Dissertation > Excellent graduate degree dissertation topics show

Research on Phosphorus Oxychloride-Catalyzed Aniline N-Alkylation

Author: WangBo
Tutor: LiXiaoNian
School: Zhejiang University of Technology
Course: Industrial Catalysis
Keywords: phosphorus oxychloride γ-Al2O3 Aniline ethanol catalysis N-ethyl aniline N N-Diethyl aniline
CLC: O643.32
Type: Master's thesis
Year: 2011
Downloads: 75
Quote: 0
Read: Download Dissertation

Abstract


Alkylation of arylamines is one of the important technics to synthesize fine chemicals, there are many synthetic routes and methods. N-alkyl arylamines and there derivatives are important intermediates in the production of dyes, pharmaceuticals, pesticides, petrochemicals and so on. It currently still one of the hot direction of synthetic study. In this study, we have summarized previous work, in view of aniline can not completely transformed in the reaction system of“aniline + ethanol + phosphorus oxychloride”, through the optimization of reaction process, make aniline completely transformed, eventually N-ethyl aniline and N, N-diethyl aniline were synthesized. In a certain extent, reduced the production cost and improved the economic benefit. In view of the above question, the main content of this paper is as follows:1. Establishment of reaction atmosphereAccording to a lot of literature reports, Aromatic amine N-alkylation reaction using alcohols compounds as alkylating agent always under reduction atmosphere, but the reaction system of“aniline + ethanol + phosphorus oxychloride”can not acquire well result. In consideration of the oxidability of phosphorus oxychloride, we adopted nitrogen as shielding gas, reacted under inert atmosphere. The result showed that inert atmosphere greatly improved aniline conversion. Therefore, this paper confirmed nitrogen as shielding gas for experiment.2. Synthesis of N-ethyl aniline and N, N-diethyl anilineUsing phosphorus oxychloride as a catalyst, aniline reacted with ethanol, the optimal reaction condition as follows: V （aniline） : V （ethanol） : V （phosphorus oxychloride） = 55 : 70 : 2, reaction temperature 493 K, N2 pr- essure 4.0 MPa, reaction time 8 h. N, N-diethyl aniline yield of 67.82% with the total yield of N-ethyl aniline and N, N-diethyl aniline of 95% was obtained while the conversion of aniline was 100%.3. Influence of different additives on the reactionThanks toγ-Al2O3 and ZSM-5 are good N-alkylating catalyst, so we addedγ-Al2O3 and ZSM-5 to the reaction system of“aniline + ethanol + phosphorus oxychloride”separately. Well reaction result was acquired uneder the optimal reaction condition as follows: V （aniline） : V （ethanol） : V （phosphorus oxychloride） : m（γ-Al2O3）= 55 : 70 : 2 : 3, reaction temp- erature 493 K, N2 pressure 4.0 MPa, reaction time 8 h. N-ethyl aniline yield of 79.26% with the total yield of N-ethyl aniline and N, N-diethyl aniline of 98% was obtained while the conversion of aniline was 100%.

Related Dissertations

  1. Preparation of Epichlorohydrin from Crude Glycerol of Biodiesel By-product,TQ223.26
  2. Study on the Synthesis and Adsorption Behaviour of Chitosan Derivative,TS254.9
  3. Studies on Prediction Models for Fruit Decay and Shelf-Life of Postharvest Strawberry,TS255.4
  4. Studies on Prediction Models for Fruit Decay and Shelf-Life of Postharvest Chinese Bayberry,S667.6
  5. Synthesis and Reactions of Organo Lithium, Potassium, Magnesium Compounds,O621.13
  6. Physical Modification of the Soybean Protein Concentrate by Alcohol Extraction,TS201.21
  7. Synthesis and Structures of Silyl-bridged Metal Complexes,O627
  8. Synthesis and Asymmetric Catalytic Behaviors of Chiral Imine and Dimines Schiff Bases,O621.3
  9. PtRh / Pt 5 / C Catalyst Preparation, Characterization and Electrocatalytic Oxidation of Ethanol,TM911.4
  10. Construction of an integrated large-scale feed mills with an annual output of 170,000 tons integrated feed mill design and construction,S816
  11. Sulfonamide substitution reaction catalyzed asymmetric,O621.25
  12. Syntheses, Structures and Properties of Transition Metal Complexes Based on Pyridyl Ligands,O627.2
  13. Cp-PMO and Co-PMO: Preparation, Characterization and Catalytic Performance,O643.3
  14. The Experimental Study of Radiofrequency Ablation Combined with Percutaneous Ethanol Injection in Vivo Rabbit Liver,R817.5
  15. Reactions and Catalysis of β-diketiminato Metals Complexes,O643.32
  16. Study on the Solubilities of Chlorobenzene and Copper Sulphate in Subcritical Water and Ethanol in Supcritical Carbon Dioxide,O645.1
  17. Depolymerization of Polybutylene Terephthalate in Subcritical Aqueous Acid Solution and Sub/superctitical Ethanol,O631.3
  18. Study on the Ytterbium Chloride Catalyzed Synthesis of Pyridones and the Synthesis and Application of D-Mannitol Derivative Ligands,O621.36
  19. Study on Hydrolysis of Cellulose by Polyoxometalate,TQ352.1
  20. Degradation of Aniline by Photosynthetic Bacteria,X703
  21. Study on Supramolecular Effect of Cyclodextrin and Alcohol System,O641.3

CLC: > Mathematical sciences and chemical > Chemistry > Physical Chemistry ( theoretical chemistry ),chemical physics > Chemical kinetics,catalysis > Catalytic > Catalytic reaction
© 2012 www.DissertationTopic.Net  Mobile