废CeO x -MnO x 基SCR脱硝催化剂还原酸浸综合回收铈锰

doi:10.16085/j.issn.1000-6613.2021-2435

化工进展 ›› 2022, Vol. 41 ›› Issue (9): 5122-5131.DOI: 10.16085/j.issn.1000-6613.2021-2435

废CeO _x -MnO _x 基SCR脱硝催化剂还原酸浸综合回收铈锰

余正伟¹^,²^,³(), 张晓霞², 雷杰², 李澳², 王光应⁴, 丁祥¹, 龙红明¹^,²()

^1.冶金减排与资源综合利用教育部重点实验室（安徽工业大学），安徽马鞍山 243002
^2.安徽工业大学冶金工程学院，安徽马鞍山 243002
^3.冶金过程节能与污染控制安徽省教育厅工程技术研究中心，安徽马鞍山 243002
^4.安徽元琛环保科技股份有限公司，安徽合肥 230012

收稿日期:2021-11-26 修回日期:2022-04-12 出版日期:2022-09-25 发布日期:2022-09-27
通讯作者: 龙红明
作者简介:余正伟（1984—），男，博士，讲师，研究方向为固废资源化利用。E-mail：yuzhengwei@ahut.edu.cn。
基金资助:
国家自然科学基金(51704009);冶金减排与资源综合利用教育部重点实验室开放基金(JKF21-07);冶金过程节能与污染控制安徽省教育厅工程技术研究中心开放基金(GKF20-2)

Comprehensive recovery of cerium and manganese from waste CeO _x -MnO _x -based SCR denitrification catalysts by reductive acid leaching

YU Zhengwei¹^,²^,³(), ZHANG Xiaoxia², LEI Jie², LI Ao², WANG Guangying⁴, DING Xiang¹, LONG Hongming¹^,²()

^1.Key Laboratory of Metallurgical Emission Reduction & Resources Recycling (Anhui University of Technology), Ministry of Education, Maanshan 243002, Anhui, China
^2.School of Metallurgical Engineering, Anhui University of Technology, Maanshan 243002, Anhui, China
^3.Energy Saving and Pollution Control in Metallurgical Process Engineering Technology Research Center of Education Department of Anhui Province, Maanshan 243002, Anhui, China
^4.Anhui Yuanchen Environmental Protection Technology Company Limited, Hefei 230012, Anhui, China

Received:2021-11-26 Revised:2022-04-12 Online:2022-09-25 Published:2022-09-27
Contact: LONG Hongming

摘要/Abstract

摘要：

废选择性催化还原（SCR）脱硝催化剂中含有大量的有价金属，直接废弃易造成资源浪费及环境污染。以废CeO _x -MnO _x 基SCR脱硝催化剂为原料，采用热力学分析结合湿法冶金实验方法，研究了浸出条件对Ce、Mn元素浸出率的影响。结果表明，废催化剂直接酸浸Ce、Mn元素浸出率低，还原-酸浸Ce、Mn元素热力学条件上可行，抗坏血酸对Ce、Mn高价氧化物有明显的还原作用。当抗坏血酸质量分数为30%、硫酸浓度2mol/L、液固比6∶1、搅拌速度350r/min、80℃恒温反应5h时，Ce、Mn的浸出率分别达到92.09%、95.51%。加入抗坏血酸后，部分Ce⁴⁺和Mn⁴⁺还原为Ce³⁺和Mn²⁺，Ce⁴⁺/Ce的比值由75.82%降低到71.62%，Mn⁴⁺/Mn的比值由29.39%降低到27.17%，同时削弱了高价Ce辅助低价Mn向高价Mn转化的作用，使得Ce、Mn高效浸出，为CeO _x -MnO _x 基废催化剂中Ce、Mn资源化利用奠定了基础。

关键词: 选择催化还原, 废催化剂, 酸浸, 还原, 回收, 资源化利用

Abstract:

