从抛光废料中回收稀土

张宇

doi:10.3969/j.issn.1000-6532.2023.05.006

从抛光废料中回收稀土

doi: 10.3969/j.issn.1000-6532.2023.05.006

张宇

连云港高品再生资源有限公司，江苏　连云港　222302

详细信息

作者简介:
张宇（1981-），男，硕士，主要从事含稀土废料再生的研究与生产

中图分类号: TD985：TF803.2
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- 被引次数: 0
出版历程
- 收稿日期: 2022-04-02

Recovery of Rare Earths from Polishing Waste

Zhang Yu

Lianyungang Gaopin Renewable Resources Co., Ltd, Lianyungang, Jiangsu, China

摘要

摘要: 这是一篇冶金工程领域的论文。以稀土抛光粉废料为原料，通过正交实验设计，首先进行废料与硫酸铵和硫酸氢铵混合物的焙烧实验，使稀土氧化物转化为硫酸盐。实验考查3个因素，每个因素取3个水平，选用正交表L₉(3⁴)，安排了9个实验，统计分析实验结果：焙烧温度取480 ℃，焙烧时间取3 h，质量比取1.8∶1。然后在酸浸液中加入0.2%的硫脲作还原剂，研究用稀硫酸从焙烧固相中浸出稀土的工艺条件。实验考查4个因素，每个因素取4个水平，选用正交表L₁₆(4⁵)，安排了16个实验，统计分析实验结果：酸浸温度取90 ℃，硫酸浓度取0.5 mol/L，浸出时间取4 h，稀硫酸与焙烧固相的液固比（质量）取4:1，稀土的浸出率可达97.8%～98.0%。
- 冶金工程 /
- 焙烧 /
- 稀土抛光粉废料 /
- 稀土浸出率 /
- 正交实验设计
Abstract: This is an essay in the field of metallurgical engineering. Using rare earth polishing powder waste as raw material, an orthogonal experimental design was used to convert rare earth oxides into sulfates by first conducting roasting experiments of the waste with a mixture of ammonium sulfate and ammonium bisulfate. The orthogonal experiment with 3 factors and 3 levels was carried out by using the orthogonal table L₉(3⁴) and statistically analyzed the test results: the roasting temperature was 480 ℃, the roasting time was 3 h, and the mass ratio was 1.8:1. In the second step, 0.2% thiourea was added to the acid leaching solution as reducing agent, and the technological conditions of leaching rare earth from the calcined solid phase with dilute sulfuric acid were studied. The orthogonal experiment with 4 factors and 4 levels was carried out by using the orthogonal table L₁₆(4⁵). The experimental result shows that on the condition of lixiviating temperature being 90 ℃, sulfuric acid thickness being 0.5 mol/L, lixiviating time being 4 h, liquid-to-solid quality ratio being 4∶1, the extraction rate of rare earths will reach 97.8%~98.0% in mass fraction.
- Metallurgical engineering /
- Roasting /
- Waste of rare earth polishing powder /
- Recovery rate of rare earth /
- Orthogonal test design

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图 1 工艺流程

Figure 1. Process flow chart

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表 1 抛光粉废料主要成分/%

Table 1. Main components of polishing powder waste

CeO₂	La₂O₃	Pr₆O₁₁	Nd₂O₃	Y₂O₃	CaO	Fe₂O₃	Al₂O₃	SiO₂
61.88	32.44	0.47	<0.1	<0.1	0.05	0.08	0.03	4.55

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表 2 焙烧实验的影响因素和水平

Table 2. Influencing factors and levels of roasting test

因素水平	1	2	3
A: 焙烧温度/℃	300	390	480
B: 焙烧时间/h	1	2	3
C: 质量比	1.3∶1	1.8∶1	2.3∶1

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表 3 焙烧正交实验

Table 3. Roasting orthogonal test

实验序号	列号/因素				浸出率
	1	2	3	4	Y/%
	A	B	C		Y/%
1	1	1	1	1	14.2
2	1	2	2	2	41.9
3	1	3	3	3	62.4
4	2	1	2	3	58.7
5	2	2	3	1	80.1
6	2	3	1	2	80.5
7	3	1	3	2	73.6
8	3	2	1	3	74.0
9	3	3	2	1	93.6
k₁	39.5	48.8	56.2	62.6
k₂	73.1	65.3	64.7	65.3
k₃	80.4	78.8	72.0	65.0
r_色度	40.9	30.0	15.8	2.7

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表 4 焙烧方差分析

Table 4. Variance analysis of roasting test

方差来源	平方和	自由度	均方	F 值	显著性
A	2855.1	2	1427.5	217.3	**
B	1354.5	2	677.3	103.1	**
C	375.2	2	187.6	28.6
误差	13.1	2	6.6
总和	4597.9	8		F_0.05(2,2)=19.00

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表 5 稀土浸出实验的影响因素和水平

Table 5. Influence factors and levels of rare earth leaching test

因素水平	1	2	3	4
A:反应温度/ ℃	30	50	70	90
B:硫酸浓度/(mol/L)	0.2	0.5	1.0	2
C:浸出时间/h	1	2	3	4
D:液固比(质量比)	2∶1	3∶1	4∶1	5∶1

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表 6 浸出正交实验

Table 6. Orthogonal test of leaching

实验序号	列号/因素					稀土浸出率 Y/%
	1	2	3	4	5
	A	B	C	D
1	1	1	1	1	1	57.7
2	1	2	2	2	2	76.9
3	1	3	3	3	3	78.7
4	1	4	4	4	4	80.2
5	2	1	2	3	4	81.8
6	2	2	1	4	3	78.7
7	2	3	4	1	2	79.7
8	2	4	3	2	1	75.7
9	3	1	3	4	2	92.6
10	3	2	4	3	1	97.6
11	3	3	1	2	4	74.7
12	3	4	2	1	3	68.6
13	4	1	4	2	3	93.2
14	4	2	3	1	4	89.3
15	4	3	2	4	1	87.8
16	4	4	1	3	2	74.8
k₁	73.4	81.3	71.5	73.8	79.7
k₂	79.0	85.6	78.8	80.1	81.0
k₃	83.4	80.2	84.1	83.2	79.8
k₄	86.3	74.8	87.7	84.8	81.5
r	12.9	10.8	16.2	11.0	1.8

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表 7 浸出方差分析

Table 7. Variance analysis of leaching test

方差来源	平方和	自由度	均方	F 值	显著性
A	378.8	3	126.3	39.8	*
B	236.9	3	79.0	24.9	*
C	594.8	3	198.3	62.5	*
D	283.3	3	94.4	29.8	*
误差	9.5	3	3.2
总和	1503.3	15		F_0.05(3,3)=9.28

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