四元体系（Li+， Mg2+//Cl-， borate-H2O）308.15 K相平衡与相图研究

doi:10.11949/0438-1157.20201690

摘要/Abstract

摘要：

采用等温溶解平衡法，开展四元体系Li⁺， Mg²⁺//Cl^-， borate–H₂O固液相平衡与相图研究，测定平衡溶液的液相组成、密度、折射率和pH。该四元体系相图中存在的盐类矿物为：LiCl·H₂O、Li₂B₄O₇·3H₂O、 MgCl₂·6H₂O、Mg₂B₆O₁₁·15H₂O和锂光卤石LiCl·MgCl₂·7H₂O，其中锂光卤石LiCl·MgCl₂·7H₂O是异成分复盐，溶液中MgCl₂存在下章氏硼镁石（MgB₄O₇·9H₂O）不稳定，转化为多水硼镁石（Mg₂B₆O₁₁·15H₂O）。多水硼镁石结晶区最大，表明镁硼酸盐易于结晶析出，而锂光卤石结晶区最小。采用Pitzer热力学模型对该四元体系的溶解度进行理论预测，计算相图与实验相图吻合较好。该四元体系的稳定相平衡与相图研究，可为含锂硼盐湖老卤中锂、镁、硼产品开发及其综合利用提供理论依据。

关键词: 盐湖卤水体系, 相平衡与相图, 锂盐, 镁硼酸盐, Pitzer模型

Abstract:

Solid-liquid phase equilibria and phase diagrams for the quaternary system (Li⁺, Mg²⁺//Cl^-, borate–H₂O) were investigated, and the compositions in liquid phase, densities, refractive indices and pH were measured experimentally by using isothermal dissolution equilibrium method. There are five minerals corresponding to LiCl·H₂O, Li₂B₄O₇·3H₂O, MgCl₂·6H₂O, Mg₂B₆O₁₁·15H₂O, and the lithium carnallite LiCl·MgCl₂·7H₂O existed in this system. Mg₂B₆O₁₁·15H₂O occupies the greatest part of phase region, while LiCl·MgCl₂·7H₂O covers the smallest. The mineral LiCl·MgCl₂·7H₂O belongs to the incongruent double salt, and hungchaoite (MgB₄O₇·9H₂O) is transformed into Mg₂B₆O₁₁·15H₂O in the concentrated MgCl₂ aqueous solution. The crystalline area of inderite is the largest, indicating that magnesium borate is easy to crystallize, while the crystalline area of lithium carnallite is the smallest. The solubility of this quaternary system were predicted using Pitzer thermodynamics model, and the calculated solubility agreed well with experimental data. The phase equilibrium study of this quaternary system (Li⁺, Mg²⁺//Cl^-, borate-H₂O) will provide a theoretical basis to promote the development of lithium, magnesium and boron products and to guide the comprehensive utilization of this precious salt lake brine resources.

Key words: salt lake brine system, phase equilibria and phase diagram, lithium salts, magnesium borate, Pitzer model

中图分类号:

O 642.4⁺2

李栋婵, 王嘉宇, 王士强. 四元体系（Li⁺， Mg²⁺//Cl^-， borate-H₂O）308.15 K相平衡与相图研究[J]. 化工学报, 2021, 72(6): 3170-3178.

LI Dongchan, WANG Jiayu, WANG Shiqiang. Phase equilibria and phase diagram of the quaternary system (Li⁺, Mg²⁺//Cl^-, borate-H₂O) at 308.15 K[J]. CIESC Journal, 2021, 72(6): 3170-3178.

