壳聚糖-薄荷精油微胶囊的制备及其性能

doi:10.19398/j.att.202103032

摘要/Abstract

摘要：

为了开发缓释型芳香功能材料和纺织品,通过单凝聚法制备薄荷精油微胶囊,以粒径和包埋率为指标,通过单因素法优化薄荷精油微胶囊的制备工艺,利用扫描电子显微镜(SEM)观察微胶囊表面形态;通过红外分析固化前后囊壁分子基团的变化,并测试了薄荷精油微胶囊的缓释性、热稳定性等。结果表明,薄荷精油微胶囊的制备工艺为:以Span80和Tween80复配作为乳化剂,选择分子量约为30000的壳聚糖为壁材,芯材薄荷油与壁材壳聚糖质量比为1∶1,加入质量分数为100%(对壳聚糖用量)的戊二醛固化1 h。薄荷精油微胶囊的平均粒径约为2.8 μm,包埋率达66.67%,常温条件一个月后保留率为65.24%,高温(120℃)2 h后保留率为76.23%,红外分析表明壳聚糖经固化后形成交联结构,热重分析表明薄荷精油微胶囊具有良好的热稳定性。薄荷精油经过微囊化处理后提高了稳定性,有利于进一步拓宽应用范围。

关键词: 壳聚糖, 薄荷精油, 单凝聚, 微胶囊

Abstract:

In order to develop slow-release aromatic functional materials and fabrics, this paper uses single coacervation method to prepare peppermint essential oil microcapsules. Taking particle size and embedding rate as indexes, the preparation process of peppermint essential oil microcapsules is optimized by single factor method. Scanning electron microscope (SEM) is adopted to observe the surface morphology on microcapsules, and infrared analysis is used to analyze the changes of molecular groups in capsule wall before and after curing, and the slow release performance and thermal stability, etc. of peppermint essential oil microcapsules are determined. The results show that the preparation process of peppermint essential oil microcapsules is as follows: by compounding Span80 and Tween80 as an emulsifier, chitosan with a molecular weight of about 30000 is selected as wall material, and the mass ratio between the core material peppermint oil and the wall material chitosan is 1:1, and glutaraldehyde with a mass fraction of 100% (for chitosan) is added for curing for 1 hour. The average particle size of peppermint essential oil microcapsules is about 2.8 μm, and the embedding rate is up to 66.67%. The retention rate is 65.24% after one month at normal temperature and 76.23% after 2 h at high temperature (120℃). Infrared analysis suggests that chitosan forms a cross-linked structure after curing, and thermogravimetric analysis shows that peppermint essential oil microcapsules have good thermal stability. After microencapsulation, the stability of peppermint essential oil is enhanced, which is beneficial to further expansion of the application scope.

Key words: chitosan, peppermint oil, single coacervation, microcapsules

中图分类号:

TS195.5

王秋萍, 倪张根, 崔慧明, 林涛, 杨云, 张瑞萍. 壳聚糖-薄荷精油微胶囊的制备及其性能[J]. 现代纺织技术, 2022, 30(2): 148-158.

WANG Qiuping, NI Zhanggen, CUI Huiming, LIN Tao, YANG Yun, ZHANG Ruiping. Preparation and properties of chitosan-peppermint oil microcapsules[J]. Advanced Textile Technology, 2022, 30(2): 148-158.

