S_2O_8~(2-)/TiO_2催化合成乙酸正丁酯
|
摘要
通过浸渍—焙烧法制备了固体超强酸S_2O_8~(2-)/TiO_2催化剂,并以醋酸和正丁醇为原料合成了乙酸正丁酯.考察了催化剂的焙烧温度、酸/醇比、反应时间等因素对反应的影响.结果表明S_2O_8~(2-)/TiO_2的最佳制备条件为:过硫酸铵浸渍浓度0.5mol/L,焙烧温度500℃,焙烧时间3h,在最佳反应条件下,乙酸正丁酯的酯化率可达97.8%,催化剂重复使用3次后,对醋酸的转化率仍可达90.8%.
Solid super acid catalyst of S_2O_8~(2-)/TiO_2 was prepared by direct impregnation calcination processes.n-Butyl acetate was synthesized from acetic acid and n-butanol.The influences of calcination temperature of catalyst,ratio of acid to alcohol,reaction time on the reaction condition were investigated.The results showed that the optimum preparation condition of S_2O_8~(2-)/TiO_2 is concentration of ammonium persulfate 0.50 mol/L and baking temperature of500 ℃for 3h.Under the optimum condition,the esterification rate of 97.8% was attained.After the catalyst was used repeatedly for three times,the conversion rate of acetic acid was still up to 90.8%.
Solid super acid catalyst of S_2O_8~(2-)/TiO_2 was prepared by direct impregnation calcination processes.n-Butyl acetate was synthesized from acetic acid and n-butanol.The influences of calcination temperature of catalyst,ratio of acid to alcohol,reaction time on the reaction condition were investigated.The results showed that the optimum preparation condition of S_2O_8~(2-)/TiO_2 is concentration of ammonium persulfate 0.50 mol/L and baking temperature of500 ℃for 3h.Under the optimum condition,the esterification rate of 97.8% was attained.After the catalyst was used repeatedly for three times,the conversion rate of acetic acid was still up to 90.8%.
引文
[1]王景芸.SO2-4/MxOy型固体超强酸改性研究进展[J].化学与粘合,2010,32(1):42-45.
[2]周海峰.体酸催化酯化反应的研究进展[J].精细与专用化学品,2004,12(23):1-6.
[3]单秋杰.负载型杂多酸盐催化合成乙酸正丁酯[J].化学工业与工程技术,2008,29(3):38-40.
[4]李冰,沈丹,李婷,等.磺化硅胶催化合成乙酸正丁酯的研究[J].广州化工,2013,41(22):82-83.
[5]胡春燕,李双全.稀土固体超强酸Gd3+-SO2-4/ZrO2催化合成乙酸正丁酯[J].湿法冶金,2011,30(4):344-345.
[6]訾俊峰.固体超强酸WO3/ZrO2催化合成乙酸正丁酯[J].许昌学院学报,2012,31(5):1-2.
[7]吴良彪.固体超强酸催化合成乙酸正丁酯的研究[J].广东化工,2010,37(4):110-111.
[8]秦传高,曹崇江,钟秦.固体超强酸SO2-4/ZrO2对乙酸正丁酯的催化合成研究[J].江苏化工,2007,35(4):35-36.
[9]莫晓兰,张昭,王优,等.固体超强酸SO2-4/ZrO2的制备及表征[J].钛工业进展,2011,28(2):14-18.
[10]王占领.S2O2-8/TiO2-Al2O3-ZrO2固体超强酸的制备及催化活性研究[J].化学工程师,2010,180(9):13-15.
[11]秦中立,范望喜,曾亮.固体超强酸S2-2O8/TiO2-ZrO2催化合成三氟甲基硝基苯[J].湖北大学学报(自然科学版),2010,32(2):175-176.
[12]喜兰,田孟超,赵旭娜.固体超强酸SO2-4/TiO2-ZnO催化合成柠檬酸三丁酯[J].化学研究与应用,2011,23(2):214-215.
[13]李运山,张文雯,黄一波,等.金属负载型阳离子交换树脂催化合成乙酸正丁酯[J].化工技术与开发,2011,40(1):9-12.
[14]任玉荣,贾树勇,侴晓玉,等.氯化亚锡催化合成乙酸丁酯的研究[J].吉林师范大学学报(自然科学版),2004,25(2):87-88.
[2]周海峰.体酸催化酯化反应的研究进展[J].精细与专用化学品,2004,12(23):1-6.
[3]单秋杰.负载型杂多酸盐催化合成乙酸正丁酯[J].化学工业与工程技术,2008,29(3):38-40.
[4]李冰,沈丹,李婷,等.磺化硅胶催化合成乙酸正丁酯的研究[J].广州化工,2013,41(22):82-83.
[5]胡春燕,李双全.稀土固体超强酸Gd3+-SO2-4/ZrO2催化合成乙酸正丁酯[J].湿法冶金,2011,30(4):344-345.
[6]訾俊峰.固体超强酸WO3/ZrO2催化合成乙酸正丁酯[J].许昌学院学报,2012,31(5):1-2.
[7]吴良彪.固体超强酸催化合成乙酸正丁酯的研究[J].广东化工,2010,37(4):110-111.
[8]秦传高,曹崇江,钟秦.固体超强酸SO2-4/ZrO2对乙酸正丁酯的催化合成研究[J].江苏化工,2007,35(4):35-36.
[9]莫晓兰,张昭,王优,等.固体超强酸SO2-4/ZrO2的制备及表征[J].钛工业进展,2011,28(2):14-18.
[10]王占领.S2O2-8/TiO2-Al2O3-ZrO2固体超强酸的制备及催化活性研究[J].化学工程师,2010,180(9):13-15.
[11]秦中立,范望喜,曾亮.固体超强酸S2-2O8/TiO2-ZrO2催化合成三氟甲基硝基苯[J].湖北大学学报(自然科学版),2010,32(2):175-176.
[12]喜兰,田孟超,赵旭娜.固体超强酸SO2-4/TiO2-ZnO催化合成柠檬酸三丁酯[J].化学研究与应用,2011,23(2):214-215.
[13]李运山,张文雯,黄一波,等.金属负载型阳离子交换树脂催化合成乙酸正丁酯[J].化工技术与开发,2011,40(1):9-12.
[14]任玉荣,贾树勇,侴晓玉,等.氯化亚锡催化合成乙酸丁酯的研究[J].吉林师范大学学报(自然科学版),2004,25(2):87-88.