中共混均匀,得到磁性聚烯烃发泡组合物,其中聚烯烃发泡组合物由75份均聚PP(熔融指数为3g/10min)、24份HMSPP(熔融指数为3g/10min)和1份成核剂纳米粘土(粒径为8μm)组成;
S3,将上述磁性聚烯烃发泡组合物加入单螺杆挤出机的料仓中,设定挤出机的前半区温度为220℃,后半区温度为150℃,挤出机转速为45rpm,进行挤出,同时在挤出机的压缩段通过注气***加入超临界二氧化碳气体,气体流量控制在8L/min,经过挤出机的模头挤出发泡并冷却切粒,即得磁性吸油聚烯烃泡沫材料。
实施例3
本实施例提供的磁性吸油聚烯烃泡沫材料的制备方法,具体步骤如下:
S1,将经干燥处理的99份四氧化三铁(粒径为100nm)置于共混机中,加入1份偶联剂KR-210(二异硬脂酰基钛酸乙二酯),在常温下以220rpm的搅拌速度混合搅拌10min,然后静置30min,制得改性四氧化三铁;
S2,取10份上述改性四氧化三铁与90份聚烯烃发泡组合物在共混机中共混均匀,得到磁性聚烯烃发泡组合物,其中聚烯烃发泡组合物由70份均聚PP(熔融指数为5g/10min)、29.5份POE(熔融指数为3g/10min)和0.5份成核剂碳酸钙(粒径为5μm)组成;
S3,将上述磁性聚烯烃发泡组合物加入单螺杆挤出机的料仓中,设定挤出机的前半区温度为200℃,后半区温度为150℃,挤出机转速为35rpm,进行挤出,同时在挤出机的压缩段通过注气***加入超临界二氧化碳气体,气体流量控制在15L/min,经过挤出机的模头挤出发泡并冷却切粒,即得磁性吸油聚烯烃泡沫材料。
对比例
将99份均聚PP(熔融指数为3.6g/10min)和1份成核剂滑石粉(粒径为10μm)加入混合机中混合均匀;然后加入单螺杆挤出机的料仓中,设定挤出机的前半区温度为200℃,后半区温度为150℃,挤出机转速为35rpm,进行挤出,同时在挤出机的压缩段通过注气***加入超临界二氧化碳气体,气体流量控制在5L/min,经过挤出机的模头发泡并冷却切粒,得到聚烯烃泡沫材料。
将本发明实施例1~3和对比例中制备的聚烯烃泡沫材料,饱和吸附柴油之后,放入挤压设备进行脱油,再重复上述吸油和脱油的操作,测试材料在重复使用5次后的吸油率;根据标准ISO 4590-2016进行开孔率测试;根据标准GB/T6343-2009测试样品的堆密度;通过接触角测定仪测试样品的接触角。
表1实施例1~3和对比例中的聚烯烃泡沫材料的性能测试结果
本发明的制备方法工艺简单,制造成本低,可工业化生产,所制备的磁性吸油聚烯烃泡沫材料与常规的聚烯烃泡沫材料相比,具有良好的疏水亲油性能和磁性,在磁场作用下可移动便于回收,可多次重复使用并保持较高的吸油率。
以上所述仅为本发明的优选实施例,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,包括以下步骤:
S1,将经干燥处理的四氧化三铁置于共混机中,加入偶联剂,在常温下搅拌混合均匀后静置,制得改性四氧化三铁;
S2,将所述改性四氧化三铁与聚烯烃发泡组合物在共混机中共混均匀,得到磁性聚烯烃发泡组合物;
S3,将所述磁性聚烯烃发泡组合物加入单螺杆挤出机的料仓中进行挤出,同时在挤出机的压缩段通过注气***加入超临界气体,经过挤出机的模头挤出发泡,然后冷却切粒,即得所述磁性吸油聚烯烃泡沫材料。
2.根据权利要求1所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,按重量份数计:在所述步骤S1中,四氧化三铁为99~99.5份,偶联剂为0.5~1份;在所述步骤S2中,改性四氧化三铁为5~15份,聚烯烃发泡组合物为85~95份。
3.根据权利要求1或2所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,在所述步骤S1中,所述偶联剂包括γ-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、三异硬脂酰基酞酸酯和二异硬脂酰基钛酸乙二酯中的任意一种或多种。
4.根据权利要求1所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,在所述步骤S2中,按质量百分比计,所述聚烯烃发泡组合物由98.5~99.5%的聚烯烃和0.5~1.5%的成核剂组成。
5.根据权利要求4所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,所述聚烯烃包括PP、PE和POE中的任意一种或多种。
6.根据权利要求4所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,所述成核剂包括碳酸钙、氧化钙、云母、滑石粉、纳米粘土和高岭土中的任意一种或多种。
7.根据权利要求1所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,在所述步骤S3中,所述单螺杆挤出机的挤出工艺为:挤出机的前半区温度为190~220℃,后半区温度为140~190℃,挤出机转速为9~55rpm。
8.根据权利要求1所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,在所述步骤S3中,所述注气***的气体流量控制在3~15L/min。
9.根据权利要求1所述的一种磁性吸油聚烯烃泡沫材料的制备方法,其特征在于,在所述步骤S3中,所述超临界气体为超临界二氧化碳或者超临界氮气。
10.一种采用权利要求1~9任意一项所述的方法制备的磁性吸油聚烯烃泡沫材料,其特征在于,所述磁性吸油聚烯烃泡沫材料的开孔率大于95%,堆密度为0.03~0.08g/cm3,粒子粒径为3~5mm。
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