摘要
以碱木质素为原料通过Reimer-Tiemann反应和Knoevenagel反应"锚"接3-乙酰基-7-二乙胺基香豆素(DEC)合成碱木质素基-g-3-丙烯酰基-7-二乙胺基香豆素(LDC)。探讨了氯仿、三甲胺和DEC用量,合成时间及温度等因素的影响,并确定其合成工艺。采用羟基自由基的清除率为指标评价了碱木质素基-g-3-丙烯酰基-7-二乙胺基香豆素抗紫外线性能。结果表明,醛基碱木质素的合成条件为m(碱木质素)∶m(氯仿)=1∶5、时间1 h、温度70℃、三甲胺用量为0.3 g,醛基碱木质素得率79.34%、醛基质量分数4.58%、纯度为93.07%。LDC的合成工艺条件为n(醛基)∶n(DEC)=1∶1、时间8 h、温度70℃,碱木质素基-g-3-丙烯酰基-7-二乙胺基香豆素的得率为90.28%、DEC接枝率为23.96%、纯度为94.88%。碱木质素基-g-3-丙烯酰基-7-二乙胺基香豆素对羟基自由基的清除率是83.82%,较碱木质素对羟基自由基的清除率提高了90.59%。
Alkali lignin-g-3-propylene acyl-7-diethylamine coumarin（ LDC） was synthesized through Reimer-Tiemann and Knoevenagel reaction from alkali lignin. 3-acetyl-7-diethylamine coumarin（ DEC） was attached to alkali lignin. Factors of the amount of chloroform,trimethylamine and DEC as well as the reaction time and temperature were investigated and the synthetic technology was determined. UV resistance of LDC was evaluated by the scavenging rate of hydroxyl radical. The suitable synthetic technology of alkali lignin aldehyde is alkali 1 ∶ 5 of lignin / chloroform,0. 3 g of trimethylamine（ 35% of aqueous solution）,one hour of reaction time and 70 ℃ of reaction temperature,and the aldehyde content of alkali lignin aldehyde is 4. 58%,the purity is 79. 34% and the yield is 93. 07%. The synthetic technology of LDC is 1 ∶ 1 of aldehyde / DEC at molar ratio,eight hours of reaction time and 70 ℃ of reaction temperature,and the DEC content of LDC is 23. 96%,the purity is 90. 28% and the yield is 94. 88%. The hydroxyl radical scavenging rate of LDC is 83. 82%,higher 90. 59% than that of alkali lignin.
出处
《东北林业大学学报》
CAS
CSCD
北大核心
2013年第12期84-88,98,共6页
Journal of Northeast Forestry University
基金
国家林业局公益项目(200904072)
中央高校基本科研业务费专项资金(DL09BB30)
