CN115110204B - 一种聚乳酸复合熔喷过滤材料及其制备方法 - Google Patents
一种聚乳酸复合熔喷过滤材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及熔喷过滤材料技术领域,具体涉及一种聚乳酸复合熔喷过滤材料及其制备方法,包括原料为聚乳酸80~100份、马来酸酐8~10份、过氧化二异丙苯1~2份、聚已内酯20~40份、聚已内酯二醇3~8份、纤维素纳米晶8~15份、驻极体2~5份、无水乙醇10~20份;使用马来酸酐接枝的聚乳酸,与聚乳酸、聚已内酯、聚已内酯二醇、纤维素纳米晶和驻极体熔融共混,后输送到计量泵、熔融模头,在高速热气流的牵引下落入接收网中,冷却后经卷绕得到的聚乳酸复合熔喷过滤材料,制得的聚乳酸复合熔喷过滤材料具有较大的断裂强力和断裂伸长率,增强了机械强度和韧性,增强过滤性能,可再生可生物降解,有利于节约资源和保护环境。
Description
技术领域
本发明涉及熔喷过滤材料技术领域,具体涉及一种聚乳酸复合熔喷过滤材料及其制备方法。
背景技术
熔喷是一种产业化制备亚微米/微米、甚至纳米超细纤维技术,其流程短、生产效率高、污染少,熔喷非织造材料轻质、蓬松、多孔、孔隙率高,这些特性赋予其在过滤、清洁、吸油、保暖等领域具有显著应用价值。随着新型冠状病毒等全球安全突发性事件的发生,熔喷非织造材料在在空气过滤领域再次占据重要地位,其产品市场也越来越大。
目前,超过90%的熔喷非织造布都是用聚丙烯制成的。但聚丙烯来源于石油,属于不可再生资源,并且在自然环境中无法降解,其废弃物处置造成了诸多环境问题。随着我国提出“碳达峰”“碳中和”的目标愿景,以及国内外各地区先行“禁塑”政策的细化和推进,为了保护环境和节约资源,满足人类对可降解绿色环保材料的迫切需求,必须寻找可生物降解的熔喷原料。聚乳酸(PLA)材料的原料为乳酸,可通过玉米、小麦中的淀粉发酵得到,聚乳酸在自然界中可被微生物分解,最终降解为CO2和H2O,是一种新型的生态环保材料,具有可生物降解性和环境友好性。用聚乳酸制备熔喷非织造材料,用于空气过滤领域,可在一定程度上缓解能源匮乏与环境污染等问题。
然而,PLA熔喷材料及技术的大规模工业化进程较缓,单一PLA熔喷材料在应用方面仍存在诸多局限性,因其本身存在韧性、耐热性差等缺点,需要探索工业化PLA熔喷材料及技术。
发明内容
本发明的目的在于提供一种聚乳酸复合熔喷过滤材料及其制备方法,制得的聚乳酸复合熔喷过滤材料具有较大的断裂强力和断裂伸长率,增强了机械强度和韧性,增强过滤性能,可再生可生物降解,有利于节约资源和保护环境。
为了达到上述目的,本发明提供如下技术方案:
一种聚乳酸复合熔喷过滤材料,包括以下质量份数的原料:聚乳酸80~100份,马来酸酐8~10份,过氧化二异丙苯1~2份,聚已内酯20~40份,聚已内酯二醇3~8份,纤维素纳米晶8~15份,驻极体2~5份,无水乙醇10~20份;
聚乳酸复合熔喷过滤材料的制备方法,包括以下步骤:
步骤一:取质量份数的过氧化二异丙苯和无水乙醇,搅拌溶解,得到过氧化二异丙苯溶液;
步骤二:取质量份数的聚乳酸,破碎过80~200目筛,加入过氧化二异丙苯溶液,室温下磁力搅拌2~3h,然后加入质量份数的马来酸酐,继续磁力搅拌2~3h,后使用双螺杆挤出机,熔融挤出,得到马来酸酐接枝聚乳酸;
步骤三:取质量份数的聚已内酯、聚已内酯二醇和纤维素纳米晶放置于45~55℃的烘箱中干燥24h,取步骤一得到的马来酸酐接枝聚乳酸放置于50~60℃的烘箱中干燥12h,取质量份数的驻极体放置于80~105℃的烘箱中干燥8~12h,将干燥后的聚已内酯、聚已内酯二醇、纤维素纳米晶、马来酸酐接枝聚乳酸和驻极体混合均匀,加入到密炼机中,设置温度为180~200℃,熔融共混8~10min,得到熔融混合物;
