高孔隙率生物炭研制及其处理废水中磷酸盐

李佳璇; 王平; 万斯; 陈润华

doi:10.13801/j.cnki.fhclxb.20230131.001

高孔隙率生物炭研制及其处理废水中磷酸盐

doi: 10.13801/j.cnki.fhclxb.20230131.001

李佳璇¹,
王平^1, ,,
万斯²,
陈润华^1, ,

1.
中南林业科技大学环境科学与工程学院，长沙 410007
2.
湖南有色金属研究院有限责任公司，长沙 410100

基金项目: 湖南省自然科学基金重大项目(2021JC0001)；湖南省自然科学基金面上项目(2022JJ31014)；湖南省科技创新引领计划项目(2021GK4059；2020SK2006)；湖南省环保厅环保科研项目(HBKT-2022010)；湖南省教育厅科学研究项目(22A0193)

详细信息

通讯作者:
王平，博士，教授，博士生导师，研究方向为水土污染控制　E-mail：csfuwp@163.com

陈润华，博士，副教授，硕士生导师，研究方向为功能材料的研发与应用　E-mail：chen12@csuft.edu.cn

中图分类号: X703；TB33
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出版历程
- 收稿日期: 2022-11-30
- 修回日期: 2023-01-04
- 录用日期: 2023-01-08
- 网络出版日期: 2023-02-01
- 刊出日期: 2023-11-01

High porosity biochar and its treatment of phosphate in wastewater

LI Jiaxuan¹,
WANG Ping^{1
, ,},
WAN Si²,
CHEN Runhua^{1
, ,}

1.
College of Environmental Science and Engineering, Central South University of Forestry and Technology, Changsha 410007, China
2.
Hunan Research Institute for Nonferrous Metals CO., LTD., Changsha 410100, China

Funds: Major Program Natural Science Foundation of Hunan Province of China (2021JC0001); Natural Science Foundation of Hunan Province (2022JJ31014); Hunan Provincial Key Research Plan Program of China (2021GK4059; 2020SK2006); Environmental Research Project of Hunan Environmental Protection Department (HBKT-2022010); Hunan Provincial Education Department Scientific Research Project (22A0193)

摘要

摘要: 生物炭是缺氧状态下生物质热解的产物；然而，常见的生物炭表面积小、孔隙结构不发达、表面活性基团少，吸附效果差。本文以高粱(GC)和柚子皮(YC)为原料，利用4种物质进行表面处理制备得到生物炭，其中制备的高粱/KOH(GC-KH)和柚子皮/KOH(YC-K)粉末表面孔状明显，证实了该工艺的可行性。GC-KH比表面积为2096.05 m²/g，平均孔径4.12 nm，在其表面含有丰富的含氧官能团，为吸附提供了良好的结构空间和活性位点。通过批量实验，探讨了不同因素对磷酸盐吸附的影响，评估了离子强度。等温线结果表明GC-KH对磷酸盐的吸附发生在单分子层表面，在pH值为7时GC-KH对磷酸盐最大吸附能力为74.73 mg/g，具有反应迅速等显著优势，为废水中磷酸盐的高效去除提供了创新路径。
- 生物炭 /
- 比表面积 /
- 磷酸盐 /
- 改性材料 /
- 吸附
Abstract: Biochar is a product of pyrolysis of biomass under anoxic conditions; however, common biochar has a small surface area, underdeveloped pore structure, few surface active groups, and poor adsorption effect. In this work, biochar was prepared from sorghum (GC) and grapefruit peel (YC) by surface treatment using four substances to obtain biochar, where the prepared sorghum/KOH (GC-KH) and grapefruit peel/KOH (YC-K) powders had obvious surface porosity, confirming the feasibility of the process. With a specific surface area of 2096.05 m²/g and an average pore size of 4.12 nm, GC-KH is rich in oxygen-containing functional groups on its surface, providing a good structural space and active sites for adsorption.The effect of different factors on phosphate adsorption was explored by batch experiments to assess the ionic strength. Results of isotherms showed that the adsorption of phosphate by GC-KH occurred on the surface of the monomolecular layer, and the maximum adsorption capacity of phosphate by GC-KH was 74.73 mg/g at pH=7. It has significant advantages such as rapid response, which provides an innovative pathway for the efficient removal of phosphate from wastewater.
- biochar /
- specific surface /
- phosphate /
- modified materials /
- adsorption

