(NH4)2SO4和Na2SO4混合溶液中(NH4)2SO4结晶动力学及铁/铝/锰/铬等离子对(NH4)2SO4结晶的影响规律

doi:10.16085/j.issn.1000-6613.2022-0542

化工进展 ›› 2023, Vol. 42 ›› Issue (1): 488-496.DOI: 10.16085/j.issn.1000-6613.2022-0542

(NH₄)₂SO₄和Na₂SO₄混合溶液中(NH₄)₂SO₄结晶动力学及铁/铝/锰/铬等离子对(NH₄)₂SO₄结晶的影响规律

范嘉昊¹^,²(), 张洋²(), 范兵强², 张贺东², 郑诗礼², 邹兴¹

^1.北京科技大学冶金与生态工程学院，北京 100084
^2.中国科学院过程工程研究所战略金属资源绿色循环利用国家工程研究中心，北京 100190

收稿日期:2022-04-01 修回日期:2022-06-06 出版日期:2023-01-25 发布日期:2023-02-20
通讯作者: 张洋
作者简介:范嘉昊（1997—），男，硕士研究生，研究方向工业结晶。E-mail：g20198253@xs.ustb.edu.cn。
基金资助:
国家重点研发计划(2018YFC1900505)

Crystallization kinetics of (NH₄)₂SO₄ in mixed solution of (NH₄)₂SO₄ and Na₂SO₄ and the influence of Fe/Al/Mn/Cr ions on crystallization

FAN Jiahao¹^,²(), ZHANG Yang²(), FAN Binqiang², ZHANG Hedong², ZHENG Shili², ZOU Xing¹

^1.School of Metallurgical and Ecological Engineering，University of Science & Technology Beijing, Beijing 100084, China
^2.National Engineering Research Center for Green Recycling of Strategic Metal Resources, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China

Received:2022-04-01 Revised:2022-06-06 Online:2023-01-25 Published:2023-02-20
Contact: ZHANG Yang

摘要/Abstract

摘要：

湿法冶金、三元前体制备等过程均会产生含硫酸钠与硫酸铵的高盐废水。研究高盐废水中硫酸铵的结晶动力学，并考察常见金属离子的影响规律对高盐废水处理具有重要意义。本文以含硫酸钠与硫酸铵混合溶液中硫酸铵的结晶过程为例，系统考察了硫酸铵的结晶动力学及铁、铝、锰、铬对硫酸铵结晶的影响规律。含硫酸钠与硫酸铵混合溶液硫酸铵结晶动力学研究结果表明，硫酸铵生长速率和成核速率方程分别为为 $B = 1.303 × 10 - 16 G 1.069 M T 1.801$ ， $G = 15.708 σ 1.387$ ；在硫酸钠与硫酸铵混合体系中，溶液过饱和度影响硫酸铵成核及生长速率，溶液过饱和度减小，晶体的成核及生长速率都会减小，与单体系硫酸铵结晶动力学结果相比，动力学参数均有所下降。铁、铝、锰、铬对硫酸铵结晶的影响规律研究结果表明，铁、铝抑制了硫酸铵晶面生长，结晶粒度减小；锰、铬对硫酸铵结晶有一定的促进作用，结晶粒度增大。金属离子改变了硫酸铵晶习，锰使结晶呈现三棱柱状，铁、铝使硫酸铵结晶片状生长。不同金属离子条件下的结晶动力学方程表明，铁和铝对结晶成核过程作用更为显著，锰和铬可以促进硫酸铵生长过程。

关键词: 硫酸铵, 金属离子, 结晶, 动力学

Abstract:

Processes such as hydrometallurgy and ternary precursor preparation will produce high-salt wastewater containing sodium sulfate and ammonium sulfate. It is of great significance to study the crystallization kinetics of ammonium sulfate in high-salt wastewater and investigate the influence of common metal ions for the treatment of high-salt wastewater. Taking the crystallization process of ammonium sulfate in a mixed solution containing sodium sulfate and ammonium sulfate as an example, the crystallization kinetics of ammonium sulfate and the influence of ferrum, aluminum, manganese and chromium on the crystallization of ammonium sulfate were systematically investigated. The results of the crystallization kinetics of ammonium sulfate in the mixed solution containing sodium sulfate and ammonium sulfate showed that the nucleation rate and growth rate equations of ammonium sulfate were: $B = 1.303 × 10 - 16 G 1.069 M T 1.801$ and $G = 15.708 σ 1.387$ . In the mixed system of sodium sulfate and ammonium sulfate, the supersaturation of the solution affected the nucleation and growth rate of ammonium sulfate. With the decrease of saturation, the nucleation and growth rate of crystals would decrease. Compared with the results of single-system ammonium sulfate crystallization kinetics, the kinetic parameters all decreased. The research results of the effect of ferrum, aluminum, manganese and chromium on the crystallization of ammonium sulfate indicated that ferrum and aluminum inhibited the growth of ammonium sulfate crystal planes and reduced the crystal size, while manganese and chromium can promote the crystallization of ammonium sulfate and increase the crystal size. Metal ions changed the crystal habit of ammonium sulfate. Manganese made the crystal appear triangular prism, while ferrum and aluminum made the ammonium sulfate crystal grow in flakes. The kinetic equations of crystallization under the conditions of different metal ions showed that ferrum and aluminum had more significant effects on the crystallization nucleation process, while manganese and chromium can promote the growth process of ammonium sulfate.

