三元体系KCl + CaCl2 + H2O 298.2、323.2及348.2 K相平衡研究及计算

doi:10.11949/0438-1157.20230470

摘要/Abstract

摘要：

采用等温溶解平衡法开展了298.2、323.2、348.2 K三元体系KCl + CaCl₂ + H₂O相平衡研究，测定了平衡液相组成及密度，采用Schreinemakers湿渣法和X射线粉晶衍射法确定了平衡固相组成。研究发现：298.2 K时，该体系为简单三元体系，无复盐形成，相图由1个三元共饱点、2条单变量曲线和2个结晶相区组成；323.2和348.2 K时，该体系为复杂三元体系，有复盐氯钾钙石（KCl·CaCl₂）形成，相图均由2个三元共饱点、3条单变量曲线和3个结晶相区组成。对比该三元体系278.2、298.2、308.2、323.2、348.2 K相图可知：随温度升高，CaCl₂结晶形式发生变化，CaCl₂·6H₂O（278.2、298.2 K）→CaCl₂·4H₂O（308.2 K）→CaCl₂·2H₂O（323.2、348.2 K）；KCl结晶面积在323.2 K时最大，氯钾钙石结晶面积随温度升高而增大。采用Pitzer-Simonson-Clegg模型进行了三元体系KCl + CaCl₂ + H₂O（298.2、323.2、348.2 K）热力学计算，理论计算值与实验值吻合较好。

关键词: 相平衡, 溶解性, 水合物, PSC模型, 氯钾钙石

Abstract:

The composition of equilibrium liquid of the ternary system KCl + CaCl₂ + H₂O were determined by isothermal dissolution method at 298.2, 323.2, and 348.2 K. The density and composition of the equilibirum liquid phase were measured experimentally. The equilibirum solid phase composition was determined by Schreinemakers wet residue method and X-ray diffraction method. It is found that at 298.2 K, the system is a simple ternary system without double salt formation, and the phase diagram consists of one ternary invariant point, two univariate curves and two crystalline phase regions. The ternary system belongs to complex type system with the formation of double salt chlorocalcite (KCl·CaCl₂) at 323.2 and 348.2 K. And the phase diagrams consist of two invariant points, three univariate curves and three crystallization regions. By comparing the phase diagrams of the ternary system at 278.2, 298.2, 308.2, 323.2, and 348.2 K, it can be found that with the temperature increasing, the crystallization form of CaCl₂ changes from CaCl₂·6H₂O (278.2, 298.2 K), CaCl₂·4H₂O (308.2 K) to CaCl₂·2H₂O (323.2, 348.2 K). The crystallization area of KCl is the largest at 323.2 K, and the size of the double salt chlorocalcite crystallization region increases with the temperature increasing. The thermodynamics calculations of KCl + CaCl₂ + H₂O at 298.2, 323.2, and 348.2 K were carried out by Pitzer-Simonson-Clegg model, and the calculation values agree well with the experimental values.

Key words: phase equilibria, solubility, hydrate, PSC model, chlorocalcite

中图分类号:

O 642.4

于旭东, 李琪, 陈念粗, 杜理, 任思颖, 曾英. 三元体系KCl + CaCl₂ + H₂O 298.2、323.2及348.2 K相平衡研究及计算[J]. 化工学报, 2023, 74(8): 3256-3265.

Xudong YU, Qi LI, Niancu CHEN, Li DU, Siying REN, Ying ZENG. Phase equilibria and calculation of aqueous ternary system KCl + CaCl₂ + H₂O at 298.2, 323.2, and 348.2 K[J]. CIESC Journal, 2023, 74(8): 3256-3265.

