高效稳定的MoS2-TiO2纳米复合催化剂用于浆态床菲催化加氢

doi:10.1016/S1872-2067(22)64184-6

催化学报 ›› 2023, Vol. 46: 125-136.DOI: 10.1016/S1872-2067(22)64184-6

高效稳定的MoS₂-TiO₂纳米复合催化剂用于浆态床菲催化加氢

杨成功^a^,^b, 王冬娥^a^,^*(), 黄蓉^a^,^b, 韩健强^a, 塔娜^c, 马怀军^a, 曲炜^a, 潘振栋^a, 王从新^a, 田志坚^a^,^c^,^*()

^a中国科学院大连化学物理研究所, 洁净能源国家实验室, 辽宁大连 116023
^b中国科学院大学, 北京 100049
^c中国科学院大连化学物理研究所, 催化基础国家重点实验室, 辽宁大连 116023

收稿日期:2022-09-06 接受日期:2022-10-13 出版日期:2023-03-18 发布日期:2023-02-21
通讯作者: *电子信箱: tianz@dicp.ac.cn (田志坚), dewang@dicp.ac.cn (王冬娥)
基金资助:
新疆自治区重点研发计划(2017B02007-1);新疆自治区重点研发计划(2017B02007-2)

Highly active and stable MoS₂-TiO₂ nanocomposite catalyst for slurry-phase phenanthrene hydrogenation

Chenggong Yang^a^,^b, Donge Wang^a^,^*(), Rong Huang^a^,^b, Jianqiang Han^a, Na Ta^c, Huaijun Ma^a, Wei Qu^a, Zhendong Pan^a, Congxin Wang^a, Zhijian Tian^a^,^c^,^*()

^aDalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cState Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian116023, Liaoning, China

Received:2022-09-06 Accepted:2022-10-13 Online:2023-03-18 Published:2023-02-21
Contact: *E-mail: tianz@dicp.ac.cn (Z. Tian), dewang@dicp.ac.cn (D. Wang)
Supported by:
Autonomous Region Key R&D Program of Xin Jiang(2017B02007-1);Autonomous Region Key R&D Program of Xin Jiang(2017B02007-2)

摘要/Abstract

摘要：

浆态床加氢是一种先进的非常规石油资源(重油等)加氢提质技术, 它采用分散型催化剂以提高催化剂与原料中的沥青质等大分子的接触程度. 沥青质等大分子中多环芳烃的快速转化是浆态床重油加氢技术的挑战, 因此设计高活性的加氢催化剂是浆态床加氢技术的关键. 作为典型的二维层状材料, 分散型MoS₂催化剂表现出较好的催化加氢性能. 然而, 纳米尺寸的分散型MoS₂催化剂的稳定性有待提高, 在高温高压下MoS₂片层会折叠并聚集成较大的颗粒以降低其表面能. MoS₂颗粒的生长会导致其悬浮性降低和边缘活性位点暴露量减少, 因而降低催化剂的活性和寿命. 因此, 急需设计开发高性能的分散型MoS₂纳米催化剂, 从而解决MoS₂层在高温高压条件下的折叠和聚集难题, 提高MoS₂纳米催化剂的催化加氢活性和稳定性. 纳米复合材料的构建可以有效地解决活性组分的团聚问题. 近年来, Janus纳米复合材料因其在催化方面的广泛应用引起了科研人员的关注. 此外, 复合材料中各组分的种类对其催化活性有显著影响. 早期研究表明, 与Al₂O₃, SiO₂, MgO或其他金属氧化物相比, TiO₂复合MoS₂催化剂具有较高的催化加氢活性.

