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Improved Regioselective Mononitration of o-Xylene over HBEA-500 Zeolite Catalyst

  • Shi, Chun J. (School of Applied Chemistry and Environmental Engineering, Bengbu College) ;
  • Tai, Yan F. (School of Applied Chemistry and Environmental Engineering, Bengbu College) ;
  • Liu, Hong T. (School of Chemical Engineering, Hefei University of Technology)
  • Received : 2013.07.08
  • Accepted : 2013.08.14
  • Published : 2013.11.20

Abstract

Keywords

Experimental

Quantities are recorded in the footnotes to the appropriate tables. All reactions were carried out in a 50 mL two-necked round bottomed flask equipped with a water condenser and a magnetic stirrer. In a typical experiment, a mixture of zeolite HBEA-25 (Si/Al = 25, 0.11g), o-xylene (0.60 mL, 5 mmol ), nitric acid ( 65%, 0.68 mL, 10 mmol ) in acetic anhydride (5.0 mL) at room temperature for 10 h. When the reaction was over, the zeolite was removed by filtration and the filter liquor was washed with NaHCO3 (3 × 10 mL) and water (3 × 10 mL). The organic phase separated was dried with anhydrous sodium sulfate, and filtrated to give a straw yellow liquid residue. The isomer distribution and yields of products were estimated from the peak areas based on the internal standard technique using gas chromatography. The straw yellow products with further purification by column chromatography, and were identified by comparison of their analytical data with those of authentic samples.

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