熔融结晶法提纯邻碘苯胺工艺
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摘要
利用熔融结晶法对邻碘苯胺混合物进行分离提纯,考察并分析了降温速率、结晶终温、养晶时间、升温速率和发汗终温对产品收率和纯度的影响。邻碘苯胺质量分数为70. 95%时的最佳结晶工艺:以降温速率0. 3 K/5 min降温到结晶终温301. 15 K,使固体熔融液结晶,养晶时间为2 h;再升温发汗,升温速率为0. 2 K/5 min,升到发汗终温至313. 15 K结束。实验得到质量分数为99. 07%的邻碘苯胺,产品收率为61. 75%。
Crude o-iodoaniline mixtures are separated and purified by melt crystallization. Effects of cooling rate,final temperature in the crystallization process,crystal growing time,heating rate and final temperature in the sweating process on the yield and purity of the product are investigated and analyzed.The results show that 99. 07% o-iodoaniline can be obtained with a yield of 61. 75% when the initial concentration of o-iodoaniline in crude mixtures is 70. 95%,the cooling rate is 0. 3 K·min~(-1),the final crystallization temperature is 301. 15 K,crystal growing time is 2 h and the heating rate in sweating process is 0. 2 K·min~(-1) and the final sweating temperature is 313. 15 K.
Crude o-iodoaniline mixtures are separated and purified by melt crystallization. Effects of cooling rate,final temperature in the crystallization process,crystal growing time,heating rate and final temperature in the sweating process on the yield and purity of the product are investigated and analyzed.The results show that 99. 07% o-iodoaniline can be obtained with a yield of 61. 75% when the initial concentration of o-iodoaniline in crude mixtures is 70. 95%,the cooling rate is 0. 3 K·min~(-1),the final crystallization temperature is 301. 15 K,crystal growing time is 2 h and the heating rate in sweating process is 0. 2 K·min~(-1) and the final sweating temperature is 313. 15 K.
引文
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[7]史成玲,刘秀杰,孟杰,等.邻碘和邻溴苯胺的合成[J].天津理工大学学报,2010,26(6):60-62.
[8]朱静,李天祥,张耀,等.一种邻碘苯胺的制备方法:CN,106542958A[P].2017-3-29.
[9]孙少文,杨光军,丁建生,等.熔融结晶工艺开发[J].化学工程,2008,36(12):18-20.
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[11]Wynn Nicholas P.Separate organics by melt crystallization[J].Chemical Engineering Progress,1992,88(3):52-60.
[12]Wellinghoff G,Wintermantel K.Melt crystallization theoretical premises and technicallimitations[J].International Chemical Engineering,1994,34(1):17-27.
[13]Berry David A,Ng Ka M.Synthesis of crystallization-distillation hybrid separation process[J].AIChE,1997,43(7):1751-1762.
[14]许奎,朱静,刘博文,等.邻碘苯胺与对碘苯胺固液相图测定及数据关联[J].化学工程,2018,46(1):43-45.
[2]Kabalka G W,Wang L,Namboodiri V,et al.Rapid microwave-enhanced,solventless Sonogashira coupling reaction on alumina[J].Tetrahedron Letters,2000,41(27):5151-5154.
[3]Deng H,Li Z,Ke F,et al.Cu-catalyzed three-component synthesis of substituted benzothiazoles in water[J].Chemistry-A European Journal,2012,18(16):4840-4843.
[4]谭文.邻卤苯胺与芳香腈环化反应合成苯丙咪唑衍生物及其应用研究[D].成都:四川师范大学,2014.
[5]Alonso D A,Njera C,Pacheco M C.Oxime-derived palladium complexes as very efficient catalysts for the heck-mizorokireaction[J].Advanced Synthesis&Catalysis,2002,344(2):172-183.
[6]Xu K,Zhu J,Li T.Measurement and correlation of dissolution equilibrium of o-iodoaniline and p-iodoanilinein pure solvents[J].Journal of Chemical&Engineering Data,2018,63(1):217-224.
[7]史成玲,刘秀杰,孟杰,等.邻碘和邻溴苯胺的合成[J].天津理工大学学报,2010,26(6):60-62.
[8]朱静,李天祥,张耀,等.一种邻碘苯胺的制备方法:CN,106542958A[P].2017-3-29.
[9]孙少文,杨光军,丁建生,等.熔融结晶工艺开发[J].化学工程,2008,36(12):18-20.
[10]李士雨,秦文军.熔融结晶技术用于制备高纯对二氯苯[J].化工装备技术,1994,(4):1-4.
[11]Wynn Nicholas P.Separate organics by melt crystallization[J].Chemical Engineering Progress,1992,88(3):52-60.
[12]Wellinghoff G,Wintermantel K.Melt crystallization theoretical premises and technicallimitations[J].International Chemical Engineering,1994,34(1):17-27.
[13]Berry David A,Ng Ka M.Synthesis of crystallization-distillation hybrid separation process[J].AIChE,1997,43(7):1751-1762.
[14]许奎,朱静,刘博文,等.邻碘苯胺与对碘苯胺固液相图测定及数据关联[J].化学工程,2018,46(1):43-45.