图/表 24

图1 不同乳化剂的微胶囊粒径分布

Fig.1 Particle size distribution of microcapsules with different emulsifiers

图2 不同乳化剂的微胶囊平均粒径和分散指数

Fig.2 Average particle size and PDI of microcapsules with different emulsifiers

表1 不同乳化剂的微胶囊包埋率和平均粒径

Tab.1 Embedding rate and average particle size of microcapsules with different emulsifiers

乳化剂种类	包埋率/%	平均粒径/μm
无乳化剂	47.20	4.9
Tween80	52.15	3.7
Span80	41.30	3.1
Span80、Tween80复合	56.37	2.4

图3 不同分子量壳聚糖的微胶囊粒径分布

Fig.3 Particle size distribution of chitosan microcapsules with different molecular weights

图4 不同分子量壳聚糖的微胶囊平均粒径和分散指数

Fig.4 Average particle size and PDI of chitosan microcapsules with different molecular weights

表2 不同分子量壳聚糖的微胶囊包埋率和平均粒径

Tab.2 Embedding rate and average particle size of chitosan microcapsules with different molecular weights

分子量/万	包埋率/%	平均粒径/μm
3	61.08	1.6
5	46.37	2.4
20	33.30	3.2

表3 不同芯壁比的微胶囊包埋率和平均粒径

Tab.3 Embedding rate and average particle size of microcapsules with different core wall ratios

芯壁比	包埋率/%	平均粒径/μm
1:2	56.03	2.0
1:1	61.08	1.6
2:1	52.27	1.9

图5 不同絮凝剂用量和pH值体系透过率

Fig.5 Transmissivity of the system with different dosage of flocculant and pH value

图6 不同絮凝pH值的微胶囊粒径分布

Fig.6 Particle size distribution of microcapsules at different pH values of flocculation

图7 不同絮凝pH值的微胶囊平均粒径和分散指数

Fig.7 Average particle size and PDI of microcapsules with different pH values of flocculation

表4 不同絮凝剂加入方式微胶囊的包埋率和平均粒径

Tab.4 Embedding rate and average particle size of microcapsules with different flocculant addition methods

絮凝剂加入方式	包埋率/%	平均粒径/μm
正向	65.74	1.7
逆向	41.73	2.3

图8 不同搅拌速度的微胶囊粒径分布

Fig.8 Particle size distribution of microcapsules at different stirring speeds

图9 不同搅拌速度的微胶囊平均粒径和分散指数

Fig.9 Average particle size and PDI of microcapsules at different stirring speeds

表5 不同搅拌速度制备微胶囊包埋率和平均粒径

Tab.5 Embedding rate and average particle size of microcapsules at different stirring speeds

搅拌速度/(r·min^-1)	包埋率/%	平均粒径/μm
500	65.74	2.1
1000	46.28	1.3
1500	43.58	0.9

图10 不同固化pH的微胶囊粒径分布

Fig.10 Particle size distribution of microcapsules with different curing pH values

图11 不同固化pH的微胶囊平均粒径和分散指数

Fig.11 Average particle size and PDI of microcapsules with different curing pH

表6 不同固化pH值的微胶囊包埋率和平均粒径

Tab.6 Embedding rate and average particle size of microcapsules with different curing pH values

pH值	包埋率/%	平均粒径/μm
4	27.38	0.3
7	38.56	0.5
9	65.74	1.7

表7 不同固化温度的微胶囊包埋率和平均粒径

Tab.7 Embedding rate and average particle size of microcapsules at different curing temperatures

温度/℃	包埋率/%	平均粒径/μm
5	65.74	1.7
40	66.67	3.3

图12 不同固化剂用量的微胶囊粒径分布

Fig.12 Particle size distribution of microcapsules with different dosages of curing agent

图13 不同固化剂用量的微胶囊平均粒径和分散指数注:固化剂用量为对壳聚糖重量百分比

Fig.13 Average particle size and PDI of microcapsules with different dosages of curing agent

图14 薄荷微胶囊的扫描电镜图

Fig.14 Scanning electron microscopy of mint microcapsules

图15 壳聚糖和交联后壳聚糖红外图谱

Fig.15 Infrared spectra of chitosan and crosslinked chitosan

图16 不同固化剂用量对芯材保留率的影响

Fig.16 Retention rate of core material with different amounts of curing agent

图17 微胶囊热重

Fig.17 Thermogravimetric analysis of microcapsules

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