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愈创木基型多聚体木素模型物合成工艺条件的优化
Optimization of Synthesis Process Conditions of Polymeric Guaiacyl-type Lignin Model Compound
【摘要】 采用正交试验法研究了β-O-4结构愈创木基型多聚体木素模型物合成工艺条件,优化得出适宜的聚合条件为:时间4.5h,反应温度55℃,溴代乙酰基愈创木酚在二甲基甲酰胺中的质量浓度22%,K2CO3与溴代乙酰基愈创木酚质量比0.7;适宜的还原条件为:时间10h,反应温度40℃,未还原聚合物在二甲基亚砜中的质量浓度1.6%,NaBH4与未还原聚合物质量比1.4。聚合过程中反应时间影响最大,其次为反应温度、溴代乙酰基愈创木酚在二甲基甲酰胺中的质量浓度,最后是K2CO3与溴代乙酰基愈创木酚质量比;还原过程中未还原聚合物在二甲基亚砜中的质量浓度影响最大,其次为NaBH4与未还原聚合物质量比、反应时间,最后是温度。另外,采用1H-NMR表征了最优条件下合成所得的木素模型聚合物。
【Abstract】 The optimum conditions and influential factors of synthesis process of polymeric guaiacyl-type lignin model compound linked by β-O-4 were studied.The optimum conditions of polymerization were: time 4.5h,temperature 55℃,mass concentration of bromoacetyl guaiacol in N,N-dimethyl formamide(DMF) 22%,mass ratio of potassium carbonate to bromoacetyl guaiacol 0.7;the optimum conditions of reduction were: time 10h,temperature 40℃,mass concentration of unreduced polymer in dimethyl sulfoxide(DMSO) 1.6%,mass ratio of sodium borohydride to unreduced polymer 1.4.The influence of factors on polymerization: time>temperature>mass concentration of bromoacetyl guaiacol in DMF>mass ratio of potassium carbonate to bromoacetyl guaiacol;the influence of factors on reduction: mass concentration of unreduced polymer in DMSO>mass ratio of sodium borohydride to unreduced polymer>time > temperature.The polymeric lignin model compound synthesized at the optimal conditions were characterized with 1H-NMR.
- 【文献出处】 造纸科学与技术 ,Paper Science & Technology , 编辑部邮箱 ,2009年01期
- 【分类号】TS712
- 【被引频次】11
- 【下载频次】149