CN116426012A - 一种改性壳聚糖可降解复合保鲜膜的制备方法 - Google Patents
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Abstract
本发明涉及一种改性壳聚糖可降解复合保鲜膜的制备方法。将壳聚糖溶解于冰醋酸水溶液得到壳聚糖溶解液；将上述壳聚糖溶解液与甘油三酯添加液以及棕榈酸添加液混合并搅拌均匀制备膜液；将上述膜液超声脱气后均匀涂布至平板容器中；膜液烘干后与平板容器分离即得到改性壳聚糖复合保鲜膜。改性壳聚糖复合保鲜膜同时兼顾优良的溶胀度、机械性能和阻水性能。甘油三酯和壳聚糖、棕榈酸之间形成分子间氢键，使膜结构更加致密，明显提升了复合保鲜膜的机械性能，具有优异的拉伸强度和断裂伸长率，同时提高保鲜膜的阻水性能，能够有效防止营养物质流失，延长果蔬的保鲜时间。符合GB/T 10457‑2021《食品用塑料自粘保鲜膜质量通则》中的要求。
Description
技术领域
本发明涉及环境技术领域，属于可生物降解材料，特别是涉及一种改性壳聚糖可降解复合保鲜膜及制备方法。
背景技术
随着人们对环保和食品质量安全的愈加重视，同时传统的高分子材料包装的缺点逐渐显现，如不可生物降解、不可回收、处理难度大、污染环境等，使得研究者致力于将可生物降解聚合物材料作为食品包装、保鲜材料。一些碳水化合物聚合物，如淀粉、纤维素衍生物、壳聚糖和果胶，是可生物降解和可食用的物质，绿色无毒，已被用作包装材料，可以延长食品保质期，被认为是具有工业化发展前景的可降解包装材料。
在众多碳水化合物聚合物中，壳聚糖是一种低乙酰基取代形式的甲壳素和天然碳水化合物共聚物，由β-(1-4)-2-乙酰氨基-D-葡萄糖和β-(1-4)-2-氨基-D-葡萄糖单元组成。具有很好的成膜性、通透性和吸附性且易进行结构修饰和改性，是一种性能优良的天然高分子功能膜材料。由于壳聚糖膜的制作工艺简单，并且膜的制备过程不涉及有毒物质，绿色且安全，因此，壳聚糖广泛应用于食品工业。除此之外，壳聚糖是世界上第二丰富的多糖，可以从丰富的可再生资源中获得，主要是贝类工业的废物，成本低廉。因此，具有良好的商业化潜质。然而，壳聚糖属亲水性聚合物，以其为基质制得的复合膜相比于市面上成熟的聚乙烯、聚氯乙烯膜，阻湿性较差，在高湿度下容易吸湿溶解成为限制其广泛应用的一个重要因素，因此需要对壳聚糖进行改性。
壳聚糖分子内含有羧基和氨基两种活性基团，为改性提供了多种可能，如交联、共聚、共混、离子化或壳聚糖分子链上的氨基与过渡金属离子形成配位络合物等。壳聚糖膜的改性通常以壳聚糖为成膜基质，添加多糖(淀粉、果胶、纤维素及其衍生物等)、蛋白质(肌原纤维蛋白、胶原蛋白、酪蛋白等)、脂质(甘油、植物精油、硬脂酸等)或者纳米材料(纳米二氧化钛、纳米氧化锌等)进行制备，以此提高膜的机械性能、阻隔性能、抗菌性能和抗氧化性能。目前大部分壳聚糖成膜溶剂为冰醋酸，壳聚糖单体通过分子内或分子间氢键、范德华力、物理缠结等作用交联，均匀分散在冰醋酸溶液中，形成三维网状结构。当壳聚糖与不同物质复合时，分子上的羟基、氨基等活性基团可与添加物上的羟基、乙酰基、羧基等发生氢键、静电、疏水作用，使复合膜结构更加紧密，进而结构影响性能，单一壳聚糖膜的机械性能、阻水性、抗菌活性得以增强。混合均匀且脱气后的膜液，在烘箱中烘干后能形成具有可生物降解性、良好阻气性、抑菌性的复合膜，提高食品安全性、延长食品货架期。可是现在技术仍存在无法兼顾溶胀度、阻水性能和机械性能的问题。
发明内容
为了解决现有技术的问题，其目的在于通过调配不同组分的添加量，以GB/T10457-2021《食品用塑料自粘保鲜膜质量通则》中PBAT指标为评价标准，探究最佳成膜配比，以改善单一壳聚糖膜阻水性能差、高湿度环境下容易吸湿溶解、力学性能差以及改性复合膜无法兼顾多种性能等问题。
本发明为改善以上问题，将壳聚糖基质与棕榈酸、甘油三酯进行共混改性，将膜液脱气、干燥后得到具有优良溶胀度，阻水性能和机械性能的可生物降解性复合薄膜。
本发明提供了一种改性壳聚糖基可降解复合保鲜膜的制备方法，包括以下步骤：
(1)将壳聚糖溶解于冰醋酸水溶液得到壳聚糖溶解液；
(2)将上述壳聚糖溶解液与甘油三酯添加液以及棕榈酸添加液混合并搅拌均匀制备膜液；
(3)将上述膜液超声脱气后均匀涂布至平板容器中；膜液烘干后与平板容器分离即得到改性壳聚糖复合保鲜膜。
所述步骤(1)中优选壳聚糖与冰醋酸水溶液的用量比为(0.5-2.0)g:100mL。
所述步骤(1)中优选壳聚糖溶解于体积分数为1-3％的冰醋酸水溶液中。
所述步骤(2)中优选甘油三酯与乙二醇的用量比为(50-150)mg:100mL，甘油三酯添加液与壳聚糖溶解液的用量比为(3.0-6.0)mL:100mL。
所述步骤(2)中优选棕榈酸与乙醇的用量比为(1-3)g:30mL，棕榈酸添加液与壳聚糖溶解液的用量比为(0.3-0.6)mL:100mL。
所述步骤(2)中优选搅拌速度为600-800r/min，搅拌时间为0.5-1.5h。
所述步骤(3)中优选膜液超声脱气时间为0.5-1.5h，超声频率为35-45kHz.
