AlCl3·6H2O在FeCl3、CaCl2、KCl及KCl–FeCl3溶液中溶解度的实验及预测

doi:10.11949/0438-1157.20221368

摘要/Abstract

摘要：

如何将AlCl₃·6H₂O从众多组分中选择性地结晶分离是从煤矸石中提Al的关键，而AlCl₃·6H₂O在煤矸石酸浸体系中的热力学平衡数据对于结晶过程的控制至关重要。在25~85℃的温度范围内，测定了不同温度和溶液浓度下AlCl₃·6H₂O在FeCl₃、CaCl₂、KCl及KCl-FeCl₃溶液中的溶解度。实验发现温度对AlCl₃·6H₂O在所有溶液体系中溶解度的影响均不明显，溶解度只随温度的升高略有增加；溶液浓度是影响溶解度的主要因素，AlCl₃·6H₂O在所有溶液体系中的溶解度均随溶液浓度的升高而明显下降，分析其原因是由于溶液浓度的增大使得Cl^–同离子效应增强。为了提高OLI软件预测结果的准确性，对其嵌入Bromley-Zemaitis模型中“Al³⁺–Cl^-”离子对的交互参数进行了修正。随后验证了修正模型的实用性，结果表明它可应用于AlCl₃·6H₂O在FeCl₃、CaCl₂及KCl的任意单、混溶液中溶解度的预测。

关键词: AlCl₃·6H₂O, 溶解性, 相平衡, 热力学性质, 全组分模型

Abstract:

How to selectively crystallize and separate AlCl₃·6H₂O from many components is the key to extracting Al from coal gangue, and the thermodynamic equilibrium data of AlCl₃·6H₂O in the acid leaching system of coal gangue is very important for the control of the crystallization process. The solubilities of AlCl₃·6H₂O in FeCl₃, CaCl₂, KCl and KCl-FeCl₃ solutions were measured and modeled at temperatures from 25℃ to 85℃ in this work. The effects of temperature and solution concentration on the solubility of AlCl₃·6H₂O were studied. The concentration of solution was found to be the main factor which affected the solubility. Solubility of AlCl₃·6H₂O in all solutions was found to decrease obviously with increasing concentration of solution due to the common ion effect of added Cl^-. The effect of temperature on the solubility of AlCl₃·6H₂O in all solutions was slight for the little increment of solubility with increasing temperature. New Bromley–Zemaitis activity coefficient model parameters for the Al³⁺-Cl^- ion pair were obtained by using experimental solubility data. Then the practicability of the modified model was verified, and the results show that it could be used to predict the solubility of AlCl₃·6H₂O in any single and mixed solution of FeCl₃, CaCl₂ and KCl.

Key words: AlCl₃·6H₂O, solubility, phase equilibrium, thermodynamic properties, full speciation model

中图分类号:

TQ 013.1

程文婷, 李杰, 徐丽, 程芳琴, 刘国际. AlCl₃·6H₂O在FeCl₃、CaCl₂、KCl及KCl–FeCl₃溶液中溶解度的实验及预测[J]. 化工学报, 2023, 74(2): 642-652.

Wenting CHENG, Jie LI, Li XU, Fangqin CHENG, Guoji LIU. Experiment and prediction for the solubility of AlCl₃·6H₂O in FeCl₃, CaCl₂, KCl and KCl-FeCl₃solutions[J]. CIESC Journal, 2023, 74(2): 642-652.

图/表 17

图1 溶解度测定装置a—磁力搅拌器;b—水槽;c—投入式恒温器;d—碘瓶;e—磁力转子

Fig.1 Experimental set-up used in the solubility measurementa—magnetic stirrer; b—water tank; c—input-thermostat; d—iodine flask; e—magnetic rotor

图2 不同温度下AlCl3·6H2O在水中的溶解度随时间的变化

Fig.2 Solubility of AlCl3·6H2O in pure water at different temperatures

图3 不同温度下AlCl3·6H2O在水中的溶解度变化与文献中数据的比较

Fig.3 Comparison of solubility of AlCl3·6H2O in pure water at different temperatures with references

表1 在用OLI-HKF计算热力学平衡常数时所涉及到主要组分的热力学数据

Table 1 Thermochemical data for the main species used by OLI-HKF to calculate equilibrium constants

