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锐钛型介孔偏钛酸催化剂的制备及其催化酯化性能
Preparation of mesoporous anatase metatitanic acid catalyst and its catalytic esterification properties
【摘要】 以工业偏钛浆为原料,通过水洗、碱洗、酸洗处理制备了锐钛型介孔偏钛酸催化剂,将催化剂用于α-蒎烯酯化反应中考察其催化性能,采用FT-IR、XRD、SEM、BET手段对催化剂的晶相结构、形貌、表面积、孔径等结构进行了表征。结果表明,最佳制备条件为:温度30℃,碱洗pH=8.5,酸洗pH=4.0;处理后的偏钛酸催化剂基本没有SO42,且晶型没有发生明显变化,均为锐钛矿相,最佳条件下制备的偏钛酸催化剂孔径分布均匀,晶粒团聚较少,比表面积为334.82 m2/g,平均孔径为3.96 nm,催化α-蒎烯酯化生成草酸龙脑酯含量可达48.59%,皂化后水蒸气蒸馏收集龙脑,m1(正龙脑)∶m2(异龙脑)=59.27∶37.07。
【Abstract】 Mesoporous anatase metatitanic acid catalyst was prepared by water washing,caustic washing,acid washing with industrial partial titanium pulp as raw material,then applied to the esterification reaction of α-pinene to investigate the catalytic effects.The catalysts were characterized by FTIR、XRD、SEM and BET.The results showed that the optimal preparation condition was temperature 30 ℃,caustic washing pH=8.5,acid washing pH=4.0.SO42 was barely detected in the catalysts after the treatment,and all crystal form was in anatase phase without any significant change.The metatitanic acid catalyst prepared under optimal conditions has a homogeneous pore distribution,less grain agglomeration,a specific surface area of 334.82 m2/g and an average pore size of 3.96 nm.In the optimal catalysis of α-pinene by metatitanic acid,48.59% bornyl oxalate is obtained;steam distillation is employed after saponification to collected product,where the ratio of borneol to isoborneol reaches 59.27∶37.07.
【Key words】 metatitanic acid; α-pinene; catalytic esterification; bornyl oxalate;
- 【文献出处】 化工进展 ,Chemical Industry and Engineering Progress , 编辑部邮箱 ,2013年07期
- 【分类号】TQ426
- 【被引频次】8
- 【下载频次】254