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首页> 外文期刊>Catalysis science & technology >Preparation of highly active phosphated TiO2 catalysts via continuous sol-gel synthesis in a microreactor
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Preparation of highly active phosphated TiO2 catalysts via continuous sol-gel synthesis in a microreactor

机译：制备高活性含磷酸盐的二氧化钛通过连续的溶胶-凝胶法合成的催化剂微反应器

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摘要

Microreactors, featuring mu m-sized tubes, offer greater flexibility and precise control of chemical processes compared to conventional large-scale reactors, due to their elevated surface-to-volume ratio and modular construction. However, their application in catalyst production has been largely neglected. Herein, we present the development of a microreactor process for the one-step sol-gel preparation of phosphated TiO2 - a catalyst which has been recently demonstrated to be an eco-friendly material for the selective synthesis of the platform chemical 5-hydroxymethylfurfural (5-HMF) from bio-derived glucose. In order to establish catalyst preparation-property-performance relationships, 18 samples were prepared according to a D-optimal experimental plan with a central point. The key properties of these samples (porosity, crystallite size, mole bulk fraction of P) were correlated, using quadratic and interaction models, with the catalytic performance (conversion, selectivity, reaction rate) of 5-HMF synthesis as a test reaction. The optimal calculated catalyst features were set as target parameters to optimise catalyst synthesis applying quadratic correlation functions. An optimal catalyst was obtained, validating the models employed, with a yield of almost 100% and a space-time yield of ca. 3 orders of magnitude higher than that of a conventional batch process (26.8 vs. 0.07 g(cat) h(-1) cm(reactor)(-3)). The high yield could be mainly attributed to the optimal hydrolysis ratio and temperature. Controlling the TiO2 crystallite size and surface acidity in conjunction with fine-tuning of the porous properties in the microreactor led to increased glucose conversion (95.6 vs. 78.7%), surface based formation rates of 5-HMF (0.047 vs. 0.008 g(5-HMF) h(-1) m(cat)(-2)), and selectivity towards 5-HMF (55.5 vs. 50.0%) of the optimal catalyst in relation to the batch-prepared material.
机译：微反应器,μm-sized管,报价更大的灵活性和精确的控制比传统的化学过程大规模的反应堆,由于他们的高团和模块化的建设。然而,他们在催化剂生产中的应用在很大程度上被人们忽视了。微反应器的发展过程一步溶胶-凝胶制备含磷酸盐的二氧化钛-一个最近演示了催化剂是一种环保材料的选择性化学合成的平台从bio-derived 5-hydroxymethylfurfural (5-HMF)葡萄糖。preparation-property-performance关系,根据D-optimal 18个样本准备实验计划的中心点。这些样本的特性(孔隙度、微晶尺寸,摩尔体积分数P)相关,使用二次和交互模型,与催化性能(5-HMF转换、选择性、反应速率)合成作为测试反应。计算催化剂特性设置为目标参数优化催化剂合成应用二阶相关函数。最优催化剂得到了验证模型使用,和产量的近100%ca的时空产量。3个数量级高于传统的批处理过程(26.8和0.07 g (cat) h(1)厘米(反应堆)(3))。可以主要归因于高收益最佳的水解率和温度。控制二氧化钛微晶尺寸和表面酸度与微调的微反应器导致多孔属性增加葡萄糖转化率(78.7% vs 95.6),基于表面形成5-HMF率(0.047 vs。0.008克(5-HMF) h (1) m (cat)(2)),和选择性对5-HMF (50.0% vs 55.5)的最优相对于batch-prepared催化剂材料。

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