所述步骤(3)中优选膜液烘干温度为30-55℃，烘干时间为15-25h。
通过本发明所提出的以上技术方案与现有技术相比，能够取得下列有益效果：
(1)通过下表中的数据可知，本发明提供的新型制备方法能够使改性壳聚糖复合保鲜膜同时兼顾优良的溶胀度、机械性能和阻水性能。(2)甘油三酯可以和壳聚糖、棕榈酸之间形成分子间氢键，使膜结构更加致密，明显提升了复合保鲜膜的机械性能，具有优异的拉伸强度和断裂伸长率，使保鲜膜更具韧性，同时使保鲜膜具有较低的水蒸气透过率，提高保鲜膜的阻水性能，能够有效防止营养物质的流失，延长果蔬的保鲜时间。符合GB/T10457-2021《食品用塑料自粘保鲜膜质量通则》中的要求。(3棕榈酸分子中含有亲水基团(-COOH)，在水中溶胀程度大，使得本发明在具备良好机械性能的前提下，溶胀度优于现有技术水平，为光或微生物的降解反应提供有利条件，说明该复合保鲜膜中的高分子链更易被降解为小分子量化合物，可以有效缩短保鲜膜的降解周期。(4)本发明工艺简单，生产过程中不涉及有毒物质，绿色且安全，适宜推广工业化生产。
表1本方法制备的保鲜膜与现有技术性能对比
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
1.将壳聚糖溶解于体积分数为1％的冰醋酸水溶液中得到壳聚糖溶解液，其中壳聚糖与冰醋酸水溶液的用量比为0.5g:100mL。
2.在壳聚糖溶解液中加入甘油三酯添加液及棕榈酸添加液搅拌得到膜液，搅拌速度为600r/min，搅拌时间为0.5h。甘油三酯添加液为甘油三酯与乙二醇的混合物，其中甘油三酯与乙二醇的用量比为50mg:100mL，甘油三酯添加液与壳聚糖溶解液的用量比为3.0mL:100mL。棕榈酸添加液为棕榈酸与乙醇的混合物，其中棕榈酸与乙醇的用量比为1g:30mL，棕榈酸添加液与壳聚糖溶解液的用量比为0.3mL:100mL。
3.将上述混合后的膜液超声脱气后均匀涂布至平板容器中，在膜液烘干后与平板容器分离即得到复合膜。膜液超声脱气时间为0.5h，超声频率为35kHz。膜液烘干温度为30℃，烘干时间为15h。
实施例2
1.将壳聚糖溶解于体积分数为3％的冰醋酸水溶液中得到壳聚糖溶解液，其中壳聚糖与冰醋酸水溶液的用量比为2.0g:100mL。
2.在壳聚糖溶解液中加入6.0mL甘油三酯添加液及0.6mL棕榈酸添加液搅拌得到膜液，搅拌速度为800r/min，搅拌时间为1.5h。甘油三酯添加液为甘油三酯与乙二醇的混合物，其中甘油三酯与乙二醇的用量比为150mg:100mL，甘油三酯添加液与壳聚糖溶解液的用量比为6.0mL:100mL。棕榈酸添加液为棕榈酸与乙醇的混合物，其中棕榈酸与乙醇的用量比为3g:30mL，棕榈酸添加液与壳聚糖溶解液的用量比为0.6mL:100mL。
3.将上述混合后的膜液超声脱气后均匀涂布至平板容器中，在膜液烘干后与平板容器分离即得到复合膜。膜液超声脱气时间为1.5h，超声频率为45kHz。膜液烘干温度为55℃，烘干时间为25h。
实施例3
1.将壳聚糖溶解于体积分数为2％的冰醋酸水溶液中得到壳聚糖溶解液，其中壳聚糖与冰醋酸水溶液的用量比为1g:100mL。
2.在壳聚糖溶解液中加入甘油三酯添加液及棕榈酸添加液搅拌得到膜液，搅拌速度为700r/min，搅拌时间为1.0h。甘油三酯添加液为甘油三酯与乙二醇的混合物，其中甘油三酯与乙二醇的用量比为100mg:100mL，甘油三酯添加液与壳聚糖溶解液的用量比为5.0mL:100mL。棕榈酸添加液为棕榈酸与乙醇的混合物，其中棕榈酸与乙醇的用量比为2g:30mL，棕榈酸添加液与壳聚糖溶解液的用量比为0.5mL:100mL。
3.将上述混合后的膜液超声脱气后按一定量转移至平板容器中，在膜液烘干后与平板容器分离即得到复合膜。膜液超声脱气时间为1.0h，超声频率为40kHz。膜液烘干温度为40℃，烘干时间为20h。
壳聚糖复合保鲜膜性能测试：(1)溶胀度的测定：保鲜膜干燥至恒重后将其放入烧杯中，用塑料包装覆盖50mL蒸馏水，24h后取出并称量湿膜的重量，利用两次的质量差计算溶胀度；(2)透明度的测定：在800nm下，用紫外可见光分光光度计测定透过率；(3)水蒸气透过率的测定：在称量瓶中装入干燥无水氯化钙以提供相对湿度为0％的环境，用干燥膜将称量瓶口密封并称重，然后使复合膜两侧保持一定的蒸气压差，24h后再次称重，通过两次的质量差计算水蒸气透过率；(4)机械性能的测定：使用万能材料试验机测量薄膜的拉伸强度和断裂伸长率，初始夹持间距为5cm，延伸速度为1mm/s。