图/表 8

参考文献 35

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No.	Composition of liquid phase（w）/%					J?necke index（J）			Solid phase
No.	Li⁺	Mg²⁺	Cl^-	B₄O₇^2-	H₂O	J(Mg²⁺)	J(B₄O₇^2-)	J(H₂O)	Solid phase
1,E₁	0.28	0.01	0.00	3.20	96.51	2.00	100.15	26028.88	Inderite+Lb
2	0.30	0.01	0.51	2.31	96.87	1.87	67.57	24416.78	Inderite+Lb
3	0.33	0.01	0.88	1.88	96.90	1.70	50.08	22241.73	Inderite+Lb
4	0.44	0.01	1.55	1.65	96.35	1.28	33.10	16657.46	Inderite+Lb
5	0.50	0.02	1.99	1.35	96.14	2.23	23.60	14485.54	Inderite+Lb
6	0.64	0.03	2.89	1.02	95.42	2.61	13.88	11189.12	Inderite+Lb
7	0.86	0.05	4.12	0.92	94.05	3.21	9.26	8156.13	Inderite+Lb
8	1.47	0.09	7.51	0.58	90.35	3.38	3.41	4576.09	Inderite+Lb
9	2.08	0.10	10.70	0.40	86.72	2.67	1.67	3126.82	Inderite+Lb
10	2.88	0.10	14.88	0.27	81.87	1.94	0.82	2147.90	Inderite+Lb
11,F₁	3.44	0.11	17.76	0.21	78.48	1.79	0.54	1726.44	Inderite+Lb+Lc
12	3.35	0.11	17.31	0.24	78.99	1.84	0.63	1783.48	Lb+Lc
13	4.04	0.10	20.83	0.18	74.85	1.39	0.39	1407.75	Lb+Lc
14,E₂	6.55	0.00	33.36	0.18	59.91	0.00	0.25	704.81	Lb+Lc
15,E₃	5.34	2.21	33.72	0.00	58.73	19.12	0.00	685.45	Bis+Lc
16	4.09	0.01	20.86	0.13	74.91	0.14	0.28	1409.36	Inderite+Lc
17	4.18	0.02	21.33	0.13	74.34	0.27	0.28	1366.70	Inderite+Lc
18	4.10	0.10	21.18	0.18	74.44	1.37	0.39	1379.83	Inderite+Lc
19	5.61	1.15	31.76	0.49	60.99	10.48	0.70	749.93	Inderite+Lc
20	6.47	1.70	37.79	0.50	53.54	13.05	0.60	554.45	Inderite+Lc
21	5.85	2.17	36.01	0.41	55.56	17.48	0.52	603.90	Inderite+Lc
22,F₂	5.58	2.37	35.19	0.56	56.30	19.52	0.72	625.69	Inderite+Lc+Lcar
23	5.26	2.41	33.63	0.59	58.11	20.74	0.79	674.72	Inderite+Lcar
24,E₄	4.93	2.84	33.44	0.00	58.79	24.76	0.00	691.41	Bis+Lcar
25,F₃	4.85	2.68	32.14	0.96	59.37	23.99	1.35	716.98	Inderite+Lcar+Bis
26	3.99	4.12	31.84	1.19	58.86	37.10	1.68	715.03	Inderite+Bis
27	2.54	5.65	29.22	0.55	62.04	55.96	0.85	828.95	Inderite+Bis
28	2.07	6.34	28.75	0.70	62.14	63.63	1.10	841.36	Inderite+Bis
29	2.10	6.15	28.40	0.57	62.78	62.58	0.91	861.92	Inderite+Bis
30	1.37	4.96	21.23	0.51	71.93	67.40	1.09	1318.76	Inderite+Bis
31	0.83	4.24	16.39	0.46	78.08	74.47	1.27	1850.29	Inderite+Bis
32	0.41	3.66	12.57	0.44	82.92	83.60	1.57	2555.37	Inderite+Bis
33,E₅	0.00	3.19	9.12	0.42	87.27	100.00	2.06	3690.87	Inderite+Bis

