Preparation of Rice Husk Carbon-based Solid Acid Catalyst for the Dehydration of Xylose to Furfural†

doi:10.7503/cjcu20160040

Abstract

Abstract:

A carbon-based solid acid catalyst, prepared by the sulfonation of rice husk carbon, was proved to be an efficient and environmental benign catalyst for the dehydration of xylose to furfural. The catalyst was characterized by Fourier transform infrared spectroscopy(FTIR), elemental analysis and Scanning Electronic Microscopy(SEM). The total acid site concentrations of the catalyst samples were obtained using standard acid-base back titration. The acid site concentration of 1.03 mmol/g was obtained when the 4.0 g of rice husk carbon was sulfonated by 15 mL of H₂SO₄ at 150 ℃ for 8 h. The effects of solvent, reaction temperature and time on the dehydration of xylose to furfural catalyzed by the rice husk carbon-based solid acid catalyst were studied. The results indicate that the yield of furfural increases gradually with the increase of reaction temperature and with the prolonger of the reaction time. The catalytic performance of the synthesized catalyst is better when using DMSO as reaction solvent than that of using water as solvent. A maximum furfural yield of 75.8% was achieved. The repeated usability and regeneration of the catalyst was investigated.

Key words: Carbon-based solid acid catalyst, Sulfonation, Xylose, Furfural

CLC Number:

O643.3

TrendMD:

LIANG Yu, CHEN Zhihao, LIANG Baoyan, HU Zhe, YANG Xiaomin, WANG Zichen. Preparation of Rice Husk Carbon-based Solid Acid Catalyst for the Dehydration of Xylose to Furfural^†[J]. Chem. J. Chinese Universities, 2016, 37(6): 1123.

Figures/Tables 7

Fig.1 Effect of sulfonation time on the acid site density of rice husk-derived carbon-based solid acid catalystPreparation conditions: rice husk-based carbon(4.0 g), H2SO4(15 mL), 150 ℃.

Fig.2 FTIR spectrum of rice husk-derived carbon-based solid acid catalystPreparation conditions: rice husk-based carbon(4.0 g), H2SO4(15 mL), 150 ℃, 8 h.

Table 1 Elemental analysis of rice husk-derived carbon and rice husk-derived carbon-based solid acid catalyst*

Sample	Elemental content(%)
Sample	N	C	H	S
RHC	0.56	61.56	1.31	0.32
Catalyst	0.50	59.47	1.73	2.22

Fig.3 SEM image of rice husk-derived carbon-based solid acid catalystPreparation conditions: rice husk-based carbon(4.0 g), H2SO4(15 mL), 150 ℃, 8 h.

Table 2 Effect of reaction temperature on the dehydration of xylose to furfural*

Temperature/℃	120	140	160	180
Yield of furfural(%)	8.2	30.0	45.7	72.3

Table 3 Effect of reaction time on the dehydration of xylose to furfural*

Time/h	2	4	6	7	8
Yield off urfural(%)	36.3	45.7	51.4	58.8	75.8

Table 4 Reused ability of the catalyst*

Cycle	Yield of urfural(%)	Acid site density/(mmol·g^-1)
0	72.3	1.03
1	72.2	1.04
2	58.7	0.85
3	44.4	0.65

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