Preparation and characterization of H4SiW12O40@MIL-100(Fe) and its catalytic performance for synthesis of 4,4'-MDA

Yunhuan Kong; Xiaomeng Cheng; Hualiang An; Xinqiang Zhao; Yanji Wang

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Preparation and characterization of H₄SiW₁₂O₄₀@MIL-100(Fe) and its catalytic performance for synthesis of 4,4'-MDA

第25届中国过程控制会议专栏 | Updated：2026-01-06

- Preparation and characterization of H₄SiW₁₂O₄₀@MIL-100(Fe) and its catalytic performance for synthesis of 4,4'-MDA
- Chinese Journal of Chemical Engineering Vol. 26, Issue 2, Pages: 330-336(2018)
- Affiliations：
  
  Hebei Provincial Key Lab of Green Chemical Technology and Efficient Energy Saving, School of Chemical Engineering and Technology, Hebei University of Technology,Tianjin,China,300130
- Author bio：
- Funds：
- DOI：
  CLC：
- Published：2018
- Accepted：
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摘要

Abstract

The catalytic performance of commonly used heteropolyacids (H

SiW

and H

PMo

) for the synthesis of 4

4'-methylenedianiline (4

4'-MDA) from aniline and formaldehyde was evaluated and the result showed that H

SiW

with moderate acid strength exhibited the best catalytic performance. Then H

SiW

@MIL-100(Fe) was prepared by encapsulating H

SiW

within the pores of MIL-100(Fe) to facilitate its recovery and reuse. The prepared H

SiW

@MIL-100(Fe) was characterized by means of FT-IR

adsorption-desorption

XRD

TG and then the catalytic performance was evaluated. The result showed that H

SiW

was highly dispersed in the pores of MIL-100(Fe)

and both the Keggin structure of H

SiW

and the crystal skeleton structure of MIL-100(Fe) could be effectively preserved. Furthermore

SiW

@MIL-100(Fe) showed exce

llent catalytic performance under the following reaction conditions:a molar ratio of aniline to formaldehyde=5

a mass ratio of catalyst to formaldehyde=1.2

a reaction temperature of 120℃ and a reaction time of 6 h. Under the above reaction conditions

the conversion of aniline was 41.1%

and the yield and selectivity of 4

4'-MDA were 81.6% and 79.2%

respectively. Unfortunately

an appreciable loss in the catalytic activity of the recovered H

SiW

@MIL-100(Fe) was observed because of the blocking of the pores and the change of the acidity resulted from the adsorption of alkaline organics such as aniline and 4

4'-MDA. The adsorbed alkaline organics could be cleaned up when the recovered catalyst was washed by methanol and DMF. Then the catalyst was effectively reused up to three cycles without much loss in its activity.

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