陕西科技大学学报(自然科学版)
陝西科技大學學報(自然科學版)
협서과기대학학보(자연과학판)
JOURNAL OF SHAANXI UNIVERSITY OF SCIENCE & TECHNOLOGY
2015年
4期
60-64
,共5页
王学川%任静%强涛涛%王晓芹
王學川%任靜%彊濤濤%王曉芹
왕학천%임정%강도도%왕효근
二乙醇胺%氯丙烯%N,N-二(2-羟乙基)-2-氨基丙烯%合成
二乙醇胺%氯丙烯%N,N-二(2-羥乙基)-2-氨基丙烯%閤成
이을순알%록병희%N,N-이(2-간을기)-2-안기병희%합성
diethanolamine%allylchloride%N,N-bis(2-hydroxyethyl)-2-amine-propenyl%syn-t hesis
以二乙醇胺和氯丙烯为原料,在碱性条件下,控制温度、时间和摩尔比反应生成N,N‐二(2‐羟乙基)‐2‐氨基丙烯,由核磁氢谱(1 H‐NMR)、红外光谱(FT‐IR)、元素分析、XRD表征了合成产物的结构和结晶性,用热重分析仪表征了产物的热稳定性.根据产物中叔胺的含量来确定最佳的合成工艺:反应温度为50℃,反应时间为70 min ,单体的摩尔比为n(二乙醇胺)∶n(氯丙烯)=1∶1.1,目标产物的产率可达到96%以上.
以二乙醇胺和氯丙烯為原料,在堿性條件下,控製溫度、時間和摩爾比反應生成N,N‐二(2‐羥乙基)‐2‐氨基丙烯,由覈磁氫譜(1 H‐NMR)、紅外光譜(FT‐IR)、元素分析、XRD錶徵瞭閤成產物的結構和結晶性,用熱重分析儀錶徵瞭產物的熱穩定性.根據產物中叔胺的含量來確定最佳的閤成工藝:反應溫度為50℃,反應時間為70 min ,單體的摩爾比為n(二乙醇胺)∶n(氯丙烯)=1∶1.1,目標產物的產率可達到96%以上.
이이을순알화록병희위원료,재감성조건하,공제온도、시간화마이비반응생성N,N‐이(2‐간을기)‐2‐안기병희,유핵자경보(1 H‐NMR)、홍외광보(FT‐IR)、원소분석、XRD표정료합성산물적결구화결정성,용열중분석의표정료산물적열은정성.근거산물중숙알적함량래학정최가적합성공예:반응온도위50℃,반응시간위70 min ,단체적마이비위n(이을순알)∶n(록병희)=1∶1.1,목표산물적산솔가체도96%이상.
The N ,N‐bis(2‐hydroxyethyl)‐2‐amino‐propenyl was prepared by using diethano‐lamine and allyl chloride as raw materials under alkaline conditions .According to the content of the tertiary amine the best synthesis conditions were determined .The reaction temperature was 50 ℃ ,the reaction time was 70 min ,the molar ratio of monomers was n(diethanolamine)∶ n(allyl chloride) = 1∶1 .1 ,the yield of target product was above 96% .The structure and crystallinity of product was characterized by means of 1 H‐NMR spectrum (1 H‐NMR) ,infra‐red spectroscopy (FT‐IR) ,elemental analysis and X‐ray diffraction .The thermal stability of the product was characterized through thermal gravimetric analysis instrument .