N-异冰片基丙烯酰胺的合成研究
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TQ236

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松香松节油精深加工技术集成与示范(2018YFD0600402)


Study on Synthesis of N-Isobornyl Acrylamide
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Integration and demonstration of rosin turpentine deep processing technology(2018YFD0600402)

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    摘要:

    以丙烯腈和天然可再生资源莰烯为原料,在无溶剂条件下催化合成了N-异冰片基丙烯酰胺(NIBAM)。探索了催化剂种类及用量、物料配比、反应温度、反应时间对反应选择性和NIBAM得率的影响。采用正交实验确定了适宜的合成工艺条件:以FeCl3为催化剂,催化剂用量为10%(以总物料质量计),莰烯与丙烯腈和水的摩尔比为1:3:1,反应温度120 ℃,反应时间12 h。在此条件下,反应选择性和NIBMA的得率分别为97.6%和90.3% 。采用HRMS、FT-IR和NMR等分析技术对产物结构进行了表征。

    Abstract:

    N-Isobornyl Acrylamide (NIBAM) was synthesized from acrylonitrile and natural renewable resource camphene under solvent-free conditions. Effects of the types and the dosages of catalysts, molar ratio of camphene to acrylonitrile and water, reaction temperature and reaction time on the reaction selectivity and the yield of NIBAM were investigated, and the optimum reaction conditions were determined by or-thogonal tests as follows: the molar ratio of camphene to acrylonitrile and water was 1:3:1; FeCl3 was adopted as the catalyst, and the amount of FeCl3 was 10%; reaction temperature 120 ℃, reaction time 12 h. The reaction electivity and the average yield of NIBAM under the aforesaid conditions were 90.3% and 97.6%, respectively. The structure of NIBAM was determined by HRMS, FT-IR and NMR.

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周新成,陶钰,张成龙,徐徐,杨益琴,王石发. N-异冰片基丙烯酰胺的合成研究[J].精细化工,2020,37(4):

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  • 收稿日期:2019-08-05
  • 最后修改日期:2019-10-09
  • 录用日期:2019-10-13
  • 在线发布日期: 2020-03-23
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