Waste selective catalytic reduction (SCR) denitrification catalyst contains amounts of valuable metals, which directly landfill will cause resources waste and environmental pollution. The effects of leaching conditions on selective acid leaching of Ce and Mn elements from waste CeO _x -MnO _x SCR denitrification catalyst were investigated by thermodynamic analysis and hydrometallurgy experimental study. The results confirmed that the direct-acid leaching rates of Ce and Mn from waste CeO _x -MnO _x SCR catalyst were very low, the reduction-acid leaching of Ce and Mn was feasible under thermodynamic conditions, and the ascorbic acid had obvious reduction effect on Ce and Mn high-valence oxides. When the experimental conditions were as follows: ascorbic acid mass ratio of 30%, sulfuric acid concentration of 2mol/L, liquid-solid ratio of 6∶1, stirring speed of 350r/min and constant temperature of 80℃ with reaction time of 5h, the leaching rates of Ce and Mn reached 92.09% and 95.51%, respectively, and the mass ratios of Ce⁴⁺/Ce and Mn⁴⁺/Mn decreased from 75.82% to 71.62% and 29.39% to 27.17%, respectively. It was indicated that the addition of the ascorbic acid reduced part of Ce⁴⁺ (Mn⁴⁺) to Ce³⁺ (Mn²⁺) and weakened the positive effect of high valence Ce on the transition of Mn from the low-valence, thus improving the leaching rates of Ce and Mn, which had laid the groundwork for resource utilization of Ce and Mn in waste CeO _x -MnO _x -based SCR denitrification catalysts.

Key words: selective catalytic reduction (SCR), waste catalysts, acid leaching, reduction, recovery, resource utilization

中图分类号:

TF11.31

余正伟, 张晓霞, 雷杰, 李澳, 王光应, 丁祥, 龙红明. 废CeO _x -MnO _x 基SCR脱硝催化剂还原酸浸综合回收铈锰[J]. 化工进展, 2022, 41(9): 5122-5131.

YU Zhengwei, ZHANG Xiaoxia, LEI Jie, LI Ao, WANG Guangying, DING Xiang, LONG Hongming. Comprehensive recovery of cerium and manganese from waste CeO _x -MnO _x -based SCR denitrification catalysts by reductive acid leaching[J]. Chemical Industry and Engineering Progress, 2022, 41(9): 5122-5131.

图/表 20

表1 废CeO x -MnO x 基SCR脱硝催化剂化学成分（质量分数，%）

TiO₂	MnO	CeO₂	SO₃	CaO	MgO	Na₂O	K₂O	其他
72.53	11.20	2.57	3.80	2.57	1.14	0.48	0.60	5.11

图1 废CeO x -MnO x 基烟气脱硝催化剂XRD图谱

图2 废CeO x -MnO x 基SCR脱硝催化剂XPS图谱

表2 以XPS能谱峰面积计算化合价比例

样品	化合价比例/%
Ce³⁺/Ce	22.67
Ce⁴⁺/Ce	77.33
Mn²⁺/Mn	23.22
Mn³⁺/Mn	41.88
Mn⁴⁺/Mn	34.49

表3 Ce-H2O系各反应在25℃下对应的φ-pH函数关系

序号	平衡反应	φ-pH关系式
a	O₂+4H⁺+4e^- $̿$ 2H₂O	φ=1.2290-0.0592pH
b	H⁺+2e^- $̿$ H₂	φ=-0.0592pH
c	O₂+2H⁺+2e^- $̿$ H₂O₂	φ=0.682-0.0592pH
d	C₆H₆O₆+2H⁺+2e^- $̿$ C₆H₈O₆	φ=0.39-0.0592pH
（1）	Ce³⁺+3e^- $̿$ Ce	φ=-2.3239+0.0197lg $α C e 3 +$
（2）	Ce⁴⁺+e^- $̿$ Ce³⁺	φ=1.7432+0.0592lg（ $α C e 4 +$ / $α C e 3 +$ ）
（3）	Ce₂O₃+6H⁺ $̿$ 2Ce³⁺+3H₂O	pH=10.1936-3lg $α C e 3 +$
（4）	CeO₂+4H⁺ $̿$ Ce⁴⁺+2H₂O	pH=-2.096-1/4lg $α C e 4 +$
（5）	2CeO₂+2H⁺+2e^- $̿$ Ce₂O₃+H₂O	φ=-0.5606-0.0592pH
（6）	CeO₂+4H⁺+e^- $̿$ Ce³⁺+2H₂O	φ=1.2485-0.2366pH-0.0592lg $α C e 3 +$
（7）	Ce₂O₃+6H⁺+6e^- $̿$ 2Ce+3H₂O	φ=-1.7209-0.0592pH

