基于碱/硫脲协同活化制备多元掺杂活性炭

doi:10.3969/j.issn.0253-2417.2021.04.011

摘要/Abstract

摘要：

以葵花秆为原料，利用其自身含有的磷元素为磷源，硫脲为氮源、硫源，通过KOH、硫脲协同活化制备N、P、S三元掺杂活性炭。探讨了活化温度对掺杂活性炭吸附性能的影响，并通过氮气吸附-脱附等温线、X射线光电子能谱（XPS）分析了掺杂活性炭的孔隙结构及其表面化学性质；采用恒电流充放电（GCD）、循环伏安法（CV）考察了掺杂活性炭作为超级电容器电极材料的电化学性能。研究结果表明：随着活化温度的升高，掺杂活性炭的碘吸附值呈先上升后下降的趋势，活化温度900℃时碘吸附值达到最大，为2 080 mg/g。碱和硫脲的协同活化作用有利于促进掺杂活性炭比表面积和总孔容积的提高，活化温度900℃得到的样品P，T-900的比表面积和总孔容积高达2 517 m²/g和1.73 cm³/g。P，T-900含有较丰富的N、P和S，质量分数分别为1.9%、0.52%和2.46%。在6 mol/L KOH电解液中进行测试，当电流密度为1 A/g时，P，T-900的比电容达到259 F/g；当电流密度为10 A/g时，其比电容达230 F/g，初始电容保持率高达88.8%。

关键词: 碱/硫脲复合, 协同活化, 多元掺杂, 电化学性能, 活性炭

Abstract:

N, P and S multi-doped activated carbon was prepared from sunflower straw by the synergistic activation of KOH and thiourea with its own phosphorus element as phosphorus source, thiourea as nitrogen source and sulfur source. The effect of activation temperature on the adsorption performance of doped activated carbon was discussed. The pore structure and surface chemical properties of doped activated carbon were analyzed by nitrogen adsorption desorption isotherm and X-ray photoelectron spectroscopy(XPS); the electrochemical performance of doped activated carbon as electrode material for supercapacitor was investigate by galvanostatic dharge discharge(GCD) and cyclic voltammetry(CV). The results showed that as the increase of activation temperature, the iodine adsorption value of doped activated carbon increased first and then decreased; when the activation temperature was 900℃, the iodine adsorption value reached the maximum(2 080 mg/g). The synergistic activation of alkali and thiourea was beneficial to enhance the specific surface area and total pore volume of doped activated carbon, the specific surface area and total pore volume of doped activated carbon P, T-900, which was obtained under activation temperature 900℃, were 2 517 m²/g and 1.73 cm³/g, respectively. The doped activated carbon P, T-900 contained nitrogen(N), phosphorus(P) and sulfur(S) elements, and their mass fractions were 1.9%, 0.52% and 2.46% respectively. When the current density was 1 A/g, the specific capacitance of P, T-900 reached 259 F/g in 6 mol/L KOH electrolyte. When the current density was 10 A/g, the specific capacitance of P, T-900 reached 230 F/g, and the initial capacitance retention was as high as 88.8%.

Key words: alkali/thiourea composition, synergistic activation, multi-doped, electrochemical performance, activated carbon

中图分类号:

TQ35

王琼, 杨旋, 蔡政汉, 陈燕丹, 黄彪, 林冠烽. 基于碱/硫脲协同活化制备多元掺杂活性炭[J]. 林产化学与工业, 2021, 41(4): 77-84.

Qiong WANG, Xuan YANG, Zhenghan CAI, Yandan CHEN, Biao HUANG, Guanfeng LIN. Preparation of Multi-doped Activated Carbon Based on Alkali/Thiourea Synergistic Activation[J]. Chemistry and Industry of Forest Products, 2021, 41(4): 77-84.

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样品 samples	原料用量raw material amount/g			活化温度/℃ activation temp.	得率/% yield	碘吸附值/(mg·g^-1) iodine value
样品 samples	KOH	硫脲 thiourea	炭化料 carbonized material	活化温度/℃ activation temp.	得率/% yield	碘吸附值/(mg·g^-1) iodine value
P, T-800	15	5	5	800	23.2	1188.2
P, T-850	15	5	5	850	22.9	1832.9
P, T-900	15	5	5	900	22.3	2080.0
P, T-950	15	5	5	950	15.3	1850.9
P, T-1000	15	5	5	1000	12.7	1834.5
P-900	15	0	5	900	38.4	1684.4
T-900	0	5	5	900	18.0	644.8
C-900	0	0	5	900	41.3	789.7

样品 samples	S_BET/(m²·g^-1)	V_T/(cm³·g^-1)	V_micro/(cm³·g^-1)	V_meso/(cm³·g^-1)	d/nm
P, T-900	2517.2	1.73	0.14	1.59	2.75
P-900	1882.5	0.96	0.77	0.19	0.85
T-900	576.4	0.41	0.24	0.17	0.57
C-900	833.0	0.48	0.22	0.26	2.33

样品samples	C/%	O/%	P/%	N/%	S/%
P, T-900	79.00	16.11	0.52	1.90	2.46
P-900	78.63	18.73	0.69	1.46	0.50
T-900	78.86	12.69	0.62	6.56	1.27
C-900	88.26	9.65	0.38	1.47	0.24
C-500	66.16	29.99	0.48	3.11	0.27

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