CN114081869A - 一种微胶囊镶嵌壳聚糖固体香氛及其制备方法与应用 - Google Patents

一种微胶囊镶嵌壳聚糖固体香氛及其制备方法与应用 Download PDF

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CN114081869A
CN114081869A CN202111196647.2A CN202111196647A CN114081869A CN 114081869 A CN114081869 A CN 114081869A CN 202111196647 A CN202111196647 A CN 202111196647A CN 114081869 A CN114081869 A CN 114081869A
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chitosan
essential oil
solid fragrance
microcapsule
polylactic acid
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CN114081869B (zh
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胡剑峰
朱泽铭
瞿金清
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South China University of Technology SCUT
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Abstract

本发明公开了一种微胶囊镶嵌壳聚糖固体香氛及其制备方法及应用，其是将聚乳酸和精油按多种质量比溶解在二氯甲烷中；随后在得到的聚乳酸‑精油溶液中加入聚乙烯醇溶液，得到初乳液；再将聚乙烯醇溶液和乳化剂加入到初乳液中，乳化后洗涤，最后在冷冻干燥机中冷冻干燥得到微胶囊。再将微胶囊加入到壳聚糖溶液中，使其充分混合，冷冻干燥后浸渍在植物精油中，制备得到固体香氛。本发明具有以下优点：制备方法简单，壳聚糖固体香氛释放精油时间持久；还通过外壳层提高了微胶囊的抗冲击性能和耐化学品性，保证产品的质量稳定性和储存稳定性。