表2实施例与对比例不同性能的比较
将各实施例与表1中若干其他种类的复合保鲜膜对比可得，壳聚糖/没食子酸复合膜机械性能较好，但阻水性能和溶胀度表现较差；而壳聚糖/果胶复合膜虽然阻水性能和溶胀度表现优异，但机械性能不符合国家标准。在满足GB/T 10457-2021《食品用塑料自粘保鲜膜质量通则》PBAT指标中力学性能要求下，各实施例均表现出均衡、优良的溶胀度、阻水性能和机械性能。可能是因为壳聚糖、棕榈酸和甘油三酯分子间形成了氢键的相互作用，使分子间连接更紧密，进而使膜结构更加致密，有效遏制水分扩散，机械性能和阻水性能更好，同时也验证了甘油三酯作为增塑剂的可能性。另外，棕榈酸分子中含有亲水基团(-COOH)，在水中的溶胀程度大，因此各实施例在具有优良的机械性能和阻水性能的同时具有较优的溶胀度，有利于其后续的光或生物降解反应，缩短降解周期。实施例2中棕榈酸添加量最多而溶胀度降低的原因可能为甘油三酯添加量的增多使分子间作用力增大，溶剂分子进入膜分子内部受阻，进而导致溶胀度降低。综上，经过棕榈酸及甘油三酯的协同改性，壳聚糖复合保鲜膜的各项性能均有显著提升，符合具有广阔的工业化生产前景。
本发明公开和提出的技术方案，本领域技术人员可通过借鉴本文内容，适当改变条件路线等环节实现，尽管本发明的方法和制备技术已通过较佳实施例子进行了描述，相关技术人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和技术路线进行改动或重新组合，来实现最终的制备技术。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，他们都被视为包括在本发明精神、范围和内容中。
Claims (8)
1.一种改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，包括以下步骤：
(1)将壳聚糖溶解于冰醋酸水溶液得到壳聚糖溶解液；
(2)将上述壳聚糖溶解液与甘油三酯添加液以及棕榈酸添加液混合并搅拌均匀制备膜液；
(3)将上述膜液超声脱气后均匀涂布至平板容器中；膜液烘干后与平板容器分离即得到改性壳聚糖复合保鲜膜。
2.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(1)中壳聚糖与冰醋酸水溶液的用量比为(0.5-2.0)g:100mL。
3.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(1)中壳聚糖溶解于体积分数为1-3％的冰醋酸水溶液中。
4.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(2)中甘油三酯与乙二醇的用量比为(50-150)mg:100mL，甘油三酯添加液与壳聚糖溶解液的用量比为(3.0-6.0)mL:100mL。
5.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(2)中棕榈酸与乙醇的用量比为(1-3)g:30mL，棕榈酸添加液与壳聚糖溶解液的用量比为(0.3-0.6)mL:100mL。
6.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(2)中搅拌速度为600-800r/min，搅拌时间为0.5-1.5h。
7.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(3)中膜液超声脱气时间为0.5-1.5h，超声频率为35-45kHz。
8.如权利要求1所述的改性壳聚糖基可降解复合保鲜膜的制备方法，其特征是，所述步骤(3)中膜液烘干温度为30-55℃，烘干时间为15-25h。
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