Key words: ammonium sulfate, metal ion, crystallization, kinetics

中图分类号:

TQ113.7

范嘉昊, 张洋, 范兵强, 张贺东, 郑诗礼, 邹兴. (NH₄)₂SO₄和Na₂SO₄混合溶液中(NH₄)₂SO₄结晶动力学及铁/铝/锰/铬等离子对(NH₄)₂SO₄结晶的影响规律[J]. 化工进展, 2023, 42(1): 488-496.

FAN Jiahao, ZHANG Yang, FAN Binqiang, ZHANG Hedong, ZHENG Shili, ZOU Xing. Crystallization kinetics of (NH₄)₂SO₄ in mixed solution of (NH₄)₂SO₄ and Na₂SO₄ and the influence of Fe/Al/Mn/Cr ions on crystallization[J]. Chemical Industry and Engineering Progress, 2023, 42(1): 488-496.

图/表 12

图1 蒸发结晶装置示意图1—低温循环冷却器；2—夹套结晶器；3—电动搅拌器；4—球形冷凝管；5—冷却水浴；6—真空泵；7—锥形瓶

表1 硫酸铵悬浮密度及相对过饱和度

取样编号	m/kg	$M T$ /kg·m^-3	σ
1	4.19×10^-5	4.19	0.014
2	7.99×10^-5	7.99	0.042
3	12.01×10^-4	12.01	0.035
4	19.13×10^-4	19.13	0.05
5	14.24×10^-4	14.24	0.04
6	19.77×10^-4	19.77	0.075
7	23.55×10^-4	23.55	0.05
8	25.52×10^-4	25.52	0.014
9	26.08×10^-4	26.08	0.042

表1 硫酸铵悬浮密度及相对过饱和度

取样编号	m/kg	$M T$ /kg·m^-3	σ
1	4.19×10^-5	4.19	0.014
2	7.99×10^-5	7.99	0.042
3	12.01×10^-4	12.01	0.035
4	19.13×10^-4	19.13	0.05
5	14.24×10^-4	14.24	0.04
6	19.77×10^-4	19.77	0.075
7	23.55×10^-4	23.55	0.05
8	25.52×10^-4	25.52	0.014
9	26.08×10^-4	26.08	0.042

图2 硫酸铵的粒径分布

图3 硫酸铵的粒数密度分布函数拟合

表2 以1号结晶样品为例计算μ0和μ1

粒度/μm	累加百分数/%	ΔL/μm	$L j ¯$ /μm	n_j /μm^-4	μ₀_j /μm^-3	μ₁_j /μm^-2
0	0	50	25	0	0	0
50	0	50	75	0	0	0
100	1.8113208	50	125	4.39072×10^-15	2.19536×10^-13	2.7442×10^-11
150	6.5660377	50	175	4.20031×10^-15	2.10015×10^-3	3.67527×10^-11
200	6.5660377	50	225	0	0	0
250	10.0377358	50	275	7.90341×10^-16	3.95171×10^-14	1.08672×10^-11
300	21.4339623	100	350	6.29213×10^-16	6.29213×10^-14	2.20225×10^-11
400	26.7169811	100	450	1.37241×10^-16	1.37241×10^-14	6.17587×10^-12
500	30.9433962	100	550	6.01347×10^-17	6.01347×10^-15	3.30741×10^-12
600	43.3962264	100	650	1.07342×10^-16	1.07342×10^-14	6.97722×10^-12
700	46.7924528	100	750	1.9057×10^-17	1.9057×10^-15	1.42927×10^-12
800	46.7924528	100	850	0	0	0
900	58.5660377	100	950	3.25071×10^-17	3.25071×10^-15	3.08818×10^-12
1000	83.8490566	500	1250	6.12872×10^-18	3.06436×10^-15	3.83045×10^-12
1500	100	500	1750	1.42677×10^-18	7.13386×10^-16	1.24843×10^-12
2000					μ₀=5.71396×10^-13	μ₁=1.23141×10^-10