Description

一种微胶囊镶嵌壳聚糖固体香氛及其制备方法与应用
技术领域
本发明属于功能材料领域，涉及一种微胶囊镶嵌壳聚糖固体香氛及其制备方法与应用。
背景技术
微胶囊具体来说是指将某一目的物(芯或内相)用各种天然的或合成的高分子化合物连续薄膜(壁或外相)完全包覆起来，而对目的物的原有化学性质丝毫无损，然后逐渐地通过某些外部刺激或缓释作用使目的物的功能再次在外部呈现出来，或者依靠囊壁的屏蔽作用起到保护芯材的作用，微胶囊的直径一般为1～500μm，壁的厚度为0.5～150μm。其中，被包埋的物质称为芯材，包括香精香料、酸化剂、甜味剂、色素、脂类、维生素、矿物质、酶、微生物、气体以及其它各种饲料添加剂，包埋芯材实现微囊胶化的物质称为壁材。
聚乳酸，又称为聚丙交酯，是通过乳酸聚合得到的聚酯类聚合物。聚乳酸具有良好的抗溶剂性、优异的机械性能和物理性能。可以进行多种加工，包括挤压、吹塑、拉伸、纺丝等。由聚乳酸制备而成的材料不只具有良好的生物降解性，还具有较好的生物相容性、透明性、耐热性、手感和光泽度，由于具有以上种种优点，聚乳酸被广泛应用于内外衣服装、包装材料、纤维、非织造物、建筑、化工和医疗卫生等领域，在此作为微胶囊的壁材使用。
天然多糖因其高效、环保、可生物降解和低成本的优越特性而备受关注。例如，壳聚糖在各种形式的粉末、片状、珠状和膜中由于存在氨基和羟基官能团而表现出优异的吸附能力。壳聚糖泡沫是一种较好的泡沫材料，具有材料利用率高、生态友好、二次污染风险低的特点。
普通微胶囊和普通壳聚糖泡沫在释放芯材、保护活性物质等领域的应用上存在以下问题：(1)微胶囊壁材对环境有一定的毒害性，壁材大部分不是绿色无毒材料，降解后可能对环境产生副作用；(2)壁材微胶囊力学性能不够导致的对于芯材的保护作用受限；(3)释放吸收物质较快，通常在较短的时间内就将所吸收物质释放完毕，不能达到长久的释放功能。
发明内容
本发明的第一目的在于针对现有技术存在的问题，提供一种微胶囊镶嵌壳聚糖固体香氛的制备方法。
本发明的第二目的在于提供上述方法制备得到的微胶囊镶嵌壳聚糖固体香氛。
本发明的第三目的还在于提供所述微胶囊镶嵌壳聚糖固体香氛在制备药品、化妆品及功能型材料中的应用。
为了实现上述发明目的，本发明采用的技术方案是：
一种制备微胶囊镶嵌壳聚糖固体香氛的方法，其包括如下步骤：
(1)聚乳酸微胶囊的制备：
将聚乳酸和精油溶解在有机溶剂中；在得到的聚乳酸-精油溶液中加入聚乙烯醇溶液，超声后得到初乳液；再将聚乙烯醇溶液和乳化剂加入到初乳液中，乳化后搅拌固化，冷冻干燥得到微胶囊；
(2)壳聚糖固体香氛的制备：
将微胶囊加入到壳聚糖溶液中，混合均匀后，冷冻干燥得到微胶囊镶嵌的壳聚糖泡沫，最后将得到的泡沫在植物精油中浸渍，制备得到固体香氛。
步骤(1)所述聚乳酸与精油的质量比为(1～5)：1，优选为(1～2)：1。
步骤(1)所述精油为薰衣草、柠檬、海风、桂花、洋甘菊、百合、茉莉、玫瑰、紫罗兰、檀香、茶树、香橙、康乃馨、雪莲、姜花、薄荷、森林、郁金香、玉兰花、风信子、迷迭香、欧薄荷、茶树、黑胡椒、姜、小豆蔻、乳香、没药、亚麻籽、香茅、玫瑰、榄香、白松香、西洋杉、檀香、松木、杜松、广藿香和岩兰草中的至少一种。
步骤(1)所述溶剂为二氯甲烷、乙酸正丁酯、二甲苯、三氯甲烷中的至少一种；
步骤(1)所述聚乳酸与溶剂的质量比为1：(15～25)，优选为1:20～22。
步骤(1)中前后两次所述聚乙烯醇溶液的浓度均为0.2～0.8％，优选为0.5wt％。
步骤(1)所述聚乳酸-精油溶液与第一次加入聚乙烯醇溶液的质量比为1：(0.5～3)，优选为1:1。
步骤(1)所述初乳液与第二次加入聚乙烯醇溶液的质量比为1：(1～4)，优选为1:2。
步骤(1)所述乳化剂为阿拉伯树胶粉、失水山梨醇单油酸酯(Span 80)、山梨醇酐单油酸酯(Tween 80)、硬脂酰乳酸钠、双乙酰酒石酸单甘油酯等中的至少一种。
步骤(1)所述乳化剂与聚乳酸的质量比为(10～20)：1，优选为15:1。
步骤(1)所述乳化为在4000～8000r/min的转速下乳化10～40min，优选为在6000r/min的转速下乳化20min。
步骤(1)所述搅拌固化完成后还包括用去离子水离心洗涤的步骤。
步骤(2)所述壳聚糖溶液的质量浓度为(0.1～0.5)wt％。优选的，步骤(2)所述壳聚糖溶液所使用的溶剂为盐酸、乙酸、过氧乙酸中的至少一种与水的混合溶液；
步骤(2)所述微胶囊与壳聚糖的质量比为1：(2～10)，优选为1:5。
步骤(2)所述植物精油与步骤(1)所用精油为同一精油。
一种微胶囊镶嵌壳聚糖固体香氛，通过上述方法制备得到。
所述微胶囊镶嵌壳聚糖固体香氛在制备药品、化妆品及功能型材料中的应用。
优选的，所述微胶囊镶嵌壳聚糖固体香氛可作为化妆品等功能型精细有机化学品添加剂,使用时添加量为总质量的1-20％。优选的，使用时添加量为总质量的5-10％。
优选的，所述微胶囊镶嵌壳聚糖固体香氛可在制备胶粘剂、涂料中应用，使用时添加量为总质量的1-30％。更优选的，使用时添加量为总质量的3-20％。
本发明以聚乳酸作为壁材，植物精油为芯材制备了聚乳酸微胶囊，并且将其镶嵌到壳聚糖泡沫中，具有优异的包封性能，持续稳定的缓释效果，力学性能优异，具有广泛用途。
本发明的原理是：(1)采用水/油/水(W1/O/W2)双乳液法制备聚乳酸微胶囊，将油相与去离子水混合，声波作用形成W1/O的一次乳状液。然后将一次乳液立即注入大量PVA水溶液中，在机械搅拌下制备粗重乳液,经过一夜的磁搅拌，得到了均匀的双乳液并固化。(2)将一定比例的壳聚糖溶液和微胶囊混合，冷冻干燥得到微胶囊镶嵌的壳聚糖固体香氛。