步骤四:将步骤三中得到的熔融混合物输送到计量泵中,后输送到熔融模头中,熔融模头两侧通入高速热气流,对熔融混合物牵引后落入接收网中,后在室温环境开放场中冷却,最后经卷绕得到的聚乳酸复合熔喷过滤材料。
进一步优选,驻极体为纳米二氧化硅、多壁碳纳米管、纳米二氧化钛、纳米四氧化三铁中的一种或多种。
进一步优选,制备方法步骤四中,计量泵的温度设置为200~210℃,调节计量泵的计量速度能与输送过来的熔融混合物输送速度相匹配,使熔融模头处的熔融混合物均匀挤出,且熔融模头中一个单孔的挤出速度为10~13mL/h。
进一步优选,制备方法步骤四中熔融模头的温度为210~240℃,熔融模头两侧通入的高速热气流为,热气流温度为220~280℃,气流速度为250~350m/s。
进一步优选,制备方法步骤四中熔融模头与接收网的距离为9~10cm。
进一步优选,制备方法步骤二中,使用双螺杆挤出机设置温度为170~190℃,螺杆转速为40~50r/min。
步骤二中的反应有:
;
步骤三涉及到的反应有:
本发明的有益效果:
1、使用马来酸酐接枝的聚乳酸,与聚乳酸、聚已内酯、聚已内酯二醇、纤维素纳米晶和驻极体熔融共混,形成熔融混合物,后输送到计量泵、熔融模头,在高速热气流的牵引下落入接收网中,冷却后经卷绕得到的聚乳酸复合熔喷过滤材料,改善了单一聚乳酸熔喷材料强度、韧性、耐热性差的缺点,发展了一种可以代替PP熔喷材料的新材料,可再生可生物降解,有利于节约资源和保护环境。
2、聚已内酯、聚已内酯二醇作为本发明的增韧剂,与聚乳酸熔融共混,有利于增强聚乳酸的韧性,且聚已内酯、聚乳酸分子分别与纤维素纳米晶氢键键合、纤维素纳米晶将聚已内酯和聚乳酸分子连接到一起,聚已内酯二醇与接枝在聚乳酸分子链上的马来酸酐通过开环键合,马来酸酐接枝的聚乳酸能够与聚乳酸聚合,增加了聚乳酸分子链的长度和侧链的复杂性,使得整个分子中不同组成部分呈现互相交联的状态,从分子结构增加了聚乳酸材料的强度和韧性,相互交联的分子结构,使得聚乳酸分子不易间滑移,强度和耐热性得到了提升。
3、过氧化二异丙苯为强氧化剂,能够使得聚乳酸产生活性位点,聚乳酸分子链上的活性位点与马来酸酐结合,有利于形成马来酸酐接枝聚乳酸,马来酸酐接枝聚乳酸在聚乳酸、聚已内酯和驻极体熔融共混体系中充当增容剂,有利于改善熔融共混体系中各物质间的相容性,实现增容改性。
4、聚已内酯二醇能够与马来酸酐接枝聚乳酸发生开环聚合反应,有利于进一步增长聚乳酸的分子链长,增加聚乳酸的分子侧链长度,且聚已内酯的熔融共聚,改善了单一聚乳酸的韧性差、耐热性差的缺点。
5、驻极体为纳米二氧化硅、多壁碳纳米管、纳米二氧化钛、纳米四氧化三铁中的一种或几种,纳米级的驻极体,一方面在材料中充当润滑剂,起到润滑的作用,同时能够起到骨架支撑作用,有利于增强聚乳酸复合熔喷过滤材料的机械强度,另一方面,所选驻极体为多孔材料,能够通过静电作用或者孔道吸附作用,增强聚乳酸复合熔喷过滤材料的过滤性能。
具体实施方式
下面将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,本领域普通技术人员在没有作出创造性劳动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
一种聚乳酸复合熔喷过滤材料,包括以下质量份数的原料:聚乳酸90份,马来酸酐9份,过氧化二异丙苯1.5份,聚已内酯30份,聚已内酯二醇5份,纤维素纳米晶10份,驻极体3份,无水乙醇15份;
聚乳酸复合熔喷过滤材料的制备方法,包括以下步骤:
步骤一:取质量份数的过氧化二异丙苯和无水乙醇,搅拌溶解,得到过氧化二异丙苯溶液;
步骤二:取质量份数的聚乳酸,破碎过120目筛,加入过氧化二异丙苯溶液,室温下磁力搅拌2h,然后加入质量份数的马来酸酐,继续磁力搅拌3h,后使用双螺杆挤出机,熔融挤出,得到马来酸酐接枝聚乳酸;
