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  • Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst.

Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst.

Journal of hazardous materials (2011-09-03)
Joanna Adamiak, Dorota Kalinowska-Alichnewicz, Michał Szadkowski, Wincenty Skupiński
ABSTRACT

A new catalyst, H(3)PO(4)/MoO(3)/SiO(2), was prepared by modification of MoO(3)/SiO(2) using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Molybdenum(VI) oxide, nanopowder, 100 nm (TEM), 99.5% trace metals basis
Supelco
Chlorobenzene, analytical standard
Sigma-Aldrich
Molybdenum(VI) oxide, 99.97% trace metals basis
Sigma-Aldrich
Chlorobenzene, anhydrous, 99.8%
Sigma-Aldrich
Chlorobenzene, ACS reagent, ≥99.5%
Sigma-Aldrich
Chlorobenzene, ReagentPlus®, 99%
Sigma-Aldrich
Molybdenum(VI) oxide, puriss. p.a., 99.5%
Sigma-Aldrich
Molybdenum(VI) oxide, ReagentPlus®, ≥99.5%
Sigma-Aldrich
Molybdenum(VI) oxide, ACS reagent, ≥99.5%
Sigma-Aldrich
Chlorobenzene, suitable for HPLC, 99.9%