Preparation and characterization of mesoporous SO2-4/ZrO2 and itscatalytic synthesis of biodiesel from waste cooking oil
  
DOI:10.12166/j.zgyz.1003-7969/2019.11.010
KeyWord:sol-gel method  mesoporous SO2-4/ZrO2  solid superacid  waste cooking oil  biodiesel
FundProject:宁夏自然科学基金研究项目(NZ17094);国家自然科学基金项目(21266001)
Author NameAffiliation
ZHANG Zhi1, YUAN Hong1, 2, WANG Yunjie1 1.College of Chemistry and Chemical Engineering, North University for Nationalities, Yinchuan 750021, China2.Key Laboratory of Chemical Technology of the State Ethnic Affairs Committee, Yinchuan 750021, China 
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Abstract:
      Using sol-gel method,with hexadecyl trimethyl ammonia bromide (CTAB) as template, zirconium n-propanol as zirconium source and (NH4)2SO4 as sulfide agent,mesoporous SO2-4/ZrO2 solid superacid was prepared by calcination at different temperatures (400-600 ℃).The structure of the catalyst was characterized by ammonia temperature programmed desorption (NH3-TPD), Fourier transform infrared spectroscopy (FT-IR), physical adsorption and desorption of N2 (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM).The results showed that when calcination temperature was 500 ℃, the catalyst showed obvious tetragonal phase. With the increase of calcination temperature, the specific surface area of the catalyst increased first and then decreased.When the calcination temperature was 500 ℃, the specific surface area was the highest with 130 m2/g and and the pore size was 3.3 nm. TEM showed that the catalyst had worm-like mesoporous structure. NH3-TPD curves showed that the prepared catalyst had super acidity, and the maximum acidity was 22 cm3/g STP at 500 ℃. The catalyst was used to prepare biodiesel by transesterification of waste cooking oil with methanol. It was found that the catalyst calcinated at 500 ℃ had high catalytic activity and the yield of biodiesel reached 92.3% at 190 ℃ for 8 h. The yield of biodiesel still could reach 76.3% after the catalyst calcinated at 500 ℃ was reused for five times.
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