表2 以1号结晶样品为例计算μ0和μ1

粒度/μm	累加百分数/%	ΔL/μm	$L j ¯$ /μm	n_j /μm^-4	μ₀_j /μm^-3	μ₁_j /μm^-2
0	0	50	25	0	0	0
50	0	50	75	0	0	0
100	1.8113208	50	125	4.39072×10^-15	2.19536×10^-13	2.7442×10^-11
150	6.5660377	50	175	4.20031×10^-15	2.10015×10^-3	3.67527×10^-11
200	6.5660377	50	225	0	0	0
250	10.0377358	50	275	7.90341×10^-16	3.95171×10^-14	1.08672×10^-11
300	21.4339623	100	350	6.29213×10^-16	6.29213×10^-14	2.20225×10^-11
400	26.7169811	100	450	1.37241×10^-16	1.37241×10^-14	6.17587×10^-12
500	30.9433962	100	550	6.01347×10^-17	6.01347×10^-15	3.30741×10^-12
600	43.3962264	100	650	1.07342×10^-16	1.07342×10^-14	6.97722×10^-12
700	46.7924528	100	750	1.9057×10^-17	1.9057×10^-15	1.42927×10^-12
800	46.7924528	100	850	0	0	0
900	58.5660377	100	950	3.25071×10^-17	3.25071×10^-15	3.08818×10^-12
1000	83.8490566	500	1250	6.12872×10^-18	3.06436×10^-15	3.83045×10^-12
1500	100	500	1750	1.42677×10^-18	7.13386×10^-16	1.24843×10^-12
2000					μ₀=5.71396×10^-13	μ₁=1.23141×10^-10

表3 平均成核速率和平均生长速率

取样编号	μ₀/μm^-3	μ₁/μm^-2	$B ¯$ /μm^-3·s^-1	$G ¯$ /μm·s^-1
1	5.71396×10^-13	1.23141×10^-10	1.18142×10^-15	0.04116
2	1.28025×10^-12	3.51759×10^-10	1.04789×10^-15	0.18793
3	1.90898×10^-12	5.31568×10^-10	4.01696×10^-15	0.14552
4	4.31916×10^-12	8.03464×10^-10	1.57388×10^-14	0.23945
5	1.37625×10^-11	1.55993×10^-9	4.67263×10^-15	0.20499
6	1.656×10^-11	1.74644×10^-9	1.09063×10^-14	0.41233
7	1.00223×10^-11	2.07534×10^-9	1.71882×10^-14	0.25547
8	2.03352×10^-11	2.30801×10^-9	1.91881×10^-14	0.62046
9	3.18481×10^-11	3.27934×10^-9

表3 平均成核速率和平均生长速率

取样编号	μ₀/μm^-3	μ₁/μm^-2	$B ¯$ /μm^-3·s^-1	$G ¯$ /μm·s^-1
1	5.71396×10^-13	1.23141×10^-10	1.18142×10^-15	0.04116
2	1.28025×10^-12	3.51759×10^-10	1.04789×10^-15	0.18793
3	1.90898×10^-12	5.31568×10^-10	4.01696×10^-15	0.14552
4	4.31916×10^-12	8.03464×10^-10	1.57388×10^-14	0.23945
5	1.37625×10^-11	1.55993×10^-9	4.67263×10^-15	0.20499
6	1.656×10^-11	1.74644×10^-9	1.09063×10^-14	0.41233
7	1.00223×10^-11	2.07534×10^-9	1.71882×10^-14	0.25547
8	2.03352×10^-11	2.30801×10^-9	1.91881×10^-14	0.62046
9	3.18481×10^-11	3.27934×10^-9

图4 硫酸铵晶体粉末衍射图谱

图5 不同杂质获得的硫酸铵晶体形貌

图6 不同杂质对硫酸铵结晶粒度的影响

图7 不同浓度下杂质对硫酸铵结晶粒度的影响

表4 硫酸铵结晶动力学方程

杂质种类	浓度/mol·L^-1	成核动力学方程	生长动力学方程
Mn²⁺	0.001	$B = 4.129 × 10 - 17 G 0.454 M T 1.995$	$G = 17.267 σ 1.098$
	0.002	$B = 2.974 × 10 - 17 G 0.856 M T 1.341$	$G = 17.997 σ 1.12$
	0.003	$B = 1.517 × 10 - 17 G 0.969 M T 1.613$	$G = 15.276 σ 1.198$
Al³⁺	0.001	$B = 1.316 × 10 - 17 G 0.744 M T 2.142$	$G = 13.274 σ 1.159$
	0.002	$B = 1.307 × 10 - 17 G 0.744 M T 2.142$	$G = 12.831 σ 1.372$
	0.003	$B = 1.203 × 10 - 17 G 1.069 M T 1.801$	$G = 12.118 σ 1.272$
Fe³⁺	0.001	$B = 1.876 × 10 - 17 G 0.647 M T 1.886$	$G = 11.219 σ 1.277$
	0.002	$B = 1.611 × 10 - 17 G 0.969 M T 1.396$	$G = 10.884 σ 1.316$
	0.003	$B = 1.454 × 10 - 17 G 0.931 M T 1.576$	$G = 10.687 σ 1.386$
Cr³⁺	0.001	$B = 3.422 × 10 - 17 G 0.599 M T 1.388$	$G = 16.457 σ 1.078$
	0.002	$B = 2.747 × 10 - 17 G 0.873 M T 1.671$	$G = 18.155 σ 1.253$
	0.003	$B = 1.498 × 10 - 17 G 0.969 M T 1.613$	$G = 13.844 σ 1.361$

