Preparation and Application of Carbon Nanofibers-supported Palladium Nanoparticles Catalysts Based on Electrospinning

doi:10.15541/jim20130556

Abstract

Abstract:

Carbon nanofibers-supported palladium nanoparticle catalysts were prepared by electrospinning, chemical reduction and the subsequent high temperature carbonization methods. The experiments were carried out to investigate the influence of different reducing agents (sodium borohydride, hydrazine hydrate and hydrogen gas) on morphology of palladium nanoparticles and carbon nanofibers in detail. Catalysts were characterized by UV-Vis spectra, X-ray diffraction, fourier transform infrared spectrum, scanning electron microscope, field emission transmission electron microscope. Results show that the palladium nanoparticles are distributed uniformly on the carbon nanofibers with dimension of about 7 nm, and the catalyst is relatively flexible by using hydrogen gas as reducing agent. Then it was applied to the Heck coupling reaction to test catalytic properties and recyclability. Results indicate that the catalyst possesses excellent stability and recyclability.

Key words: electrospinning, palladium nanoparticles, Pd NPs/CNFs, Heck reaction

CLC Number:

O643

GUO Li-Ping, BAI Jie, LIANG Hai-Ou, LI Chun-Ping, SUN Wei-Yan, MENG Qing-Run. Preparation and Application of Carbon Nanofibers-supported Palladium Nanoparticles Catalysts Based on Electrospinning[J]. Journal of Inorganic Materials, 2014, 29(8): 814-820.

Figures/Tables 9

Fig.1 UV-vis diffuse reflection spectra of Pd NPs/PAN reduced by different reducing agents (A) Sodium borohydride; (B) Hydrazine hydrate; (C) Hydrogen gas

Fig. 2 XRD patterns of Pd NPs/CNFs catalysts prepared with different reducing agents (A) Sodium borohydride; (B) Hydrazine hydrate; (C) Hydrogen gas

Fig.3 FTIR spectra of PdCl2/PAN nanofibers (A) and Pd NPs/CNFs catalysts (B, C, D) prepared with different reducing agents (B) Sodium borohydride; (C) Hydrazine hydrate; (D) Hydrogen gas

Fig. 4 SEM images of PdCl2/PAN nanofibers(a) and Pd NPs /PAN nanofibers (b, c, d) prepared with different reducing agents (b) Sodium borohydride; (c) Hydrazine hydrate; (d) Hydrogen gas

Fig. 5 SEM images of Pd NPs/CNFs catalysts prepared with different reducing agents (a) Sodium borohydride; (b) Hydrazine hydrate; (c) Hydrogen gas

Fig. 6 TEM images of Pd NPs/CNFs catalysts prepared with different reducing agents (a) Sodium borohydride; (b) Hydrazine hydrate; (c) Hydrogen gas

Table 1 Comparative product yields for iodobenzene with methyl acrylate under series of catalysts

Catalyst	Temperature /℃	Reaction time /h	Catalyst /g	Conversion rate /%	Selectivity /%
a	150	10	0.0305	100	97.50
b	150	10	0.0307	100	96.09
c	150	10	0.0301	100	94.56

Table 2 Recycling experiments using Pd NPs/CNFs catalyst in the Heck coupling reaction of iodobenzene and methyl acrylate

Run	Temperature /℃	Reaction time /h	Catalyst /g	Conversion rate /%	Selectivity /%
1	150	10	0.0301	100	94.56
2	150	10	0.0300	100	96.24
3	150	10	0.0298	100	98.21
4	150	10	0.0296	100	98.43
5	150	10	0.0297	100	98.25

Fig. 7 TEM image and particle diameter distribution histograms of Pd NPs before (A) and after (B) being catalyzed the Heck reaction five times

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