No.	Composition of liquid phase（w）/%					J?necke index（J）			Solid phase
No.	Li⁺	Mg²⁺	Cl^-	B₄O₇^2-	H₂O	J(Mg²⁺)	J(B₄O₇^2-)	J(H₂O)	Solid phase
1,E₁	0.28	0.01	0.00	3.20	96.51	2.00	100.15	26028.88	Inderite+Lb
2	0.30	0.01	0.51	2.31	96.87	1.87	67.57	24416.78	Inderite+Lb
3	0.33	0.01	0.88	1.88	96.90	1.70	50.08	22241.73	Inderite+Lb
4	0.44	0.01	1.55	1.65	96.35	1.28	33.10	16657.46	Inderite+Lb
5	0.50	0.02	1.99	1.35	96.14	2.23	23.60	14485.54	Inderite+Lb
6	0.64	0.03	2.89	1.02	95.42	2.61	13.88	11189.12	Inderite+Lb
7	0.86	0.05	4.12	0.92	94.05	3.21	9.26	8156.13	Inderite+Lb
8	1.47	0.09	7.51	0.58	90.35	3.38	3.41	4576.09	Inderite+Lb
9	2.08	0.10	10.70	0.40	86.72	2.67	1.67	3126.82	Inderite+Lb
10	2.88	0.10	14.88	0.27	81.87	1.94	0.82	2147.90	Inderite+Lb
11,F₁	3.44	0.11	17.76	0.21	78.48	1.79	0.54	1726.44	Inderite+Lb+Lc
12	3.35	0.11	17.31	0.24	78.99	1.84	0.63	1783.48	Lb+Lc
13	4.04	0.10	20.83	0.18	74.85	1.39	0.39	1407.75	Lb+Lc
14,E₂	6.55	0.00	33.36	0.18	59.91	0.00	0.25	704.81	Lb+Lc
15,E₃	5.34	2.21	33.72	0.00	58.73	19.12	0.00	685.45	Bis+Lc
16	4.09	0.01	20.86	0.13	74.91	0.14	0.28	1409.36	Inderite+Lc
17	4.18	0.02	21.33	0.13	74.34	0.27	0.28	1366.70	Inderite+Lc
18	4.10	0.10	21.18	0.18	74.44	1.37	0.39	1379.83	Inderite+Lc
19	5.61	1.15	31.76	0.49	60.99	10.48	0.70	749.93	Inderite+Lc
20	6.47	1.70	37.79	0.50	53.54	13.05	0.60	554.45	Inderite+Lc
21	5.85	2.17	36.01	0.41	55.56	17.48	0.52	603.90	Inderite+Lc
22,F₂	5.58	2.37	35.19	0.56	56.30	19.52	0.72	625.69	Inderite+Lc+Lcar
23	5.26	2.41	33.63	0.59	58.11	20.74	0.79	674.72	Inderite+Lcar
24,E₄	4.93	2.84	33.44	0.00	58.79	24.76	0.00	691.41	Bis+Lcar
25,F₃	4.85	2.68	32.14	0.96	59.37	23.99	1.35	716.98	Inderite+Lcar+Bis
26	3.99	4.12	31.84	1.19	58.86	37.10	1.68	715.03	Inderite+Bis
27	2.54	5.65	29.22	0.55	62.04	55.96	0.85	828.95	Inderite+Bis
28	2.07	6.34	28.75	0.70	62.14	63.63	1.10	841.36	Inderite+Bis
29	2.10	6.15	28.40	0.57	62.78	62.58	0.91	861.92	Inderite+Bis
30	1.37	4.96	21.23	0.51	71.93	67.40	1.09	1318.76	Inderite+Bis
31	0.83	4.24	16.39	0.46	78.08	74.47	1.27	1850.29	Inderite+Bis
32	0.41	3.66	12.57	0.44	82.92	83.60	1.57	2555.37	Inderite+Bis
33,E₅	0.00	3.19	9.12	0.42	87.27	100.00	2.06	3690.87	Inderite+Bis

