碱炭比及活化温度对稻壳活性炭极微孔的影响

doi:10.15541/jim20140251

无机材料学报 ›› 2015, Vol. 30 ›› Issue (1): 17-22.DOI: 10.15541/jim20140251

碱炭比及活化温度对稻壳活性炭极微孔的影响

李大伟^{1, 2}, 马腾飞^{1, 3}, 田原宇^{1, 2}, 朱锡锋⁴, 乔英云²

(1. 中国石油大学(华东) 化工学院, 青岛266580; 2. 山东科技大学低碳能源化工重点实验室, 青岛 266590; 3. 中国石油天然气股份有限公司辽阳石化分公司, 辽阳 111003; 4. 中国科技大学安徽省生物质洁净能源重点实验室, 合肥 230026)

收稿日期:2014-05-13 修回日期:2014-07-13 出版日期:2015-01-20 网络出版日期:2014-12-29
作者简介:李大伟(1982–), 男, 讲师, 博士后. E-mail: lidaweicumt@126.com
基金资助:
国家自然科学基金(51206099);中国科学院重点部署项目(KGZD-EW-304-3);教育部新世纪优秀人才支持计划(NCET-11-1031)

Effects of Alkali/Char Ratio and Activation Temperature on Ultramicropores of Rice Husk Active Carbon

LI Da-Wei^{1, 2}, MA Teng-Fei^{1, 3}, TIAN Yuan-Yu^{1, 2}, ZHU Xi-Feng⁴, QIAO Ying-Yun²

(1. College of Chemical Engineering, China University of Petroleum (East China), Qingdao 266580, China; 2. Research Centre for Low-carbon Energy Sources, Shandong University of Science and Technology, Qingdao 266590, China; 3. PetroChina Liaoyang Petrochemical Company, Liaoyang 111003, China; 4. Key Laboratory for Biomass Clean Energy of Anhui Province, University of Science and Technology of China, Hefei 230026, China)

Received:2014-05-13 Revised:2014-07-13 Published:2015-01-20 Online:2014-12-29
About author:LI Da-Wei. E-mail: lidaweicumt@126.com
Supported by:
National Natural Science Foundation of China (51206099);Key Research Programof the Chinese Academy of Sciences (KGZD-EW-304-3);Program for New Century Excellent Talent in University of the Ministry of Education of China (NCET-11-1031)

摘要/Abstract

摘要：

采用N₂吸附、CO₂吸附和热重红外联用等技术手段, 考察了在KOH活化稻壳炭的过程中碱炭比和活化温度对活性炭极微孔的影响。结果表明: 在不同碱炭比(0.6︰1~3︰1)和活化温度(640~780℃)下制备的稻壳活性炭, 极微孔主要分布在0.42~0.70 nm。当碱炭比增加时, 极微孔孔容先增大后减小; 而当活化温度升高时, 极微孔孔容呈降低趋势。极微孔率随碱炭比或活化温度的升高而单调递减。在活化温度为640℃、碱炭比为1: 1时, 可得极微孔孔容为0.149 mL/g、极微孔率达36.3%的微孔活性炭。活性炭的极微孔孔容与其在10⁴Pa时的CO₂吸附量高度线性相关。

关键词: 活性炭, 极微孔, KOH, 稻壳

Abstract:

Porous carbons were prepared by KOH activation of rice husk char at alkali/char ratios of 0.6︰1 to 3︰1 and activation temperatures from 640℃ to 780 ℃. The obtained porous carbons were characterized using N₂ adsorption and desorption technique, CO₂ adsorption, TG-FTIR analyses. The results indicate that the ultramicropore size of the prepared porous carbons is mostly in the range of 0.42-0.70 nm. As the alkali/char ratio increases, the volume of ultramicropores first rises and then diminishes, whereas the volume of ultramicropores tends to decrease monotonously with the increase of activation temperature. A microporous carbon with ultramicropore volume of 0.149 mL/g, ultramicropore fraction of 36.3%, pore volume of 0.411 mL/g, and specific surface area of 774 m²/g, can be produced by activation at 640℃ at the alkali/char ratio of 1︰1. The ultramicropore volume of the porous carbons and their CO₂ uptake at 10⁴Pa display a strong linear relationship.

Key words: active carbon, ultramicropore, KOH, rice husk

中图分类号:

TQ424

李大伟, 马腾飞, 田原宇, 朱锡锋, 乔英云 . 碱炭比及活化温度对稻壳活性炭极微孔的影响[J]. 无机材料学报, 2015, 30(1): 17-22.

LI Da-Wei, MA Teng-Fei, TIAN Yuan-Yu, ZHU Xi-Feng, QIAO Ying-Yun. Effects of Alkali/Char Ratio and Activation Temperature on Ultramicropores of Rice Husk Active Carbon[J]. Journal of Inorganic Materials, 2015, 30(1): 17-22.

图/表 6

图 1 稻壳炭及活性炭的表征

Fig. 1 Characterizations for rice husk char and active carbons. (a) N2 adsorption/desorption isotherms; (b) Mesopore size distribution; (c) SEM image of rice husk char; (d) SEM image of K3-780

表 1 稻壳炭及活性炭的孔结构

Table 1 Textural properties of rice husk char and active carbons

	Sample	S_BET / (m²·g^-1)	V_t / (cm³·g^-1)	V_micro / (cm³·g^-1)	V_meso / (cm³·g^-1)	V_{<0.7 nm} / (cm³·g^-1)	V_{<1 nm} / (cm³·g^-1)	(V_micro / V_t) /%	(V_{<0.7 nm} / V_t) /%
	RHC	114	0.069	0.051	0.018	—	—	—	—
Effects of KOH/char ratio	K0.6-780	678	0.359	0.262	0.097	0.120	0.156	73.0	33.4
	K1-780	1199	0.600	0.479	0.121	0.139	0.196	79.8	23.1
	K2-780	1842	0.828	0.802	0.026	0.088	0.126	96.9	10.6
	K3-780	2695	1.137	1.106	0.031	0.078	0.117	97.3	6.9
Effects of activation temperature	K1-640	774	0.411	0.302	0.109	0.149	0.190	73.5	36.3
	K1-710	1041	0.527	0.422	0.105	0.149	0.202	80.1	28.3
	K1-780	1199	0.600	0.479	0.121	0.139	0.196	79.8	23.1

图 2 碱炭比对活性炭极微孔孔分布的影响

Fig. 2 Effects of alkali/char ratio on pore size distributions of ultramicropores of active carbons

图 3 活化温度对活性炭极微孔孔分布的影响

Fig. 3 Effects of activation temperature on pore size distributions of ultramicropores of active carbons

图 4 热解温度对稻壳炭(RHC)及含KOH稻壳炭(K1-0)重量及气体产物的影响

Fig. 4 Effects of heating temperature on mass and gaseous products of rice husk char (RHC) and KOH-containing char. (a) Thermogravimetric curves; FTIR spectra of gaseous products released at heating temperatures of 640℃(b), 710℃(c) and 780℃(d)

图 5 极微孔孔容与104 Pa下CO2吸附量的关系

Fig. 5 Relation between ultramicropore volume and CO2 uptake at 104 Pa

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碱炭比及活化温度对稻壳活性炭极微孔的影响

Effects of Alkali/Char Ratio and Activation Temperature on Ultramicropores of Rice Husk Active Carbon

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