低价钒溶液中铁(II)和钒(IV)、铬(III)的分离及莫尔盐的制备

殷仁涛; 罗冬梅; 陈良; 翁定崧; 肖海兵; 梁斌; 王正豪

doi:10.3969/j.issn.1000-6532.2022.04.010

低价钒溶液中铁(II)和钒(IV)、铬(III)的分离及莫尔盐的制备

四川大学化学工程学院，四川　成都　610065

基金项目: 国家自然科学基金面上项目（NSFC51774205）

详细信息

作者简介: 殷仁涛（1996-），男，硕士研究生，主要从事矿物资源绿色综合利用

通讯作者: 王正豪（1995-），男，博士，主要从事资源回收和储能材料开发

中图分类号: TD951；TF841.3

收稿日期: 2022-02-27

刊出日期: 2022-08-25

Separation of Iron(II) and Vanadium(IV)、Chromium(III) from Low Valence Vanadium Solution and Preparation of Mohr's Salt

School of Chemical Engineering, Sichuan University, Chengdu, Sichuan, China

More Information

Corresponding author: Wang Zhenghao, 2658287933@qq.com

Received Date: 27 February 2022

Publish Date: 25 August 2022

摘要

摘要:
本文以钒渣提取低价钒过程中得到的含低价钒、铬和铁的浸出液为研究对象，将真空冷却法应用于钒铁分离，铁从浸出液中以莫尔盐结晶析出，实现了铁与低价态钒、铬的高效分离并制备了莫尔盐。探究了pH值、硫酸铵添加量、反应时间、结晶时间对钒铁结晶分离行为的影响。结果表明，在真空度0.08 MPa， pH值为2.5，硫酸铵添加量（以n((NH₄)₂SO₄)/ n(FeSO₄)计）为1.2，反应140 min，结晶36 h的条件下，铁的去除率达86.42%，钒的损失率仅为0.52%，铬的损失率为1.64%，获得了纯度为99.23%的莫尔盐产品。
- 钒渣 /
- 低价钒 /
- 结晶 /
- 硫酸亚铁铵
Abstract:
In this study, the leaching solution containing vanadium(IV), chromium(III) and iron(II) obtained in the process of extracting low valence vanadium from vanadium slag was taken as the research object, and the vacuum cooling method was applied to crystallize iron(II) from the leachatein the form of Mohr’s salt, which realized the efficient separation of iron from vanadium(IV) and chromium(III) and the preparation of Mohr’s salt. The effect of pH value, ammonium sulfate addition, reaction time, and crystallization time on the separation behavior of ferrovanadium crystallization were investigated. The results showed that the removal rate of iron reached 86.42% under the conditions of the vacuum degree of 0.08 MPa, pH value of 2.5, addition of ammonium sulfate (calculated as n((NH₄)₂SO₄)/n(FeSO₄)) of 1.2, reaction for 140 min and crystallization for 36 h. The loss of vanadium and chromium were only 0.52% and 1.64%, respectively. In addition, Mohr’s salt with a purity of 99.23% was obtained.
- Vanadium slag /
- Low valence vanadium /
- Crystallize /
- (NH₄)₂Fe(SO₄)₂·6H₂O

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图 1 结晶方式的影响

Figure 1.

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图 2 (a) pH值对莫尔盐结晶除铁的影响；(b) 不同pH 值下结晶产物的XRD

Figure 2.

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图 3 (a) 反应时间对莫尔盐结晶除铁的影响；(b) 不同反应时间下结晶产物的XRD

Figure 3.

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图 4 (a) 硫酸铵用量对莫尔盐结晶除铁的影响；(b) 不同硫酸铵用量下结晶产物的XRD

Figure 4.

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图 5 (a) 结晶时间对莫尔盐结晶除铁的影响；(b) 不同结晶时间下结晶产物的XRD

Figure 5.

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图 6 结晶48 h下紫色结晶的XRD

Figure 6.

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图 7 (a)结晶产物XRD；(b)结晶产物形貌

Figure 7.

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图 8 (a)结晶产物TG-DTA；(b)纯莫尔盐TG-DTA

Figure 8.

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表 1 浸出液中的主要元素及其含量/(g·t^-1)

Table 1. Main chemical compositions in leaching solution

Cr Fe V Ti

1.045 14.890 4.792 0.044

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