羊粪炭对水体氮磷吸附条件的响应面优化及吸附机理研究

doi:10.16258/j.cnki.1674-5906.2023.12.013

生态环境学报 ›› 2023, Vol. 32 ›› Issue (12): 2216-2227.DOI: 10.16258/j.cnki.1674-5906.2023.12.013

羊粪炭对水体氮磷吸附条件的响应面优化及吸附机理研究

李卓轩¹(), 彭自然¹^,²^,^*(), 何文辉¹^,²^,³, 卫瑞璐¹, 高琳茜¹

1.上海海洋大学海洋生态与环境学院，上海 201306
2.水域环境生态上海高校工程研究中心，上海 201306
3.上海河湖生物链构建及资源化利用工程技术研究中心，上海 200433

收稿日期:2023-10-09 出版日期:2023-12-18 发布日期:2024-02-05
通讯作者: *彭自然。E-mail: zrpeng@shou.edu.cn
作者简介:李卓轩（1998年生），男，硕士研究生，研究方向为水污染控制及吸附材料。E-mail: zhuoxuan1998@163.com
基金资助:
水体污染控制与治理科技重大专项(2017ZX07205-003-R07);上海市科技计划项目(20DZ 2250700)

Response Surface Optimization and Adsorption Mechanism of Sheep Manure Charcoal on Nitrogen and Phosphorus Adsorption Conditions

LI Zhuoxuan¹(), PENG Ziran¹^,²^,^*(), HE Wenhui¹^,²^,³, WEI Ruilu¹, GAO Linxi¹

1. College of Marine Ecology and Environment, Shanghai Ocean University, Shanghai 201306, P. R. China
2. Shanghai University Engineering Research Center for Water Environment and Ecology, Shanghai 201306, P. R. China
3. Shanghai Engineering Research Center for Biochain Construction and Resource Utilization of Lakes and Rivers, Shanghai, 200433, P. R. China

Received:2023-10-09 Online:2023-12-18 Published:2024-02-05

摘要/Abstract

摘要：

为缓解水体富营养化，通过经济高效的方法降低水体氮磷含量，同时解决羊粪资源化利用问题，以羊粪球为原料在600 ℃下热解制备生物炭（YF600），利用Box-Behnken设计实验，研究浸渍比、pH、温度对YF600吸附水中NH₄⁺-N、NO₃⁻-N、PO₄³⁻-P效果的影响，运用响应面优化法确定最佳吸附条件。用吸附等温线中的Langmuir方程、Freundlich方程和吸附动力学的准一级方程、准二级方程对3种污染物的吸附过程进行拟合，并通过BET、FTIR、SEM-EDS、XRD、元素分析仪分析其理化性质和吸附机理。结果表明，对YF600吸附NH₄⁺-N、PO₄³⁻-P的影响显著性大小为：浸渍比>pH>温度，吸附NO₃⁻-N为：浸渍比>pH（温度影响不显著）。拟合出最佳吸附条件为浸渍比0.004，温度26.2 ℃，pH=6.77，此时NH₄⁺-N、NO₃⁻-N、PO₄³⁻-P的单位吸附量分别为14、2.08、4.93 mg∙g⁻¹，实验结果与预测值基本吻合，说明YF600复合吸附氮磷效果较好，该模型具有可行性。Langmuir方程拟合更好证明其以単分子层吸附为主；准二级动力学模型能更好地反映YF600的吸附效率。表征结果为YF600比表面积达63.91 m²∙g⁻¹，表面有大量褶皱且分布着不规则微孔，含丰富的羧基、酯基、羟基等含氧官能团和Mg、Ca、Fe、Al、Na、Si等多种元素，且Ca²⁺、Mg²⁺含量高，O/C高，以上理化性质使其具备良好的脱氮除磷性能，其氮磷吸附机理主要为离子交换、静电吸附和络合沉淀作用。研究结果表明，YF600复合吸附多种不同形式氮磷效果良好且工艺简单、生产成本低，对YF600氮磷吸附机理进行了解释分析，旨在为羊粪资源化利用与羊粪炭优化污水处理工艺提供理论依据。

关键词: 生物炭, 羊粪, 铵态氮, 磷酸盐, 硝态氮, 响应面

Abstract:

