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采用微波辐射法,在相转移催化剂四丁基溴化铵作用下,用预先被NaOH碱化的甲壳低聚糖(CHOS)与溴化正丁烷反应制备N-正丁基甲壳低聚糖(C_4-CHOS)。目标产物C_4-CHOS的结构通过FTIR图谱及XRD图谱分析得到验证。实验结果表明,当NaOH与甲壳低聚糖质量比为2∶1、碱化温度70℃、碱化时间60min、反应时间60min、反应温度80℃、溴代正丁烷质量为甲壳低聚糖的6.35倍、四丁基溴化铵与甲壳低聚糖质量比为0.03∶1时,具有较好的综合性能:起泡性为43.33%,稳泡性为87.18%,乳化性为76.74%。C_4-CHOS的临界胶束浓度(CMC)为0.016%,表面张力约为65.3mN/m;亲水亲油平衡值(HLB)测定结果为10.73。同步热分析表明C_4-CHOS在205℃之前都是稳定的。
Microwave irradiation was used to prepare N-n-butyl chitooligosaccharides by chitooligosaccharides (CHOS) alkalized with NaOH and n-butylammonium bromide under the action of phase transfer catalyst tetrabutylammonium bromide C_4-CHOS). The structure of the target product C_4-CHOS was verified by FTIR and XRD patterns. The results showed that when the mass ratio of NaOH to chitooligosaccharides is 2:1, the alkalization temperature is 70 ℃, the alkalization time is 60min, the reaction time is 60min, the reaction temperature is 80 ℃, the mass of n-butyl bromide is chitooligosaccharides 6.35 times. The mass ratio of tetrabutylammonium bromide to chitooligosaccharides is 0.03:1, the foaming property is 43.33%, the foam stability is 87.18% and the emulsifiability is 76.74%. The critical micelle concentration (CMC) of C_4-CHOS was 0.016%, the surface tension was about 65.3mN / m, and the HLB was 10.73. Simultaneous thermal analysis showed that C_4-CHOS was stable before 205 ℃.