Large Scale Halogen-free Synthesis of Metal-organic Framework Material Fe-MIL-100

doi:10.11901/1005.3093.2016.563

Chinese Journal of Materials Research

2017, Vol. 31

Issue (8): 569-575 DOI: 10.11901/1005.3093.2016.563

Orginal Article

Current Issue | Archive | Adv Search

Large Scale Halogen-free Synthesis of Metal-organic Framework Material Fe-MIL-100

Xiangping YANG¹, Xiaoxue GUO¹, Chenghua ZHANG^2,³(

), Yong YANG^2,³, Yongwang LI^2,³

1 College of Chemical Engineering, China University of Petroleum (HD), Qingdao 266000, China
2 National Engineering Laboratory of Coal Indirect Liquefaction, Synfuels China Co. Ltd., Beijing 101407, China
3 State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China

Cite this article:

Xiangping YANG, Xiaoxue GUO, Chenghua ZHANG, Yong YANG, Yongwang LI. Large Scale Halogen-free Synthesis of Metal-organic Framework Material Fe-MIL-100. Chinese Journal of Materials Research, 2017, 31(8): 569-575.

Download:

HTML

PDF(2277KB)
Export: BibTeX | EndNote (RIS)

Abstract

Hierarchically porous iron (Ⅲ) trimesate Fe-MIL-100 were synthesized by hydro-thermal route of HF free in a large scale, with ironic nitrate and trimesic acid as raw materials. The structure and morphology of Fe-MIL-100 were characterized by X-ray diffraction (XRD), N₂ physical adsorption, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TG). The effect of temperature, HNO₃ addition, time and post-treatment on the structure of Fe-MIL-100 were investigated. The results show that the prepared Fe-MIL-100 has high crystallinity with BET surface area up to 1744 m²/g. The prepared materials have good thermal stability, which can withstand temperature up to 520 ^°C before decomposition in nitrogen.

Key words: composite large scale synthesis Fe-MIL-100 hydrothermal synthesis

Received: 26 September 2016

ZTFLH:

TQ050.4

Fund: Supported by National Natural Science Foundation of China (No.91545109) and International Cooperation in Science and Technology of Shanxi Province (No.2014081004)

	Service

	E-mail this article
	Add to citation manager
	E-mail Alert
	RSS
	（）
	Articles by authors
	Xiangping YANG
	Xiaoxue GUO
	Chenghua ZHANG
	Yong YANG
	Yongwang LI

URL:

https://www.cjmr.org/EN/10.11901/1005.3093.2016.563 OR https://www.cjmr.org/EN/Y2017/V31/I8/569

Fig.1 XRD patterns of Fe-MIL-100 with different temperature

Fig.2 XRD patterns of samples with different amount of HNO₃

Fig.3 N₂ adsorption/desorption isotherm of samples with different amount of HNO₃ at -196℃

Fig.4 Optical photograph of sample (a), SEM images (b~d) of prepared samples with different amount of HNO₃ (HNO₃/Fe = 1, 2, 4 respectively)

Table 1 Textural properties of Fe-MIL-100 with different amount of HNO₃

Fig.5 XRD patterns of samples with different reaction times

Fig.6 N₂ adsorption/desorption isotherm of samples with different reaction times at -196℃

Table 2 Textural properties of Fe-MIL-100 with different time of crystallization

Fig.7 FTIR spectra of samples with different washing time

Fig.8 N₂ adsorption/desorption isotherm of samples under different washing time at -196℃

Table 3 Textural properties of Fe-MIL-100 with different washing time

Fig.9 XRD patterns of samples with different value of Fe/H₃BTC

Fig.10 N₂ adsorption/desorption isotherm of samples with different value of Fe/H₃BTC at -196℃

