Phase equilibria for quaternary system Rb+, Cs+, Mg2+ // SO42- - H2O at 298.2 K

doi:10.11949/0438-1157.20200159

Abstract

Abstract:

Phase equilibria for the quaternary system Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O at 298.2 K was studied by an isothermal dissolution equilibrium method. The solubilities, densities, and refractive indices of the system at equilibrium were also determined experimentally. Based on the measured data, the stable phase diagram, and diagrams of density vs composition, refractive index vs composition were plotted. The results show that the quaternary system belongs to a complex type at 298.2 K with the double salts Cs₂SO₄·MgSO₄·6H₂O, Rb₂SO₄·MgSO₄·6H₂O, and solid solution [(Rb, Cs)₂SO₄] formed. The phase diagram consists of 4 invariant points, 9 univariant curves, and 6 crystallization zones. Invariant points E₁, E₂, and E₃belong to commensurate type, while invariant point E₄ belongs to incommensurate type. The crystallization zones corrsepond to 3 single salts Rb₂SO₄, MgSO₄·7H₂O, Cs₂SO₄, 2 double salts Cs₂SO₄·MgSO₄·6H₂O and Rb₂SO₄·MgSO₄·6H₂O, 1 solid solution [(Rb, Cs)₂SO₄]. The crystallization zone of double salt Rb₂SO₄·MgSO₄·6H₂O is the largest, while the crystallization zone of single salt Cs₂SO₄ is the smallest, which indicating that Rb₂SO₄·MgSO₄·6H₂O is most easily crystallized. The densities and refractive indices change regularly with the changing of Cs₂SO₄content of the solution. The stable phase diagram of the system will provide a theoretical basis for the development and utilization of resources such as rubidium and cesium in the magnesium sulfate subtype salt lake brine.

Key words: phase equilibria, isothermal dissolution equilibrium method, double salt, solid solution, solubility

摘要：

采用等温溶解平衡法研究了298.2 K下四元体系Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O的相平衡关系，测定了该体系的溶解度、密度以及折射率，并绘制了相应的稳定相图、水图、密度-组成图和折射率-组成图。研究表明：298.2 K下，该四元体系为复杂四元体系，有复盐Cs₂SO₄·MgSO₄·6H₂O和Rb₂SO₄·MgSO₄·6H₂O以及固溶体[(Rb, Cs）₂SO₄]生成。其稳定相图由4个四元共饱点、9条单变量曲线以及6个结晶区组成。四元共饱点中E₁、E₂、E₃为相称共饱点，E₄为不相称共饱点。6个结晶相区分别对应3种单盐Rb₂SO₄、MgSO₄·7H₂O、Cs₂SO₄，2种复盐Cs₂SO₄·MgSO₄·6H₂O、Rb₂SO₄·MgSO₄·6H₂O和1种固溶体[(Rb,Cs）₂SO₄]。其中，复盐Rb₂SO₄·MgSO₄·6H₂O结晶区最大，表明其在该体系中最易结晶析出；Cs₂SO₄结晶区最小。平衡液相的密度和折射率随着溶液中Cs₂SO₄含量变化呈规律性变化。该体系稳定相图将为硫酸镁亚型盐湖卤水中的铷、铯等资源开发利用提供理论依据。

关键词: 相平衡, 等温溶解平衡法, 复盐, 固溶体, 溶解度

CLC Number:

O 642

Ying ZENG, Peijun CHEN, Xudong YU. Phase equilibria for quaternary system Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O at 298.2 K[J]. CIESC Journal, 2020, 71(8): 3460-3468.

曾英, 陈佩君, 于旭东. 四元体系Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O 298.2 K相平衡研究[J]. 化工学报, 2020, 71(8): 3460-3468.

Figures/Tables 11

References 30

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System	Composition of equilibrium solution, w(B)/%^①			Equilibrated solid phase^②	Ref.
System	w(Rb₂SO₄)	w(Cs₂SO₄)	w(MgSO₄)	Equilibrated solid phase^②	Ref.
Rb⁺, Mg²⁺ // SO₄^2- - H₂O	3.77	0.00	25.67	RM + M₇	[29]
	4.31	0.00	26.75	RM + M₇	this work
	33.60	0.00	0.69	Rb₂SO₄+ RM	[29]
	31.69	0.00	0.63	Rb₂SO₄+ RM	this work
Cs⁺, Mg²⁺ // SO₄^2- - H₂O	0.00	10.59	24.39	CM + M₇	[29]
	0.00	12.97	26.72	CM + M₇	this work
	0.00	63.56	0.46	Cs₂SO₄+ CM	[29]
	0.00	64.27	0.32	Cs₂SO₄+ CM	this work