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图 1 高粱(GC)和柚子皮(YC)粉末制备生物炭的工艺流程

Figure 1. Process flow diagram for the preparation of biochar from sorghum (GC) and grapefruit peel (YC) powder

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图 2 不同倍数下高粱粉末 ((a), (b))、GC-H ((c), (d)) 和GC-S ((e), (f)) 的SEM图像

Figure 2. SEM images of sorghum powder ((a), (b)), GC-H ((c), (d)) and GC-S ((e), (f)) at different magnifications

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图 3 高粱粉末、GC-H和GC-S的孔径分布图 ((a)~(c)) 和N₂吸附脱附等温线 ((e)~(g))

STP— Standard temperature and pressure

Figure 3. Pore size distribution ((a)-(c)) and N₂ adsorption and desorption isotherms ((e)-(g)) of sorghum powder, GC-H and GC-S, respectively

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图 4 不同倍数下GC-Na ((a), (b))、GC-KC ((c), (d))、GC-KO ((e), (f)) 和GC-KH ((g), (h)) 的SEM图像

Figure 4. SEM images of GC-Na ((a), (b)), GC-KC ((c), (d)), GC-KO ((e), (f)) and GC-KH ((g), (h)) at different magnifications

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图 5 GC-Na、GC-KC、GC-KO和GC-KH的孔径分布图 ((a)~(d)) 和N₂吸附脱附等温线 ((e)~(h))

Figure 5. Pore size distribution ((a)-(d)) and N₂ adsorption and desorption isotherms ((e)-(h)) of GC-Na, GC-KC, GC-KO and GC-KH respectively

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图 6 高粱粉末、GC-S和GC-KH的FTIR图谱

Figure 6. FTIR spectras of sorghum powder, GC-S and GC-KH

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图 7 不同倍数下柚子皮粉末 ((a), (b))、YC ((c), (d)) 和YC-K ((e), (f)) 的SEM图像

Figure 7. SEM images of grapefruit peel powder ((a), (b)), YC ((c), (d)) and YC-K ((e), (f)) at different magnifications

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图 8 柚子皮粉末、YC和YC-K的孔径分布图 ((a)~(c)) 和N₂吸附脱附等温线 ((e)~(g))

Figure 8. Pore size distribution ((a)-(c)) and N₂ adsorption and desorption isotherms ((e)-(g)) of grapefruit peel powder, YC and YC-K, respectively

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图 9 GC-KH投加量 (a)、pH (b)、共存离子 (c)、不同温度下反应时间(d)和不同温度下初始浓度 (e) 对GC-KH吸附磷酸盐效果的影响

Figure 9. Effect of GC-KH dosage (a), pH (b), coexisting ions (c), reaction time at different temperatures (d), initial concentration at different temperatures (e) on the effect of phosphate adsorption by GC-KH

m—Mass; q_t—Amount adsorbed at time t; q_e—Amount adsorbed when adsorption equilibrium is reached; C_e—Concentration of pollutant in the solution after removal; C₀—Initial concentration

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图 10 GC-KH吸附磷酸盐的伪一阶动力学模型 (a)、伪二阶动力学模型 (b)；不同温度下GC-KH吸附磷酸盐的Langmuir模型和Freundlich模型 (c)、D-R模型 (d) 及热力学 (f)

Figure 10. Pseudo-first-order kinetic model (a) and Pseudo-second-order kinetic model (b) for phosphate adsorption by GC-KH; Langmuir and Freundlich models (c), D-R model (d) and thermodynamics (f) of phosphate adsorption by GC-KH at different temperatures

θ—Isotherm constant; T—Absolute temperature; K_d—Thermodynamic equilibrium constant

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表 1 产物及其说明

Table 1. Products and their descriptions

Sample	Description
GC-H	Sorghum powder carbonised product after water treatment
GC-S	Sorghum powder carbonised product after FeSO₄ treatment
GC-Na	GC-S activated product after Na₂C₂O₄ treatment
GC-KC	GC-S activated by K₂C₂O₄ treatment
GC-KO	GC-S activated product after CH₃COOK treatment
GC-KH	GC-S activated by KOH treatment
YC	Pomelo peel powder carbonised by FeSO₄ treatment
YC-K	YC activated product after KOH treatment