步骤三:取质量份数的聚已内酯、聚已内酯二醇和纤维素纳米晶放置于50℃的烘箱中干燥24h,取步骤一得到的马来酸酐接枝聚乳酸放置于55℃的烘箱中干燥12h,取质量份数的驻极体放置于90℃的烘箱中干燥10h,将干燥后的聚已内酯、聚已内酯二醇、纤维素纳米晶、马来酸酐接枝聚乳酸和驻极体混合均匀,加入到密炼机中,设置温度为190℃,熔融共混9min,得到熔融混合物;
步骤四:将步骤三中得到的熔融混合物输送到计量泵中,后输送到熔融模头中,熔融模头两侧通入高速热气流,对熔融混合物牵引后落入接收网中,后在室温环境开放场中冷却,最后经卷绕得到的聚乳酸复合熔喷过滤材料。
实施例2
一种聚乳酸复合熔喷过滤材料,包括以下质量份数的原料:聚乳酸100份,马来酸酐10份,过氧化二异丙苯2份,聚已内酯40份,聚已内酯二醇8份,纤维素纳米晶15份,驻极体5份,无水乙醇20份;
聚乳酸复合熔喷过滤材料的制备方法,包括以下步骤:
步骤一:取质量份数的过氧化二异丙苯和无水乙醇,搅拌溶解,得到过氧化二异丙苯溶液;
步骤二:取质量份数的聚乳酸,破碎过200目筛,加入过氧化二异丙苯溶液,室温下磁力搅拌3h,然后加入质量份数的马来酸酐,继续磁力搅拌3h,后使用双螺杆挤出机,熔融挤出,得到马来酸酐接枝聚乳酸;
步骤三:取质量份数的聚已内酯、聚已内酯二醇和纤维素纳米晶放置于55℃的烘箱中干燥24h,取步骤一得到的马来酸酐接枝聚乳酸放置于60℃的烘箱中干燥12h,取质量份数的驻极体放置于105℃的烘箱中干燥12h,将干燥后的聚已内酯、聚已内酯二醇、纤维素纳米晶、马来酸酐接枝聚乳酸和驻极体混合均匀,加入到密炼机中,设置温度为200℃,熔融共混10min,得到熔融混合物;
步骤四:将步骤三中得到的熔融混合物输送到计量泵中,后输送到熔融模头中,熔融模头两侧通入高速热气流,对熔融混合物牵引后落入接收网中,后在室温环境开放场中冷却,最后经卷绕得到的聚乳酸复合熔喷过滤材料。
实施例3
一种聚乳酸复合熔喷过滤材料,包括以下质量份数的原料:聚乳酸80份,马来酸酐8份,过氧化二异丙苯1份,聚已内酯20份,聚已内酯二醇3份,纤维素纳米晶8份,驻极体2份,无水乙醇10份;
聚乳酸复合熔喷过滤材料的制备方法,包括以下步骤:
步骤一:取质量份数的过氧化二异丙苯和无水乙醇,搅拌溶解,得到过氧化二异丙苯溶液;
步骤二:取质量份数的聚乳酸,破碎过80目筛,加入过氧化二异丙苯溶液,室温下磁力搅拌2h,然后加入质量份数的马来酸酐,继续磁力搅拌2h,后使用双螺杆挤出机,熔融挤出,得到马来酸酐接枝聚乳酸;
步骤三:取质量份数的聚已内酯、聚已内酯二醇和纤维素纳米晶放置于45℃的烘箱中干燥24h,取步骤一得到的马来酸酐接枝聚乳酸放置于50℃的烘箱中干燥12h,取质量份数的驻极体放置于80℃的烘箱中干燥8h,将干燥后的聚已内酯、聚已内酯二醇、纤维素纳米晶、马来酸酐接枝聚乳酸和驻极体混合均匀,加入到密炼机中,设置温度为180℃,熔融共混8min,得到熔融混合物;
步骤四:将步骤三中得到的熔融混合物输送到计量泵中,后输送到熔融模头中,熔融模头两侧通入高速热气流,对熔融混合物牵引后落入接收网中,后在室温环境开放场中冷却,最后经卷绕得到的聚乳酸复合熔喷过滤材料。
对比例1为单一成分聚乳酸熔喷过滤材料;
对比例2为未加驻极体的聚乳酸复合熔喷过滤材料,其余条件与实施例1相同;
使用万能拉力机进行力学性质测试,试样尺寸为80mm×10mm×2mm,过滤效果以过滤截留粒径0.25微米颗粒的百分比表示,试样厚度为2mm,得到的结果如表所示;
由上表所示,本发明方法所制备的聚乳酸复合熔喷过滤材料具有较大的断裂强力、较大的断裂伸长率,过滤百分比高,强度高、韧性好。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应所述以权利要求的保护范围为准。
