A novel cerium (III) salt of Dawson type tungstophosphoric acid (Ce
2
P
2
W
18
O
62
·16H
2
O) was prepared by doping cerous nitrate in H
6
P
2
W
18
O
62
·13H
2
O powder and characterized by thermogravimetry and differential thermal analyses (TG/DTA)
Fourier transform infrared spectroscopy (FT-IR)
X-ray powder diffraction (XRD)
pyridine infrared spectroscopy (Py-IR) and scanning electron microscopy (SEM). Its catalytic activity was evaluated by the probe reaction of synthesis of n-butyl acetate with acetic acid and n-butanol. The effects of various parameters such as molar ratio of n-butanol to acetic acid
reaction temperature
reaction time
and catalyst amount have been studied by single factor experiment. The results show that Ce
2
P
2
W
18
O
62
·16H
2
O behaved as an excellent heterogeneous catalyst in the synthesis of n-butyl acetate. The optimum synthetic conditions were determined as follows:molar ratio of n-butanol to acetic acid at 2.0:1.0
mass of the catalyst being 1.44% of the total reaction mixture
reaction temperature of 120 ℃ and reaction
time of 150 min. Under above conditions
the conversion of acetic acid was above 97.8%. The selectivity of n-butyl acetate based on acetic acid was
in all cases
nearly 100%. The catalysts could be recycled and still exhibited high catalytic activity with 90.4% conversion after five cycles of reaction. It was found by means of TG-DTA and Py-IR that the catalyst deactivation was due to the adsorption of a complex of by-product on the active sites on catalysts surface or the catalyst loss in its separation from the products. Compared with using sulfuric acid as catalyst
the present procedure with Ce
2
P
2
W
18
O
62
·16H
2
O is a green productive technology due to simple process
higher yield
catalyst recycling and no corrosion for the production facilities.
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Related Author
Xiaocheng Lin
Youjie Huang
Ling Li
Changshen Ye
Jie Chen
Ting Qiu
Lu Qing
Shan Falong
Related Institution
Engineering Research Center of Reaction Distillation, Fujian Province University, College of Chemical Engineering, Fuzhou University
College of Environment and Resources, Fuzhou University
College of Chemical Engineering, Qingdao University of Science and Technology
College of Chemical Engineering, Zhejiang University of Technology
State Key Laboratory of Advanced Optical Polymer and Manufacturing Technology, College of Chemical Engineering, Qingdao University of Science and Technology