System	Composition of equilibrium solution, w(B)/%^①			Equilibrated solid phase^②	Ref.
System	w(Rb₂SO₄)	w(Cs₂SO₄)	w(MgSO₄)	Equilibrated solid phase^②	Ref.
Rb⁺, Mg²⁺ // SO₄^2- - H₂O	3.77	0.00	25.67	RM + M₇	[29]
	4.31	0.00	26.75	RM + M₇	this work
	33.60	0.00	0.69	Rb₂SO₄+ RM	[29]
	31.69	0.00	0.63	Rb₂SO₄+ RM	this work
Cs⁺, Mg²⁺ // SO₄^2- - H₂O	0.00	10.59	24.39	CM + M₇	[29]
	0.00	12.97	26.72	CM + M₇	this work
	0.00	63.56	0.46	Cs₂SO₄+ CM	[29]
	0.00	64.27	0.32	Cs₂SO₄+ CM	this work

No.	Composition of equilibrium solution, w(B)/%				J?necke index of dry salt,J(B)/(g·(100 g S)^-1)				Equilibrated solid phase^①
No.	w(Rb₂SO₄)	w(Cs₂SO₄)	w(MgSO₄)	w(H₂O)	J(Rb₂SO₄)	J(Cs₂SO₄)	J(MgSO₄)	J(H₂O)	Equilibrated solid phase^①
1, A	28.18	15.97	0.00	55.85	63.83	36.17	0.00	126.50	Rb₂SO₄ + S
2, E₁	30.25	15.82	0.66	53.27	64.74	33.85	1.41	114.00	Rb₂SO₄+ S + RM
3, B	0.95	61.78	0.00	37.27	1.51	98.49	0.00	59.41	Cs₂SO₄+ S
4, E₂	2.03	58.44	0.41	39.12	3.33	96.00	0.67	64.26	Cs₂SO₄+ S + CM
5, C	0.00	64.27	0.32	35.41	0.00	99.50	0.50	54.82	Cs₂SO₄+ CM
6	1.67	61.67	0.38	36.28	2.62	96.78	0.60	56.94	Cs₂SO₄+ CM
7, E₂	2.03	58.44	0.41	39.12	3.33	96.00	0.67	64.26	Cs₂SO₄+ S + CM
8	3.87	56.65	0.56	38.92	6.34	92.74	0.92	63.72	S + CM
9	6.96	53.67	0.46	38.91	11.39	87.86	0.75	63.69	S + CM
10	12.91	49.41	0.64	37.04	20.51	78.47	1.02	58.83	S + CM
11	17.80	44.59	0.38	37.23	28.36	71.03	0.61	59.31	S + CM
12	20.76	37.59	0.36	41.29	35.36	64.03	0.61	70.33	S + CM
13	22.57	32.02	0.37	45.04	41.07	58.26	0.67	81.95	S + CM
14	24.87	27.10	0.44	47.59	47.45	51.71	0.84	90.80	S + CM
15	26.19	23.85	0.44	49.52	51.88	47.25	0.87	98.10	S + CM
16	26.71	20.42	0.46	52.41	56.12	42.91	0.97	110.13	S + CM
17	28.04	18.65	0.48	52.83	59.44	39.54	1.02	112.00	S + CM
18, E₄	29.38	16.45	0.48	53.69	63.44	35.52	1.04	115.94	S + RM + CM
19, D	0.00	12.97	26.72	60.31	0.00	32.68	67.32	151.95	CM + M₇
20	0.72	11.68	25.71	61.89	1.89	30.65	67.46	162.40	CM + M₇
21	1.89	10.15	25.75	62.21	5.00	26.86	68.14	164.62	CM + M₇
22, E₃	2.92	9.55	25.07	62.46	7.78	25.44	66.78	166.38	CM + M₇+ RM
23	3.10	9.58	19.25	68.07	9.71	30.00	60.29	213.19	CM + RM
24	5.39	11.46	11.91	71.24	18.74	39.85	41.41	247.71	CM + RM
25	8.86	13.36	5.25	72.53	32.25	48.64	19.11	264.03	CM + RM
26	11.52	15.27	3.53	69.68	37.99	50.37	11.64	229.82	CM + RM
27	16.68	15.18	1.82	66.32	49.53	45.07	5.40	196.91	CM + RM
28	21.28	16.34	1.21	61.17	54.80	42.08	3.12	157.53	CM + RM
29	24.34	16.08	0.90	58.68	58.90	38.92	2.18	142.01	CM + RM
30	27.55	15.95	0.80	55.70	62.19	36.00	1.81	125.73	CM + RM
31, E₄	29.38	16.45	0.48	53.69	63.44	35.52	1.04	115.94	S + RM + CM
32, E	4.31	0.00	26.75	68.94	13.88	0.00	86.12	221.96	RM + M₇
33	3.92	1.91	26.45	67.72	12.14	5.92	81.94	209.79	RM + M₇
34	3.53	5.29	26.56	64.62	9.98	14.95	75.07	182.65	RM + M₇
35	3.08	7.92	25.87	63.13	8.35	21.48	70.17	171.22	RM + M₇
36, E₃	2.92	9.55	25.07	62.46	7.78	25.44	66.78	166.38	CM + M₇+ RM
37, F	31.69	0.00	0.63	67.68	98.05	0.00	1.95	209.41	Rb₂SO₄+ RM
38	30.93	1.61	0.54	66.92	93.50	4.87	1.63	202.30	Rb₂SO₄+ RM
39	30.65	3.15	0.54	65.66	89.26	9.17	1.57	191.21	Rb₂SO₄+ RM
40	31.25	5.88	0.49	62.38	83.07	15.63	1.30	165.82	Rb₂SO₄+ RM
41	30.51	7.48	0.49	61.52	79.29	19.44	1.27	159.88	Rb₂SO₄+ RM
42	30.22	9.22	0.48	60.08	75.70	23.10	1.20	150.50	Rb₂SO₄+ RM
43	29.08	13.21	0.49	57.22	67.97	30.88	1.15	133.75	Rb₂SO₄+ RM
44, E₁	30.25	15.82	0.66	53.27	64.74	33.85	1.41	114.00	Rb₂SO₄+ S +RM