本文通过一步溶剂热法合成了一系列不同MoS₂含量的Janus MoS₂-TiO₂纳米复合催化剂, 并研究了其在浆态床催化菲加氢中的活性和稳定性. 高分辨透射电镜结果表明, Janus MoS₂-TiO₂纳米复合催化剂由TiO₂纳米粒子(10‒15 nm)和MoS₂片层(堆积层数为1‒3和片层长度为2‒10 nm)组成. 活性位模型计算和NO化学吸附测试表明, 与MoS₂和负载型MoS₂/TiO₂催化剂相比, Janus MoS₂-TiO₂纳米复合催化剂中的MoS₂层具有更高的MoS₂分散度, 暴露出更多的边缘配位不饱和Mo原子. X射线光电子能谱结果表明, 通过形成Mo‒O‒Ti键成功构建了具有强MoS₂-TiO₂相互作用的Janus结构, 并出现了TiO₂向MoS₂的电子转移现象. 从TiO₂到MoS₂的电子转移会削弱Mo‒S键并在基面产生大量配位不饱和Mo原子. 浆态床催化菲加氢反应结果表明, Janus MoS₂-TiO₂纳米复合催化剂上菲转化率最高可达91.6%. 而MoS₂催化剂上菲转化率仅为50.4%. 催化剂的稳定性评价结果表明, 经过7次菲催化加氢循环反应后, Janus MoS₂-TiO₂-15纳米复合催化剂上菲转化率降低了25.1%, 保持在68.6%, 仍高于新鲜的MoS₂催化剂上菲的转化率. 然而经过7次菲催化加氢循环反应后, MoS₂催化剂上菲的转化率下降了49.6%, 仅为25.4%. 与MoS₂催化剂相比, Janus MoS₂-TiO₂纳米复合催化剂在高温高压下表现出更高的菲催化加氢活性和稳定性.

结合反应后的催化剂表征, 其高活性可归因于大量配位不饱和Mo原子的暴露. 而其高稳定性主要是源于其稳定的Mo‒O‒Ti键提供的MoS₂-TiO₂强相互作用, 可以有效地将MoS₂层锚定在TiO₂纳米粒子表面, 避免MoS₂层卷曲、折叠和团聚. 综上, 将二维层状催化剂与另一种纳米材料耦合形成Janus纳米复合催化剂是设计和构建在高温高压条件下具有较好催化性能和稳定性的二维层状催化剂的有效途径.

关键词: 纳米复合催化剂, 高MoS₂分散度, 配位不饱和Mo原子, MoS₂-TiO₂相互作用, 催化加氢

Abstract:

MoS₂-TiO₂ nanocomposite catalysts with Janus structure were synthesized via facile one-step solvothermal method. X-ray diffraction, high resolution transmission electron microscope, NO chemisorption and X-ray photoelectron spectroscopy were applied to characterize the composition and nanostructure of the MoS₂-TiO₂ nanocomposite catalysts. Experimental results revealed that the MoS₂-TiO₂ nanocomposite catalysts with Janus structure were composed of MoS₂ layers (few stacked layers of 1-3 and short slabs of 2-10 nm) and TiO₂ nanoparticles (10-15 nm), which have strong MoS₂-TiO₂ interaction with transferring electrons from TiO₂ to MoS₂. Catalytic performance of MoS₂-TiO₂ nanocomposite catalysts for phenanthrene hydrogenation was investigated and compared with that of MoS₂ catalyst in an autoclave reactor with high temperature and high pressure. The phenanthrene conversion over the MoS₂-TiO₂ nanocomposite catalyst with MoS₂ content of 15.0 wt% (MoS₂-TiO₂-15) can reach 91.6%, which was much higher than 50.4% for MoS₂ catalyst and 76.8% for conventional supported MoS₂/TiO₂-15 catalyst. After 7 cycles of phenanthrene hydrogenation reaction, the phenanthrene conversion over MoS₂-TiO₂-15 nanocatalyst remained at 68.6%, while the phenanthrene conversion over MoS₂ catalyst was reduced to only 25.4%. The MoS₂-TiO₂ nanocomposite catalysts exhibit significantly enhanced catalytic activity and stability for slurry phase hydrogenation. The enhanced catalytic activity originates from the exposure of abundant coordinatively unsaturated Mo atoms. The enhanced stability results from the Janus structure with stable MoS₂-TiO₂ interaction and Mo-O-Ti bonds, which anchor MoS₂ layers on the surface of TiO₂ nanoparticles to avoid the curling, folding and agglomeration of MoS₂ layers. This is an important finding on slurry phase catalytic hydrogenation performances of MoS₂-based nanocomposite catalysts with Janus structure. Shedding light on the research of Janus nanocomposite catalysts in catalytic hydrogenation is significantly crucial for the development of effective and stable hydrogenation catalysts.

Key words: Nanocomposite catalyst, High MoS₂ dispersion, Coordinatively unsaturated Mo atom, MoS₂-TiO₂ interaction, Catalytic hydrogenation

杨成功, 王冬娥, 黄蓉, 韩健强, 塔娜, 马怀军, 曲炜, 潘振栋, 王从新, 田志坚. 高效稳定的MoS₂-TiO₂纳米复合催化剂用于浆态床菲催化加氢[J]. 催化学报, 2023, 46: 125-136.