图/表 15

图1 二元体系KCl + H2O、CaCl2 + H2O 298.2、323.2、348.2 K溶解度数据对比

Fig.1 Comparison of solubility data of the binary systems KCl + H2O, CaCl2+H2O at 298.2, 323.2, and 348.2 K

表1 三元体系KCl + CaCl2 + H2O 在298.2、323.2和348.2 K的固液相平衡数据

Table 1 Solid-liquid phase equilibria data of the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

编号	密度 ρ/(g/cm³)	液相组成 w(B)×10²		湿固相组成 w(B)×10²		平衡固相
编号	密度 ρ/(g/cm³)	w(KCl)	w(CaCl₂)	w(KCl)	w(CaCl₂)	平衡固相
T = 298.2 K
1, A	1.1837	26.18	0.00	—	—	KCl
2	1.1919	23.23	2.77	59.29	1.54	KCl
3	1.1953	21.07	5.16	59.94	2.63	KCl
4	1.2130	18.31	8.14	53.82	4.57	KCl
5	1.2217	15.55	11.26	72.01	3.67	KCl
6	1.2459	12.07	15.57	51.16	8.68	KCl
7	1.2605	9.80	19.19	62.52	8.00	KCl
8	1.2847	7.58	22.71	80.77	4.75	KCl
9	1.3010	5.58	26.41	71.16	7.82	KCl
10	1.3383	4.91	28.74	53.74	14.18	KCl
11	1.3490	4.07	31.84	67.50	10.44	KCl
12	1.3873	3.58	34.72	66.73	11.79	KCl
13	1.3961	3.34	36.81	63.62	13.41	KCl
14	1.4252	3.18	40.47	63.92	14.24	KCl
15	1.4503	3.52	43.08	77.75	9.21	KCl
16	1.4615	3.31	44.41	50.94	21.71	KCl
17, S₁	1.4664	2.81	45.62	1.10	48.59	KCl + CaCl₂·6H₂O
18, B	1.4570	0.00	44.83	—	—	CaCl₂·6H₂O
T = 323.2 K
1, C	1.2032	29.87	0.00	—	—	KCl
2	1.2119	26.52	3.28	65.74	1.57	KCl
3	1.2149	23.39	6.46	73.40	2.19	KCl
4	1.2327	20.21	10.18	67.70	4.27	KCl
5	1.2474	17.00	13.43	66.42	5.55	KCl
6	1.2600	13.40	17.67	67.87	6.64	KCl
7	1.2792	10.97	21.21	65.99	8.06	KCl
8	1.2954	8.55	25.18	65.82	9.29	KCl
9	1.3149	6.40	29.11	67.27	10.41	KCl
10	1.3532	6.09	31.26	65.90	11.46	KCl
11	1.3908	5.12	36.74	71.33	11.29	KCl
12	1.4188	4.87	40.10	72.83	11.56	KCl
13	1.4559	5.01	42.97	76.87	12.51	KCl
14	1.4843	5.28	44.98	75.73	13.47	KCl
15	1.5001	5.63	47.10	74.76	13.45	KCl
16	1.5131	5.84	48.83	73.58	14.40	KCl
17	1.5526	7.23	50.86	33.33	36.61	KCl
18, S₂	1.5571	7.40	51.88	40.08	54.27	KCl + KCl·CaCl₂
19	1.5556	7.24	52.74	10.14	52.97	KCl·CaCl₂
20	1.5508	5.01	55.02	26.21	57.97	KCl·CaCl₂
21, S₃	1.5511	4.24	55.07	7.48	61.15	KCl·CaCl₂ + CaCl₂·2H₂O
22	1.5496	4.10	55.18	2.57	62.16	CaCl₂·2H₂O
23	1.5384	2.18	55.58	2.05	60.68	CaCl₂·2H₂O
24, D	1.5366	0.00	56.74	—	—	CaCl₂·2H₂O
T = 348.2 K
1, E	1.2992	33.08	0.00	—	—	KCl
2	1.3057	29.78	3.64	77.93	1.56	KCl
3	1.3153	26.22	7.07	75.07	2.30	KCl
4	1.3236	22.94	10.43	70.94	4.52	KCl
5	1.3442	19.10	14.59	61.73	7.51	KCl
6	1.3490	15.64	19.79	65.71	9.51	KCl
7	1.3889	12.42	24.19	77.24	7.93	KCl
8	1.4435	10.21	28.66	68.01	10.59	KCl
9	1.4597	7.70	33.05	69.57	12.08	KCl
10	1.5251	7.16	38.38	71.84	12.05	KCl
11	1.5890	6.50	41.34	65.19	15.48	KCl
12	1.6241	6.42	43.68	67.34	15.57	KCl
13	1.6385	7.09	46.21	66.84	16.23	KCl
14, S₄	1.6511	9.36	48.36	19.73	44.10	KCl + KCl·CaCl₂
15	1.6612	7.99	51.52	19.08	53.98	KCl·CaCl₂
16	1.6708	5.85	53.98	17.23	55.68	KCl·CaCl₂
17	1.6765	4.66	55.38	10.18	56.31	KCl·CaCl₂
18, S₅	1.6820	3.69	56.56	8.79	60.30	KCl·CaCl₂ + CaCl₂·2H₂O
19	1.7013	2.43	56.82	1.34	63.88	CaCl₂·2H₂O
20	1.7214	1.95	57.12	1.16	63.62	CaCl₂·2H₂O
21, F	1.7432	0.00	58.84	—	—	CaCl₂·2H₂O

