| 张 志1，袁 红1，2，王云杰1.介孔SO2-4/ZrO2的制备、表征及其催化
煎炸废油合成生物柴油[J].中国油脂,2019,44(11):47~51.[ZHANG Zhi1, YUAN Hong1, 2, WANG Yunjie1.Preparation and characterization of mesoporous SO2-4/ZrO2 and itscatalytic synthesis of biodiesel from waste cooking oil[J].China Oils and Fats,2019,44(11):47~51.] |
| 介孔SO2-4/ZrO2的制备、表征及其催化
煎炸废油合成生物柴油 |
| Preparation and characterization of mesoporous SO2-4/ZrO2 and itscatalytic synthesis of biodiesel from waste cooking oil |
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| DOI：10.12166/j.zgyz.1003-7969/2019.11.010 |
| 中文关键词: 溶胶凝胶法 介孔SO2-4/ZrO2 固体超强酸 煎炸废油 生物柴油 |
| 英文关键词:sol-gel method mesoporous SO2-4/ZrO2 solid superacid waste cooking oil biodiesel |
| 基金项目:宁夏自然科学基金研究项目（NZ17094）；国家自然科学基金项目（21266001） |
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| 中文摘要: |
| 采用溶胶凝胶法，使用十六烷基三甲基溴化氨（CTAB）为模板剂，正丙醇锆为锆源，（NH4)2SO4为硫化剂，经不同温度（400～600 ℃）煅烧制备介孔SO2-4/ZrO2固体超强酸。并利用氨程序升温脱附（NH3-TPD）、傅里叶红外光谱（FT-IR）、N2物理吸脱附（BET）、X射线衍射（XRD）和透射电子显微镜（TEM）对样品结构进行表征。结果显示：当煅烧温度为500 ℃时制备的催化剂出现明显的四方晶相，随着煅烧温度的升高，催化剂的比表面积先增加后减小，500 ℃时最大，比表面积为130 m2/g，孔径为3.3 nm；TEM显示所制备的催化剂均具有蠕虫状介孔结构；NH3-TPD曲线显示所制备的催化剂均具有超强酸性，500 ℃时酸量最大，为22 cm3/g STP。将该催化剂用于煎炸废油和甲醇酯交换制备生物柴油试验，发现500 ℃煅烧的催化剂具有较高的催化活性，于190 ℃下反应8 h生物柴油收率达到92.3%。催化剂重复利用5次后，生物柴油收率仍能达到76.3%。 |
| 英文摘要: |
| 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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