空气氧化再生Pd-C催化剂的研究-.docVIP

空气氧化法再生Pd/C催化剂的初步研究 Preliminary study of Air oxidation regenerated Pd/C catalyst 摘要：研究了空气氧化法再生PTA精制用Pd/C催化剂的过程，以4-CBA为评价指标，考察了氧气含量、氧化温度、氧化时间和空气流量对Pd/C催化剂活性的影响，用XRD和TEM对再生Pd/C催化剂进行表征。结果表明： 空气氧化再生Pd/C催化剂的适宜条件为空气流量80mL/min， 氧化时间60min， 氧化温度180℃，4-CBA的转化率可达到99.34%；TEM表征结果表明空气氧化再生能够使催化剂中大颗粒的金属钯明显减小，可以使得Pd晶粒在载体表面有效地再分散。 Abstract: In this study the process of air oxidizing regeneration of Pd/C catalyst used in PTA refining is researched. Based on the indication of 4-CBA, factors including the oxygen content, oxidation temperature, oxidation time and air flow were evaluated on how they impacted the activity of Pd/C catalyst, and to characterize the reactivated catalyst XRD and TEM were adopted to analyse the feature. Results show the optimum conditions for recycling Pd/C catalyst are: air low 50mL/min, oxidation time 60min and temperature 180℃, the conversion rate of 4-CBA under this could be up to 99.34%; TEM observation revealed the oxidizing regeneration was able to minish big particles of metal palladium in size and disperse the crystalline grains more effectively on the surface of carriers. 关键词：Pd/C催化剂 PTA 空气氧化 再生 Key words: Pd/C catalyst PTA air oxidation reactivation 中图分类号：TQ032 　 文献标识码：A PTA精制生产中所用的Pd/C催化剂，是聚酯工业中用量较大的贵金属催化剂之一，催化活性较高，其制备技术由Engelhard、Montictni等外国公司所垄断。PTA加氢精制过程影响因素较多，Pd/C催化剂的寿命相对较短，一般为1~1.5年。 Pd/C catalyst used in PTA refining production, is one of the previous /noble metal catalysts with big consumption in polyester industry, and highly efficient in catalysing, while its preparing technologies are mostly monopolized by overseas companies like Engelhard, Montictni. Due to the complication involved in actual PTA hydrorefining, Pd/C catalyst is relatively short of service life, 1~1.5 years in average only. 国内一些研究院及大学自上世纪80年代起，对Pd/C催化剂失活和制备开发进行研究。造成Pd/C催化剂寿命较短和失活的原因主要为有机杂质堵塞催化剂孔道、催化剂表面Pd的流失和烧结 [1-2]。针对Pd/C催化剂不同的失活原因，主要的再生方法有：碱洗[3]、酸洗[4]和超临界CO2萃取再生[5]等，但这些方法都不能有效地解决金属Pd的烧结失活问题。 Since 1980s some institutes and colleges in China h