光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
4期
1031-1034
,共4页
刘晓欢%王春鹏%王基夫%许玉芝%储富祥
劉曉歡%王春鵬%王基伕%許玉芝%儲富祥
류효환%왕춘붕%왕기부%허옥지%저부상
木质素模型化合物%二氢丁香酚%丙烯酰氯%聚合活性
木質素模型化閤物%二氫丁香酚%丙烯酰氯%聚閤活性
목질소모형화합물%이경정향분%병희선록%취합활성
Lignin mode compound%Dihydroeugenol%Acryloyl chloride%Polymerization activity
以木质素模型化合物二氢丁香酚(DH)为原料,利用丙烯酰氯(AC)进行接枝改性制备丙烯酸二氢丁香酚酯(DH-AC)。采用傅里叶变换红外光谱(FTIR)、气相色谱-质谱联用仪(GC-MS)、核磁共振氢谱(1H-NMR)和凝胶色谱(GPC)等分析手段研究了丙烯酸二氢丁香酚酯的结构以及聚合活性。FTIR结果表明二氢丁香酚经过丙烯酰氯改性后,3495cm-1为酚羟基伸缩振动吸收峰完全消失,在1762cm-1处有新的酯基峰生成,同时在1631和981cm-1出现CC的特征吸收峰,表明丙烯酸酯官能团已成功接枝到二氢丁香酚上。1H-NMR分析结果显示DH-AC在δ=5.6的酚羟基质子峰完全消失,同时在δ=6.0,6.4和6.7出现了三个不同的质子峰,这主要是由于乙烯基CHCH2结构的引入,该结果进一步证明目标产物丙烯酸二氢丁香酚酯结构的正确性。GC-MS结果表明目标产物丙烯酸二氢丁香酚酯的纯度为98.63%。GPC结果显示DH-AC在偶氮二异丁氰(AIBN)作为引发剂的存在下,DH-AC可以发生聚合反应,均聚物相对分子质量结果为:Mw(37400),Mn(23400),Mw/Mn=1.60,表明丙烯酸二氢丁香酚酯单体具有高的聚合活性。丙烯酸二氢丁香酚酯(DH-AC)的制备和性能研究为开发新型木质素基高分子材料奠定了理论基础。
以木質素模型化閤物二氫丁香酚(DH)為原料,利用丙烯酰氯(AC)進行接枝改性製備丙烯痠二氫丁香酚酯(DH-AC)。採用傅裏葉變換紅外光譜(FTIR)、氣相色譜-質譜聯用儀(GC-MS)、覈磁共振氫譜(1H-NMR)和凝膠色譜(GPC)等分析手段研究瞭丙烯痠二氫丁香酚酯的結構以及聚閤活性。FTIR結果錶明二氫丁香酚經過丙烯酰氯改性後,3495cm-1為酚羥基伸縮振動吸收峰完全消失,在1762cm-1處有新的酯基峰生成,同時在1631和981cm-1齣現CC的特徵吸收峰,錶明丙烯痠酯官能糰已成功接枝到二氫丁香酚上。1H-NMR分析結果顯示DH-AC在δ=5.6的酚羥基質子峰完全消失,同時在δ=6.0,6.4和6.7齣現瞭三箇不同的質子峰,這主要是由于乙烯基CHCH2結構的引入,該結果進一步證明目標產物丙烯痠二氫丁香酚酯結構的正確性。GC-MS結果錶明目標產物丙烯痠二氫丁香酚酯的純度為98.63%。GPC結果顯示DH-AC在偶氮二異丁氰(AIBN)作為引髮劑的存在下,DH-AC可以髮生聚閤反應,均聚物相對分子質量結果為:Mw(37400),Mn(23400),Mw/Mn=1.60,錶明丙烯痠二氫丁香酚酯單體具有高的聚閤活性。丙烯痠二氫丁香酚酯(DH-AC)的製備和性能研究為開髮新型木質素基高分子材料奠定瞭理論基礎。
이목질소모형화합물이경정향분(DH)위원료,이용병희선록(AC)진행접지개성제비병희산이경정향분지(DH-AC)。채용부리협변환홍외광보(FTIR)、기상색보-질보련용의(GC-MS)、핵자공진경보(1H-NMR)화응효색보(GPC)등분석수단연구료병희산이경정향분지적결구이급취합활성。FTIR결과표명이경정향분경과병희선록개성후,3495cm-1위분간기신축진동흡수봉완전소실,재1762cm-1처유신적지기봉생성,동시재1631화981cm-1출현CC적특정흡수봉,표명병희산지관능단이성공접지도이경정향분상。1H-NMR분석결과현시DH-AC재δ=5.6적분간기질자봉완전소실,동시재δ=6.0,6.4화6.7출현료삼개불동적질자봉,저주요시유우을희기CHCH2결구적인입,해결과진일보증명목표산물병희산이경정향분지결구적정학성。GC-MS결과표명목표산물병희산이경정향분지적순도위98.63%。GPC결과현시DH-AC재우담이이정청(AIBN)작위인발제적존재하,DH-AC가이발생취합반응,균취물상대분자질량결과위:Mw(37400),Mn(23400),Mw/Mn=1.60,표명병희산이경정향분지단체구유고적취합활성。병희산이경정향분지(DH-AC)적제비화성능연구위개발신형목질소기고분자재료전정료이론기출。
Dihydroeugenol acrylate was synthesized by the reaction of acryloyl chloride (AC ) with lignin mode compound di-hydroeugenol (DH) in the presence of TEA and characterized by using FTIR ,GC/MS ,1 H-NMR and GPC. FTIR spectra showed that ,after the esterification with acryloyl chloride ,the intensity of stretching vibration peak of O - H (centered at 3 495 cm -1 ) of DH was disappeared. At the same time ,a new peak appeared at 1 762 cm-1 which was assigned to ester group. Addi-tionally ,the appearance of 1 631 and 981 cm -1 were attributed to the carbon-carbon double bond confirmed the success in the synthesis of DH-AC. 1 H-NMR spectra showed that ,after the esterification with acryloyl chloride ,the proton signal of O- H at 5.5 ppm was disappeared. Meanwhile ,the appearance of three new proton signals at 6.0 ppm ,6.4 and 6.7 ppm ,attributed to the vinylic protons ,indicated that acryloyl chloride was successfully grafted onto DH. The results further confirmed the struc-tures of the DH-AC. GC-MS results showed the DH-AC had a high purity of 98.63%. GPC results showed that dihydroeugenol acrylate could polymerize in the 1 ,4-dioxane using a thermal initiator of AIBN (2.0 Wt% of total monomers). The weight aver-age molecular mass (Mw) of the homopolymer is 37 400 g · mol-1 ,and the number average molecular mass is 23 400 g · mol-1 with a polydispersity index Mw/Mn of 1.60 ,indicating that the dihydroeugenol acrylate has high polymerization activity .This strategy provides a novel approach for extending the comprehensive utilization of lignin .