No.	Composition of equilibrium solution, w(B)/%				J?necke index of dry salt,J(B)/(g·(100 g S)^-1)				Equilibrated solid phase^①
No.	w(Rb₂SO₄)	w(Cs₂SO₄)	w(MgSO₄)	w(H₂O)	J(Rb₂SO₄)	J(Cs₂SO₄)	J(MgSO₄)	J(H₂O)	Equilibrated solid phase^①
1, A	28.18	15.97	0.00	55.85	63.83	36.17	0.00	126.50	Rb₂SO₄ + S
2, E₁	30.25	15.82	0.66	53.27	64.74	33.85	1.41	114.00	Rb₂SO₄+ S + RM
3, B	0.95	61.78	0.00	37.27	1.51	98.49	0.00	59.41	Cs₂SO₄+ S
4, E₂	2.03	58.44	0.41	39.12	3.33	96.00	0.67	64.26	Cs₂SO₄+ S + CM
5, C	0.00	64.27	0.32	35.41	0.00	99.50	0.50	54.82	Cs₂SO₄+ CM
6	1.67	61.67	0.38	36.28	2.62	96.78	0.60	56.94	Cs₂SO₄+ CM
7, E₂	2.03	58.44	0.41	39.12	3.33	96.00	0.67	64.26	Cs₂SO₄+ S + CM
8	3.87	56.65	0.56	38.92	6.34	92.74	0.92	63.72	S + CM
9	6.96	53.67	0.46	38.91	11.39	87.86	0.75	63.69	S + CM
10	12.91	49.41	0.64	37.04	20.51	78.47	1.02	58.83	S + CM
11	17.80	44.59	0.38	37.23	28.36	71.03	0.61	59.31	S + CM
12	20.76	37.59	0.36	41.29	35.36	64.03	0.61	70.33	S + CM
13	22.57	32.02	0.37	45.04	41.07	58.26	0.67	81.95	S + CM
14	24.87	27.10	0.44	47.59	47.45	51.71	0.84	90.80	S + CM
15	26.19	23.85	0.44	49.52	51.88	47.25	0.87	98.10	S + CM
16	26.71	20.42	0.46	52.41	56.12	42.91	0.97	110.13	S + CM
17	28.04	18.65	0.48	52.83	59.44	39.54	1.02	112.00	S + CM
18, E₄	29.38	16.45	0.48	53.69	63.44	35.52	1.04	115.94	S + RM + CM
19, D	0.00	12.97	26.72	60.31	0.00	32.68	67.32	151.95	CM + M₇
20	0.72	11.68	25.71	61.89	1.89	30.65	67.46	162.40	CM + M₇
21	1.89	10.15	25.75	62.21	5.00	26.86	68.14	164.62	CM + M₇
22, E₃	2.92	9.55	25.07	62.46	7.78	25.44	66.78	166.38	CM + M₇+ RM
23	3.10	9.58	19.25	68.07	9.71	30.00	60.29	213.19	CM + RM
24	5.39	11.46	11.91	71.24	18.74	39.85	41.41	247.71	CM + RM
25	8.86	13.36	5.25	72.53	32.25	48.64	19.11	264.03	CM + RM
26	11.52	15.27	3.53	69.68	37.99	50.37	11.64	229.82	CM + RM
27	16.68	15.18	1.82	66.32	49.53	45.07	5.40	196.91	CM + RM
28	21.28	16.34	1.21	61.17	54.80	42.08	3.12	157.53	CM + RM
29	24.34	16.08	0.90	58.68	58.90	38.92	2.18	142.01	CM + RM
30	27.55	15.95	0.80	55.70	62.19	36.00	1.81	125.73	CM + RM
31, E₄	29.38	16.45	0.48	53.69	63.44	35.52	1.04	115.94	S + RM + CM
32, E	4.31	0.00	26.75	68.94	13.88	0.00	86.12	221.96	RM + M₇
33	3.92	1.91	26.45	67.72	12.14	5.92	81.94	209.79	RM + M₇
34	3.53	5.29	26.56	64.62	9.98	14.95	75.07	182.65	RM + M₇
35	3.08	7.92	25.87	63.13	8.35	21.48	70.17	171.22	RM + M₇
36, E₃	2.92	9.55	25.07	62.46	7.78	25.44	66.78	166.38	CM + M₇+ RM
37, F	31.69	0.00	0.63	67.68	98.05	0.00	1.95	209.41	Rb₂SO₄+ RM
38	30.93	1.61	0.54	66.92	93.50	4.87	1.63	202.30	Rb₂SO₄+ RM
39	30.65	3.15	0.54	65.66	89.26	9.17	1.57	191.21	Rb₂SO₄+ RM
40	31.25	5.88	0.49	62.38	83.07	15.63	1.30	165.82	Rb₂SO₄+ RM
41	30.51	7.48	0.49	61.52	79.29	19.44	1.27	159.88	Rb₂SO₄+ RM
42	30.22	9.22	0.48	60.08	75.70	23.10	1.20	150.50	Rb₂SO₄+ RM
43	29.08	13.21	0.49	57.22	67.97	30.88	1.15	133.75	Rb₂SO₄+ RM
44, E₁	30.25	15.82	0.66	53.27	64.74	33.85	1.41	114.00	Rb₂SO₄+ S +RM

