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浅谈化学实验中羧甲基壳聚糖的合成方法
壳聚糖(chitosan ,CTS)作为一种至关重要的大分子有机化合物,被广泛应用于化工、医疗、食品制造等各个行业。但是由于壳聚糖性质特殊,除酸外,不溶于水性溶剂,且CTS在浓酸当中还会水解,因此它的实践用途并非十分广泛。故对壳聚糖进行结构修饰,极大程度地改变其溶解性能。 本课题以壳聚糖为原料,在碱性条件下,用氯乙酸对壳聚糖进行化学改性研究,合成具有良好水溶性的羧甲基壳聚糖。其次考察合成条件如反应温度、时间、氯乙酸质量对合成羧甲基壳聚糖的取代度的影响情况。同时也用红外光谱的分析方法测定产物结构及取代度。实验结果表明,反应1h到反应3h间,产品的羧甲基取代度一直增加;反应40℃到反应60℃间,产品的羧甲基取代度先增加再减少;氯乙酸质量从2.0g加到2.8g,产品的羧甲基取代度先增加再减少。结论:取反应时间为2小时,反应温度为50℃,氯乙酸质量为2.4g,可以得到取代度较高的羧甲基壳聚糖。 关键词:壳聚糖;氯乙酸法;取代度;羧甲基壳聚糖 ABSTRACT Chitosan (CTS), as an important macromolecule organic compound, is widely used in chemical industry, medical treatment, food manufacturing and other industries. But because of its special properties, besides acid, it is insoluble in water-borne solvents, and CTS can hydrolyze in concentrated acid, so its practical use is not very extensive. Therefore, the structure modification of chitosan can greatly change its solubility. In this paper, chitosan was used as raw material to synthesize carboxymethyl chitosan with good water solubility by chemical modification of chitosan with chloroacetic acid under alkaline conditions. Secondly, the effects of synthesis conditions such as reaction temperature, time and quality of chloroacetic acid on the degree of substitution of carboxymethyl chitosan were investigated. The structure and degree of substitution of the product were also determined by infrared spectroscopy. The results show that the degree of carboxymethyl substitution of the product increases from 1 h to 3 h, increases first and then decreases from 40 to 60 and the degree of carboxymethyl substitution of the product increases first and then decreases when the mass of chloroacetic acid increases from 2.0 g to 2.8 G. CONCLUSION: Carboxymethyl chitosan with high degree of substitution can be obtained with reaction time of 2 hours, reaction temperature of 50 C and mass of chloroacetic acid of 2.4 G. Key words: chitosan; chloroacetic acid method; degree of substitution; carboxymethyl chitosan
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