表1 三元体系KCl + CaCl2 + H2O 在298.2、323.2和348.2 K的固液相平衡数据

Table 1 Solid-liquid phase equilibria data of the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

编号	密度 ρ/(g/cm³)	液相组成 w(B)×10²		湿固相组成 w(B)×10²		平衡固相
编号	密度 ρ/(g/cm³)	w(KCl)	w(CaCl₂)	w(KCl)	w(CaCl₂)	平衡固相
T = 298.2 K
1, A	1.1837	26.18	0.00	—	—	KCl
2	1.1919	23.23	2.77	59.29	1.54	KCl
3	1.1953	21.07	5.16	59.94	2.63	KCl
4	1.2130	18.31	8.14	53.82	4.57	KCl
5	1.2217	15.55	11.26	72.01	3.67	KCl
6	1.2459	12.07	15.57	51.16	8.68	KCl
7	1.2605	9.80	19.19	62.52	8.00	KCl
8	1.2847	7.58	22.71	80.77	4.75	KCl
9	1.3010	5.58	26.41	71.16	7.82	KCl
10	1.3383	4.91	28.74	53.74	14.18	KCl
11	1.3490	4.07	31.84	67.50	10.44	KCl
12	1.3873	3.58	34.72	66.73	11.79	KCl
13	1.3961	3.34	36.81	63.62	13.41	KCl
14	1.4252	3.18	40.47	63.92	14.24	KCl
15	1.4503	3.52	43.08	77.75	9.21	KCl
16	1.4615	3.31	44.41	50.94	21.71	KCl
17, S₁	1.4664	2.81	45.62	1.10	48.59	KCl + CaCl₂·6H₂O
18, B	1.4570	0.00	44.83	—	—	CaCl₂·6H₂O
T = 323.2 K
1, C	1.2032	29.87	0.00	—	—	KCl
2	1.2119	26.52	3.28	65.74	1.57	KCl
3	1.2149	23.39	6.46	73.40	2.19	KCl
4	1.2327	20.21	10.18	67.70	4.27	KCl
5	1.2474	17.00	13.43	66.42	5.55	KCl
6	1.2600	13.40	17.67	67.87	6.64	KCl
7	1.2792	10.97	21.21	65.99	8.06	KCl
8	1.2954	8.55	25.18	65.82	9.29	KCl
9	1.3149	6.40	29.11	67.27	10.41	KCl
10	1.3532	6.09	31.26	65.90	11.46	KCl
11	1.3908	5.12	36.74	71.33	11.29	KCl
12	1.4188	4.87	40.10	72.83	11.56	KCl
13	1.4559	5.01	42.97	76.87	12.51	KCl
14	1.4843	5.28	44.98	75.73	13.47	KCl
15	1.5001	5.63	47.10	74.76	13.45	KCl
16	1.5131	5.84	48.83	73.58	14.40	KCl
17	1.5526	7.23	50.86	33.33	36.61	KCl
18, S₂	1.5571	7.40	51.88	40.08	54.27	KCl + KCl·CaCl₂
19	1.5556	7.24	52.74	10.14	52.97	KCl·CaCl₂
20	1.5508	5.01	55.02	26.21	57.97	KCl·CaCl₂
21, S₃	1.5511	4.24	55.07	7.48	61.15	KCl·CaCl₂ + CaCl₂·2H₂O
