东北林业大学学报
東北林業大學學報
동북임업대학학보
JOURNAL OF NORTHEAST FORESTRY UNIVERSITY
2013年
12期
84-88,98
,共6页
马艳丽%王海登%方桂珍%李大奇%杨正美
馬豔麗%王海登%方桂珍%李大奇%楊正美
마염려%왕해등%방계진%리대기%양정미
醛基化碱木质素%碱木质素基-g-3-丙烯酰基-7-二乙胺基香豆素%合成
醛基化堿木質素%堿木質素基-g-3-丙烯酰基-7-二乙胺基香豆素%閤成
철기화감목질소%감목질소기-g-3-병희선기-7-이을알기향두소%합성
Alkali lignin aldehyde%Alkali lignin-g-3-propylene acyl-7-diethylamine coumarin%Synthesis
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%。
以堿木質素為原料通過Reimer-Tiemann反應和Knoevenagel 反應“錨”接3-乙酰基-7-二乙胺基香豆素( DEC)閤成堿木質素基-g-3-丙烯酰基-7-二乙胺基香豆素( LDC)。探討瞭氯倣、三甲胺和DEC用量,閤成時間及溫度等因素的影響,併確定其閤成工藝。採用羥基自由基的清除率為指標評價瞭堿木質素基-g-3-丙烯酰基-7-二乙胺基香豆素抗紫外線性能。結果錶明,醛基堿木質素的閤成條件為m(堿木質素)∶m(氯倣)=1∶5、時間1 h、溫度70℃、三甲胺用量為0.3 g,醛基堿木質素得率79.34%、醛基質量分數4.58%、純度為93.07%。LDC的閤成工藝條件為n(醛基)∶n( DEC)=1∶1、時間8 h、溫度70℃,堿木質素基-g-3-丙烯酰基-7-二乙胺基香豆素的得率為90.28%、DEC接枝率為23.96%、純度為94.88%。堿木質素基-g-3-丙烯酰基-7-二乙胺基香豆素對羥基自由基的清除率是83.82%,較堿木質素對羥基自由基的清除率提高瞭90.59%。
이감목질소위원료통과Reimer-Tiemann반응화Knoevenagel 반응“묘”접3-을선기-7-이을알기향두소( DEC)합성감목질소기-g-3-병희선기-7-이을알기향두소( LDC)。탐토료록방、삼갑알화DEC용량,합성시간급온도등인소적영향,병학정기합성공예。채용간기자유기적청제솔위지표평개료감목질소기-g-3-병희선기-7-이을알기향두소항자외선성능。결과표명,철기감목질소적합성조건위m(감목질소)∶m(록방)=1∶5、시간1 h、온도70℃、삼갑알용량위0.3 g,철기감목질소득솔79.34%、철기질량분수4.58%、순도위93.07%。LDC적합성공예조건위n(철기)∶n( DEC)=1∶1、시간8 h、온도70℃,감목질소기-g-3-병희선기-7-이을알기향두소적득솔위90.28%、DEC접지솔위23.96%、순도위94.88%。감목질소기-g-3-병희선기-7-이을알기향두소대간기자유기적청제솔시83.82%,교감목질소대간기자유기적청제솔제고료90.59%。
Alkali lignin-g-3-propylene acyl-7-diethylamine coumarin ( LDC) was synthesized through Reimer-Tiemann and Kno-evenagel 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 syn-thetic 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 alde-hyde/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%, high-er 90.59%than that of alkali lignin.