CN106867089A - 一种透气性复合薄膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种透气性复合薄膜及其制备方法,该复合薄膜由如下重量百分比的组分制备而成:60%‑82%的聚烯烃树脂聚合物、2%‑8%微纳米晶纤维素粒子、0.4%‑1%抗氧剂、15%‑30%分散剂、0.1%‑0.5%润滑剂、0.2%‑1%偶联剂。其制备方法如下:将微纳米晶纤维素水分散液和偶联剂分散均匀;再加入分散剂混合均匀,并干燥得预处理填料;将所得到的预处理填料、聚烯烃树脂、抗氧剂、润滑剂添加到双螺杆挤出机中,经过熔融挤出、冷却和造粒得透气性复合薄膜组成物,热压延制备平整薄膜;再浸入清洗剂中,超声、干燥;双向拉伸并进行热定型处理,得透气性复合薄膜。该复合薄膜透气性能高效、机械性能优良。
Description
技术领域
本发明涉及复合薄膜领域,具体涉及一种透气性复合薄膜及其制备方法。
背景技术
纤维素是一种自然界中蕴藏最丰富的天然可再生高分子化合物,以纤维素为原料的产品广泛应用于燃料乙醇、造纸、渗透膜、塑料、电子产品、医药工程、电工及工业加工等领域,具有环保可降解、热稳定性好、化学稳定性高、介电常数高等优良特性。近几年,大批科研人员致力于将纤维素改性和增强用以制备高性能的薄膜材料,主要用于过滤、渗透膜和锂电池隔膜材料。传统透气膜是一种填充一定份数无机粒子填料的聚合物薄膜,在拉伸情况下无机填料周围形成尺寸可控的孔洞,可允许水蒸气和空气等气体的通过,同时不允许液体通过,主要用于生产婴儿纸尿裤、女性卫生巾、户外运动服饰等制成品。工业生产上主要是将透气膜的组合物在一定温度下通过挤出、造粒、流延或吹塑后再进行拉伸,此时只有聚合物基体树脂可以被拉伸,而添加的无机粒子填料无法被拉伸,从而在无机粒子填料周围产生了仅供水蒸气或空气等气体可通过的细微孔洞。
中国专利201110203184.8公开了一种低透气量透气膜的组合物及其制备方法,其组分包括:聚烯烃树脂混合物、透气量调节剂、表面改性的微米级无机粒子、抗氧剂、润滑剂和偶联剂。其优点在于纳微米无机填料能够提高透气膜的力学性能,同时表面偶联改性的无机粒子增加了与聚烯烃基体树脂的相容性,但不足之处在于高添加量(30%-55%)的微米无机粒子不能够很好地均匀分散在基体树脂中,从而影响了薄膜材料的透气均匀性。
中国专利201110125458.6公开了一种聚烯烃薄膜及其制备方法,其组分包括:聚烯烃树脂、成孔剂和萃取剂。其优点在于所采用传统湿法制备的聚丙烯烃薄膜的结构小、数量多,但其采用两步高体积百分比浓度的萃取过程,其萃取溶剂为N,N’-二甲基甲酰胺、二氯甲烷、三氯甲烷等属于高污染、有毒溶剂,可对人体和环境造成巨大伤害。
发明内容
本发明的目的在于提供一种透气性复合薄膜及其制备方法,以制备一种透气性能高效、机械性能优良的复合薄膜。
本发明的目的通过以下技术方案实现。
一种透气性复合薄膜,该透气性复合薄膜由以下重量百分比的组分制备而成:
优选的,所述聚烯烃树脂混合物为线性低密度聚乙烯(LLDPE)、低密度聚乙烯(LDPE)、中密度聚乙烯(MDPE)、高密度聚乙烯(HDPE)、均聚聚丙烯(HPP)、乙烯-丙烯共聚物(EPM)、乙烯-丁烯共聚物(ENR)、乙烯-辛烯共聚物(POE)、乙烯-丙烯酸酯-甲基丙烯酸缩水甘油酯(GMA)和乙烯-丙烯-非共轭二烯(EPDM)中的单种或多种的共混物。
优选的,所选微纳米晶纤维素粒子的粒径尺寸分布在50nm-50μm;所述微纳米晶纤维素优选于麻、麦秆、稻草、蔗渣、棉花和植物种皮中的一种以上。
优选的,所述分散剂为不同聚合程度的聚乙二醇:进一步优选为PEG-200,PEG-400,PEG-600,PEG-1000,PEG-2000,PEG-4000和PEG-6000中的一种以上,主要用于包覆微纳米晶纤维素粒子,阻止其发生团聚,经浸洗过程除去后可形成更多均匀分散透气孔道。
