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摘要环己烷氧化反应的主要产物有环己醇、环己酮和己二酸，他们均是用途广泛的化工原料。世界上90％以上的环己酮采用环己烷氧化法来生产，环己酮主要用于医药、油漆、涂料、橡胶及农药等工业，另外在印刷和塑料的回收方面也有很大的用量。如何高选择性地氧化己烷一直是一个具有挑战性的课题。采用基于浸渍-吸附法制备Au/C催化剂，利用XRD，FI-IR，BET,N２吸附和UV—Vis等手段表征了材料的晶相组成，晶粒尺寸，热稳定性及其催化性能，研究其环己烷选择氧化性能，并确定最佳制备条件及最佳环己烷选择氧化工艺条件。结果显示，使用浸渍-吸附法制备Au/C催化剂的质量分数为1％的Au／C催化效果最佳，纳米金颗粒直径小于2 nm且分布均匀，其较佳反应条件为5O℃，pH 9．5，催化剂0 .22 g，水溶液中质量分数为7.5％的环己烷，环己烷在1 h内，选择性及转化率均可同时达到100％。上述研究表明基于浸渍-吸附法制备Au/C催化剂，且在该多相催化反应上反应时间短，活性高，选择性高。24357
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Au/C CATALYST PREPARATION, CHARACETERIZATION AND PERFORMANCE STUDY
ABSTRACT
The main product of the oxidation reaction of cyclohexane cyclohexanol, cyclohexanone and adipic acid，They are widely used chemicals，More than 90 percent of the world cyclohexanone cyclohexane oxidation to produce，Cyclohexanone is mainly used in pharmaceutical, paint, paint, rubber and pesticides and other industrial，Also in terms of printing and recycling plastics is also a great amount of。How high selective oxidation of hexane has been a challenging task。Based impregnation - adsorption prepared Au / C catalyst，Based impregnation - adsorption prepared Au / C catalyst utilization XRD, FI-IR, BET, N2 adsorption and UV-Vis and other means to characterize the crystalline phase of the material composition, grain size, thermal stability and catalytic properties studied cyclohexane oxidation resistance, and to determine the optimal preparation conditions and the best conditions for selective oxidation of cyclohexane。The results show that the use of immersion - adsorption prepared Au / C catalyst mass fraction of 1% Au / C catalytic best, nano-gold particles smaller than 2 nm in diameter and uniform distribution, the optimal reaction conditions for the 5O ℃, pH 9 .5 catalyst 0 .22 g, mass fraction of the aqueous solution of 7.5% cyclohexane, within 1 h, while the selectivity and conversion rate can reach 100%. Based on these studies show that impregnation - adsorption prepared Au / C catalyst, and the reaction time is short on the heterogeneous catalysis, high activity and high selectivity.
目录
1 绪论 .5
1.1 本课题的研究背景及意义5
1.2 纳米Au催化剂的研究意义5
2 文献综述7
2.1 环己烷、环己酮和环己醇的物化性质.7
2.2 环己烷选择性氧化生产环己醇、环己酮的进展.7
2.3 环己烷氧化制KA油研究进展.8
2.4 环己烷氧化反应工业化生产技术现状.9
2.4.1 硼酸催化氧化法.9
2.4.2 钴盐催化氧化法.9
2.4.3 无催化氧化法.10
2.5 负载型纳米金催化剂的制备方法.11
2.5.1 沉积—沉淀法(DP 法) 11
2.5.2 浸渍法(IMP 法) .11
2.5.3 共沉淀法(CP 法) 11
2.5.4 离子交换法(IE 法) 11
2.5.5 化学蒸发沉积法(CVD 法) .11
2.5.6 光化学沉积法(FD 法) 12
2.5.7 一步水热合成法(HY 法) 12
2.5.8 金属有机配合物固载法(OGCG 法) 12
2.6 金催化剂概述.12
2.6.1 金催化剂发展简史.12
2.6.2 金催化剂的构成要素.13
2.6.3 金催化剂的特点.13
2.6.4 金催化剂用于环己烷氧化反应的研究进展.13
3 实验部分.15
3.1 原料、药品及设备15
3.2 催化剂的制备.16
3.3 环己烷的氧化反应.17
3.4 催化剂的表征.18