Table 4 Textural properties s of Fe-MIL-100 with different value of Fe/H₃BTC

Fig.11 TG and heat flow of Fe-MIL-100

[1]	Rodenas T, Van Dalen M, García-Pérez E, et al.Visualizing MOF mixed matrix membranes at the nanoscale: towards structure-performance relationships in CO2/CH4 separation over NH2-MIL-53(Al)@PI[J]. Adv. Funct. Mater., 2014, 24: 249
[2]	Gascon J, Corma A, Kapteijn F, et al.Metal organic framework catalysis: Quo vadis?[J]. ACS Catal., 2014, 4: 361
[3]	Farrusseng D, Aguado S, Pinel C.Metal-organic frameworks: opportunities for catalysis[J]. Angewandt. Chem. Int. Ed., 2009, 48: 7502
[4]	Wang C, Xie Z G, deKrafft K E, et al. Doping Metal-organic frameworks for water oxidation, carbon dioxide reduction, and organic photocatalysis[J]. J. Am. Chem. Soc., 2011, 133: 13445
[5]	Yaghi O M, O’Keeffe M, Ockwig N W, et al. Reticular synthesis and the design of new materials[J]. Nature, 2003, 423: 705
[6]	Zhao D, Timmons D J, Yuan D Q, et al.Tuning the topology and functionality of metal-organic frameworks by ligand design[J]. Account. Chem. Res., 2011, 44: 123
[7]	Horcajada P, Surblé S, Serre C, et al.Synthesis and catalytic properties of MIL-100(Fe), an iron(III) carboxylate with large pores[J]. Chem. Commun., 2007, (27): 2820
[8]	Férey G, Serre C, Draznieks C M, et al.A hybrid solid with giant pores prepared by a combination of targeted chemistry, simulation, and powder diffraction[J]. Angewandt. Chem. Int. Ed., 2004, 43: 6456
[9]	Volkringer C, Popov D, Loiseau T, et al.Synthesis, single-crystal X-ray microdiffraction, and NMR characterizations of the giant pore metal-organic framework aluminum trimesate MIL-100[J]. Chem. Mater., 2009, 21: 5695
[10]	Mowat J P S, Miller S R, Slawin A M Z, et al. Synthesis, characterisation and adsorption properties of microporous scandium carbox ylates with rigid and flexible frameworks[J]. Micropor. Mesopor. Mater., 2011, 142: 322
[11]	Lieb A, Leclerc H, Devic T, et al.MIL-100(V)-a mesoporous vanadium metal organic framework with accessible metal sites[J]. Micropor. Mesopor. Mater., 2012, 157: 18
[12]	Wang D K, Wang M T, Li Z H.Fe-based metal-organic frameworks for highly selective photocatalytic benzene hydroxylation to phenol[J]. ACS Catal., 2015, 5: 6852
[13]	Zhu B J, Yu X Y, Jia Y, et al.Iron and 1, 3, 5-benzenetricarboxylic metal-organic coordination polymers prepared by solvothermal method and their application in efficient As(V) removal from aqueous solutions[J]. J. Phys. Chem., 2012, 116C: 8601
[14]	Horcajada P, Serre C, Vallet-Regí M, et al.Metal-organic frameworks as efficient materials for drug delivery[J]. Angewandt. Chem. Int. Ed., 2006, 45: 5974
[15]	Plaza M G, Ribeiro A M, Ferreira A, et al.Rodrigues, Separation of C3/C4 hydrocarbon mixtures by adsorption using a mesoporous iron MOF: MIL-100(Fe)[J]. Micropor. Mesopor. Mater., 2012, 153: 178
[16]	Kurfi?tova L, Seo Y K, Hwang Y K, et al.High activity of iron containing metal-organic-framework in acylation of p-xylene with benzoyl chloride[J]. Catal. Today, 2012, 179: 85
[17]	Dhakshinamoorthy A, Alvaro M, Hwang Y K, et al.Intracrystalline diffusion in metal organic framework during heterogeneous catalysis: influence of particle size on the activity of MIL-l00 (Fe) for oxidation reactions[J]. Dalton Trans., 2011, 40: 10719
[18]	Ahmed I, Jeon J, Khan N A, et al.Synthesis of a metal-organic framework, iron-benezenetricarboxylate, from dry gels in the absence of acid and salt[J]. Cryst. Growth Des., 2012, 12: 5878
[19]	Vimont A, Leclerc H, Maugé F, et al.Creation of controlled br?nsted acidity on a zeotypic mesoporous chromium(III) carboxylate by grafting water and alcohol molecules[J]. J. Phys. Chem., 2007, 111C: 383

