钒渣酸浸提铁工艺优化及复合光催化剂的制备

doi:10.16085/j.issn.1000-6613.2023-2241

摘要/Abstract

摘要：

钒渣来自转炉钒渣，含有大量铁元素，它的二次利用具有重大的经济价值与现实意义。本文以H₂SO₄为酸浸液，利用响应面法优化酸浸工艺参数，后通过煅烧-水热法成功制备出ɑ-Fe₂O₃/Bi₂WO₆复合光催化剂，在模拟可见光作用下光降解染料废水甲基橙（MO）。结果表明，响应面优化酸浸实验的最佳工艺参数为H₂SO₄浓度2.8mol/L、酸浸温度98℃、酸浸时间138min、固液比1∶4.2，钒渣中Fe的浸出率为71.0%；以钒渣为铁源，采用沉淀-煅烧法制备出α-Fe₂O₃后，通过水热法合成VS-Fe₂O₃/Bi₂WO₆，其光降解性能明显优于商业Fe₂O₃/Bi₂WO₆，VS-Fe₂O₃的最佳掺杂量为10％，当H₂O₂投加量为19.58mmol/L、pH=6.5、催化剂投加量为0.4g/L、MO初始浓度为10mg/L、光反应6h时，MO去除率达96%，COD去除率为88.4%，出水COD为13.34mg/L，符合《污水综合排放标准》一级标准，光反应速率常数为纯相Bi₂WO₆的4.8倍；MO的降解机理主要为H₂O₂协同VS-Fe₂O₃/Bi₂WO₆作用下的光芬顿反应。本文可为钒渣高效、清洁的资源化利用及其在光催化领域的资源化利用提供参考。

关键词: 钒渣, 酸浸, 响应面, 光催化, 钨酸铋

Abstract:

Vanadium slag, derived from converter vanadium slag, contains a large amount of iron, and its secondary utilization has significant economic value and practical significance. In this paper, H₂SO₄was used as the acid leaching solution, and the response surface method was used to optimize the acid leaching process parameters. Subsequently, the α-Fe₂O₃/Bi₂WO₆ composite photocatalyst was successfully prepared by the calcination-hydrothermal method for the photodegradation of methyl orange (MO), a dye wastewater, under simulated visible light. The results showed that the optimal process parameters for acid leaching were as follows: H₂SO₄concentration of 2.8mol/L, acid leaching temperature of 98℃, acid leaching time of 138min and solid-liquid ratio of 1∶4.2. Under these optimal parameters, the iron leaching efficiency from vanadium slag was 71.0%. After preparing α-Fe₂O₃ from vanadium slag using a precipitation-calcination method, the photodegradation performance of the VS-Fe₂O₃/Bi₂WO₆ composite synthesized via hydrothermal treatment was found to be significantly superior to that of the commercial Fe₂O₃/Bi₂WO_6. The optimal doping amount of VS-Fe₂O₃was 10%. When the H₂O₂dosage was 19.58mmol/L, pH was 6.5, catalyst dosage was 0.4g/L, initial concentration of wastewater was 10mg/L and photoreaction was carried out for 6h, the removal rate of MO was 96% and the COD removal rate was 88.4%. The effluent COD concentration of 13.34mg/L met the requirements of the “Integrated Wastewater Emission Standard” level A standard and the rate constant ofthe photoreaction was 4.8 times that of the pure Bi₂WO₆phase. The degradation mechanism of MO was primarily due to the photo-Fenton reaction under the action of H₂O₂ synergistic VS-Fe₂O₃/Bi₂WO₆. This paper can provide a reference for the efficient and clean resource utilization of vanadium slag and its resource utilization in photocatalysis.

Key words: vanadium slag, acid leaching, response surface, photocatalysis, Bi₂WO₆

中图分类号:

TD98

蒋莉萍, 张雪乔, 钟晓娟, 魏于凡, 肖利, 郭旭晶, 羊依金. 钒渣酸浸提铁工艺优化及复合光催化剂的制备[J]. 化工进展, 2025, 44(1): 538-548.

