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›› 2006, Vol. 6 ›› Issue (5): 789-793.

• 生化工程专栏 • 上一篇    下一篇

微波间歇法快速制备高粘均分子量和高脱乙酰度的壳聚糖

李巧霞,宋宝珍,仰振球,樊红雷   

  1. 中国科学院过程工程研究所
  • 出版日期:2006-10-20 发布日期:2006-10-20

Preparation of Chitosan with High Viscosity-average Molecular Weight and High Degree of Deacetylation by Rapid Interim Microwave Heating Method

LI Qiao-xia,SONG Bao-zhen,YANG Zhen-qiu,FAN Hong-lie   

  1. 中国科学院过程工程研究所
  • Online:2006-10-20 Published:2006-10-20

摘要: 使用微波间歇法可快速制备高脱乙酰度和高粘均分子量的壳聚糖. 单因素实验确定的工艺条件为微波功率800 W,将45%(w)的氢氧化钠溶液与250~380 mm的20 g甲壳素粉以8:1的体积比混合,在100℃下反应10 min,洗涤、微波干燥后在相同条件下再反应1次,共20 min,可制得脱乙酰度为94.5%、粘均分子量1.48×106的白色壳聚糖粉末. 其他制备条件相同,使用电加热法间歇处理甲壳素粉3次,反应共5 h,可以得到脱乙酰度为96.2%、粘均分子量为3.8×105的褐色壳聚糖粉末. 微波间歇法所制壳聚糖的结晶度高,内部有规整的有序结构,用它制备的膜致密,性能优于用电加热法所制壳聚糖制备的膜.

关键词: 壳聚糖, 粘均分子量, 脱乙酰度, 微波间歇法

Abstract: Chitosan with high degree of deacetylation (DD=94.5%) and high viscosity-average molecular weight (Mv=1.48′106) was prepared by rapid interim microwave heating method. Influential factors such as particle size of chitin, concentration of sodium hydroxide solution, ratio of liquid to solid, reaction temperature, reaction time and reaction cycle were investigated. 45%(w) sodium hydroxide solution was mixed with 20 g chitin with particle size 250~380 mm by volumetric ratio of liquid to solid 8:1 and reacted for 10 min at 100℃ under microwave (800 W, 2450 MHz). Then, the mixture was treated by washing and drying to obtain chitosan with DD of 72.3% and Mv of 2.06×106. Finally, under the same reaction conditions, this chitosan was treated with 45% NaOH solution under microwave for another 10 min to obtain chitosan with DD of 94.5% and Mv of 1.48×106. Compared with traditional interim electricity heating method, the proposed method not only shortened the reaction time from 5 h to 20 min but also improved the molecular weight from 3.8×105 to 1.48×106 which has close degree of deacetylation. FT-IR and XRD spectra showed that the chitosan with high DD (94.5%) and high Mv (1.48×106) had high crystallinity and order structure and the film made of the chitosan had better properties than the film made from the chitosan with 96.2% DD and 3.8×105 Mv produced by interim electricity heating method.

Key words: chitosan, viscosity-average molecular weight, degree of deacetylation, interim microwave heating method