In this study, biochar (YF600) was prepared through the pyrolysis of sheep dung at 600 ℃ to cost-effectively mitigate water eutrophication, lower nitrogen, and phosphorus levels, thus addressing the efficient utilization of sheep manure as a valuable resource. Box-Behnken design was used to investigate the effects of impregnation ratio, pH, and temperature on the adsorption of NH₄⁺-N, PO₄³⁻-P and NO₃⁻-N in water by YF600. The optimal adsorption conditions were determined using response surface methodology. The adsorption processes for the targeted pollutants were modeled using Langmuir and Freundlich isotherm equations. Additionally, pseudo-first-order and pseudo-second-order kinetic equations were applied to characterize the adsorption kinetics. The adsorption mechanism was comprehensively characterized by BET, FTIR, SEM-EDS, XRD, and elemental analyzers. The results showed that the key factors influencing the adsorption of NH₄⁺-N, PO₄³⁻-P by YF600 were immersion ratio, pH, and temperature in turn. In the case of NO₃⁻-N adsorption, the immersion ratio was more influential than pH, with temperature was not significant. The optimal adsorption conditions were: immersion ratio of 0.004, temperature of 26.2 ℃, and a pH=6.77. Under these specified conditions, the respective adsorption capacities for NH₄⁺-N, NO₃⁻-N, and PO₄³⁻-P were found to be 14 mg∙g⁻¹, 2.08 mg∙g⁻¹, and 4.93 mg∙g⁻¹. These observations closely aligned with the predicted values, suggesting that YF600 effectively adsorbed nitrogen and phosphorus, supporting the feasibility of the model. Better fitness of the Langmuir equation suggested monolayer adsorption dominated. Meanwhile, the pseudo-second-order kinetic model better captured the adsorption efficiency of YF600. In addition, Our results revealed that YF600 possessed a specific surface area of 63.91 m²∙g⁻¹, featuring numerous folds on the surface and irregular micropores. The biochar was found to be rich in carboxyl, ester, hydroxyl, and other oxygen-containing functional groups, and it contained a variety of elements, including Mg, Ca, Fe, Al, Na, Si. Among these parameters, higher concentrations of Ca²⁺, Mg²⁺, and O/C ratio were observed. These physicochemical properties confer excellent nitrogen and phosphorus removal capabilities of YF600. The nitrogen and phosphorus adsorption mechanism of YF600 primarily involve ion exchange, electrostatic adsorption, and complex precipitation. This study demonstrated that YF600 effectively adsorbs various forms of nitrogen and phosphorus, offering a straightforward process with low production costs. The study provided a theoretical foundation for the resource utilization of sheep manure and optimization of sewage treatment processes through the application of sheep manure biochar.

Key words: biochar, sheep manure, ammonium nitrogen, phosphate, nitrate nitrogen, response surface

中图分类号:

TQ424
X52

李卓轩, 彭自然, 何文辉, 卫瑞璐, 高琳茜. 羊粪炭对水体氮磷吸附条件的响应面优化及吸附机理研究[J]. 生态环境学报, 2023, 32(12): 2216-2227.

LI Zhuoxuan, PENG Ziran, HE Wenhui, WEI Ruilu, GAO Linxi. Response Surface Optimization and Adsorption Mechanism of Sheep Manure Charcoal on Nitrogen and Phosphorus Adsorption Conditions[J]. Ecology and Environment, 2023, 32(12): 2216-2227.

图/表 19

参考文献 62

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标号	因素	水平
A	浸渍比	0.001、0.003、0.005
B	吸附温度/℃	20、25、30
C	pH	5、7、9

标号	因素	水平
A	浸渍比	0.001、0.003、0.005
B	吸附温度/℃	20、25、30
C	pH	5、7、9

序号	浸渍比	摄氏度/ ℃	pH	NH₄⁺-N 吸附量/ (mg∙g⁻¹)	PO₄³⁻-P 吸附量/ (mg∙g⁻¹)	NO₃⁻-N 吸附量/ (mg∙g⁻¹)
1	0.001	20	7	8.14	1.66	0.89
2	0.005	20	7	11.38	4.26	2.02
3	0.001	30	7	7.66	2.52	0.91
4	0.005	30	7	12.38	4.52	2.08
5	0.001	25	5	6.23	2.35	1.17
6	0.005	25	5	8.22	3.80	2.37
7	0.001	25	9	6.38	2.84	0.83
8	0.005	25	9	10.27	4.92	1.79
9	0.003	20	5	8.77	3.68	1.98
10	0.003	30	5	11.17	3.95	2.01
11	0.003	20	9	11.25	4.73	1.35
12	0.003	30	9	11.01	4.90	1.32
13	0.003	25	7	14.11	4.84	1.88
14	0.003	25	7	13.94	4.55	1.77
15	0.003	25	7	13.86	4.66	1.87
16	0.003	25	7	14.39	4.88	1.75
17	0.003	25	7	13.88	4.93	1.88