No.	J(Cs₂SO₄)	Density, ρ/(g?cm^-3)	Refractive index, n_D	No.	J(Cs₂SO₄)	Density, ρ/(g?cm^-3)	Refractive index, n_D
1, A	36.17	1.5180	1.3766	23	30.00	1.3494	1.3841
2, E₁	33.85	1.5100	1.3767	24	39.85	1.2974	1.3704
3, B	98.49	2.0126	1.4102	25	48.64	1.2851	1.3640
4, E₂	96.00	2.0253	1.4109	26	50.37	1.3046	1.3640
5, C	99.50	1.9803	1.4084	27	45.07	1.3537	1.3660
6	96.78	2.0130	1.4104	28	42.08	1.4146	1.3700
7, E₂	96.00	2.0253	1.4109	29	38.92	1.4452	1.3723
8	92.74	2.0223	1.4100	30	36.00	1.4891	1.3746
9	87.86	2.0114	1.4090	31, E₄	35.52	1.4917	1.3754
10	78.47	1.9685	1.4032	32, E	0.00	1.3261	1.3914
11	71.03	1.8375	1.3978	33	5.92	1.3442	1.3921
12	64.03	1.7240	1.3923	34	14.95	1.4207	1.3938
13	58.26	1.6658	1.3878	35	21.48	1.4268	1.3943
14	51.71	1.6321	1.3839	36, E₃	25.44	1.4458	1.3945
15	47.25	1.5786	1.3812	37, F	0.00	1.3675	1.3660
16	42.91	1.5626	1.3795	38	4.87	1.3772	1.3668
17	39.54	1.5251	1.3773	39	9.17	1.3959	1.3680
18, E₄	35.52	1.4917	1.3754	40	15.63	1.4351	1.3695
19, D	32.68	1.4082	1.3995	41	19.44	1.4473	1.3708
20	30.65	1.4153	1.3983	42	23.10	1.4684	1.3718
21	26.86	1.4178	1.3976	43	30.88	1.4993	1.3745
22, E₃	25.44	1.4458	1.3945	44, E₁	33.85	1.5100	1.3767

Phase equilibria for quaternary system Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O at 298.2 K

四元体系Rb⁺, Cs⁺, Mg²⁺ // SO₄^2- - H₂O 298.2 K相平衡研究

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