食品科学 ›› 2024, Vol. 45 ›› Issue (1): 173-180.doi: 10.7506/spkx1002-6630-20230316-163

• 食品工程 • 上一篇    

壳聚糖微花的制备及影响其形貌的因素

焦思宇,许丁予,姚先超,何丽欣,林日辉   

  1. (广西民族大学化学化工学院,林产化学与工程国家民委重点实验室暨广西林产化学与工程重点实验室,广西林产化学与工程协同创新中心,广西 南宁 530006)
  • 发布日期:2024-02-05
  • 基金资助:
    国家自然科学基金地区科学基金项目(21766004);广西自然科学基金项目(2019GXNSFAA185008); 广西高校中青年教师科研基础能力提升项目(2023KY0175)

Preparation of Chitosan Microflower and Factors Affecting Its Morphology

JIAO Siyu, XU Dingyu, YAO Xianchao, HE Lixin, LIN Rihui   

  1. (State Ethnic Affairs Commission Guangxi Key Laboratory of Chemistry and Engineering of Forest Products, Guangxi Collaborative Innovation Center for Chemistry and Engineering of Forest Products, School of Chemistry and Chemical Engineering, Guangxi Minzu University, Nanning 530006, China)
  • Published:2024-02-05

摘要: 以壳聚糖(chitosan,CS)为原料,在其溶解过程中通过超声和过氧化氢对其进行辅助溶解,之后通过离子交联法,将三聚磷酸钠(sodium tripolyphosphate,TPP)由下而上地注入到CS溶液中,并通过冷冻干燥得到了壳聚糖微花(chitosan microflower,CSMF),并对其进行一系列表征,研究影响其成花的因素。结果发现CSMF粒径在1~2 μm;CSMF的傅里叶红外变换光谱在532 cm-1出现了磷酸根基团的振动峰;CSMF的晶型由CS的半结晶结构变为了水合多晶型结构;CSMF的X射线光电子能谱结果显示其产生了C—N+键;而热重分析结果显示CSMF的热稳定性较CS稍有降低;并且发现预处理方式、超声时间、CS溶液温度和CS与TPP质量比会影响CSMF的花状结构,而超声功率和过氧化氢添加量不会影响其花状结构,进而推测其成花机理为将原CS降解成在一定分子质量范围内的短长链CS,然后在一定的温度下TPP与降解后相对较长的CS链交联形成微花结构的底座,与降解后相对较短的CS链交联形成纳米片,最后再通过CS结构上面的—NH3+与磷酸根离子之间的相互作用,将纳米片自组装到底座上,进而生成了微花结构。

关键词: 壳聚糖;三聚磷酸钠;壳聚糖微花

Abstract: Chitosan (CS) was dissolved with the aid of ultrasound and hydrogen peroxide treatment. Then, sodium tripolyphosphate (TPP) was introduced as a crosslinker into CS solution from bottom to top. Finally, chitosan microflower (CSMF) was obtained by collecting the resulting precipitate and freeze-drying it. CSMF was characterized and the factors affecting its formation were studied. The results showed that the size of CSMF was 1–2 μm in diameter. The Fourier transform infrared (FTIR) spectrum of CSMF showed a vibration peak of phosphate group at 532 cm-1. The crystal form of CS changed from semi-crystalline structure to hydrated polycrystalline structure after conversion into CSMF. X-ray photoelectron spectroscopy (XPS) showed that CSMF produced C-N+ bond, and thermogravimetric analysis (TGA) showed that the thermal stability of CSMF was slightly lower than that of CS. Also, it was found that pretreatment method, ultrasonic time, CS solution temperature and CS/TPP ratio (m/m) but not ultrasound power or hydrogen peroxide addition could affect the flower-shaped structure of CSMF. Furthermore, it was inferred that the formation mechanism of CSMF was related to that fact that after the degradation of CS into short- or long-chain CS within a certain molecular mass range, relatively longer and shorter degraded CS chains were crosslinked by TPP to respectively form the pedestal of the microflower structure and nanosheets which were self-assembled on the substate through the interaction between the –NH3+ and phosphate ions in the structure of CS.

Key words: chitosan; sodium tripolyphosphate; chitosan microflower

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