锐钛型介孔偏钛酸催化剂的制备及其催化酯化性能

化工进展

锐钛型介孔偏钛酸催化剂的制备及其催化酯化性能

刘小琴1，张煌2，郑辉东1，郭川1，陈剑峰1，侯英俊1，王碧玉1

1福州大学化学化工学院，福建福州 350108；2福建青松股份有限公司，福建建阳 354200

出版日期:2013-07-05 发布日期:2013-07-05

Preparation of mesoporous anatase metatitanic acid catalyst and its catalytic esterification properties

LIU Xiaoqin1，ZHANG Huang2，ZHENG Huidong1，GUO Chuan1，CHEN Jianfeng1，HOU Yingjun1，WANG Biyu1

1College of Chemistry and Chemical Engineering，Fuzhou University，Fuzhou 350108，Fujian，China；2Fujian Green Pine Co.，Ltd.，Jianyang 354200，Fujian，China

Online:2013-07-05 Published:2013-07-05

摘要/Abstract

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。

关键词: 偏钛酸, α-蒎烯, 催化酯化, 草酸龙脑酯

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

刘小琴1，张煌2，郑辉东1，郭川1，陈剑峰1，侯英俊1，王碧玉1. 锐钛型介孔偏钛酸催化剂的制备及其催化酯化性能[J]. 化工进展.

LIU Xiaoqin1，ZHANG Huang2，ZHENG Huidong1，GUO Chuan1，CHEN Jianfeng1，HOU Yingjun1，WANG Biyu1. Preparation of mesoporous anatase metatitanic acid catalyst and its catalytic esterification properties[J]. Chemical Industry and Engineering Progree.

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