组分	$V ¯ P, 25 0$ / (cm³·mol^-1)	$C ¯ P, 25 0$ / (J·K^-1·mol^-1)	$Δ S ¯ f, 25 0$ / (J·K^-1·mol^-1)	$Δ H ¯ f, 25 0$ / (kJ·mol^-1)	$Δ G ¯ f, 25 0$ / (kJ·mol^-1)
H⁺	0	0	0	0	0
OH^-	-4.18	-137.19	-10.711	-229.99	-157.3
H₂O	18.1	75.3	69.95	-285.83	-237.19
Al³⁺	44.4	-135.98	-325.1	-530.67	-483.7
Fe³⁺	42.8	-142.737	-277.522	-49.6023	-17.2457
Ca²⁺	18.06	-31.50	-56.48	-543.083	-552.79
K⁺	9.06	8.28432	101.044	-252.17	-282.462
Cl^–	17.8	-123.18	56.735	-167.08	-131.29

表1 在用OLI-HKF计算热力学平衡常数时所涉及到主要组分的热力学数据

Table 1 Thermochemical data for the main species used by OLI-HKF to calculate equilibrium constants

组分	$V ¯ P, 25 0$ / (cm³·mol^-1)	$C ¯ P, 25 0$ / (J·K^-1·mol^-1)	$Δ S ¯ f, 25 0$ / (J·K^-1·mol^-1)	$Δ H ¯ f, 25 0$ / (kJ·mol^-1)	$Δ G ¯ f, 25 0$ / (kJ·mol^-1)
H⁺	0	0	0	0	0
OH^-	-4.18	-137.19	-10.711	-229.99	-157.3
H₂O	18.1	75.3	69.95	-285.83	-237.19
Al³⁺	44.4	-135.98	-325.1	-530.67	-483.7
Fe³⁺	42.8	-142.737	-277.522	-49.6023	-17.2457
Ca²⁺	18.06	-31.50	-56.48	-543.083	-552.79
K⁺	9.06	8.28432	101.044	-252.17	-282.462
Cl^–	17.8	-123.18	56.735	-167.08	-131.29

表2 主要组分的七个HKF参数值

Table 2 Values of seven HKF parameters for the main species

组分	α₁×10	α₂×10^-2	α₃	α₄×10^-4	γ₁	γ₂×10^-4	ω×10^-5
H⁺	0	0	0	0	0	0	0
OH^-	1.2527	0.0738	1.8423	-2.782	4.15	-10.35	1.724
Al³⁺	-3.3404	-17.1108	14.9917	-2.0716	10.7	-8.06	2.8711
Fe³⁺	-3.1784	-15.542	11.859	-2.1365	11.08	-9.9808	2.7025
Ca²⁺	-0.1974	7.252	5.2966	-2.4792	9	-2.522	1.2366
K⁺	3.559	-1.473	5.435	-2.712	7.4	-1.791	0.1927
Cl^-	4.032	4.801	5.563	-2.847	-4.40	-5.714	1.456

表3 AlCl3·6H2O热力学平衡方程的经验参数

Table 3 Coefficients for thermodynamic equilibrium constants of AlCl3·6H2O

A	B	C	D
-93.1444	-7955.7916	16.7452	-0.0419

表4 AlCl3·6H2O在水中的溶解度（平衡时间：6 h）

Table 4 Solubility of AlCl3·6H2O （1） in H2O （2）（Equilibration time： 6 h）

温度/℃	用不同单位形式表示的溶解度(以AlCl₃计)
温度/℃	$C 1 / (g ⋅ L - 1)$	$M 1 / (m o l ⋅ L - 1)$	$m 1 / (m o l ⋅ (k g H 2 O) - 1)$
25	386.124	2.8958	3.3622
35	385.658	2.8923	3.3754
45	385.598	2.8918	3.3896
50	386.728	2.9003	3.4100
55	386.437	2.8981	3.4112
65	387.280	2.9045	3.4287
70	388.439	2.9131	3.4453
75	388.881	2.9165	3.4514
85	390.593	2.9293	3.4682

表4 AlCl3·6H2O在水中的溶解度（平衡时间：6 h）

Table 4 Solubility of AlCl3·6H2O （1） in H2O （2）（Equilibration time： 6 h）

温度/℃	用不同单位形式表示的溶解度(以AlCl₃计)
温度/℃	$C 1 / (g ⋅ L - 1)$	$M 1 / (m o l ⋅ L - 1)$	$m 1 / (m o l ⋅ (k g H 2 O) - 1)$
25	386.124	2.8958	3.3622
35	385.658	2.8923	3.3754
45	385.598	2.8918	3.3896
50	386.728	2.9003	3.4100
55	386.437	2.8981	3.4112
65	387.280	2.9045	3.4287
70	388.439	2.9131	3.4453
75	388.881	2.9165	3.4514
85	390.593	2.9293	3.4682