22	1.5496	4.10	55.18	2.57	62.16	CaCl₂·2H₂O
23	1.5384	2.18	55.58	2.05	60.68	CaCl₂·2H₂O
24, D	1.5366	0.00	56.74	—	—	CaCl₂·2H₂O
T = 348.2 K
1, E	1.2992	33.08	0.00	—	—	KCl
2	1.3057	29.78	3.64	77.93	1.56	KCl
3	1.3153	26.22	7.07	75.07	2.30	KCl
4	1.3236	22.94	10.43	70.94	4.52	KCl
5	1.3442	19.10	14.59	61.73	7.51	KCl
6	1.3490	15.64	19.79	65.71	9.51	KCl
7	1.3889	12.42	24.19	77.24	7.93	KCl
8	1.4435	10.21	28.66	68.01	10.59	KCl
9	1.4597	7.70	33.05	69.57	12.08	KCl
10	1.5251	7.16	38.38	71.84	12.05	KCl
11	1.5890	6.50	41.34	65.19	15.48	KCl
12	1.6241	6.42	43.68	67.34	15.57	KCl
13	1.6385	7.09	46.21	66.84	16.23	KCl
14, S₄	1.6511	9.36	48.36	19.73	44.10	KCl + KCl·CaCl₂
15	1.6612	7.99	51.52	19.08	53.98	KCl·CaCl₂
16	1.6708	5.85	53.98	17.23	55.68	KCl·CaCl₂
17	1.6765	4.66	55.38	10.18	56.31	KCl·CaCl₂
18, S₅	1.6820	3.69	56.56	8.79	60.30	KCl·CaCl₂ + CaCl₂·2H₂O
19	1.7013	2.43	56.82	1.34	63.88	CaCl₂·2H₂O
20	1.7214	1.95	57.12	1.16	63.62	CaCl₂·2H₂O
21, F	1.7432	0.00	58.84	—	—	CaCl₂·2H₂O

图2 三元体系KCl + CaCl2 + H2O 298.2 K固液相图

Fig.2 Solid-liquid diagram of the ternary system KCl + CaCl2 + H2O at 298.2 K

图3 共饱点S1处平衡固相XRD谱图

Fig.3 XRD pattern of the invariant point S1

图4 三元体系KCl + CaCl2 + H2O 323.2 K固液相图

Fig.4 Solid-liquid diagram of the ternary system KCl + CaCl2 + H2O at 323.2 K

图5 三元体系KCl + CaCl2 + H2O 348.2 K固液相图

Fig.5 Solid-liquid diagram of the ternary system KCl + CaCl2 + H2O at 348.2 K

图6 共饱点S2处平衡固相XRD谱图

Fig.6 XRD pattern of the invariant point S2

图7 共饱点S3处平衡固相XRD谱图

Fig.7 XRD pattern of the invariant point S3

图8 共饱点S4处平衡固相XRD谱图

Fig.8 XRD pattern of the invariant point S4

图9 共饱点S5处平衡固相XRD谱图

Fig.9 XRD pattern of the invariant point S5

图10 三元体系KCl + CaCl2 + H2O对比相图Sy—KCl; Chle—KCl·CaCl2; KC—2KCl·CaCl2·2H2O; Ant—CaCl2·6H2O; Sin—CaCl2·2H2O

