Chinese Journal of Applied Chemistry ›› 2020, Vol. 37 ›› Issue (4): 433-439.DOI: 10.11944/j.issn.1000-0518.2020.04.190251

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An Efficient Method for Improved Preparation of C.I. Pigment Red 177 Intermediate

ZHANG Tianyongab,Ren Zhongjinga,LI Bina*(),JIANG Shuanga*(),SHI Jixinga,SHI Zhiqiangc,LÜ Dongjunde   

  1. aTianjin Key Laboratory of Applied Catalysis Science and Technology,School of Chemical Engineering and Technology,Tianjin University,Tianjin 300354,China
    bCollaborative Innovation Center of Chemical Science and Engineering(Tianjin),Tianjin 300072,China
    cDepartment of Chemical Engineering,Renai College,Tianjin University,Tianjin 301636,China
    dYuhong Pigment Co. Ltd, Dezhou,Shandong 253000,China
    eShangdong Engineering Technology Research Center for the Whole Process Control of Organic Pigment's Cleaner Production, Dezhou,Shandong 253000,China
  • Accepted:2020-02-18 Published:2020-04-01 Online:2020-04-10
  • Contact: LI Bin,JIANG Shuang
  • Supported by:
    Supported by the National Natural Science Foundation of China(No.21908161), the Tianjin Science and Technology Innovation Platform Program(No.14TXGCCX00017), the Natural Science Foundation of Tianjin(No.16JCYBJC20800)

Abstract:

The effect of batch addition of the catalyst (copper powder) on the reaction rate during the synthesis of 4,4'-diamino-1,1'-dianthraquinone-3,3'-disulfonic acid (DAS) was investigated systematically. The results indicate that 55 ℃ is the preferred reaction temperature. Copper powder and sodium bromate with a mass ratio of of 2:5 are first added, and the second portion of catalyst with a mass ratio of 1:5 copper powder to sodium bromate is then added during the reaction. The reaction time could be saved for 2~3 h compared to adding copper powder at one time (the mass ratio of copper powder to sodium bromate is 3:5). The copper salt mixed in DAS could be removed efficiently by addition of citric acid during the preparation process, which can improve the purity of DAS. When the mass ratio of copper powder to citric acid is 6:1, the content of copper salt in DAS is less than 0.001%. In addition, the influence of the residual amount of the filtrate after distillation on the yield of DAS is also explored and the yield of DAS is above 95% when the remaining amount of filtrate is 20 mL. The results of this study also indicate that to further improve the yield of the reaction, more efficient catalyst is needed.

Key words: C.I. Pigment red 177 intermediate, catalyst, copper powder, citric acid