Phase equilibria and calculation of quaternary system LiCl+MgCl2+CaCl2+H2O at 323.2 K

doi:10.11949/0438-1157.20230115

Abstract

Abstract:

The solid-liquid phase equilibria of the quaternary system LiCl+MgCl₂+CaCl₂+H₂O at 323.2 K were studied by the isothermal dissolution method. The density, refractive index and composition of liquid phase were determined experimentally. The phase diagram of the quaternary system at 323.2 K was plotted. The results show that there are two double salts LiCl·MgCl₂·7H₂O and 2MgCl₂·CaCl₂·12H₂O formed in the quaternary system, belonging to a complex system. The phase diagram of this quaternary system consists of three invariant points, seven univariate curves, five crystallization fields corresponding to MgCl₂·6H₂O, LiCl·H₂O, CaCl₂·2H₂O, LiCl·MgCl₂·7H₂O, 2MgCl₂·CaCl₂·12H₂O. Comparing the phase diagram of the quaternary system at 323.2 K and 298.2 K, it has found that with the increase of temperature, calcium chloride is converted from CaCl₂·6H₂O and CaCl₂·4H₂O to CaCl₂·2H₂O, the crystallization fields of LiCl·MgCl₂·7H₂O and MgCl₂·6H₂O decrease and the crystallization fields of LiCl·H₂O and 2MgCl₂·CaCl₂·12H₂O increase, which indicates that increasing temperature is beneficial to the precipitation of LiCl·H₂O and 2MgCl₂·CaCl₂·12H₂O. The solubility of the quaternary system was calculated by using the PSC model, and the calculated results were basically consistent with the experimental results.

Key words: phase equilibria, aqueous solution, solubility, thermodynamic properties, lithium salt

摘要：

采用等温溶解平衡法开展了323.2 K四元体系LiCl+MgCl₂+CaCl₂+H₂O的固液相平衡研究，测定了平衡液相组成及密度、折射率，并绘制了相应的相图。研究发现：323.2 K时，该体系有复盐LiCl·MgCl₂·7H₂O和2MgCl₂·CaCl₂·12H₂O生成，属于复杂四元体系，其相图包含3个共饱点，7条单变量曲线，5个结晶区（MgCl₂·6H₂O、LiCl·H₂O、CaCl₂·2H₂O、LiCl·MgCl₂·7H₂O、2MgCl₂·CaCl₂·12H₂O）。对比298.2 K下该四元体系的相图，发现随着温度升高，氯化钙从CaCl₂·6H₂O、CaCl₂·4H₂O转化成CaCl₂·2H₂O，LiCl·MgCl₂·7H₂O和MgCl₂·6H₂O结晶区减小，LiCl·H₂O和2MgCl₂·CaCl₂·12H₂O结晶区增大，表明温度升高有利于LiCl·H₂O和2MgCl₂·CaCl₂·12H₂O析出。采用PSC模型对该四元体系进行了溶解度计算，计算结果与实验结果基本吻合。

关键词: 相平衡, 水溶液, 溶解性, 热力学性质, 锂盐

CLC Number:

O 642.4

Ke CHEN, Li DU, Ying ZENG, Siying REN, Xudong YU. Phase equilibria and calculation of quaternary system LiCl+MgCl₂+CaCl₂+H₂O at 323.2 K[J]. CIESC Journal, 2023, 74(5): 1896-1903.

陈科, 杜理, 曾英, 任思颖, 于旭东. 四元体系LiCl+MgCl₂+CaCl₂+H₂O 323.2 K相平衡研究及计算[J]. 化工学报, 2023, 74(5): 1896-1903.

Figures/Tables 11

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仪器名称	生产厂家	型号	精度值
电子分析天平	赛多利斯科学仪器（北京）有限公司	PRACTUM224-ICN	±0.0001 g
恒温培养箱	重庆英博实验仪器有限公司	SHH-250	±0.2 K
阿贝折射仪	上海仪电物理光学仪器公司	WYA	±0.0001
超级恒温水浴	常州国华电器有限公司	HH-501	±0.2 K
超纯水机	四川优普超纯科技有限公司	UPT-II-20T	—
回旋振荡器	常州市金坛友联仪器研究所	HY-5B	—
火焰原子吸收光谱仪	赛默飞世尔科技（中国）有限公司	ICE-3300	—
X射线衍射仪	日本理学	Ultima IV	—

仪器名称	生产厂家	型号	精度值
电子分析天平	赛多利斯科学仪器（北京）有限公司	PRACTUM224-ICN	±0.0001 g
恒温培养箱	重庆英博实验仪器有限公司	SHH-250	±0.2 K
阿贝折射仪	上海仪电物理光学仪器公司	WYA	±0.0001
超级恒温水浴	常州国华电器有限公司	HH-501	±0.2 K
超纯水机	四川优普超纯科技有限公司	UPT-II-20T	—
回旋振荡器	常州市金坛友联仪器研究所	HY-5B	—
火焰原子吸收光谱仪	赛默飞世尔科技（中国）有限公司	ICE-3300	—
X射线衍射仪	日本理学	Ultima IV	—

