CN107400249B - 一种香蕉纤维素薄膜的制备方法及其应用 - Google Patents
一种香蕉纤维素薄膜的制备方法及其应用 Download PDFInfo
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Abstract
本发明提供一种香蕉纤维素薄膜的制备方法及其应用,香蕉茎秆纤维首先经过酸碱处理,然后利用离子液体对纤维素进行溶解与改性,再经混合溶液洗涤等一系列制备工艺,获得再生纤维素薄膜。纤维素的离子液体溶解属于物理溶解,较好地保留了纤维素的天然特性,使得该薄膜具有良好的机械性能、生物可降解性和水果保鲜效果。
Description
技术领域
本发明涉及保鲜包装技术领域,特别涉及一种香蕉纤维素薄膜的制备方法及其应用。
背景技术
近年来,随着人们环保意识的不断提高,以及对食品品质要求越来越高,具有可生物降解的绿色环保包装材料被广泛关注。传统塑料类保鲜包装材料的大量和过度化使用带来严重的“白色污染”,而纤维素基材料具有可生物降解、可再生以及生物安全性好等特点,纤维素基水果保鲜包装替代材料的开发符合环境保护和包装材料绿色化的发展趋势。水果保鲜包装材料要求具有良好的保湿性、机械强度、传热传质性等,在贮藏过程中,保持果实的水分和完好性,同时能较好地将生理作用产生的热传递出来,提高保鲜的效果。
然而,由于具有极强氢键的作用,纤维素是植物纤维中最稳定的成份,纤维素基水果保鲜包装材料的制备需要进行改性,以改善其使用性能。常利用化学方法将纤维素改性为纤维素黄酸盐或铜胺络合物,然后再生得到再生纤维素,该方法破坏了纤维素原有的天然特性,造成制备的再生纤维素聚合度降低,机械强度下降,成膜性差。针对化学改性的缺点,本发明通过改进纤维素制备薄膜的方法,使得纤维素溶解和改性后制备的薄膜具有很好的性能。
发明内容
鉴以此,本发明提出一种香蕉纤维素薄膜的制备方法,实现纤维素薄膜的机械性能好、保鲜效果好、生物可降解。
本发明的技术方案是:一种香蕉纤维素薄膜的制备方法,包括以下步骤:
(1)香蕉茎秆刮麻得到香蕉茎秆纤维,剪切,加入酸溶液后进行水浴加热,用水清洗香蕉茎秆纤维至pH呈中性;
(2)将步骤(1)处理后的香蕉茎秆纤维置于碱溶液中再进行水浴加热,用水清洗至pH呈中性,得碱化纤维,烘干备用;
(3)干燥后的碱化纤维加入离子液体1-烯丙基-3-甲基咪唑氯盐中,进行搅拌加热溶解,得溶液并均匀倾倒在玻璃平板上,用涂膜器迅速刮制成均匀的薄膜;
(4)将玻璃平板及薄膜一同放入乙醇和蒸馏水的混合溶液中,用去离子水清洗,得再生的纤维素薄膜;
(5)将再生的纤维素薄膜置于玻璃干燥器内,室温下自热干燥,得产品纤维素薄膜。
优选地,所述步骤(1)中,所述酸溶液为1~3g/L的H2SO4溶液,且固液比为1:15~25。
优选地,所述步骤(1)中,水浴加热温度为45~55℃,水浴加热时间为1.8~2.2h。
优选地,所述步骤(2)中,所述碱溶液为150~250g/L的NaOH溶液。
优选地,所述步骤(2)中,水浴加热温度为25~35℃,水浴加热时间为1~1.7h。
优选地,所述步骤(3)中,搅拌转速为180~220r/min,溶解温度为85~100℃,溶解时间为2.5~3.5h。
优选地,所述步骤(4)中,每隔3~7min更换去离子水,清洗2~5次。
优选地,所述步骤(5)中,干燥时间为20~30h。
本发明还包括制备方法制得的香蕉纤维素薄膜。
优选地,所述香蕉纤维素薄膜应用于保鲜果蔬。
与现有技术相比,本发明的有益效果是:
香蕉茎秆纤维首先经过酸碱处理,然后利用离子液体对纤维素进行溶解与改性,经混合溶液洗涤等一系列制备工艺,获得再生纤维素薄膜。纤维素的离子液体溶解属于物理溶解,较好地保留了纤维素的天然特性,经过使得该薄膜具有良好的机械性能、生物可降解性和水果保鲜效果。
附图说明
