CN109971010B - 一种淀粉复合膜材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种淀粉复合膜材料及其制备方法。该制备方法先将甲酸纳米木素和聚乙烯醇的混合物、甲酸纳米木素和聚环氧乙烯的混合物分别均匀分散于淀粉液中,然后分别在恒温恒湿环境中静置,即获得疏水性能显著改善的淀粉复合膜材料;甲酸纳米木素的质量为淀粉的1%‑3%,聚乙烯醇或聚环氧乙烯与淀粉的质量比为(1‑10)∶10。本发明先将甲酸制浆后得到的木质素制成纳米级别,然后与淀粉复合,制备出淀粉复合膜材料,经试验可显著改善其疏水性能,能实现甲酸木素高值化利用,提升淀粉复合膜应用性能,为利用甲酸纳米木素分散技术制备高疏水性淀粉/聚乙烯醇或淀粉/聚环氧乙烯复合材料提供了技术支持,具有很好的实用性。
Description
技术领域
本发明属于淀粉复合膜技术领域,具体涉及一种淀粉复合膜材料及其制备方法。
背景技术
传统石油塑料具有的持久耐用特性使其成为包装、涂料、建筑和卫生领域的理想材料。然而,化石材料不易被生物降解,其废弃物在环境中的积累对人类健康构成了严重威胁。正是这种环境保护意识的增强,使得淀粉、纤维素、蛋白质等天然原料成为取代不可再生生物降解材料的研究日益得到重视。目前,由于淀粉的低成本和全世界丰富的可获得性,在食品、造纸和纺织等领域,研究者对淀粉材料的研究产生了浓厚兴趣。其中,淀粉/聚乙烯醇或淀粉/聚氧化乙烯食品包装膜是开发具有理想性能新型高分子材料的有效途径,对开发绿色可降解生物材料具有重要价值。然而,聚乙烯醇和聚氧化乙烯含有大量的亲水性官能团,复合膜疏水性能欠缺。
化学交联是改善淀粉疏水性能的常用方式,通过乙二醛、戊二醛和碳酸镐铵化学交联可有效降低其亲水性能。但通过物理方法来改善淀粉膜的疏水性能的研究很少,技术不成熟。
发明内容
发明目的:针对现有技术中存在的问题,本发明的目的在于提供一种淀粉复合膜材料的制备方法,实现木质素的高值化利用,提升淀粉复合膜的应用性能。本发明的另一个目的是提供一种上述制备方法所获得的淀粉复合膜材料。
技术方案:为了解决上述问题,本发明所采用的技术方案如下:
一种淀粉复合膜材料的制备方法,先将甲酸纳米木素和聚乙烯醇的混合物、甲酸纳米木素和聚环氧乙烯的混合物分别均匀分散于淀粉液中,然后分别在恒温恒湿环境中静置,即可获得疏水性能显著改善的淀粉复合膜材料;其中,甲酸纳米木素的质量为淀粉质量的1%-3%,聚乙烯醇或聚环氧乙烯与淀粉的质量比为(1-10)∶10。
所述的淀粉复合膜材料的制备方法,具体包括以下步骤:
(1)取甲酸木质素,溶于四氢呋喃中,磁力搅拌使其均匀分散转移至透析袋中,使用去离子水透析,制得甲酸纳米木素;
(2)取甲酸纳米木素和聚乙烯醇的混合物、甲酸纳米木素和聚环氧乙烯的混合物,分别向两种混合物中加入淀粉液,分别置于恒温磁力搅拌器中搅拌,并超声,使纳米木素分散均匀;
(3)将步骤(2)中的体系转移至培养皿中,恒温恒湿环境中静置2天以上,制得淀粉复合膜;所述恒温的温度为25℃,恒湿的湿度为50%。
所述的淀粉复合膜材料的制备方法,甲酸纳米木素的用量为淀粉质量的1%-3%。
所述的淀粉复合膜材料的制备方法,聚乙烯醇或聚氯乙烯的质量与淀粉质量的比值为(1-10)∶10。
所述的淀粉复合膜材料的制备方法,淀粉为玉米淀粉。
所述的淀粉复合膜材料的制备方法,淀粉液中,淀粉的质量分数为1%。
所述的淀粉复合膜材料的制备方法,步骤(2)中,恒温磁力搅拌器的温度为90℃,搅拌速度为400rpm,超声时间为10min。
所述的淀粉复合膜材料的制备方法制备得到的淀粉复合膜材料。
