The present invention belongs to the technical field of
fluorochemical industry, and specifically relates to a
spinel-type
composite oxide catalyst and a preparation method thereof. The general formula of the catalyst is AB2O4, and its preparation method includes: (1) mixing the raw materials at the A-site and the B-site, dissolving them in deionized water, adding
citric acid monohydrate, and mixing and stirring to obtain a
sol; (2) evaporating the
sol to obtain a dry gel, then
drying the dry gel, subsequently performing pretreatment on the dried dry gel, and performing
calcination after pretreatment to obtain a
spinel-type
composite oxide catalyst; (3) placing the
spinel-type
composite oxide catalyst in a fixed-
bed reactor, and simultaneously introducing N2 and HF for fluorination treatment. By using adjustable
ion types and ratios at the A-site and the B-site to optimize the
surface structure and active sites of the catalyst, combined with the
citric acid-assisted
sol-
gel method and specific pretreatment,
calcination, and fluorination treatment processes, the stability, catalytic activity, and selectivity of the catalyst are significantly improved.