与现有技术相比，本发明具有以下优点：
1)制备的聚乳酸微胶囊为白色或灰白色均匀球体，平均粒径1-5μm；水分质量含量≤5％；临界应力最高能达到100mN，机械性能好；
2)制备的聚乳酸微胶囊，不仅通过内壳层的包封控制了芯材料缓释速率，还通过外壳层提高了微胶囊的抗冲击性能和耐化学品性，保证产品的质量稳定性和储存稳定性；
3)聚乳酸微胶囊的制备方法可用于包封多种活性物质，原料来源广泛，壳层原料价格便宜；
4)制备工艺简单，生产的聚乳酸微胶囊可以应用在食品、药品、化妆品等领域，还可以广泛应用于功能型材料领域，拓宽微胶囊的使用范围。
5)制备的壳聚糖固体香氛为灰白色固体，香味释放周期长。
具体实施方式
以下通过具体实施例来对发明作进一步的说明，结合试验进一步说明本发明的有益效果。但这些实施例只是为了说明，不是对本发明的限制。
本发明制备的聚乳酸微胶囊的性能表征方法如下：外观的测试：自然光下观察并记录，光学显微镜；平均粒径：马尔文粒径分析仪；临界应力用微控系统(Model 403A)测定；所述聚乳酸型号为4060D，分子量大约为320000。所述聚乙烯醇型号为PVA-1788。
实施例1
聚乳酸微胶囊镶嵌壳聚糖固体香氛的原料配方如下表。
组分 重量份数
聚乳酸(4060D,纯度≧95％) 1
溶剂：二氯甲烷 21.25
茶树精油(纯度≧99％) 1
玫瑰精油(纯度≧99％) 1
壳聚糖 5
溶剂：醋酸 7.5
乳化剂：阿拉伯树胶粉 15
聚乙烯醇(PVA-1788) 0.8
去离子水 78.4
制备方法的由以下步骤制成：
(1)聚乳酸微胶囊的制备：
按照上表将聚乳酸、茶树精油和玫瑰精油按质量比(1:1:1)在21.25份的二氯甲烷磁力搅拌0.5h溶解；随后在得到的聚乳酸-精油溶液中加入1:1质量比的聚乙烯醇溶液(0.5wt％)，超声15min，得到初乳液；再将质量比为1:2的聚乙烯醇溶液(0.5wt％)和15份的乳化剂加入到初乳液中，在6000r/min的转速下乳化20min，之后过夜搅拌固化，完成后使用去离子水在2000r/min的离心机中洗涤三次，最后在冷冻干燥机中冷冻干燥72h得到微胶囊。微胶囊的平均粒径为1±0.05微米，临界应力为50mN。
(2)壳聚糖固体香氛的制备：
将微胶囊加入到0.5wt％的壳聚糖-醋酸溶液中，搅拌1h使其充分混合，冷冻干燥后得到微胶囊镶嵌的壳聚糖固体香氛，最后将得到的泡沫在茶树精油和玫瑰精油中浸渍1h，使壳聚糖固体香氛孔道充分吸收植物精油。
产品指标：该固体香氛可以持续3个月保持香味释放。
实施例2
聚乳酸微胶囊镶嵌壳聚糖固体香氛的原料配方如下表。
Figure BDA0003303237930000061
Figure BDA0003303237930000071
制备方法的由以下步骤制成：
(1)聚乳酸微胶囊的制备：
将聚乳酸、薰衣草精油和香茅精油按质量比(1:1:1)在29.06份的乙酸正丁酯磁力搅拌0.5h溶解；随后在得到的聚乳酸-精油溶液中加入1:1质量比的聚乙烯醇溶液(0.5wt％)，超声15min，得到初乳液；再将质量比为1：2的聚乙烯醇溶液(0.5wt％)和15份的乳化剂加入到初乳液中，在4000r/min的转速下乳化20min，之后过夜搅拌固化，完成后使用去离子水在4000r/min的离心机中洗涤三次，最后在冷冻干燥机中冷冻干燥72h得到微胶囊。微胶囊的平均粒径为5±0.1微米，临界应力为100mN。
(2)壳聚糖固体香氛的制备：
将微胶囊加入到0.5wt％的壳聚糖-醋酸溶液中，搅拌1h使其充分混合，冷冻干燥后得到微胶囊镶嵌的壳聚糖固体香氛，最后将得到的泡沫在植物精油中浸渍1h，使壳聚糖固体香氛孔道充分吸收植物精油。
产品指标：该固体香氛可以持续3个月保持香味释放。
实施例3
用于车载空气清新的聚乳酸微胶囊的配方如下表：
组分 重量份数
聚乳酸(4060D,纯度≧95％) 1
溶剂：二氯甲烷 21.25
香茅精油(纯度≧99％) 1
牛至精油(纯度≧99％) 1
乳化剂：阿拉伯树胶粉 15
聚乙烯醇(PVA-1788) 0.8
制备方法的由以下步骤制成：
(1)聚乳酸微胶囊的制备：
将聚乳酸、香茅精油和牛至精油按质量比(1:1:1)溶解在二氯甲烷中；随后在得到的聚乳酸-精油溶液中加入1:1质量比的聚乙烯醇溶液(0.5wt％)，超声15min，得到初乳液；再将质量比为1:2的聚乙烯醇溶液(0.5wt％)和乳化剂加入到初乳液中，在6000r/min的转速下乳化20min，之后过夜搅拌固化，完成后使用去离子水在4000r/min的离心机中洗涤三次，最后在冷冻干燥机中冷冻干燥72h得到微胶囊。微胶囊的平均粒径为1±0.05微米，临界应力为50mN。
(2)壳聚糖固体香氛的制备：
将微胶囊加入到0.5wt％的壳聚糖-醋酸溶液中，搅拌1h使其充分混合，冷冻干燥后得到微胶囊镶嵌的壳聚糖固体香氛，最后将得到的泡沫在植物精油中浸渍1h，使壳聚糖固体香氛孔道充分吸收植物精油。
产品指标：该固体香氛可以持续3个月保持香味释放。
以上详细描述了本发明的较佳具体实施例，是发明人花费了大量人才财力和时间，在多次试验出来的结果，应当理解，本领域的普通技术无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此，凡本技术领域中技术人员依本发明构思在现有技术基础上通过逻辑分析、推理或者根据有限的实验可以得到的技术方案，均应该在由本权利要求书所确定的保护范围之中。

