碳质纤维固载Pd催化剂制备及其催化性能研究

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李成林,李铁夫,王瑶.碳质纤维固载Pd催化剂制备及其催化性能研究[J].,2022,62(1):1-8

碳质纤维固载Pd催化剂制备及其催化性能研究

Preparation of Pd immobilized on carbonaceous fiber and its catalytic performance study

DOI：10.7511/dllgxb202201001

中文关键词:碳质纤维氧化 Suzuki反应催化剂载体

英文关键词:carbonaceous fiber oxidation Suzuki reaction catalyst supporter

基金项目:科技部国家重点研发计划资助项目(2016YFE0109800).

作者	单位
李成林,李铁夫,王瑶

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中文摘要:

以乙炔为碳源、铜粉为催化剂制备碳质纤维(CF)，采用氧化剂(硝酸、硫酸或过氧化氢)对所制备的碳质纤维进行氧化处理，将氧化后的碳质纤维固载Pd制备Pd/CF催化剂，并考察其在溴苯和苯硼酸Suzuki反应中的催化性能．利用傅里叶变换红外光谱仪(FT-IR)、电感耦合等离子体发射光谱仪(ICP-OES)和场发射扫描电子显微镜(FE-SEM)对碳质纤维、氧化后的碳质纤维以及Pd/CF催化剂进行表征．结果表明，合成的碳质纤维整体形貌呈直线形状，纤维内含有大量的碳碳双键．氧化处理后，纤维形貌没有明显变化，但检测出碳氧双键．3种氧化剂处理得到的Pd/CF催化剂中，硝酸氧化CF制得的催化剂(Pd/CF-N)活性和稳定性最好．以硝酸为氧化剂考察了硝酸浓度、氧化时间、氧化温度对Pd/CF-N催化活性的影响，结果表明在所考察的参数范围内，Pd/CF-N的活性随着氧化时间和氧化温度的增加而增加，与硝酸浓度关系不大．最佳氧化条件下制备的Pd/CF-N在Suzuki反应中产物收率为93%，重复使用5次后，仍能保持较高的活性．

英文摘要:

Carbonaceous fiber (CF) was prepared with acetylene as the carbon source and copper powder as the catalyst. Three oxidants, including nitric acid, sulfuric acid and hydrogen peroxide were used to oxidize the prepared CF, and the oxidized CF was immobilized with Pd to prepare Pd/CF catalyst. The effect of Pd/CF catalyst in Suzuki reaction of bromobenzene and phenylboronic acid was investigated. Fourier transform infrared spectroscopy (FT-IR), inductively coupled plasma emission spectrometer (ICP-OES) and field emission scanning electron microscopy (FE-SEM) were used to characterize CF, oxidized CF and Pd/CF catalysts. Characterization results show that the morphologies of CF before and after oxidation are similar in linear shape. The carbon carbon double bond is detected in the as synthesized CF, and after oxidation treatment, the carbon oxygen double bond is detected. Among Pd/CF catalysts treated with three oxidants, the catalyst (Pd/CF-N) prepared by oxidizing CF with nitric acid has the best performance in both activity and stability. Therefore, the effects of nitric acid concentration, oxidation time and oxidation temperature on the activity of Pd/CF-N were further investigated. The results show that within the scope of the investigated parameters, the activity of Pd/CF-N increases with the increase of oxidation time and temperature, and has little relationship with the concentration of nitric acid. Pd/CF-N catalyst prepared under optimal condition has the best catalytic performance in Suzuki reaction with a product yield of 93%. The catalyst can be reused for 5 cycles without significant loss in activity.

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碳质纤维固载Pd催化剂制备及其催化性能研究

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