离子交换法从低品位石煤钒矿浸出液提钒工艺研究

赵笑益; 程倩; 王望泊; 宁新霞; 程文康; 曹欢; 康敏; 王勇

doi:10.13779/j.cnki.issn1001-0076.2022.03.010

离子交换法从低品位石煤钒矿浸出液提钒工艺研究

1.
西安西北有色地质研究院有限公司, 陕西西安 710054

2.
陕西省矿产资源综合利用工程技术研究中心, 陕西西安 710054

基金项目:
陕西省重点研发计划项目-低品位石煤钒矿干式选矿抛尾-无污染化学提钒工艺及尾渣资源化处理关键技术研究(2022ZDLSF07-10)

详细信息

作者简介: 赵笑益(1980-), 男, 高级工程师, 矿物加工工程专业

通讯作者: 程倩(1991-), 女, 工程师, 矿物加工工程专业

中图分类号: TF841.3;TF803.2

收稿日期: 2022-01-01

刊出日期: 2022-06-25

Study on Vanadium Extraction from Leachate of Low Grade Vanadium Ore by Ion Exchange Method

1.
Xi'an Northwest Geological Institute of Nonferrous Metals Co. Ltd., Xi'an 710054, China

2.
Engineering & Technology Center for Comprehensive Utilization of Mineral Resource of Shaanxi Province, Xi'an 710054, China

More Information

Corresponding author: CHENG Qian

Received Date: 01 January 2022

Publish Date: 25 June 2022

摘要

摘要:
采用离子交换法对石煤钒矿通过拌酸保温熟化—堆浸所得浸出液进行了提钒工艺研究, 主要考察离子交换法提钒工艺, 树脂类型、溶液pH值、动态吸附对钒吸附率的影响。试验结果表明, 含钒浸出液经中和—氧化后调节pH=1.88得到交换前液, 优选吸附性能较好的阴离子交换树脂D201, 进行动态吸附, V₂O₅饱和吸附容量217.66 mg/mL湿树脂; 以4% NaOH+4% NaCl配比的解吸剂对D201进行动态解吸, 解吸液中V₂O₅含量最高达到119.49 g/L, 在解吸液体积(mL)与湿树脂体积(mL)比为3.7时, 树脂解吸率已超过99%;所得解吸液经酸性铵盐一步沉钒法制备得到品位超过98%的高纯V₂O₅产品。本试验提供了一种操作方便、成本低廉的提钒工艺, 树脂D201具有对钒吸附容量大、吸附率高、处理量大等优势, 富钒解吸液无需净化处理, 利用铵盐一步沉钒法最终得到合格产品, 并且避免了萃取工艺带来的废水处理难度大的问题, 工艺适应性强。
- 石煤钒矿 /
- 离子交换法 /
- 阴离子交换树脂D201
Abstract:
The ion exchange method was used to study the extraction process of vanadium from the leaching solution of stone coal vanadium ore obtained by mixing acid, heat preservation, maturation and heap leaching. The influence of resin type, pH value of solution and dynamic adsorption on vanadium adsorption rate was mainly investigated. The experimental results showed that the vanadium-containing leaching solution was neutralized and oxidized to obtain the pre-exchange solution by adjusting pH=1.88, and the anion exchange resin D201 with better adsorption performance was selected for dynamic adsorption. The saturated adsorption capacity of V₂O₅ was 217.66 mg/mL wet resin. The dynamic desorption of D201 was carried out with 4%NaOH + 4%NaCl. The maximum content of V₂O₅ in the desorption solution was 119.49 g/L. When the volume ratio of desorption solution (mL) to wet resin (mL) was 3.7, the desorption rate of resin was over 99%. The obtained analytical solution was prepared by one-step precipitation of vanadium with acidic ammonium salt to obtain high-purity V₂O₅ products with a grade of over 98%. This experiment provides a convenient operation and low cost of vanadium extraction process. The resin D201 has the advantages of large adsorption capacity, high adsorption rate and large treatment capacity for vanadium. The vanadium-rich analytical solution does not need purification treatment. The ammonium salt one-step precipitation method is used to obtain qualified products, and the difficulty of wastewater treatment caused by the extraction process is avoided. The process is highly adaptable.
- stone coal vanadium ore /
- ion exchange method /
- anion exchange resin D201

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图 1 试验流程图

Figure 1.

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图 2 V-H₂O系ε-pH图

Figure 2.

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图 3 中和—氧化流程

Figure 3.

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图 4 pH值不同树脂静态吸附情况

Figure 4.

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图 5 D201动态吸附情况

Figure 5.

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图 6 动态解吸试验结果

Figure 6.

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表 1 浸出液成分分析

Table 1. Component analysis of leaching solution

成分	V₂O₅	TFe	Al₂O₃	Na₂O	K₂O
含量/(g·L^-1)	2.50	7.63	7.97	0.096	1.51

成分	SiO₂	U	Hg	Ti	CaO
含量/(mg·L^-1)	0.12	5.76	0.002	37.1	0.16

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表 2 中和—氧化试验结果

Table 2. Neutralization-oxidation experimental results

溶液类型	pH	氧化还原电位/mV	V/mL	V₂O₅含量/(g·L^-1)	V₂O₅分布率/%
浸出液	0.72	476	1000	3.43	/
中和上清液	1.84	/	530	2.97	49.18
一洗水	2.48	/	500	1.26	19.68
二洗水	2.05	/	555	0.94	16.30
三洗水	2.70	/	510	0.37	5.90
四洗水	2.84	/	890	0.09	2.50
中和渣	/	/	54.17 g	0.38%	6.43
合计	/	/	/	/	100.00
氧化后液	2.10	915	/	2.25	/

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表 3 不同交换树脂静态吸附情况

Table 3. Static adsorption of different exchange resin

树脂类型	交换前液(1)	2 h交换尾液(1)	2 h吸附容量(2)	吸附率/%	24 h交换尾液(1)	24 h吸附容量(2)	吸附率/%	90 h交换尾液(1)	90 h吸附容量(2)	吸附率/%
D202	2.33	0.99	134.00	57.51	0.75	154.80	67.81	0.61	165.07	73.82
D201	2.14	0.48	166.00	77.57	0.28	183.33	86.92	0.12	195.06	94.39
D314	2.14	0.60	154.00	71.96	0.39	172.20	81.78	0.15	189.80	92.99
备注：(1)单位为g/L-V₂O₅；(2)单位为mg/mL湿树脂。

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表 4 静态解吸试验结果

Table 4. Static analytical experimental results

树脂类型	解吸剂	树脂V₂O₅总含量/mg	解吸液V₂O₅含量/(g·L^-1)	解吸率/%
	4%NaOH+4%NaCl	273.54	2.24	99.98
D201	4%NaOH	246.46	1.47	89.24
	4%NaCl	238.55	0.11	6.76

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