[1]	PAN Xinyuan, JIANG Jin, REN Yunfei, LIU Li, LI Jinghui, ZHANG Mingya. Microstructure and Property of Ti / Steel Composite Pipe Prepared by Hot Extrusion[J]. 材料研究学报, 2023, 37(9): 713-720.
[2]	LIU Ruifeng, XIAN Yunchang, ZHAO Rui, ZHOU Yinmei, WANG Wenxian. Microstructure and Properties of Titanium Alloy/Stainless Steel Composite Plate Prepared by Spark Plasma Sintering[J]. 材料研究学报, 2023, 37(8): 581-589.
[3]	JI Yuchen, LIU Shuhe, ZHANG Tianyu, ZHA Cheng. Research Progress of MXene Used in Lithium Sulfur Battery[J]. 材料研究学报, 2023, 37(7): 481-494.
[4]	WANG Wei, XIE Zelei, QU Yishen, CHANG Wenjuan, PENG Yiqing, JIN Jie, WANG Kuaishe. Tribological Properties of Graphene/SiO₂ Nanocomposite as Water-based Lubricant Additives[J]. 材料研究学报, 2023, 37(7): 543-553.
[5]	ZHANG Tengxin, WANG Han, HAO Yabin, ZHANG Jiangang, SUN Xinyang, ZENG You. Damping Enhancement of Graphene/Polymer Composites Based on Interfacial Interactions of Hydrogen Bonds[J]. 材料研究学报, 2023, 37(6): 401-407.
[6]	SHAO Mengmeng, CHEN Zhaoke, XIONG Xiang, ZENG Yi, WANG Duo, WANG Xuhui. Effect of Si²⁺ Ion Beam Irradiation on Performance of C/C-ZrC-SiC Composites[J]. 材料研究学报, 2023, 37(6): 472-480.
[7]	DU Feifei, LI Chao, LI Xianliang, ZHOU Yaoyao, YAN Gengxu, LI Guojian, WANG Qiang. Preparation of TiAlTaN/TaO/WS Composite Coatings by Magnetron Sputtering and their Cutting Properties on Titanium Alloy[J]. 材料研究学报, 2023, 37(4): 301-307.
[8]	ZHANG Jinzhong, LIU Xiaoyun, YANG Jianmao, ZHOU Jianfeng, ZHA Liusheng. Preparation and Properties of Temperature-Responsive Janus Nanofibers[J]. 材料研究学报, 2023, 37(4): 248-256.
[9]	WANG Gang, DU Leilei, MIAO Ziqiang, QIAN Kaicheng, DU Xiangbowen, DENG Zeting, LI Renhong. Interfacial Properties of Polyamide 6-based Composites Reinforced with Polydopamine Modified Carbon Fiber[J]. 材料研究学报, 2023, 37(3): 203-210.
[10]	LIN Shifeng, XU Dongan, ZHUANG Yanxin, ZHANG Haifeng, ZHU Zhengwang. Preparation and Mechanical Properties of TiZr-based Bulk Metallic Glass/TC21 Titanium Alloy Dual-layered Composites[J]. 材料研究学报, 2023, 37(3): 193-202.
[11]	MIAO Qi, ZUO Xiaoqing, ZHOU Yun, WANG Yingwu, GUO Lu, WANG Tan, HUANG Bei. Pore Structure, Mechanical and Sound Absorption Performance for Composite Foam of 304 Stainless Steel Fiber/ZL104 Aluminum Alloy[J]. 材料研究学报, 2023, 37(3): 175-183.
[12]	ZHANG Kaiyin, WANG Qiuling, XIANG Jun. Microwave Absorption Properties of FeCo/SnO₂ Composite Nanofibers[J]. 材料研究学报, 2023, 37(2): 102-110.
[13]	ZHOU Cong, ZAN Yuning, WANG Dong, WANG Quanzhao, XIAO Bolv, MA Zongyi. High Temperature Properties and Strengthening Mechanism of (Al₁₁La₃+Al₂O₃)/Al Composite[J]. 材料研究学报, 2023, 37(2): 81-88.
[14]	LUO Yu, CHEN Qiuyun, XUE Lihong, ZHANG Wuxing, YAN Youwei. Preparation of Double-layer Carbon Coated Na₃V₂(PO₄)₃ as Cathode Material for Sodium-ion Batteries by Ultrasonic-assisted Solution Combustion and Its Electrochemical Performance[J]. 材料研究学报, 2023, 37(2): 129-135.
[15]	LIU Zhihua, YUE Yuanchao, QIU Yifan, BU Xiang, YANG Tao. Preparation of g-C₃N₄/Ag/BiOBr Composite and Photocatalytic Reduction of Nitrate[J]. 材料研究学报, 2023, 37(10): 781-790.

No Suggested Reading articles found!

Viewed

Full text

Abstract

Cited

Shared

Discussed