Fig.10 Comparison of phase diagrams of the ternary system KCl + CaCl2 + H2O

表2 三元体系KCl + CaCl2 + H2O 298.2、323.2和348.2 K单盐参数

Table 2 Single salt parameters of the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

体系	α_MX	$α M X 1$	B_MX	$B M X 1$	W_1,MX	U_1,MX	V_1,MX	文献
T = 298.2 K								[32]
KCl-H₂O	13	0	9.1029	0	-3.7326	-3.1452	0.3974
CaCl₂-H₂O	13	2	57.5105	163.5972	23.2003	71.0962	-79.9384
T = 323.2 K
KCl-H₂O	13	0	10.4427	0	-3.2804	-2.3879	0.4077
CaCl₂-H₂O	13	2	90.4708	88.6000	15.0772	57.7981	-60.2934
T = 348.2 K
KCl-H₂O	13	0	15.4538	0	0.2626	6.1647	-4.7684
CaCl₂-H₂O	13	2	119.6073	14.5708	4.9119	39.4562	-37.3883

表2 三元体系KCl + CaCl2 + H2O 298.2、323.2和348.2 K单盐参数

Table 2 Single salt parameters of the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

体系	α_MX	$α M X 1$	B_MX	$B M X 1$	W_1,MX	U_1,MX	V_1,MX	文献
T = 298.2 K								[32]
KCl-H₂O	13	0	9.1029	0	-3.7326	-3.1452	0.3974
CaCl₂-H₂O	13	2	57.5105	163.5972	23.2003	71.0962	-79.9384
T = 323.2 K
KCl-H₂O	13	0	10.4427	0	-3.2804	-2.3879	0.4077
CaCl₂-H₂O	13	2	90.4708	88.6000	15.0772	57.7981	-60.2934
T = 348.2 K
KCl-H₂O	13	0	15.4538	0	0.2626	6.1647	-4.7684
CaCl₂-H₂O	13	2	119.6073	14.5708	4.9119	39.4562	-37.3883

表3 三元体系KCl + CaCl2 + H2O 298.2、323.2和348.2 K混合参数

Table 3 Mixing parameters of the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

T/K	W_MNX	Q_MNX	U_MNX	文献
298.2	216.2946	-333.0332	254.5483	[32]
323.2	201.1790	-322.7688	255.6148
348.2	157.8346	-267.3083	217.4444

表4 三元体系KCl + CaCl2 + H2O 298.2、323.2和348.2 K各盐溶度积常数

Table 4 Ksp of solid phase in the ternary system KCl + CaCl2 + H2O at 298.2， 323.2， and 348.2 K

固相	T/K	K_sp	文献
KCl	298.2	8.1347	[32]
	323.2	12.7311
	348.2	16.9827
CaCl₂·6H₂O	298.2	7.4367×10³
CaCl₂·2H₂O	323.3	2.5202×10⁶
CaCl₂·2H₂O	348.2	6.3200×10⁵
KCl·CaCl₂	323.2	2.9535×10⁸
KCl·CaCl₂	348.2	7.8489×10⁷

图11 三元体系KCl + CaCl2 + H2O 298.2(a)、323.2(b)、348.2 K(c)实验与计算相图

Fig.11 Experimental and calculated phase diagrams of the ternary system KCl + CaCl2 + H2O at 298.2(a), 323.2(b), and 348.2 K(c)

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三元体系KCl + CaCl₂ + H₂O 298.2、323.2及348.2 K相平衡研究及计算

Phase equilibria and calculation of aqueous ternary system KCl + CaCl₂ + H₂O at 298.2, 323.2, and 348.2 K

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