表4 硫酸铵结晶动力学方程

杂质种类	浓度/mol·L^-1	成核动力学方程	生长动力学方程
Mn²⁺	0.001	$B = 4.129 × 10 - 17 G 0.454 M T 1.995$	$G = 17.267 σ 1.098$
	0.002	$B = 2.974 × 10 - 17 G 0.856 M T 1.341$	$G = 17.997 σ 1.12$
	0.003	$B = 1.517 × 10 - 17 G 0.969 M T 1.613$	$G = 15.276 σ 1.198$
Al³⁺	0.001	$B = 1.316 × 10 - 17 G 0.744 M T 2.142$	$G = 13.274 σ 1.159$
	0.002	$B = 1.307 × 10 - 17 G 0.744 M T 2.142$	$G = 12.831 σ 1.372$
	0.003	$B = 1.203 × 10 - 17 G 1.069 M T 1.801$	$G = 12.118 σ 1.272$
Fe³⁺	0.001	$B = 1.876 × 10 - 17 G 0.647 M T 1.886$	$G = 11.219 σ 1.277$
	0.002	$B = 1.611 × 10 - 17 G 0.969 M T 1.396$	$G = 10.884 σ 1.316$
	0.003	$B = 1.454 × 10 - 17 G 0.931 M T 1.576$	$G = 10.687 σ 1.386$
Cr³⁺	0.001	$B = 3.422 × 10 - 17 G 0.599 M T 1.388$	$G = 16.457 σ 1.078$
	0.002	$B = 2.747 × 10 - 17 G 0.873 M T 1.671$	$G = 18.155 σ 1.253$
	0.003	$B = 1.498 × 10 - 17 G 0.969 M T 1.613$	$G = 13.844 σ 1.361$

表5 不同浓度杂质条件下硫酸铵结晶平均成核速率和平均生长速率

杂质种类	浓度/mol·L^-1	$B ¯$ /μm^-3·s^-1	$G ¯$ /μm·s^-1
Mn²⁺	0.001	1.76419×10^-14	0.66714
	0.002	1.13867×10^-14	0.82653
	0.003	9.17748×10^-15	0.33817
Al³⁺	0.001	7.42176×10^-15	0.61249
	0.002	6.34097×10^-15	0.37135
	0.003	1.76419×10^-15	0.24965
Fe³⁺	0.001	5.25004×10^-15	0.44396
	0.002	3.54196×10^-15	0.34471
	0.003	1.19991×10^-15	0.14457
Cr³⁺	0.001	1.05465×10^-14	0.74411
	0.002	8.94551×10^-15	0.37585
	0.003	5.11125×10^-15	0.25918

表5 不同浓度杂质条件下硫酸铵结晶平均成核速率和平均生长速率

杂质种类	浓度/mol·L^-1	$B ¯$ /μm^-3·s^-1	$G ¯$ /μm·s^-1
Mn²⁺	0.001	1.76419×10^-14	0.66714
	0.002	1.13867×10^-14	0.82653
	0.003	9.17748×10^-15	0.33817
Al³⁺	0.001	7.42176×10^-15	0.61249
	0.002	6.34097×10^-15	0.37135
	0.003	1.76419×10^-15	0.24965
Fe³⁺	0.001	5.25004×10^-15	0.44396
	0.002	3.54196×10^-15	0.34471
	0.003	1.19991×10^-15	0.14457
Cr³⁺	0.001	1.05465×10^-14	0.74411
	0.002	8.94551×10^-15	0.37585
	0.003	5.11125×10^-15	0.25918

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(NH₄)₂SO₄和Na₂SO₄混合溶液中(NH₄)₂SO₄结晶动力学及铁/铝/锰/铬等离子对(NH₄)₂SO₄结晶的影响规律

Crystallization kinetics of (NH₄)₂SO₄ in mixed solution of (NH₄)₂SO₄ and Na₂SO₄ and the influence of Fe/Al/Mn/Cr ions on crystallization

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