优选的,所述润滑剂为高级脂肪酸脂类、金属皂类、脂肪酰胺类和石蜡中的一种以上。进一步优选为硬脂酸、硬脂酸锌、硬脂酸钙、油酸酰胺、低分子PE蜡、低分子PP蜡、OPE(氧化聚乙烯)蜡、天然石蜡、液体石蜡等。所选用润滑剂可降低物料与加工机械及物料分子之间的相互摩擦,从而改善了复合物的加工性能以及提高复合材料的热稳定性能。
优选的,所述微纳米晶纤维素经偶联剂处理,所用偶联剂为含有氨基、巯基、环氧基、酰氧基和乙烯基中的一种以上基团的硅烷偶联剂;进一步优选为γ-氨丙基三甲氧基硅烷(KH590)、γ-氨丙基三乙氧基硅烷(KH550)、γ-(2,3-环氧丙氧)丙基二甲氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、γ-巯丙基三乙氧基硅烷(KH580)、γ-巯丙基三甲氧基硅烷、乙烯基三甲氧基硅烷和乙烯基三乙氧基硅烷中的一种以上。
优选的,所述抗氧剂为酚类、芳香胺类、受阻酚类、亚磷酸脂类和硫代二丙酸双酯中的一种以上;进一步优选为抗氧剂1010、1076、164、264、CA、DNP、DLTP、TNP、BHT。抗氧剂在聚合物加工和应用体系中少量存在时,可延缓或抑制聚合物氧化过程,从而避免色泽变化并延长使用寿命。
以上所述的一种透气性复合薄膜的制备方法,包括如下步骤:
(1)将微纳米晶纤维素粒子水分散液和偶联剂分散均匀,得预分散液;
(2)将预分散液和分散剂混合均匀,并在烘箱中干燥获得预处理填料;
(3)将所得到的预处理填料、聚烯烃树脂混合物、抗氧剂、润滑剂通过喂料***添加到双螺杆挤出机中,经过熔融挤出、冷却和造粒制得透气性复合薄膜组成物粒料;
(4)将透气性复合薄膜组成物粒料分别在170-190℃的温度以及20t-40t的压力下进行热压延或挤出制备出平整的复合薄膜;
(5)将平整的复合薄膜浸入清洗剂中,经超声除去分散剂并干燥处理;
(6)将步骤(5)所得干燥复合薄膜进行双向拉伸,拉伸倍率为0.5-1.5,在80-120℃条件下进行热定型处理,使薄膜中的基材分子链充分取向,热定型处理时间为5-15min,制得具有微纳米孔的透气性复合薄膜。
优选的,所述双螺杆挤出机为同向旋转双螺杆挤出机,长径比L/D为40-50,螺杆转速≥80rpm,挤出温度设定180-220℃。
优选的,步骤(5)所述超声的频率为40-200kHz;所述清洗剂为水、乙醇、异丙醇和丙酮中的一种以上。
通过透气性复合薄膜的透水率实测,可以分析出微纳米晶纤维素的含量影响着复合膜材料的力学性能,另外,分散剂的种类及用量在很大程度上决定了复合膜材料的透水率。
与现有技术相比,本发明具有如下优点:
(1)本发明在聚烯烃树脂中添加刚性棒状有机粒子微纳米晶纤维素能够提高复合薄膜的亲水性、热稳定性以及力学性能;
(2)本发明对微纳米晶纤维素表面进行偶联处理,可以提高其与基体树脂的界面兼容性;
(3)本发明中分散剂聚乙二醇的加入可以有效阻止微纳米晶纤维素粒子发生团聚现象;
(4)本发明复合薄膜后处理过程中所用清洗剂环保、安全,可回收重复利用;
(5)本发明在将复合薄膜进行拉伸取向之前进行浸泡处理,除去分散剂,所得到复合薄膜成品的孔道尺寸更小、数量更多,此外易于控制孔道的形状;
(6)本发明具有膜孔呈现微纳米级非直线孔道结构的特点。
附图说明
图1是本发明透气性复合薄膜的表面扫描电镜图。
图2是本发明透气性复合薄膜的断面扫描电镜图。
具体实施方式
以下结合实例与附图对本发明的实施方式作进一步的具体说明,但本发明的实施方式不限于此。
实施例1
(1)将3.2kg浓度为25g/L的微纳米晶大豆种皮纤维素水分散液(粒径为50nm-2μm)和6g硅烷偶联剂KH580在高速分散机(1000rpm)中分散均匀,再加入300g分散剂聚乙二醇PEG-200在高速混合机(1000rpm)中混合均匀,并将其混合物在烘箱中干燥获得预处理填料;