表3 Ce-H2O系各反应在25℃下对应的φ-pH函数关系

序号	平衡反应	φ-pH关系式
a	O₂+4H⁺+4e^- $̿$ 2H₂O	φ=1.2290-0.0592pH
b	H⁺+2e^- $̿$ H₂	φ=-0.0592pH
c	O₂+2H⁺+2e^- $̿$ H₂O₂	φ=0.682-0.0592pH
d	C₆H₆O₆+2H⁺+2e^- $̿$ C₆H₈O₆	φ=0.39-0.0592pH
（1）	Ce³⁺+3e^- $̿$ Ce	φ=-2.3239+0.0197lg $α C e 3 +$
（2）	Ce⁴⁺+e^- $̿$ Ce³⁺	φ=1.7432+0.0592lg（ $α C e 4 +$ / $α C e 3 +$ ）
（3）	Ce₂O₃+6H⁺ $̿$ 2Ce³⁺+3H₂O	pH=10.1936-3lg $α C e 3 +$
（4）	CeO₂+4H⁺ $̿$ Ce⁴⁺+2H₂O	pH=-2.096-1/4lg $α C e 4 +$
（5）	2CeO₂+2H⁺+2e^- $̿$ Ce₂O₃+H₂O	φ=-0.5606-0.0592pH
（6）	CeO₂+4H⁺+e^- $̿$ Ce³⁺+2H₂O	φ=1.2485-0.2366pH-0.0592lg $α C e 3 +$
（7）	Ce₂O₃+6H⁺+6e^- $̿$ 2Ce+3H₂O	φ=-1.7209-0.0592pH

表4 Mn-H2O系各反应在25℃下对应的φ-pH函数关系

序号	平衡反应	φ-pH关系式
a	O₂+4H⁺+4e^- $̿$ 2H₂O	φ=1.2290-0.0592pH
b	H⁺+2e^- $̿$ H₂	φ=-0.0592pH
c	O₂+2H⁺+2e^- $̿$ H₂O₂	φ=0.682-0.0592pH
d	C₆H₆O₆+2H⁺+2e^- $̿$ C₆H₈O₆	φ=0.39-0.0592pH
（8）	Mn²⁺+2e^- $̿$ Mn	φ=-1.185+0.0296lg $α M n 2 +$
（9）	Mn（OH）₂+2H⁺ $̿$ Mn²⁺+2H₂O	pH=9.06-0.0592lg $α M n 2 +$
（10）	Mn（OH）₂+2H⁺+2e^- $̿$ Mn+2H₂O	φ=-0.649-0.0592pH
（11）	Mn₃O₄+2H⁺+2e^- $̿$ 3MnO+H₂O	φ=0.216-0.0592pH
（12）	Mn₃O₄+8H⁺+2e^- $̿$ 3Mn²⁺+4H₂O	φ=1.824-0.237pH-0.0887lg $α M n 2 +$
（13）	3Mn₂O₃+2H⁺+2e^- $̿$ Mn₃O₄+H₂O	φ=0.743-0.0592pH
（14）	Mn₂O₃+6H⁺+2e^- $̿$ 2Mn²⁺+3H₂O	φ=1.443-0.177pH-0.0592lg $α M n 2 +$
（15）	2MnO₂+2H⁺+2e^- $̿$ Mn₂O₃+H₂O	φ=0.819-0.0592pH
（16）	$M n O 4 -$ +4H⁺+3e^- $̿$ MnO₂+2H₂O	φ=1.754-0.1789pH+0.01972lg $α M n 4 -$
（17）	MnO₂+4H⁺+2e^- $̿$ Mn²⁺+2H₂O	φ=1.224-0.1183pH-0.02956lg $α M n 2 +$