图1为塑料薄膜、滤纸和香蕉纤维素薄膜土埋中的形貌对比图。
具体实施方式
为了更好理解本发明技术内容,下面提供具体实施例,做进一步的说明。
实施例1
一种香蕉纤维素薄膜的制备方法,包括以下步骤:
(1)香蕉茎秆刮麻得到香蕉茎秆纤维,剪切,加入1.2g/L的H2SO4溶液后进行水浴加热,香蕉茎秆纤维和硫酸的固液重量比为1:16,水浴加热温度为47℃,水浴加热时间为1.8h,用水清洗香蕉茎秆纤维至pH呈中性;
(2)将步骤(1)处理后的香蕉茎秆纤维置于156g/L的NaOH溶液中再进行水浴加热,水浴加热温度为27℃,水浴加热时间为1h,用水清洗至pH呈中性,得碱化纤维,烘干备用;
(3)干燥后的碱化纤维加入1-烯丙基-3-甲基咪唑氯盐离子液体中,进行搅拌加热溶解,搅拌转速为180r/min,溶解温度为86℃,溶解时间为2.5h,得溶液并均匀倾倒在玻璃平板上,用涂膜器迅速刮制成均匀的薄膜;
(4)将玻璃平板及薄膜一同放入乙醇和蒸馏水的混合溶液中,每隔3min更换用于清洗的去离子水,清洗2次,得再生的纤维素薄膜;
(5)将再生的纤维素薄膜置于玻璃干燥器内,室温下自热干燥,得产品纤维素薄膜,干燥时间为20h。
实施例2
一种香蕉纤维素薄膜的制备方法,包括以下步骤:
(1)香蕉茎秆刮麻得到香蕉茎秆纤维,剪切,加入2.8g/L的H2SO4溶液后进行水浴加热,香蕉茎秆纤维和硫酸的固液重量比为1:23,水浴加热温度为52℃,水浴加热时间为2.2h,用水清洗香蕉茎秆纤维至pH呈中性;
(2)将步骤(1)处理后的香蕉茎秆纤维置于246g/L的NaOH溶液中再进行水浴加热,水浴加热温度为33℃,水浴加热时间为1.7h,用水清洗至pH呈中性,得碱化纤维,烘干备用;
(3)干燥后的碱化纤维加入1-烯丙基-3-甲基咪唑氯盐离子液体中,进行搅拌加热溶解,搅拌转速为220r/min,溶解温度为100℃,溶解时间为3.5h,得溶液并均匀倾倒在玻璃平板上,用涂膜器迅速刮制成均匀的薄膜;
(4)将玻璃平板及薄膜一同放入乙醇和蒸馏水的混合溶液中,每隔7min更换用于清洗的去离子水,清洗5次,得再生的纤维素薄膜;
(5)将再生的纤维素薄膜置于玻璃干燥器内,室温下自热干燥,得产品纤维素薄膜,干燥时间为30h。
实施例3
一种香蕉纤维素薄膜的制备方法,包括以下步骤:
(1)香蕉茎秆刮麻得到香蕉茎秆纤维,剪切,加入2.4g/L的H2SO4溶液后进行水浴加热,香蕉茎秆纤维和硫酸的固液重量比为1:22,水浴加热温度为52℃,水浴加热时间为2.0h,用水清洗香蕉茎秆纤维至pH呈中性;
(2)将步骤(1)处理后的香蕉茎秆纤维置于210g/L的NaOH溶液中再进行水浴加热,水浴加热温度为30℃,水浴加热时间为1.5h,用水清洗至pH呈中性,得碱化纤维,烘干备用;
(3)干燥后的碱化纤维加入1-烯丙基-3-甲基咪唑氯盐离子液体中,进行搅拌加热溶解,搅拌转速为200r/min,溶解温度为93℃,溶解时间为3.2h,得溶液并均匀倾倒在玻璃平板上,用涂膜器迅速刮制成均匀的薄膜;
(4)将玻璃平板及薄膜一同放入乙醇和蒸馏水的混合溶液中,每隔5min更换用于清洗的去离子水,清洗3次,得再生的纤维素薄膜;
(5)将再生的纤维素薄膜置于玻璃干燥器内,室温下自热干燥,得产品纤维素薄膜,干燥时间为25h。
为了验证本发明的有益效果,进一步设置对照组,进行以下实验:
对照组1
该对照组与实施例3的区别在于:未进行步骤(2)碱处理,且步骤(3)中的离子液体为1-丁基-3甲基咪唑氯盐。
对照组2
该对照组与实施例3的区别在于:步骤(3)中溶解温度为80℃,溶解时间为4.5h。
对照组3
该对照组与实施例3的区别在于:步骤(4)中采用去离子水清洗1次。
一、纤维素薄膜的机械性能测试
实施例1~3制备的纤维素薄膜,厚度利用测厚仪、拉伸强度和断裂伸长率利用智能电子拉力试验机、水蒸气透过率利用水蒸气透光率测试仪、气体透过率利用压差法气体渗透仪进行测试。