(2)将500g线性低密度聚乙烯(LLDPE)、100g乙烯-丙烯酸酯-甲基丙烯酸缩水甘油酯(GMA)、预处理填料、4g酚类264和亚磷酸酯类BHT抗氧剂、10g润滑剂硬脂酸钙通过高速混合机(1000rpm)进行预混,得预混物料;
(3)通过计量喂料器将预混物料加入到挤出机进料口,经同向旋转双螺杆挤出机熔融挤出、冷却造粒即为透气性复合薄膜组成物成品。上述加工过程所用双螺杆挤出机长径比为50,螺杆转速90rpm,挤出温度设定为:加料口180℃,熔融段210℃,机头口模180℃;
(4)将复合薄膜组成物粒料在170℃温度和25t压力下进行热压延制备平整薄膜;
(5)将复合薄膜浸入去离子水中,经超声(200kHz)除去分散剂并干燥处理;
(6)将干燥复合薄膜进行双向拉伸,拉伸倍率为0.5,并在80℃条件下进行热定型处理,热定型时间为5min,最终制备出膜厚为60-150μm的透气膜成品,依照上述配方和制备过程,所得到的透气性复合薄膜的透气率达到2460-6530g/(m2·24h)。
本实施例所制备的透气性复合薄膜的表面和断面的扫描电镜图分别如图1和图2所示,透气孔道以非直线型空间网络状结构分布,孔隙多、广且均匀,孔径大小为100nm-10μm,孔隙率达到50%。
实施例2
(1)将2.5kg浓度为20g/L的微晶棉花纤维素水分散液(粒径为500nm-10μm)和10g硅烷偶联剂KH550在高速分散机(1000rpm)中分散均匀,再加入分散剂225g聚乙二醇PEG-400在高速混合机(1000rpm)中混合,并将其混合物在烘箱中干燥获得预处理填料;
(2)将600g低密度聚乙烯(LDPE)、100g乙烯-丙烯共聚物(EPM)、预处理填料、4g受阻酚类抗氧剂1010,10g润滑剂硬脂酸锌通过高速混合机(1200rpm)进行预混,得预混物料;
(3)通过计量喂料器将预混物料加入到挤出机进料口,经同向旋转双螺杆挤出机熔融挤出、冷却造粒即为透气性复合薄膜组成物粒料。上述加工过程所用双螺杆挤出机长径比为40,螺杆转速80rpm,挤出温度设定为:加料口180℃,熔融段205℃,机头口模180℃;
(4)将复合薄膜组成物粒料在180℃温度和40t压力下进行挤出制备平整复合薄膜;
(5)将复合薄膜浸入乙醇中,经超声(100kHz)除去分散剂并干燥处理;
(6)将干燥复合薄膜进行双向拉伸,拉伸倍率为1.5,并在100℃条件下进行热定型处理,热定型时间为15min,最终制备出膜厚为60-150μm的透气膜成品,依照上述配方和制备过程,所得到的透气性复合薄膜的透气率达到2710-4890g/(m2·24h)。
实施例3
(1)将0.5kg浓度为40g/L的微晶麻纤维素水分散液(粒径为2μm-50μm)和2g硅烷偶联剂KH590在高速分散机(1000rpm)中分散均匀,再加入分散剂150g聚乙二醇PEG1000在高速混合机(1000rpm)中混合均匀,并将其混合物在烘箱中干燥获得预处理填料;
(2)将700g高密度聚乙烯(HDPE)、120g乙烯-辛烯共聚物(POE)、预处理填料、7g受阻酚类抗氧剂1076和1g润滑剂低分子PE蜡通过高速混合机(1200rpm)进行预混;
(3)通过计量喂料器将预混物料加入到挤出机进料口,经同向旋转双螺杆挤出机熔融挤出、冷却造粒即为透气性复合薄膜组成物成品。上述加工过程所用双螺杆挤出机长径比为50,螺杆转速100rpm,挤出温度设定为:加料口180℃,熔融段220℃,机头口模180℃;
(4)将复合薄膜组成物粒料在190℃温度和20t压力下进行热压延制备平整薄膜;
(5)将复合薄膜浸乙醇中,经超声(40kHz)除去分散剂并干燥处理;
(6)将干燥复合薄膜进行双向拉伸,拉伸倍率为1,并在120℃条件下进行热定型处理,热定型时间为10min,最终制备出膜厚为60-150μm的透气膜成品,依照上述配方和制备过程,所得到的透气性复合薄膜的透气率达到2710-6500g/(m2·24h)。
