镧改性Silicalite-1封装铜纳米团簇增强糠醛加氢制糠醇的性能

doi:10.1016/S1872-2067(26)65125-X

催化学报 ›› 2026, Vol. 88: 382-392.DOI: 10.1016/S1872-2067(26)65125-X

镧改性Silicalite-1封装铜纳米团簇增强糠醛加氢制糠醇的性能

香含^a^,¹, 林露^b^,¹, 李雨^a^,^b, 衣启松^b^,^c, 姜超然^d, 陈睿^e, 刘远帅^b, 赛娜^a, 贺进逯^a, 白凤华^a^,^*(), 罗文豪^a^,^*()

^a 内蒙古大学化学化工学院, 内蒙古呼和浩特 010021
^b 中国科学院青岛生物能源与过程研究所, 山东能源研究院, 青岛新能源山东省实验室, 山东青岛 266101
^c 中铝山东新材料有限公司, 山东淄博 255052
^d 中石化(北京)化工研究院有限公司, 北京 100013
^e 南开大学材料科学与工程学院, 天津 300350

收稿日期:2026-01-22 接受日期:2026-04-07 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: w.luo@imu.edu.cn (罗文豪),
f.h.bai@imu.edu.cn (白凤华).
基金资助:
国家自然科学基金(22562020);国家自然科学基金(22078316);国家自然科学基金(22509213);中央引导地方科技发展专项资金(2024ZY0116);内蒙古青年科技英才基金(NJYT24019);内蒙古大学基金(10000-23112101/081);山东省自然科学基金(ZR2025QC1329);天津市计量科技项目(2024TJMT071)

Silicalite-1 encapsulated Cu nanoclusters with La modification for enhanced performance in hydrogenation of furfural to furfuryl alcohol

Han Xiang^a^,¹, Lu Lin^b^,¹, Yu Li^a^,^b, Qisong Yi^b^,^c, Chaoran Jiang^d, Rui Chen^e, Yuanshuai Liu^b, Na Sai^a, Jinlu He^a, Fenghua Bai^a^,^*(), Wenhao Luo^a^,^*()

^a Inner Mongolia Key Laboratory of Rare Earth Catalysis, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, Inner Mongolia, China
^b Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266101, Shandong, China; Shandong Energy Institute, Qingdao 266101, Shandong, China; Qingdao Energy Shandong Laboratory, Qingdao 266101, Shandong, China
^c Chinalco Shandong New Materials Co., Ltd., Zibo 255052, Shandong, China
^d SINOPEC (Beijing) Research Institute of Chemical Industry Co., Ltd., Beijing 100013, China
^e School of Materials Science and Engineering, Nankai University, Tianjin 300350, China

Received:2026-01-22 Accepted:2026-04-07 Online:2026-09-18 Published:2026-09-05
About author:First author contact:1 共同第一作者.
1 Contributed equally to this work.
Supported by:
The National Natural Science Foundation of China(22562020);The National Natural Science Foundation of China(22078316);The National Natural Science Foundation of China(22509213);The funding of Local Science and Technology Development Guided by Central Government(2024ZY0116);The funding of Inner Mongolia Youth Science and Technology Talents(NJYT24019);The funding of Inner Mongolia University(10000-23112101/081);The Shandong Provincial Natural Science Foundation Project(ZR2025QC1329);The Tianjin Metrology Technology(2024TJMT071)