JIANG Liping, ZHANG Xueqiao, ZHONG Xiaojuan, WEI Yufan, XIAO Li, GUO Xujing, YANG Yijin. Optimization of acid leaching process of iron from vanadium slag and preparation of composite photocatalysts[J]. Chemical Industry and Engineering Progress, 2025, 44(1): 538-548.

图/表 14

参考文献 37

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因素	水平
因素	-1	0	1
H₂SO₄浓度（A）/mol·L^-1	2	2.5	3
酸浸温度（B）/℃	90	100	110
酸浸时间（C）/min	100	120	140
固液比（D）/g·mL^-1	1∶3	1∶4	1∶5

因素	水平
因素	-1	0	1
H₂SO₄浓度（A）/mol·L^-1	2	2.5	3
酸浸温度（B）/℃	90	100	110
酸浸时间（C）/min	100	120	140
固液比（D）/g·mL^-1	1∶3	1∶4	1∶5

来源	平方和	自由度	均方	F	P	显著性
模型	2678.23	14	191.30	41.55	<0.0001	显著
H₂SO₄浓度（A）	1359.58	1	1359.58	295.32	<0.0001
酸浸温度（B）	387.15	1	387.15	84.09	<0.0001
酸浸时间（C）	59.59	1	59.59	12.94	0.0029
固液比（D）	164.06	1	164.06	35.64	<0.0001
AB	23.47	1	23.47	5.10	0.0404
AC	0.44	1	0.44	0.096	0.7612
AD	2.06	1	2.06	0.45	0.5145
BC	0.060	1	0.060	0.013	0.9107
BD	0.010	1	0.010	0.002	0.9635
CD	3.76	1	3.76	0.82	0.3812
A²	660.86	1	660.86	143.55	<0.0001
B²	56.07	1	56.07	12.18	0.0036
C²	25.11	1	25.11	5.45	0.0349
D²	68.46	1	68.46	14.87	0.0017
残差	64.45	14	4.60
失拟项	53.55	10	5.35	1.96	0.2693	不显著
纯误差	10.90	4	2.73
总和	2742.68	28

来源	平方和	自由度	均方	F	P	显著性
模型	2678.23	14	191.30	41.55	<0.0001	显著
H₂SO₄浓度（A）	1359.58	1	1359.58	295.32	<0.0001
酸浸温度（B）	387.15	1	387.15	84.09	<0.0001
酸浸时间（C）	59.59	1	59.59	12.94	0.0029
固液比（D）	164.06	1	164.06	35.64	<0.0001
AB	23.47	1	23.47	5.10	0.0404
AC	0.44	1	0.44	0.096	0.7612
AD	2.06	1	2.06	0.45	0.5145
BC	0.060	1	0.060	0.013	0.9107
BD	0.010	1	0.010	0.002	0.9635
CD	3.76	1	3.76	0.82	0.3812
A²	660.86	1	660.86	143.55	<0.0001
B²	56.07	1	56.07	12.18	0.0036
C²	25.11	1	25.11	5.45	0.0349
D²	68.46	1	68.46	14.87	0.0017
残差	64.45	14	4.60
失拟项	53.55	10	5.35	1.96	0.2693	不显著
纯误差	10.90	4	2.73
总和	2742.68	28

VS		VS_残渣
氧化物	质量分数/%	氧化物	质量分数/%
Fe₂O₃	45.32	Fe₂O₃	5.02
SiO₂	19.57	SiO₂	81.56
V₂O₅	8.31	V₂O₅	0.34
Al₂O₃	4.22	Al₂O₃	4.20
MnO	6.47	MnO	1.11
TiO₂	5.60	TiO₂	1.02
MgO	4.10	MgO	1.60
Cr₂O₃	2.95	Cr₂O₃	1.10
CaO	2.14	CaO	3.35
NiO	1.30	NiO	0.65