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1.一种制备微胶囊镶嵌壳聚糖固体香氛的方法，其特征在于包括如下步骤：
(1)聚乳酸微胶囊的制备：
将聚乳酸和精油溶解在有机溶剂中；在得到的聚乳酸-精油溶液中加入聚乙烯醇溶液，超声后得到初乳液；再将聚乙烯醇溶液和乳化剂加入到初乳液中，乳化后搅拌固化，冷冻干燥得到微胶囊；
(2)壳聚糖固体香氛的制备：
将微胶囊加入到壳聚糖溶液中，混合均匀后，冷冻干燥得到微胶囊镶嵌的壳聚糖泡沫，最后将得到的泡沫在植物精油中浸渍，制备得到固体香氛。
2.根据权利要求1所述的方法，其特征在于：步骤(1)所述聚乳酸与精油的质量比为(1～5)：1；步骤(1)所述聚乳酸与溶剂的质量比为1：(15～25)。
3.根据权利要求1所述的方法，其特征在于：步骤(1)中前后两次所述聚乙烯醇溶液的浓度均为0.2～0.8％；步骤(1)所述聚乳酸-精油溶液与第一次加入聚乙烯醇溶液的质量比为1：(0.5～3)；步骤(1)所述初乳液与第二次加入聚乙烯醇溶液的质量比为1：(1～4)。
4.根据权利要求1所述的方法，其特征在于：步骤(1)所述乳化剂与聚乳酸的质量比为(10～20)：1。
5.根据权利要求1所述的方法，其特征在于：步骤(1)所述乳化剂为阿拉伯树胶粉、失水山梨醇单油酸酯、山梨醇酐单油酸酯、硬脂酰乳酸钠、双乙酰酒石酸单甘油酯中的至少一种；
步骤(1)所述精油为薰衣草、柠檬、海风、桂花、洋甘菊、百合、茉莉、玫瑰、紫罗兰、檀香、茶树、香橙、康乃馨、雪莲、姜花、薄荷、森林、郁金香、玉兰花、风信子、迷迭香、欧薄荷、茶树、黑胡椒、姜、小豆蔻、乳香、没药、亚麻籽、香茅、玫瑰、榄香、白松香、西洋杉、檀香、松木、杜松、广藿香和岩兰草中的至少一种；
步骤(1)所述乳化为在4000～8000r/min的转速下乳化10～40min。
6.根据权利要求1所述的方法，其特征在于：步骤(2)所述壳聚糖溶液的质量浓度为(0.1～0.5)wt％；步骤(2)所述微胶囊与壳聚糖的质量比为1：(2～10)。
7.根据权利要求1所述的方法，其特征在于：步骤(2)所述壳聚糖溶液所使用的溶剂为盐酸、乙酸、过氧乙酸中的至少一种与水的混合溶液；步骤(2)所述植物精油与步骤(1)所用精油为同一精油。
8.一种微胶囊镶嵌壳聚糖固体香氛，通过权利要求1～7任一项所述方法制备得到。
9.根据权利要求8所述微胶囊镶嵌壳聚糖固体香氛在制备药品、化妆品及功能型材料中的应用。
10.根据权利要求9所述的应用，其特征在于：所述微胶囊镶嵌壳聚糖固体香氛作为化妆品功能型精细有机化学品添加剂时，使用时添加量为总质量的1-20％；所述微胶囊镶嵌壳聚糖固体香氛在制备胶粘剂、涂料中应用，使用时添加量为总质量的1-30％。
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CN115216310B (zh) * 2022-08-31 2023-11-17 华南理工大学 一种基于虫胶纳米颗粒和壳聚糖的Pickering乳化剂及其制备与应用

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