摘要/Abstract

摘要： 生物质作为一种前景广阔的可再生资源, 可用于生产高附加值的燃料与化学品. 人们已探索了大量的中间体作为生产燃料和化学品的基本构筑单元, 这些中间体也被称为生物质衍生平台分子. 其中, 糠醛(FFL)作为半纤维素经简单水解所得的重要平台分子, 可进一步转化为溶剂(如2-甲基四氢呋喃)、聚合物单体(如1,5-戊二醇)、药物分子(如5-硝基糠醛)以及航空煤油如JP-10)等多种高价值产品. 由于上述转化路线大多以糠醇(FAL)作为中间体, 因此糠醛选择性加氢制糠醇反应对于可持续的生物炼制具有重要意义.
铜基催化剂是糠醛选择性加氢制备糠醇的重要催化剂, 但其存在颗粒团聚和稳定性差等问题. 针对上述问题, 本研究通过原位封装策略, 在纯硅分子筛(S-1)中制备粒径约为3.4 nm的铜纳米团簇, 并进一步引入稀土金属镧(La)进行修饰, 构建了高效稳定的La-Cu@S-1催化剂用于糠醛选择性加氢制备糠醇. 与Cu@S-1催化剂相比, La改性催化剂的活性和选择性均有所提高. 在110 °C, 20 bar H₂压力的条件下反应3 h, La-Cu@S-1可实现糠醛转化率为98.6%, 糠醇选择性为99%, 其转换频率(TOF)高达66.7 h^-1, 在已报道的Cu-分子筛催化剂中处于领先水平. 循环实验进一步显示, La-Cu@S-1经过四次循环反应后仍能保持高糠醛产率且未发生失活; 而Cu@S-1在首次反应后糠醛产率即下降约50%, 证实La的引入显著提高了催化剂稳定性. 为了深入研究La的改性机制, 联合如高角度环形暗场扫描透射电镜、低温CO吸附红外光谱、X-射线光电子能谱、H₂程序升温还原等表征手段和理论计算, 分析了La的引入对Cu电子价态的调控及金属-载体作用的调节. 结果表明, La的引入能够通过增强的电子相互作用为铜纳米团簇提供锚定位点, 从而在液相催化反应过程中有效抑制金属的浸出和团聚. 此外, La的引入还能调控包覆铜纳米颗粒的分子筛微环境, 并在催化过程中(即使在还原性H₂气氛下)显著稳定通常难以维持的Cu⁺物种, 保持较高Cu⁺物种的占比, 从而提高了催化剂活性和稳定性.
综上, 本研究结合分子筛的空间限域效应和稀土元素La改性的协同策略, 精准调控催化剂结构并稳定金属活性组分, 有效提升了铜基催化剂在糠醛加氢制备糠醇液相催化反应中的活性和稳定性.该工作不仅揭示了稀土元素在提升金属-分子筛催化剂性能方面的应用潜力, 也为稀土催化在生物质高值化转化中的应用提供了理论支持, 同时拓展了稀土元素在可再生能源转化领域的应用前景.

关键词: 分子筛, 空间限域, 糠醛, 加氢, 稀土改性

Abstract:

Selective hydrogenation of furfural (FFL) to furfuryl alcohol (FAL) represents a pivotal paradigm in sustainable biomass valorization. In this work, nanoscale Cu clusters were encapsulated in silicalite-1 (S-1) zeolite using in-situ synthesis, and further modified by a rare-earth element of La for regulating the catalyst microenvironment. The obtained La-Cu@S-1 can provide an enhanced performance in the FFL-to-FAL transformations, with 98.6% conversion of FFL and 99% selectivity of FAL at 110 °C, 20 bar H₂, and 3 h. Besides, La-Cu@S-1 shows a good stability without apparent catalyst deactivation upon four consecutive runs. Extensive characterization research reveals that La addition could provide anchoring sites for Cu nanoclusters via an enhanced electronic interaction, thereby effectively suppressing metal leaching and agglomeration during the liquid-phase catalysis. Additionally, La addition could modulate the zeolite microenvironment of encapsulated Cu nanoparticles and notably stabilize the conventionally unstable Cu⁺ species at a high proportion, even in a reductive H₂ atmosphere during catalysis, accounting for the enhanced activity and stability. This study showcases La modification as an efficient approach to rationally develop metal-zeolite combinations with enhanced performance, promoting potential utilization and development of rare-earth elements in the valorization of biomass and other renewable energy.

Key words: Zeolites, Encapsulation, Furfural, Hydrogenation, Rare-earth element

香含, 林露, 李雨, 衣启松, 姜超然, 陈睿, 刘远帅, 赛娜, 贺进逯, 白凤华, 罗文豪. 镧改性Silicalite-1封装铜纳米团簇增强糠醛加氢制糠醇的性能[J]. 催化学报, 2026, 88: 382-392.