所制备透气性复合薄膜样品的拉伸强度依据GB13022标准测试。
所制备透气性复合薄膜的透气率(WVT)依据GB/T12704-91测定,采用正杯蒸发法将所制备的透气性复合薄膜覆盖且密封在标准透湿杯敞口面,标准透湿杯中注入一定量蒸馏水,放置在温度38℃、相对湿度2%的恒温恒湿箱内,24h内的称重变化即为透气性复合薄膜的透气率。
上述3个实施例所制备的透气性复合薄膜成品呈现以下结构特征:透气孔道为非直线型空间网络状结构分布,孔隙多、广且均匀,如图1和图2所示。
以上实施例,并非对本发明内容的组成物的用量作任何限制,凡根据本发明组成物构成、用量以及制备方法所做任何修改或等同变化,均在本发明技术性保护范围之内。
Claims (10)
1.一种透气性复合薄膜,其特征在于,该透气性复合薄膜由以下重量百分比的组分制备而成:
2.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述的聚烯烃树脂混合物为线性低密度聚乙烯、低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、均聚聚丙烯、乙烯-丙烯共聚物、乙烯-丁烯共聚物、乙烯-辛烯共聚物、乙烯-丙烯酸酯-甲基丙烯酸缩水甘油酯和乙烯-丙烯-非共轭二烯中的一种或多种的共混物。
3.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述微纳米晶纤维素粒子的粒径尺寸分布为50nm-50μm。
4.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述抗氧剂为酚类、芳香胺类、受阻酚类、亚磷酸脂类和硫代二丙酸双酯中的一种以上。
5.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述分散剂为不同聚合程度的聚乙二醇。
6.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述润滑剂为高级脂肪酸脂类、金属皂类、脂肪酰胺类和石蜡中的一种以上。
7.根据权利要求1所述的一种透气性复合薄膜,其特征在于,所述偶联剂为含有氨基、巯基、环氧基、酰氧基和乙烯基中的一种以上基团的硅烷偶联剂。
8.制备权利要求1-7任一项所述的一种透气性复合薄膜的方法,其特征在于,包括如下步骤:
(1)将微纳米晶纤维素粒子水分散液和偶联剂分散均匀,得预分散液;
(2)将预分散液和分散剂混合均匀,并在烘箱中干燥获得预处理填料;
(3)将所得到的预处理填料、聚烯烃树脂混合物、抗氧剂、润滑剂通过喂料***添加到双螺杆挤出机中,经过熔融挤出、冷却和造粒制得透气性复合薄膜组成物粒料;
(4)将透气性复合薄膜组成物粒料在170-190℃的温度以及20t-40t的压力下进行热压延或挤出制备出平整的复合薄膜;
(5)将平整的复合薄膜浸入清洗剂中,经超声除去分散剂并干燥处理;
(6)将步骤(5)所得干燥复合薄膜进行双向拉伸,拉伸倍率为0.5-1.5,在80-120℃条件下进行热定型处理,使薄膜中的基材分子链充分取向,热定型处理时间为5-15min,制得具有微纳米孔的透气性复合薄膜。
9.根据权利要求8所述的制备方法,其特征在于,步骤(3)所述的双螺杆挤出机为同向旋转双螺杆挤出机,长径比L/D为40-50,螺杆转速≥80rpm,挤出温度为180-220℃。
10.根据权利要求8所述的制备方法,其特征在于,步骤(5)所述超声的频率为40-200kHz;所述清洗剂为水、乙醇、异丙醇和丙酮中的一种以上。
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