Chenggong Yang, Donge Wang, Rong Huang, Jianqiang Han, Na Ta, Huaijun Ma, Wei Qu, Zhendong Pan, Congxin Wang, Zhijian Tian. Highly active and stable MoS₂-TiO₂ nanocomposite catalyst for slurry-phase phenanthrene hydrogenation[J]. Chinese Journal of Catalysis, 2023, 46: 125-136.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(22)64184-6

https://www.cjcatal.com/CN/Y2023/V46/I3/125

图/表 10

Table 1 Synthesis of TiO2, MoS2, and MoS2-TiO2 nanocomposite catalysts under different conditions.

Catalyst	ATM (g)	N₂H₄·H₂O (g)	TBT (g)	H₂O (mL)	Ethyl alcohol (mL)
TiO₂	0	0.63	7.7	60	40
MoS₂-TiO₂-5	0.26	0.32	13.0	60	40
MoS₂-TiO₂-15	0.52	0.63	7.7	60	40
MoS₂-TiO₂-25	0.52	0.63	4.1	60	40
MoS₂-TiO₂-35	0.52	0.63	2.5	60	40
MoS₂	0.52	0.63	0	60	40

Fig. 1. XRD patterns of bare TiO2 sample, MoS2 sample, MoS2-TiO2 samples with various MoS2 contents and MoS2/TiO2-15-I sample.

Fig. 2. HRTEM images of bare TiO2 (a), MoS2-TiO2-5 (b), MoS2-TiO2-15(c), MoS2-TiO2-25 (d), MoS2-TiO2-35 (e), MoS2/TiO2-15-I (f) and MoS2 samples (g). (h) HRTEM image and corresponding element mapping of MoS2-TiO2-15 sample.

Fig. 3. Average numbers of stacking layers, average slab lengths and MoS2 dispersion.

Fig. 4. NO adsorption capacity of MoS2 and MoS2-TiO2 nanocomposite samples with different MoS2 percentages.

Fig. 5. XPS spectra of Mo 3d (a), Ti 2p (b) for MoS2 and MoS2-TiO2 nanocomposite samples. (c) XPS spectra of Mo 3d for MoS2, supported MoS2/TiO2-15-I and MoS2-TiO2-15 nanocomposite samples. (d) Negative shifts of binding energy for Mo 3d of MoS2-TiO2 nanocomposite samples compared with that of MoS2 sample.

Fig. 6. The observed structures (a) and the proposed structural models (b) of the MoS2-TiO2 nanocomposite with Janus structure.

Fig. 7. (a) Conversions and HPs of phenanthrene over MoS2 catalyst and MoS2-TiO2 nanocomposite catalysts with different MoS2 contents. (b) Catalytic hydrogenation selectivities to PHx over MoS2 catalyst and MoS2-TiO2 nanocomposite catalysts with different MoS2 contents. (c) Conversions and HPs of phenanthrene over bare TiO2, MoS2, the mixture of bare TiO2 and MoS2, MoS2-TiO2-15-I and MoS2-TiO2-15 catalyst. (d) Catalytic hydrogenation selectivities to PHx over bare TiO2, synthesized MoS2, the mixture of bare TiO2 and MoS2, MoS2-TiO2-15-I and MoS2-TiO2-15 catalyst. Reaction conditions: MoS2 contents of catalyst 0.075 g, phenanthrene 3.0 g, solvent tridecane 30.0 g, initial pressure 8 Mpa, 350 °C, 4 h.

Fig. 8. The stability of MoS2-TiO2-15 nanocomposite catalyst and MoS2 catalyst for phenanthrene hydrogenation.

Fig. 9. (a) The XRD patterns of fresh MoS2, MoS2-C7, fresh MoS2-TiO2-15, and MoS2-TiO2-15-C7. (b) HRTEM images of fresh MoS2, MoS2-C7, fresh MoS2-TiO2-15, and MoS2-TiO2-15-C7. (c) XPS spectra of Mo 3d of fresh MoS2, MoS2-C7, fresh MoS2-TiO2-15, and MoS2-TiO2-15-C7.

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高效稳定的MoS₂-TiO₂纳米复合催化剂用于浆态床菲催化加氢

Highly active and stable MoS₂-TiO₂ nanocomposite catalyst for slurry-phase phenanthrene hydrogenation

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