有益效果:与现有的技术相比,本发明先将甲酸制浆后得到的木质素制成纳米级别,然后与淀粉复合,制备出淀粉复合膜材料,经试验可显著改善其疏水性能,能实现甲酸木质素的高值化利用,满足制浆清洁生产要求,并提升淀粉复合膜的应用性能,为利用甲酸纳米木素分散技术制备高疏水性的淀粉/聚乙烯醇或淀粉/聚环氧乙烯复合材料提供了技术支持,具有很好的实用性。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。
实施例1
(1)称取1g甲酸木质素,溶于200mL四氢呋喃(THF)中,磁力搅拌(300rpm)使其均匀分散转移至透析袋中(Mw=8000),使用去离子水透析3天制得甲酸纳米木素。
(2)称取相对淀粉质量1%的甲酸纳米木素,与淀粉质量比例分别为1∶10,3∶10,1∶2和1∶1的聚乙烯醇(PVA)加入烧杯中,然后倒入事先糊化好的10g1%的玉米淀粉液中,置于90℃恒温磁力搅拌器上,搅拌10min(400rpm),并超声10min,超声功率为100W,使甲酸纳米木素分散均匀。
(3)加热结束后,为消除水分蒸发造成的质量损失,重新计算(2)中的淀粉固含量,量取0.2g淀粉所对应体积的淀粉液6±1mL,转移至直径为6cm的培养皿中,25℃50%RH环境中放置3天制得淀粉复合膜。
(4)测定淀粉复合膜的初始接触角和180s时刻的接触角,结果如下表1。
实施例2
(1)称取1g甲酸木质素,溶于200mL四氢呋喃(THF)中,磁力搅拌(300rpm)使其均匀分散转移至透析袋中(Mw=8000),使用去离子水透析3天制得甲酸纳米木素。
(2)称取相对淀粉质量3%的甲酸纳米木素,与淀粉质量比例分别为1∶10,3∶10,1∶2和1∶1的聚乙烯醇(PVA)加入烧杯中,然后倒入事先糊化好的10g1%的玉米淀粉液中,置于90℃恒温磁力搅拌器上,搅拌10min(400rpm),并超声10min,超声功率为100W,使纳米木素分散均匀。
(3)加热结束后,为消除水分蒸发造成的质量损失,重新计算(2)中的淀粉固含量,量取0.2g淀粉所对应体积的淀粉液6±1mL,转移至直径为6cm的培养皿中,25℃50%RH环境中放置3天制得淀粉复合膜。
(4)测定淀粉复合膜的初始接触角和180s时刻的接触角,结果如下表1。
实施例3
(1)称取1g甲酸木质素,溶于200mL四氢呋喃(THF)中,磁力搅拌(300rpm)使其均匀分散转移至透析袋中(Mw=8000),使用去离子水透析3天制得甲酸纳米木素。
(2)称取相对淀粉质量1%的甲酸纳米木素,与淀粉质量比例分别为1∶10,3∶10,1∶2和1∶1的聚环氧乙烯(PEO)加入烧杯中,然后倒入事先糊化好的10g1%的玉米淀粉液中,置于90℃恒温磁力搅拌器上,搅拌10min(400rpm),并超声10min,超声功率为100W,使纳米木素分散均匀。
(3)加热结束后,为消除水分蒸发造成的质量损失,重新计算(2)中的淀粉固含量,量取0.2g淀粉所对应体积的淀粉液6±1mL,转移至直径为6cm的培养皿中,25℃50%RH环境中放置3天制得淀粉复合膜。
(4)测定淀粉复合膜的初始接触角和180s时刻的接触角,结果如下表2。
实施例4
(1)称取1g甲酸木素,溶于200mL四氢呋喃(THF)中,磁力搅拌(300rpm)使其均匀分散转移至透析袋中(Mw=8000),使用去离子水透析3天制得甲酸纳米木素。
(2)称取相对于淀粉质量3%的甲酸纳米木素,与淀粉质量比例分别为1∶10,3∶10,1∶2和1∶1的聚环氧乙烯(PEO)加入烧杯中,然后倒入事先糊化好的10g1%的玉米淀粉液中,置于90℃恒温磁力搅拌器上,搅拌10min(400rpm),并超声10min,超声功率为100W,使纳米木素分散均匀。