No.	J(Mg²⁺)	Density, ρ/(g·cm^-3)	n_D	pH
1,E₁	2.00	1.0262	1.3400	9.195
2	1.87	1.0248	1.3421	9.173
3	1.70	1.022	1.3432	9.160
4	1.28	1.0241	1.3503	9.036
5	2.23	1.0267	1.3584	9.026
6	2.61	1.0281	1.3680	8.806
7	3.21	1.0300	1.3768	8.524
8	3.38	1.0484	1.3750	8.314
9	2.67	1.0694	1.3852	8.134
10	1.94	1.0957	1.4213	7.961
11,F₁	1.79	1.1199	1.3400	7.669
12	1.84	1.1256	1.3421	7.791
13	1.39	1.1429	1.3432	6.826
14,E₂	0.00	1.2498	1.3503	4.821
15,E₃	19.12	1.3121	1.4354	3.992
16	0.14	1.1412	1.3849	6.066
17	0.27	1.1447	1.3861	5.762
18	1.37	1.1483	1.3871	5.914
19	10.48	1.2581	1.4217	4.409
20	13.05	1.3178	1.4369	4.071
21	17.48	1.3190	1.438	3.961
22,F₂	19.52	1.3207	1.4365	3.971
23	20.74	1.3191	1.4362	3.962
24,E₄	24.76	1.3090	1.4348	4.007
25,F₃	23.99	1.3187	1.4351	3.946
26	37.10	1.3180	1.4331	3.952
27	55.96	1.3208	1.4353	4.021
28	63.63	1.3252	1.4373	3.986
29	62.58	1.3258	1.4375	3.967
30	67.40	1.3285	1.4389	4.001
31	74.47	1.3296	1.4398	4.012
32	83.60	1.3311	1.4407	4.023
33,E₅	100.00	1.3375	1.4428	4.112

No.	J(Mg²⁺)	Density, ρ/(g·cm^-3)	n_D	pH
1,E₁	2.00	1.0262	1.3400	9.195
2	1.87	1.0248	1.3421	9.173
3	1.70	1.022	1.3432	9.160
4	1.28	1.0241	1.3503	9.036
5	2.23	1.0267	1.3584	9.026
6	2.61	1.0281	1.3680	8.806
7	3.21	1.0300	1.3768	8.524
8	3.38	1.0484	1.3750	8.314
9	2.67	1.0694	1.3852	8.134
10	1.94	1.0957	1.4213	7.961
11,F₁	1.79	1.1199	1.3400	7.669
12	1.84	1.1256	1.3421	7.791
13	1.39	1.1429	1.3432	6.826
14,E₂	0.00	1.2498	1.3503	4.821
15,E₃	19.12	1.3121	1.4354	3.992
16	0.14	1.1412	1.3849	6.066
17	0.27	1.1447	1.3861	5.762
18	1.37	1.1483	1.3871	5.914
19	10.48	1.2581	1.4217	4.409
20	13.05	1.3178	1.4369	4.071
21	17.48	1.3190	1.438	3.961
22,F₂	19.52	1.3207	1.4365	3.971
23	20.74	1.3191	1.4362	3.962
24,E₄	24.76	1.3090	1.4348	4.007
25,F₃	23.99	1.3187	1.4351	3.946
26	37.10	1.3180	1.4331	3.952
27	55.96	1.3208	1.4353	4.021
28	63.63	1.3252	1.4373	3.986
29	62.58	1.3258	1.4375	3.967
30	67.40	1.3285	1.4389	4.001
31	74.47	1.3296	1.4398	4.012
32	83.60	1.3311	1.4407	4.023
33,E₅	100.00	1.3375	1.4428	4.112

Species	β⁽⁰⁾	β⁽¹⁾	β⁽²⁾	C^?	θ	ψ
LiCl	0.1469	0.3134	—	-0.00324	—	—
MgCl₂	0.3455	1.6987	—	0.05489	—	—
Li₂B₄O₇	5.9118	-37.298	—	-7.3439	—	—
MgB₄O₇	-1.7318	6.2356	-139.94	-1.4978	—	—
Li⁺, Mg²⁺	—	—	—	—	-0.00743	—
Cl^-, B₄O₇^2-	—	—	—	—	0.05252	—
Li⁺,Mg²⁺,Cl^-	—	—	—	—	—	0.00
Li⁺,Mg²⁺,B₄O₇^2-	—	—	—	—	—	0.00
Li⁺, Cl^-,B₄O₇^2-	—	—	—	—	—	1.0857
Mg²⁺,Cl^-,B₄O₇^2-	—	—	—	—	—	0.7383

四元体系（Li⁺， Mg²⁺//Cl^-， borate-H₂O）308.15 K相平衡与相图研究

Phase equilibria and phase diagram of the quaternary system (Li⁺, Mg²⁺//Cl^-, borate-H₂O) at 308.15 K

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