ie7b01166_si_001.pdf (1.34 MB)
A Strategy for the Synthesis of 1,2-Dichlorotetrafluorocyclobutene from Hexachlorobutadiene and Its Reaction Pathway
journal contribution
posted on 2017-06-21, 00:00 authored by Xiaomeng Zhou, Pingli Zhang, Jinwei He, Biao ZhouIn
this paper, a novel strategy for the preparation of 1,2-dichlorotetrafluorocyclobutene
(DTB) was proposed via a catalytic gas-phase process of fluorination
using hexachlorobutadiene (HCBD) and anhydrous HF. In order to search
for suitable catalysts and reveal the reaction pathway for this synthetic
route, a series of studies were carried out. First, CrOx/ZnO catalysts with different promoters (Ni, Cu,
In, Al) were prepared by a precipitate method and the optimum reaction
conditions were investigated. The highest activity was achieved on
the Cr–Ni–Zn catalyst, whose yield of DTB reached 90%
by a multiple cycle reaction. Second, the effects of different promoters
on the properties of catalysts were studied by Brunauer–Emmett–Teller
(BET) surface area analysis, scanning electron microscopy (SEM), X-ray
diffraction (XRD), temperature-programmed desorption in ammonia (NH3-TPD), and X-ray photoelectron spectroscopy (XPS). It was
found that the Cr–Ni–Zn catalyst showed the excellent
catalytic performances with more CrOxFy species, higher oxygen concentration, and
widely distributed acid strength on its surface. Third, combining
experimental results with theoretical calculations, a reaction pathway
has been proposed. This study offers an economic synthetic route for
DTB from HCBD, which is a valuable and promising method for industrial
production.