Claims (6)
1.一种聚乳酸复合熔喷过滤材料,其特征在于,包括以下质量份数的原料:聚乳酸80~100份,马来酸酐8~10份,过氧化二异丙苯1~2份,聚已内酯20~40份,聚已内酯二醇3~8份,纤维素纳米晶8~15份,驻极体2~5份,无水乙醇10~20份;
所述聚乳酸复合熔喷过滤材料的制备方法,包括以下步骤:
步骤一:取质量份数的过氧化二异丙苯和无水乙醇,搅拌溶解,得到过氧化二异丙苯溶液;
步骤二:取质量份数的聚乳酸,破碎过80~200目筛,加入过氧化二异丙苯溶液,室温下磁力搅拌2~3h,然后加入质量份数的马来酸酐,继续磁力搅拌2~3h,后使用双螺杆挤出机,熔融挤出,得到马来酸酐接枝聚乳酸;
步骤三:取质量份数的聚已内酯、聚已内酯二醇和纤维素纳米晶放置于45~55℃的烘箱中干燥24h,取步骤一得到的马来酸酐接枝聚乳酸放置于50~60℃的烘箱中干燥12h,取质量份数的驻极体放置于80~105℃的烘箱中干燥8~12h,将干燥后的聚已内酯、聚已内酯二醇、纤维素纳米晶、马来酸酐接枝聚乳酸和驻极体混合均匀,加入到密炼机中,设置温度为180~200℃,熔融共混8~10min,得到熔融混合物;
步骤四:将步骤三中得到的熔融混合物输送到计量泵中,后输送到熔融模头中,熔融模头两侧通入高速热气流,对熔融混合物牵引后落入接收网中,后在室温环境开放场中冷却,最后经卷绕得到的聚乳酸复合熔喷过滤材料。
2.根据权利要求1所述的一种聚乳酸复合熔喷过滤材料,其特征在于,所述驻极体为纳米二氧化硅、多壁碳纳米管、纳米二氧化钛、纳米四氧化三铁中的一种或多种。
3.根据权利要求1所述的一种聚乳酸复合熔喷过滤材料,其特征在于:所述步骤四中,计量泵的温度设置为200~210℃,调节计量泵的计量速度能与输送过来的熔融混合物输送速度相匹配,使熔融模头处的熔融混合物均匀挤出,且单个熔融模头挤出速度为10~13mL/h。
4.根据权利要求1所述的一种聚乳酸复合熔喷过滤材料,其特征在于:所述步骤四中熔融模头的温度为210~240℃,熔融模头两侧通入的高速热气流为,热气流温度为220~280℃,气流速度为250~350m/s。
5.根据权利要求1所述的一种聚乳酸复合熔喷过滤材料,其特征在于:所述步骤四中熔融模头与接收网的距离为9~10cm。
6.根据权利要求1所述的一种聚乳酸复合熔喷过滤材料,其特征在于:所述步骤二中,使用双螺杆挤出机设置温度为170~190℃,螺杆转速为40~50r/min。
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Effective date of registration: 20240108 Address after: 712000 No.3, zhizhisan Road, Xinxing Textile Industrial Park, Xingping City, Xianyang City, Shaanxi Province Applicant after: Xinggu Technology (Shaanxi) Co.,Ltd. Address before: Room D240, 2nd Floor, Z1-Z4 Floor, No. 1953, Qianshan Mingzhu South Road, Xiangzhou District, Zhuhai City, Guangdong Province, 519000 Applicant before: Zhao Meiyi |
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