序号	浸渍比	摄氏度/ ℃	pH	NH₄⁺-N 吸附量/ (mg∙g⁻¹)	PO₄³⁻-P 吸附量/ (mg∙g⁻¹)	NO₃⁻-N 吸附量/ (mg∙g⁻¹)
1	0.001	20	7	8.14	1.66	0.89
2	0.005	20	7	11.38	4.26	2.02
3	0.001	30	7	7.66	2.52	0.91
4	0.005	30	7	12.38	4.52	2.08
5	0.001	25	5	6.23	2.35	1.17
6	0.005	25	5	8.22	3.80	2.37
7	0.001	25	9	6.38	2.84	0.83
8	0.005	25	9	10.27	4.92	1.79
9	0.003	20	5	8.77	3.68	1.98
10	0.003	30	5	11.17	3.95	2.01
11	0.003	20	9	11.25	4.73	1.35
12	0.003	30	9	11.01	4.90	1.32
13	0.003	25	7	14.11	4.84	1.88
14	0.003	25	7	13.94	4.55	1.77
15	0.003	25	7	13.86	4.66	1.87
16	0.003	25	7	14.39	4.88	1.75
17	0.003	25	7	13.88	4.93	1.88

参数	NH₄⁺-N吸附量/(mg∙g⁻¹)					PO₄³⁻-P吸附量/(mg∙g⁻¹)					NO₃⁻-N吸附量/(mg∙g⁻¹)
参数	平方和	自由度	F	P	显著性	平方和	自由度	F	P	显著性	平方和	自由度	F	P	显著性
模型	123.12	9	88.78	<1×10⁻⁴	极显著	17.1	9	40.60	<1×10⁻⁴	极显著	4.15	9	65.01	<1×10⁻⁴	极显著
A	23.95	1	155.43	<1×10⁻⁴	极显著	8.24	1	176.14	<1×10⁻⁴	极显著	2.12	1	419.04	<1×10⁻⁴	极显著
B	0.9	1	5.83	0.0465	显著	0.3	1	6.49	0.0383	显著	0.0046	1	0.16	0.7024
C	2.57	1	16.70	0.0047	极显著	1.61	1	34.39	6×10⁻⁴	极显著	0.011	1	107.84	<1×10⁻⁴	显著
AB	0.54	1	3.53	0.1022		0.089	1	1.91	0.2098		0.004	1	0.078	0.7884
AC	0.89	1	5.78	0.0472	显著	0.1	1	2.16	0.1855		2.25×10⁻⁸	1	2.32	0.1719
BC	1.74	1	11.31	0.012	显著	0.0028	1	0.059	0.8152		0.0012	1	0.15	0.7084
A²	50.4	1	327.05	<1×10⁻⁴	极显著	5.89	1	125.78	<1×10⁻⁴	极显著	1.32	1	40.79	<4×10⁻⁴	极显著
B²	1.98	1	12.83	0.0089	显著	0.5	1	10.72	0.0136	显著	0.01	1	9.13	0.0193	显著
C²	33.06	1	214.56	<1×10⁻⁴	极显著	0.054	1	1.15	0.3199		0.55	1	1.73	<0.2296	不显著
残差	1.08	7				0.33	7				0.013	7
失拟项	0.88	3	5.89	0.0598	不显著	0.22	3	2.82	0.1714	不显著	0.0079	3	1.97	0.2605	不显著
纯误差	0.2	4				0.11	4				0.0049	4
总误差	124.2	16				17.43	16				4.16	16

羊粪炭对水体氮磷吸附条件的响应面优化及吸附机理研究

Response Surface Optimization and Adsorption Mechanism of Sheep Manure Charcoal on Nitrogen and Phosphorus Adsorption Conditions

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污染物	CV/%	r²	r²_Adj	r²_Pred	精密度
Y₁	3.65	0.9913	0.9801	0.8842	26.862
Y₂	5.41	0.9812	0.957	0.7865	19.371
Y₃	4.68	0.9882	0.973	0.8797	28.447

参数	q_e(NH4+-N)/(mg∙g⁻¹)	q_e(PO4³⁻_-N)/(mg∙g⁻¹)	q_e(NO3⁻_-N)/(mg∙g⁻¹)
理论值	14.01	4.93	2.08
实际值1	14.00	4.91	1.98
实际值2	13.86	4.88	2.02
实际值3	13.98	4.88	2.01
平均值	13.95	4.89	2.00
偏差/%	0.4±0.64	0.77±0.28	3.5±1.1

污染物类型	Langmuir方程			Freundlich方程
污染物类型	q_m /(mg∙g⁻¹)	K_L/(L∙g⁻¹)	r²	K_F	1/n	r²
NH₄⁺-N	17.67	0.0116	0.9971	0.5215	0.6362	0.9931
NO₃⁻-N	2.46	0.1024	0.9706	0.9173	0.1997	0.937
PO₄³⁻-P	4.89	0.1621	0.9946	1.3657	0.3293	0.9644

污染物	拟一级动力学			拟二级动力学
污染物	q_e/(mg∙g⁻¹)	k₁	r²	q_e/(mg∙g⁻¹)	k₂	r²
NH₄⁺-N	5.56	0.4776	0.9695	9.59	0.2583	0.9977
NO₃⁻-N	1.29	0.3240	0.977	2.57	0.934	0.9972
PO₄³⁻-P	4.65	0.4653	0.9824	4.59	0.4266	0.9966

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