Selective phenol methylation to 2,6-dimethylphenol in a fluidized bed of iron-chromium mixed oxide catalyst with o–cresol circulation

Chemistry Central Journal

Witold Żukowski¹  Gabriela Berkowicz¹  Jerzy Baron¹  Stanisław Kandefer¹  Dariusz Jamanek²  Stefan Szarlik²  Zbigniew Wielgosz²  Maria Zielecka² 

[1] Cracow University of Technology, Faculty of Chemical Engineering and Technology, ul. Warszawska 24, Cracow, 31-155, Poland

[2] Industrial Chemistry Research Institute, ul. Rydygiera 8, Warsaw, 01-793, Poland

关键词: Iron-chromium catalyst;    Fluidized bed;    2,6-dimethylphenol;   

Others  :  1082192
DOI  :  10.1186/s13065-014-0051-6

 received in 2014-04-25, accepted in 2014-08-04,  发布年份 2014

【 摘 要 】

Background

2,6-dimethylphenol (2,6-DMP) is a product of phenol methylation, especially important for the plastics industry. The process of phenol methylation in the gas phase is strongly exothermic. In order to ensure good temperature equalization in the catalyst bed, the process was carried out using a catalyst in the form of a fluidized bed - in particular, the commercial iron-chromium catalyst TZC-3/1.

Results

Synthesis of 2,6-dimethylphenol from phenol and methanol in fluidized bed of iron-chromium catalyst was carried out and the fluidization of the catalyst was examined. Stable state of fluidized bed of iron-chromium catalyst was achieved. The measured velocities allowed to determine the minimum flow of reactants, ensuring introduction of the catalyst bed in the reactor into the state of fluidization. Due to a high content of o-cresol in products of 2,6-dimethylphenol synthesis, circulation in the technological node was proposed. A series of syntheses with variable amount of o-cresol in the feedstock allowed to determine the parameters of stationary states.

Conclusion

A stable work of technological node with o-cresol circulation is possible in the temperature range of350-380°C, and o-cresol_in/phenol_in molar ratio of more than 0.48. Synthesis of 2,6-DMP over the iron-chromium catalyst is characterized by more than 90% degree of phenol conversion. Moreover, the O-alkylation did not occur (which was confirmed by GC-MS analysis). By applying o-cresol circulation in the 2,6-DMP process, selectivity of more than 85% degree of 2,6-DMP was achieved. The participation levels of by-products: 2,4-DMP and 2,4,6-TMP were low. In the optimal conditions based on the highest yield of 2,6-DMP achieved in the technological node applying o-cresol circulation, there are 2%_mol. of 2,4-DMP and 6%_mol. of 2,4,6-TMP in the final mixture, whereas 2,4,6-TMP can be useful as a chain stopper and polymer’s molar mass regulator during the polymerization of 2,6-DMP.

【 授权许可】

   
2014 Żukowski et al.; licensee Chemistry Central Ltd.

【 图 表 】

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