表4 Mn-H2O系各反应在25℃下对应的φ-pH函数关系

序号	平衡反应	φ-pH关系式
a	O₂+4H⁺+4e^- $̿$ 2H₂O	φ=1.2290-0.0592pH
b	H⁺+2e^- $̿$ H₂	φ=-0.0592pH
c	O₂+2H⁺+2e^- $̿$ H₂O₂	φ=0.682-0.0592pH
d	C₆H₆O₆+2H⁺+2e^- $̿$ C₆H₈O₆	φ=0.39-0.0592pH
（8）	Mn²⁺+2e^- $̿$ Mn	φ=-1.185+0.0296lg $α M n 2 +$
（9）	Mn（OH）₂+2H⁺ $̿$ Mn²⁺+2H₂O	pH=9.06-0.0592lg $α M n 2 +$
（10）	Mn（OH）₂+2H⁺+2e^- $̿$ Mn+2H₂O	φ=-0.649-0.0592pH
（11）	Mn₃O₄+2H⁺+2e^- $̿$ 3MnO+H₂O	φ=0.216-0.0592pH
（12）	Mn₃O₄+8H⁺+2e^- $̿$ 3Mn²⁺+4H₂O	φ=1.824-0.237pH-0.0887lg $α M n 2 +$
（13）	3Mn₂O₃+2H⁺+2e^- $̿$ Mn₃O₄+H₂O	φ=0.743-0.0592pH
（14）	Mn₂O₃+6H⁺+2e^- $̿$ 2Mn²⁺+3H₂O	φ=1.443-0.177pH-0.0592lg $α M n 2 +$
（15）	2MnO₂+2H⁺+2e^- $̿$ Mn₂O₃+H₂O	φ=0.819-0.0592pH
（16）	$M n O 4 -$ +4H⁺+3e^- $̿$ MnO₂+2H₂O	φ=1.754-0.1789pH+0.01972lg $α M n 4 -$
（17）	MnO₂+4H⁺+2e^- $̿$ Mn²⁺+2H₂O	φ=1.224-0.1183pH-0.02956lg $α M n 2 +$

图3 还原酸浸体系热力学分析Ce-H2O系、Mn-H2O系φ-pH图

图4 废CeO x -MnO x 基SCR脱硝催化剂还原酸浸铈锰流程图

表5 还原剂种类对废CeO x -MnO x 基SCR脱硝催化剂还原酸浸Ce、Mn的影响

还原剂	温度/℃	浸出率/%		残留率/%
还原剂	温度/℃	Ce	Mn	Ti	浸出渣
无	25	29.34	32.02	87.74	86.80
无	80	59.72	72.55	87.83	81.70
抗坏血酸	80	92.08	95.51	91.20	77.90
Na₂SO₃	80	57.63	92.48	89.50	78.10
H₂O₂	80	88.49	94.10	84.73	71.10

图5 还原剂添加量对废SCR脱硝催化剂中Ce、Mn浸出率的影响

图6 硫酸浓度对废SCR脱硝催化剂中Ce、Mn浸出率的影响

图7 浸出温度对废SCR脱硝催化剂中Ce、Mn浸出率的影响

图8 浸出时间对废SCR脱硝催化剂中Ce、Mn浸出率的影响

图9 液固比对废SCR脱硝催化剂中Ce、Mn浸出率的影响

图10 搅拌速度对废SCR脱硝催化剂中Ce、Mn浸出率的影响

表6 废CeOx-MnOx基SCR脱硝催化剂还原-酸浸渣主要化学成分（质量分数，%）

TiO₂	MnO	CeO₂	SO₃	CaO	MgO	其他
93.58	0.78	0.33	0.78	0.04	0.12	4.37

图11 还原-酸浸渣后XRD图谱分析

图12 还原-酸浸渣SEM-EDS图谱分析

图13 还原剂加入前后XPS能谱

表7 以XPS能谱峰面积计算化合价比例 (%)

样品	Ce³⁺/Ce	Ce⁴⁺/Ce	Mn²⁺/Mn	Mn⁴⁺/Mn	O_β/（O_α+O_β）	O_α/（O_α+O_β）
原料	22.67	77.33	23.22	34.49	10.88	89.12
抗坏血酸加入量10%	24.18	75.82	23.82	29.39	27.16	72.84
抗坏血酸加入量20%	25.27	74.73	25.89	28.93	27.97	72.03
抗坏血酸加入量30%	28.38	71.62	36.35	27.17	33.47	66.53
抗坏血酸加入量40%	28.14	71.86	36.03	26.89	21.70	78.30

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废CeO _x -MnO _x 基SCR脱硝催化剂还原酸浸综合回收铈锰

Comprehensive recovery of cerium and manganese from waste CeO _x -MnO _x -based SCR denitrification catalysts by reductive acid leaching

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废CeO x -MnO x 基SCR脱硝催化剂还原酸浸综合回收铈锰

Comprehensive recovery of cerium and manganese from waste CeO x -MnO x -based SCR denitrification catalysts by reductive acid leaching

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废CeO _x -MnO _x 基SCR脱硝催化剂还原酸浸综合回收铈锰

Comprehensive recovery of cerium and manganese from waste CeO _x -MnO _x -based SCR denitrification catalysts by reductive acid leaching