Chem. J. Chinese Universities ›› 2021, Vol. 42 ›› Issue (5): 1589.doi: 10.7503/cjcu20200303
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WANG Changyao, WANG Shuai, DUAN Linlin, ZHU Xiaohang, ZHANG Xingmiao, LI Wei()
Received:
2020-05-28
Online:
2021-05-10
Published:
2020-09-24
Contact:
LI Wei
E-mail:weilichem@fudan.edu.cn
Supported by:
CLC Number:
TrendMD:
WANG Changyao, WANG Shuai, DUAN Linlin, ZHU Xiaohang, ZHANG Xingmiao, LI Wei. In situ Confinement Growth Strategy for Ordered Mesoporous Carbon Support Ultrasmall MoO3 Nanoparticles[J]. Chem. J. Chinese Universities, 2021, 42(5): 1589.
Fig.2 TGA curves of the OMC?US?MoO3 composites with different MoO3 contents obtained after pyrolysis at 600 ℃, respectivelyMass fraction of MoO3(%): a. 4; b. 7; c. 10; d. 16; e. 27.
Sample No. | MoO3 content(%, mass fraction) | SBET/(m2·g-1) | V/(cm3·g-1) | D/nm |
---|---|---|---|---|
1 | 4 | 796 | 0.62 | 4.7 |
2 | 7 | 693 | 0.54 | 5.7 |
3 | 10 | 652 | 0.49 | 5.5 |
4 | 16 | 574 | 0.41 | 5.4 |
5 | 27 | 428 | 0.27 | 4.6 |
Table 1 Structural and textural parameters for OMC-US-MoO3 with different content
Sample No. | MoO3 content(%, mass fraction) | SBET/(m2·g-1) | V/(cm3·g-1) | D/nm |
---|---|---|---|---|
1 | 4 | 796 | 0.62 | 4.7 |
2 | 7 | 693 | 0.54 | 5.7 |
3 | 10 | 652 | 0.49 | 5.5 |
4 | 16 | 574 | 0.41 | 5.4 |
5 | 27 | 428 | 0.27 | 4.6 |
Fig.3 SAXS(A) and WA?XRD(B) patterns of the OMC?US?MoO3 composites with different MoO3 contents obtained after pyrolysis at 600 ℃Mass fraction of MoO3(%): a. 4; b. 7; c. 10; d. 16; e. 27.
Fig.4 N2 adsorption?desorption isotherms(A) and pore size distributions(B) of the OMC?US?MoO3 composites with different MoO3 contents obtained after pyrolysis at 600 ℃Mass fraction of MoO3(%): a. 4; b. 7; c. 10; d. 16; e. 27.
Fig.5 SEM images of OMC?US?MoO3 composites with different MoO3 contents obtained after pyrolysis at 600 ℃Mass fraction of MoO3(%): (A) 4; (B) 7; (C) 10; (D) 16;(E) 27.
Fig.6 TEM images of OMC?US?MoO3?7 composites obtained after pyrolysis at 600 ℃Viewed along the hexagonal(A) and columnar(B, C) directions and HRTEM image(D) of a representative MoO3 nanoparticle.
Catalyst | Time/h | Conv.(%) | Epoxide sel.(%) | TOF/h-1 |
---|---|---|---|---|
OMC-US-MoO3-7 | 2 | 52 | >99 | 2163 |
MoO3/C | 2 | 80 | 100 | 53[ |
MoO3/SiO2 | 6 | 90 | 100 | 72[ |
Mo-MOFs | 7 | 93 | 99 | 270[ |
Mo-MCM-41 | 3 | 97 | 95 | 22[ |
Mo-SBA-15 | 3 | 99 | 93 | 40[ |
[PiperazinCH2{MoO2(Salen)}]n | 12 | 95 | 98 | 16[ |
MNP30-Si-inic-Mo | 24 | 46 | 100 | 2[ |
Table 2 Calculating TOF value for epoxidation of cyclooctene and comparing with other catalysts*
Catalyst | Time/h | Conv.(%) | Epoxide sel.(%) | TOF/h-1 |
---|---|---|---|---|
OMC-US-MoO3-7 | 2 | 52 | >99 | 2163 |
MoO3/C | 2 | 80 | 100 | 53[ |
MoO3/SiO2 | 6 | 90 | 100 | 72[ |
Mo-MOFs | 7 | 93 | 99 | 270[ |
Mo-MCM-41 | 3 | 97 | 95 | 22[ |
Mo-SBA-15 | 3 | 99 | 93 | 40[ |
[PiperazinCH2{MoO2(Salen)}]n | 12 | 95 | 98 | 16[ |
MNP30-Si-inic-Mo | 24 | 46 | 100 | 2[ |
Fig.8 Time course plots of cyclooctene epoxidation(A) and reusability(B) by using OMC?US?MoO3?7 composites as catalystReaction conditions: 40.0 mmol of cyclooctene, 40.0 mmol of 5.5 mol/L TBHP in decane, 10 mg of OMC-US-MoO3-7 catalyst(0.0048 mmol/L of MoO3), 6.0 g of 1,2-dichloroethane as solvent, and 15.0 mmol of chlorobenzene as internal standard. The reaction temperature is 80 ℃.
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