纤维素薄膜的机械性能测试结果如下表1所示:
纤维素薄膜机械强度需大幅提高以达到水果保鲜包装的实际应用要求,利用酸碱共同处理香蕉茎秆纤维,再利用离子液体1-烯丙基-3-甲基咪唑氯盐溶解,再经过反复洗涤再生得到香蕉纤维素薄膜,其机械性能有明显改善,拉伸强度可达到32.8±7.2Mpa,断裂伸长率4.0±0.5%。纤维素薄膜具有微孔结构,其水蒸气透过率和气体透过率远高于对照组以及传统的塑料薄膜,纤维素薄膜的高通透性有利于乙烯的释放,延缓硬度下降、延长贮藏期。
将对照组与实施例3进行对比,由于缺少碱处理步骤,香蕉纤维素提取不完全,在离子液体中溶解不完全,其中不溶杂质使得在后续制膜步骤中无法制得完整纤维素薄膜。
将对照组2与实施例3进行对比,由于溶解温度降至80℃,溶解时间大幅延长,制得的薄膜厚度增加,机械性能下降,水蒸气和气体透过率亦下降。
将对照组3与实施例3进行对比,由于使用去离子水仅清洗1次,所制得薄膜中离子液体残留过多,薄膜无法完全干燥且厚度明显增加,虽然机械强度无明显差异,但水蒸气和气体透过率大幅降低。
二、纤维素薄膜的果蔬保鲜应用
通过实施例制得的香蕉纤维素薄膜应用于保鲜果蔬中。
将制得的纤维素薄膜制成10×15cm的纤维素薄膜包装袋,用同样方法将市售保鲜袋制成同等规格的塑料薄膜包装袋。芒果(小台芒)和香蕉(皇帝蕉)购于本地水果市场,未经杀菌和保鲜处理。挑选大小、形状相近且无可见机械损伤与病害的果实用于实验。经挑选的果实用自来水冲洗1min,洗去表面的污物,晾干,用灭菌的厨房纸巾擦去残余水分,单果封存于纤维素薄膜包装袋或塑料薄膜包装袋内,贮藏于室温(25~30℃)或11℃,相对湿度为60~85%,分别于第7天和第14天统计和计算果皮转黄指数、病情指数、病果率、商品果率及失重率等。统计与计算方法如下:
果皮颜色共分5级:0级——全绿;1级——果蒂处稍有变黄;2级——果蒂处及以外局部变黄;3级——果实大部分表面变黄,约有1/3表面绿色;4级——果实表皮全部转黄。
果实的发病程度共分5级:0级——无病斑;1级——病斑5个以下,最大病斑直径小于5mm;2级——病斑5个左右,最大病斑直径小于8mm;3级——病斑5个以上最大病斑直径在8~15mm,病斑组织深达果肉;4级——最大病斑直径15mm以上,或有20个以上的1~5mm直径的病斑。
病果率(%)=病果数/检查总果数×100%;
商品果率(%)=(0级果数+1级病果数)/检查总果数×100%;
失重率(%)=(贮藏前果重-贮藏后果重)/贮藏前果重×100%。
1、纤维素薄膜与塑料薄膜对香蕉的保鲜效果比较:
由上表可知,塑料薄膜和纤维素薄膜包装降低了香蕉的病情指数,增加了商品果率。此外,薄膜包装可以显著减少香蕉贮运过程中的失水,室温下无包装香蕉的失重率高达15.2%,薄膜包装失重率为2.9~5.1%。由于其通透性高,纤维素薄膜包装贮藏14天的香蕉失重率为5.1%,高于塑料薄膜包装的2.9%。塑料薄膜包装的香蕉果皮转黄指数7天后即达到10,而此时纤维素薄膜包装的果皮转黄指数仅为5.25,14天后才达到8.5。由此说明,纤维素薄膜的高通透性亦有利于乙烯气体的释放,从而延缓香蕉的后熟。贮藏温度为11℃时,香蕉果实的病情指数和转黄指数显著降低,包装材料对保鲜效果的影响规律与室温贮藏时一致,即纤维素薄膜包装可延迟香蕉果实的后熟,从而延长贮藏期。
2、纤维素薄膜与塑料薄膜对芒果的保鲜效果比较:
塑料薄膜包装加速了芒果的变质腐烂。在室温和11℃保存条件下,7天和14天时塑料薄膜包装芒果的病情指数分别为8.5和3.5,高于无包装的5.25和2.75。若采用纤维素薄膜包装,病情指数大幅降低,商品果率显著提高。室温贮藏7天时纤维素薄膜包装的商品果率达80%,而塑料薄膜包装的为0,无包装的仅为10%。采用纤维素薄膜包装亦可减缓果皮转黄速度,室温贮藏7天时其果皮转黄指数为0.5,而塑料薄膜包装和无包装的果皮转黄指数高达8.5和5.25。适宜的低温可有效地抑制芒果呼吸强度,延缓果实后熟和病害的发生。从表中可知,低温冷藏可显著抑制病害发生和果皮转黄,提高商品果率,延长贮藏期;11℃贮藏条件下,包装材料对芒果保鲜效果的影响规律与室温贮藏时一致,纤维素薄膜包装可进一步提高商品果率及延长贮藏期。
保鲜实验结果表明,纤维素薄膜具有良好的水果保鲜效果。纤维素薄膜包装降低了香蕉和芒果的病情指数,增加了商品果率,降低了果皮转黄指数,延长了贮运期。
三、纤维素薄膜的生物可降解性
水果保鲜包装中大量使用了一次性塑料,而塑料材料在自然环境中难于降解,造成严重的“白色污染”。纤维素薄膜保鲜包装材料除了具有良好的生物安全性和生物相容性外,最大的特点在于其可生物降解。采用土埋法对纤维素薄膜进行生物可降解性测试,土埋法利用自然界中的微生物来进行降解试验,能较实际反映材料在自然界中的降解情况。
如图1所示,不同土埋时期塑料薄膜、滤纸及纤维素薄膜形貌变化:
土埋第1周,滤纸和纤维素薄膜表面出现黄斑,为微生物侵染的特征;土埋第2周,滤纸表面出现明显的刻蚀,并出现孔洞和裂痕,而纤维素薄膜降解更快,已经碎片化;土埋第3周,滤纸表面孔洞进一步扩大,而纤维素薄膜降解完全碎片化;土埋第4周,滤纸完全碎片化,纤维素薄膜则只有絮状残留,质量残留率为7.0%。土埋实验表明,本发明制备的纤维素薄膜在自然环境中可被完全降解,不会造成“白色污染”。
综上所述,采用本发明所提供的一种香蕉纤维素薄膜的制备方法,香蕉茎秆纤维首先经过酸碱处理,然后利用离子液体对纤维素进行溶解与改性,经混合溶液洗涤等一系列制备工艺,获得再生纤维素薄膜。纤维素的离子液体溶解属于物理溶解,较好地保留了纤维素的天然特性,经过使得该薄膜具有良好的机械性能、生物可降解性和水果保鲜效果。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种香蕉纤维素薄膜的制备方法,其特征在于,包括以下步骤:
(1)香蕉茎秆刮麻得到香蕉茎秆纤维,剪切,加入酸溶液后进行水浴加热,用水清洗香蕉茎秆纤维至pH呈中性;
(2)将步骤(1)处理后的香蕉茎秆纤维置于碱溶液中进行水浴加热,用水清洗至pH呈中性,得碱化纤维,烘干备用;
(3)干燥后的碱化纤维加入离子液体1-烯丙基-3-甲基咪唑氯盐中,进行搅拌加热溶解,得溶液并均匀倾倒在玻璃平板上,用涂膜器迅速刮制成均匀的薄膜;
(4)将玻璃平板及薄膜一同放入乙醇和蒸馏水的混合溶液中,用去离子水清洗,得再生的纤维素薄膜;
(5)将再生的纤维素薄膜置于玻璃干燥器内,室温下自热干燥,得产品纤维素薄膜,
所述步骤(1)中,所述酸溶液为1~3g/L的H2SO4溶液,且固液比为1:15~25,
所述步骤(1)中,水浴加热温度为45~55℃,水浴加热时间为1.8~2.2h,
所述步骤(2)中,所述碱溶液为150~250g/L的NaOH溶液,
所述步骤(2)中,水浴加热温度为25~35℃,水浴加热时间为1~1.7h。
2.如权利要求1所述的一种香蕉纤维素薄膜的制备方法,其特征在于,所述步骤(3)中,搅拌转速为180~220r/min,溶解温度为85~100℃,溶解时间为2.5~3.5h。
3.如权利要求1所述的一种香蕉纤维素薄膜的制备方法,其特征在于,所述步骤(4)中,每隔3~7min更换去离子水,清洗2~5次。
4.如权利要求1所述的一种香蕉纤维素薄膜的制备方法,其特征在于,所述步骤(5)中,干燥时间为20~30h。
5.一种香蕉纤维素薄膜,其特征在于,由权利要求1~4任一项所述的香蕉纤维素薄膜的制备方法制得。
6.如权利要求5所述的一种香蕉纤维素薄膜,其特征在于,应用于保鲜果蔬。
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