Han Xiang, Lu Lin, Yu Li, Qisong Yi, Chaoran Jiang, Rui Chen, Yuanshuai Liu, Na Sai, Jinlu He, Fenghua Bai, Wenhao Luo. Silicalite-1 encapsulated Cu nanoclusters with La modification for enhanced performance in hydrogenation of furfural to furfuryl alcohol[J]. Chinese Journal of Catalysis, 2026, 88: 382-392.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65125-X

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图/表 8

Scheme 1. Schematic of the in-situ encapsulation approach for the preparation of the Cu@S-1 and La-Cu@S-1.

Table 1 The physicochemical properties of S-1 and different Cu-containing zeolites.

Catalyst	Loading ^a (wt%)		D_Cu ^b (%)	S_BET ^c (m²/g)	S_micro ^c (m²/g)	V_micro ^c (cm³/g)
Catalyst	La	Cu	D_Cu ^b (%)	S_BET ^c (m²/g)	S_micro ^c (m²/g)	V_micro ^c (cm³/g)
S-1	—	—	—	495	356	0.18
Cu@S-1	—	2.1	27.3	425	314	0.16
La-Cu@S-1	0.2	1.9	30.5	428	269	0.14
Cu@S-1 (Spent) ^d	—	1.9	26.6	404	227	0.12
La-Cu@S-1 (Spent) ^d	0.2	1.8	30.5	417	205	0.11

Fig. 1. STEM image (a) and HAADF-STEM images (b,c) of Cu@S-1 (Inset: Particle size distribution of Cu). STEM image (d) and HAADF-STEM images (e,f) of La-Cu@S-1 (Inset: Particle size distribution of Cu). EDX elemental mapping spectra of Cu@S-1 (g) and La-Cu@S-1 (h).

Fig. 2. (a) Reaction pathway for the hydrogenation of FFL. Time profiles of FFL conversion and products yield over Cu@S-1 (b) and La-Cu@S-1 (c). (d) Activity and selectivity comparison of different catalysts. Reaction conditions: 0.3 g furfural, 23.56 g isopropanol, 0.3 g catalyst, 20 bar H2, 110 °C, 1000 rpm, and 3 h. Recycling experiments of Cu@S-1 (e) and La-Cu@S-1 (f). Reaction conditions: 0.3 g furfural, 23.56 g isopropanol, 0.3 g catalyst, 20 bar H2, 110 °C, 1000 rpm, and 1 h. (g) Comparison with as-reported Cu-zeolite catalysts for the hydrogenation of FFL to FAL. The TOF was defined as moles of FAL per mol of surface Cu per hour.

Fig. 3. STEM image (a) and HAADF-STEM images (b,c) of Cu@S-1 (spent) (Inset: Particle size distributions of Cu). STEM image (d) and HAADF-STEM images (e,f) of La-Cu@S-1 (spent) (Inset: Particle size distributions of Cu). EDX elemental mapping spectra of Cu@S-1 (spent) (g) and La-Cu@S-1 (spent) (h).

Fig. 4. Cu 2p3/2 XPS spectra (a) and Cu LMM XAES spectra (b) of Cu@S-1, La-Cu@S-1, Cu@S-1 (spent), and La-Cu@S-1 (spent). (c) Proportions of different Cu species in Cu@S-1, La-Cu@S-1, Cu@S-1 (Spent), and La-Cu@S-1 (Spent). (d) H2-TPR profiles of Cu@S-1 and La-Cu@S-1.

Fig. 5. FT-IR-CO spectra of Cu@S-1 (a) and La-Cu@S-1 (b). Charge density difference of Cu@S-1 (c) and La-Cu@S-1 (d). The blue, green, orange, and red spheres denote Cu, La, Si, and O atoms, respectively; The yellow and cyan regions indicate electron accumulation and depletion, respectively.

Scheme 2. Schematic of the La effect on the catalytic performance of La-Cu@S-1 in the hydrogenation of FFL to FAL.

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镧改性Silicalite-1封装铜纳米团簇增强糠醛加氢制糠醇的性能

Silicalite-1 encapsulated Cu nanoclusters with La modification for enhanced performance in hydrogenation of furfural to furfuryl alcohol

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