(3)加热结束后,为消除水分蒸发造成的质量损失,重新计算(2)中的淀粉固含量,量取0.2g淀粉所对应体积的淀粉液6±1mL,转移至直径为6cm的培养皿中,25℃和50%RH环境中放置3天制得淀粉复合膜。
(4)测定淀粉复合膜的初始接触角和180s时刻的接触角,实验结果如下表1。
表1添加纳米木素后淀粉/聚乙烯醇复合膜的疏水性能
注:PEO/淀粉膜(1∶2)复合膜的初始接触角为65.6°;180s处接触角为54.7°。
由表1可知,由于含有大量的亲水性基团,淀粉/PEO膜(1∶2)复合膜在180s内的动态接触角数值上均在70°以下,表现出极高的亲水性能。而再向不同复合比例的淀粉/聚乙烯醇复合膜中加入1%和3%的甲酸钠米木素后,得到的淀粉/聚乙烯醇复合膜初始时刻和180s末的动态接触角均有了显著的提高,且均超过了90°,证明复合膜的疏水性能确实有了极大提高。这可能是由于甲酸纳米木素的纳米尺度有效提高了复合膜的微纳尺度所致;且甲酸纳米木素也不具有普通木素所含的亲水性磺酸基;同时淀粉和聚乙烯醇中的亲水性羟基相互靠近,可能形成了木素上疏水性基团向外伸展的表面分子结构,所以有效地改善了复合膜的疏水性能。可以看到,淀粉与聚乙烯醇的比例为1∶1时,添加1%的甲酸纳米木素后复合膜的疏水性改善效果最为显著,180s后仍具有高达122.2°的接触角。这表明添加甲酸纳米木素可有效改善淀粉/聚乙烯醇复合膜的疏水性能。
表2添加纳米木素后淀粉/聚环氧乙烯复合膜的疏水性能
由表2可知,向不同复合比例的淀粉/聚乙烯醇复合膜中加入1%和3%的甲酸钠米木素后,得到的淀粉/聚乙烯醇复合膜初始时刻和180s末的动态接触角均有了显著的提高,同时甲酸钠米木素的添加量、聚环氧乙烯和淀粉比例对复合膜的疏水性能有极大影响。这可能与甲酸纳米木素的纳米尺度,疏水性苯环结构,还有复合膜形成过程中甲酸纳米木素、聚环氧乙烯和淀粉所含有的亲水性官能团间的相互作用有关。其中,在甲酸纳米木素添加量为1%,聚环氧乙烯与淀粉比例为3∶10时,复合膜在180s末的接触角最高,疏水性能改善效果最为显著。这表明添加甲酸纳米木素可有效改善淀粉/聚环氧乙烯复合膜的疏水性能。
Claims (4)
1.一种淀粉复合膜材料的制备方法,其特征在于,先将甲酸纳米木素和聚乙烯醇的混合物、甲酸纳米木素和聚环氧乙烯的混合物分别均匀分散于淀粉液中,然后分别在恒温恒湿环境中静置,即可获得疏水性能显著改善的淀粉复合膜材料;其中,甲酸纳米木素的质量为淀粉质量的1%-3%,聚乙烯醇或聚环氧乙烯与淀粉的质量比为(1-10):10;具体包括以下步骤:
(1)取甲酸木质素,溶于四氢呋喃中,磁力搅拌使其均匀分散转移至透析袋中,使用去离子水透析,制得甲酸纳米木素;
(2)取甲酸纳米木素和聚乙烯醇的混合物、甲酸纳米木素和聚环氧乙烯的混合物,分别向两种混合物中加入淀粉液,分别置于恒温磁力搅拌器中搅拌,并超声,使纳米木素分散均匀;恒温磁力搅拌器的温度为90 ℃,搅拌速度为400 rpm,超声时间为10 min;
(3)将步骤(2)中的体系转移至培养皿中,恒温恒湿环境中静置2天以上,制得淀粉复合膜;所述恒温的温度为25 ℃,恒湿的湿度为50%。
2.根据权利要求1所述的淀粉复合膜材料的制备方法,其特征在于,淀粉为玉米淀粉。
3.根据权利要求1所述的淀粉复合膜材料的制备方法,其特征在于,淀粉液中,淀粉的质量分数为1%。
4.权利要求1~3任一项所述的淀粉复合膜材料的制备方法制备得到的淀粉复合膜材料。
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