Synthesis of High Purity p-Phenylenediamine from p-Nitroaniline by Catalytic Hydrogenation

Pd/C촉매하 파라니트로아닐린 수소첨가에 의한 고순도 파라페닐렌디아민의 합성공정

  • Received : 1999.10.11
  • Accepted : 1999.11.22
  • Published : 1999.12.10

Abstract

Optimum conditions of the hydrogenation of PNA to pure PPD were determined in a three-phase slurry reactor with suspended Pd/C catalyst particles. Minimization of mass transfer resistances at the interfaces of both gas-liquid and liquid-catalyst particles and control of overall reaction rate on catalyst surface leaded to decrease the hydrogen starvation on reaction active sites and to reduce the side reactions during hydrogenation. The optimum temperature, pressure, and catalysst concentration were confirmed to be in the range of $60^{\circ}C$, 60~70 psig, and 1~2 g-cat/L, respectively. Reaction rate was zero order with respect to the concentration of PNA and 1st order with respect to the pressure of hydrogen(P). Overall rate expression of the reaction was $R_A=6.44{\times}10^6{\cdot}H{\cdot}P{\cdot}m{\cdot}$exp(-4659/T) where H is constant, m is concentration of catalyst, and T is temperature.

Keywords

hydrogenation;PNA;PPD;slurry-reactor;Pd/C catalyst

References

  1. 수첨실험 12보 반응속도 및 제품품질의 검토 일본화약(주) 정밀화학 연구부
  2. J. Am. Chem. Soc. v.81 H. C. Yao;P. H. Emmett
  3. J. Appl. Chem. Biotech. v.22 G. J. K. Acres;B. J. Cooper
  4. Elements of Chemical Reaction Engineering H. S. Fogler
  5. Catalysis Organic Synthesis A. J. Bird;D. T. Thompson(Johnson Matthey)
  6. Catalyst Technical Information Johnson Matthey Catalog
  7. Section of Catalysis Uniroyal Incorporation H. Greenfield
  8. Chem. Eng. Sci. v.41 R. A. rajadhyksa;S. L. Karwa
  9. 고순도 PPD 연구보고서 조철군;김종수;한기도
  10. Chem. Eng. Sci. v.21 T. K. Sherwood;E. J. Farkas
  11. Encyclopedia of Chemical Technology v.2 Kirk-Othmer
  12. 화학공학 v.30 김철웅;김범식;고재천;이정민