2-TPR)表征發(fā)現(xiàn),與常規(guī)浸漬法制備的Pd/C催化劑相比,氨三乙酸三鈉的引入能夠有效減小Pd的平均粒徑,并且通過調(diào)變氨三乙酸三鈉的量可以獲得Pd粒子不同大小的負載型Pd/C催化劑,隨著氨三乙酸三鈉引入量的增多(Pd摩爾含量的0.5、1、2倍),Pd粒徑由5.7nm減小至2.1nm,但是繼續(xù)增加氨三乙酸三鈉的量(Pd摩爾含量的4倍),Pd粒徑不再繼續(xù)減小。當氨三乙酸三鈉:Pd=1:1時,即Pd粒子大小約為4nm時,催化劑獲得了最佳催化反應(yīng)性能,反應(yīng)6h原料全部轉(zhuǎn)化,2,3-二氯吡啶的選擇性可達76.86%。"/>

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負載型納米Pd/C的尺寸可控制備及其2,3,6-三氯吡啶加氫性能
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西安建筑科技大學(xué)冶金工程學(xué)院,西安凱立新材料股份有限公司,西安凱立新材料股份有限公司,西安凱立新材料股份有限公司

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國家科技型中小企業(yè)創(chuàng)新資助(項目號11C26216113807)


Size-control preparation of AC supported nano Pd catalyst and its hydrogenation of 2,3,6-trichloropyridine
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School of Metallurgical Engineering, Xi’an University of Architecture and Technology,Xi’an,Xi’an KaiLi Catalyst New materials Co,Ltd.,Xi’an KaiLi Catalyst New materials Co,Ltd.,Xi’an KaiLi Catalyst New materials Co,Ltd.

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    摘要:

    在催化劑制備過程中引入氨羧絡(luò)合劑(氨三乙酸三鈉),通過配位作用穩(wěn)定并保護Pd粒子,得到納米Pd/C催化劑,研究了氨三乙酸三鈉引入量對Pd/C催化劑結(jié)構(gòu)的影響。通過X射線衍射(XRD)、X射線光電子能譜(XPS)、透射電鏡(TEM)及化學(xué)吸附(H2-TPR)表征發(fā)現(xiàn),與常規(guī)浸漬法制備的Pd/C催化劑相比,氨三乙酸三鈉的引入能夠有效減小Pd的平均粒徑,并且通過調(diào)變氨三乙酸三鈉的量可以獲得Pd粒子不同大小的負載型Pd/C催化劑,隨著氨三乙酸三鈉引入量的增多(Pd摩爾含量的0.5、1、2倍),Pd粒徑由5.7nm減小至2.1nm,但是繼續(xù)增加氨三乙酸三鈉的量(Pd摩爾含量的4倍),Pd粒徑不再繼續(xù)減小。當氨三乙酸三鈉:Pd=1:1時,即Pd粒子大小約為4nm時,催化劑獲得了最佳催化反應(yīng)性能,反應(yīng)6h原料全部轉(zhuǎn)化,2,3-二氯吡啶的選擇性可達76.86%。

    Abstract:

    Pd/C catalysts were prepared by introducing complexone (nitrilotriacetic acid trisodium salt, NTA) into Pd precursor solutions, Pd particles were stabilized by the coordination of Pd2+ and NTA. Catalysts were characterized by XRD, XPS, TEM and H2-TPR, and we found that compared with Pd/C catalyst prepared by impregnation method, the average particle size of Pd could by effectively reduced by introducing NTA during preparation. Furthermore, Pd particles could be size-controlled by adjusting the amount of NTA, the average particle size of Pd was decreased from 5.7 to 2.1 nm by increase NTA from 0.5 to 2 times of Pd (molar ratio), but Pd particle size did not continue to decrease by continue increasing the amount of NTA. The best catalytic performance was achieved when the average particle size was 4nm (NTA: Pd=1: 1), conversion was 100% and selectivity of 2,3-dichloropyridine was up to 76.86% after 6 hours of reaction.

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曾永康,陳丹,曾利輝,高武.負載型納米Pd/C的尺寸可控制備及其2,3,6-三氯吡啶加氫性能[J].稀有金屬材料與工程,2018,47(5):1637~1642.[Yongkang Zeng, Dan Chen, Lihui Zeng, Wu Gao. Size-control preparation of AC supported nano Pd catalyst and its hydrogenation of 2,3,6-trichloropyridine[J]. Rare Metal Materials and Engineering,2018,47(5):1637~1642.]
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  • 收稿日期:2018-01-19
  • 最后修改日期:2018-03-01
  • 錄用日期:2018-03-12
  • 在線發(fā)布日期: 2018-06-08
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