图4 AlCl3·6H2O在水中搅拌溶解6 h后的XRD谱图

Fig.4 XRD patterns of AlCl3·6H2O in pure water at different temperatures after 6 h

图5 不同温度时AlCl3·6H2O在FeCl3溶液中的溶解度

Fig.5 Solubility of AlCl3·6H2O in FeCl3 solutions at different temperatures

图6 不同温度时AlCl3·6H2O在CaCl2溶液中的溶解度

Fig.6 Solubility of AlCl3·6H2O in CaCl2 solutions at different temperatures

图7 不同温度时AlCl3·6H2O在KCl溶液中的溶解度

Fig.7 Solubility of AlCl3·6H2O in KCl solutions at different temperatures

图8 不同温度时AlCl3·6H2O在KCl-FeCl3混合溶液中的溶解度

Fig.8 Solubility of AlCl3·6H2O in mixed KCl-FeCl3 solutions at different temperatures

表8 AlCl3·6H2O在KCl-FeCl3-H2O中的溶解度（平衡时间：6 h）

Table 8 Solubility of AlCl3·6H2O （1） in KCl （2）-FeCl3 （3）-H2O （4）（Equilibration time： 6 h）

溶液的浓度和密度					用不同单位形式表示的溶解度 (以AlCl₃计)
M₂/(mol·L^-1)	M₃/(mol·L^-1)	m₂/(mol·(kg H₂O)^-1)	m₃/(mol·(kg H₂O)^-1)	ρ_s/(g·ml^-1)	C₁/(g·L^-1)	M₁/(mol·L^-1)	m₁/(mol·(kg H₂O)^-1)
T=25℃
0.25	0	0.2923	0	1.2523	377.606	2.8319	3.3091
0.25	0.1	0.2921	0.1002	1.2626	374.724	2.8103	3.2856
0.25	0.2	0.2920	0.1940	1.2718	370.003	2.7749	3.2409
0.25	0.4	0.2916	0.3150	1.2837	363.840	2.7287	3.1823
0.25	0.5	0.2907	0.4265	1.2947	356.597	2.6743	3.1098
0.25	0.7	0.2906	0.5452	1.3062	349.680	2.6225	3.0435
0.25	0.8	0.2905	0.6707	1.3180	345.142	2.5884	3.0076
0.25	0.9	0.2899	0.7579	1.3263	338.541	2.5389	2.9418
0.25	1.0	0.2898	0.8715	1.3371	333.771	2.5032	2.9013
0.25	1.1	0.2897	0.9957	1.3486	328.333	2.4624	2.8553
0.25	1.2	0.2888	1.0793	1.3561	320.330	2.4024	2.7753
T=50℃
0.25	0	0.2968	0	1.2420	379.939	2.8494	3.3795
0.25	0.1	0.2965	0.1098	1.2521	375.231	2.8141	3.3375
0.25	0.2	0.2962	0.2080	1.2613	370.293	2.7771	3.2906
0.25	0.4	0.2956	0.3138	1.2712	363.734	2.7279	3.2252
0.25	0.5	0.2954	0.4281	1.2813	357.475	2.6809	3.1674
0.25	0.7	0.2950	0.5561	1.2930	348.889	2.6165	3.0824
0.25	0.8	0.2945	0.6793	1.3040	344.391	2.5828	3.0473
0.25	0.9	0.2944	0.7662	1.3115	336.976	2.5272	2.9723
0.25	1.0	0.2943	0.8997	1.3232	331.210	2.4840	2.9245
0.25	1.1	0.2942	1.0065	1.3324	325.814	2.4435	2.8771
0.25	1.2	0.2940	1.0873	1.3394	320.644	2.4047	2.8284

表9 Al3+-Cl-离子对的Bromley-Zemaitis活度系数模型修正参数

Table 9 Modified Bromley-Zemaitis model parameters for Al3+-Cl- interactions

离子对	B₁	B₂	B₃	C₁	C₂	C₃	D₁	D₂	D₃
Al³⁺-Cl^-	0.09215	6.4151×10^-5	1.2147×10^-6	-3.415×10^-4	-7.513×10^-6	-6.851×10^-8	-1.084×10^-5	1.1475×10^-7	1.1082×10^-9

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AlCl₃·6H₂O在FeCl₃、CaCl₂、KCl及KCl–FeCl₃溶液中溶解度的实验及预测

Experiment and prediction for the solubility of AlCl₃·6H₂O in FeCl₃, CaCl₂, KCl and KCl-FeCl₃solutions

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