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表 2 生物炭的比表面积(BET)表征结果

Table 2. Brunauer Emmett Teller (BET) characterization results of biochar

Sample	Surface aera^a/ (m²·g⁻¹)	Pore diameter^b/ nm	Pore volume^c/ (cm³·g ⁻¹)
Sorghum powder	11.8903000	15.61590	0.023938
GC-H	65.1037000	10.83450	0.048291
GC-S	189.3184000	5.79140	0.115718
GC-Na	437.8670000	7.69350	0.350280
GC-KC	737.9431000	3.28920	0.353356
GC-KO	565.2083000	3.85950	0.307675
GC-KH	2096.0475000	4.11660	1.000354
Grapefruit peel powder	8.7806000	5.91190	0.010157
YC	144.5847000	2.76330	0.070626
YC-K	1059.8472000	2.55870	0.511210
Notes: a—BET multi-point method specific surface; b—Barret-Joyner-Halenda (BJH) method desorption (cylindrical hole model) average hole diameter; c—BJH method desorption (cylindrical pore model, 2.0-49.6 nm) pore volume.

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表 3 GC-KH吸附磷酸盐的伪一阶和伪二阶动力学参数

Table 3. Pseudo-first- and Pseudo-second-order kinetic parameters for phosphate adsorption by GC-KH

Sample	Pseudo-first-order model			Pseudo-second-order model
Sample	q_cal/(mg·g⁻¹)	k₁/(min⁻¹)	R²	q_cal/(mg·g⁻¹)	k₂/(g·mg⁻¹·min⁻¹)	R²
GC-KH (15℃)	7.6071	0.0275	0.9649	12.3916	0.0807	0.9948
GC-KH (25℃)	15.1653	0.0310	0.9689	17.3974	0.0575	0.9939
GC-KH (35℃)	17.9383	0.0288	0.9712	21.8818	0.0457	0.9971
Notes: q_cal—Adsorption capacity at equilibrium time; k₁ and k₂—Reaction rate constants of pseudo-first-order and pseudo-second-order equations, respectively; R²—Correlation coefficient.

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表 4 GC-KH吸附磷酸盐的Langmuir、Freundlich和D-R等温线参数

Table 4. Langmuir, Freundlich and D-R isotherm parameters for phosphate adsorption by GC-KH

Sample	Langmuir			Freundlich			D-R
Sample	q_m/(mg·g⁻¹)	K_L/(L·mg⁻¹)	R²	K_F/(mg·g⁻¹)	n	R²	q_m/(mol·g⁻¹)	E/(kJ·mol⁻¹)	R²
GC-KH (15℃)	44.79	0.0879	0.9829	8.45	2.72	0.9121	3.3532	5.64	0.8702
GC-KH (25℃)	49.92	0.1250	0.9738	12.21	3.12	0.9419	4.0295	7.68	0.8997
GC-KH (35℃)	74.73	0.1694	0.9445	22.87	3.59	0.9104	5.9133	11.57	0.8876
Notes: q_m—Maximum adsorption capacity of Langmuir; K_L—Langmuir adsorption constant; K_F—Freundlich adsorption constant; n—Constant related to the adsorption strength; E—Reactive energy.

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表 5 GC-KH吸附磷酸盐的热力学参数

Table 5. Thermodynamic parameters of phosphate adsorption by GC-KH

C/(mg L⁻¹)	ΔH/(kJ·mol⁻¹)	ΔS/(J·mol⁻¹·K⁻¹)	ΔG/(kJ·mol⁻¹)
C/(mg L⁻¹)	ΔH/(kJ·mol⁻¹)	ΔS/(J·mol⁻¹·K⁻¹)	15℃	25℃	35℃
20	86.5333	311.6134	−89.6581	−92.7743	−95.8904
30	72.9616	257.7752	−74.1663	−76.7441	−79.3218
40	30.8975	113.1529	−32.5572	−33.6887	−34.8202
50	36.3046	128.6047	−37.0018	−38.2879	−39.5739
60	39.3341	137.6547	−39.6052	−40.9818	−42.3583
80	34.9713	120.6423	−34.7100	−35.9164	−37.1229
100	32.4302	109.8654	−31.6088	−32.7075	−33.8061
Notes: C—Initial concentration; ΔG—Gibbs free energy change; ΔH—Enthalpy change; ΔS—Entropy change.

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