编号	密度/(g·cm^-3)	折射率 n_D	液相组成, w(B) /%				J(B)/(g/100 g)				平衡固相
编号	密度/(g·cm^-3)	折射率 n_D	LiCl	MgCl₂	CaCl₂	H₂O	LiCl	MgCl₂	CaCl₂	H₂O	平衡固相
1, E	1.3949	1.4468	0.00	23.92	19.64	56.44	0.00	54.92	45.08	129.57	Bis + Tac
2	1.3403	1.4429	1.67	24.02	19.65	54.66	3.68	52.99	43.33	120.59	Bis + Tac
3	1.3347	1.4418	4.58	22.98	17.65	54.79	10.12	50.83	39.05	121.21	Bis + Tac
4	1.3311	1.4405	8.53	21.95	14.43	55.09	18.99	48.87	32.14	122.63	Bis + Tac
5	1.3353	1.4401	12.77	21.06	11.21	54.96	28.35	46.76	24.89	122.00	Bis + Tac
6	1.3207	1.4400	17.67	20.00	7.45	54.88	39.16	44.33	16.51	121.62	Bis + Tac
7, A	1.3017	1.4374	23.26	20.73	0.00	56.01	52.87	47.13	0.00	127.32	Bis + Li-Car
8	1.3263	1.4362	22.68	20.53	3.48	53.31	48.57	43.98	7.45	114.20	Bis + Li-Car
9, F₁	1.3329	1.4411	22.54	19.83	4.64	52.99	47.95	42.18	9.87	112.77	Bis + Li-Car + Tac
10	1.3340	1.4409	23.04	17.42	4.30	55.24	51.47	38.92	9.61	123.35	Li-Car + Tac
11	1.3368	1.4419	24.51	16.84	4.18	54.47	53.83	36.99	9.18	119.66	Li-Car + Tac
12	1.3268	1.4421	30.25	12.30	4.34	53.11	64.52	26.23	9.25	113.25	Li-Car + Tac
13, B	1.3081	1.4399	36.91	9.16	0.00	53.93	80.12	19.88	0.00	117.04	Li-Car + LC
14	1.3366	1.4420	35.73	9.34	2.76	52.17	74.70	19.54	5.76	109.06	Li-Car + LC
15, F₂	1.3353	1.4434	35.30	8.94	4.29	51.47	72.75	18.41	8.84	106.08	Li-Car + LC + Tac
16	1.3217	1.4451	35.34	8.68	5.41	50.57	71.49	17.57	10.94	102.30	LC + Tac
17	1.3294	1.4468	34.70	8.25	6.79	50.26	69.76	16.58	13.66	101.05	LC + Tac
18	1.3578	1.4480	33.69	7.02	9.52	49.77	67.07	13.97	18.96	99.07	LC + Tac
19	1.3354	1.4471	32.23	5.37	11.78	50.62	65.28	10.87	23.85	102.52	LC + Tac
20	1.3197	1.4411	29.84	4.49	12.67	53.00	63.48	9.55	26.97	112.75	LC + Tac
21	1.3751	1.4558	30.15	3.56	19.04	47.25	57.16	6.74	36.10	89.60	LC + Tac
22	1.3852	1.4558	29.40	2.21	21.33	47.06	55.53	4.18	40.29	88.90	LC + Tac
23	1.4294	1.4679	28.51	2.01	27.00	42.48	49.56	3.49	46.95	73.86	LC + Tac
24, F₃	1.4198	1.4660	25.44	1.73	29.83	43.00	44.62	3.04	52.34	75.43	LC + Tac + Sin
25, C	1.4100	1.4702	27.78	0.00	30.76	41.46	47.45	0.00	52.55	70.80	LC + Sin
26, D	1.4770	1.5076	0.00	3.26	54.31	42.43	0.00	5.66	94.34	73.70	Tac + Sin
27	1.4743	1.4824	4.26	3.16	49.47	43.11	7.49	5.55	86.96	75.77	Tac + Sin
28	1.4720	1.4912	8.33	2.68	46.20	42.79	14.56	4.69	80.75	74.78	Tac + Sin
29	1.4537	1.4680	13.93	2.44	39.11	44.52	25.11	4.39	70.50	80.24	Tac + Sin
30	1.4451	1.4670	19.40	2.51	34.29	43.80	34.52	4.46	61.02	77.95	Tac + Sin
31	1.4489	1.4689	22.74	1.96	33.22	42.08	39.26	3.38	57.36	72.66	Tac + Sin

编号	密度/(g·cm^-3)	折射率 n_D	液相组成, w(B) /%				J(B)/(g/100 g)				平衡固相
编号	密度/(g·cm^-3)	折射率 n_D	LiCl	MgCl₂	CaCl₂	H₂O	LiCl	MgCl₂	CaCl₂	H₂O	平衡固相
1, E	1.3949	1.4468	0.00	23.92	19.64	56.44	0.00	54.92	45.08	129.57	Bis + Tac
2	1.3403	1.4429	1.67	24.02	19.65	54.66	3.68	52.99	43.33	120.59	Bis + Tac
3	1.3347	1.4418	4.58	22.98	17.65	54.79	10.12	50.83	39.05	121.21	Bis + Tac
4	1.3311	1.4405	8.53	21.95	14.43	55.09	18.99	48.87	32.14	122.63	Bis + Tac
5	1.3353	1.4401	12.77	21.06	11.21	54.96	28.35	46.76	24.89	122.00	Bis + Tac
6	1.3207	1.4400	17.67	20.00	7.45	54.88	39.16	44.33	16.51	121.62	Bis + Tac
7, A	1.3017	1.4374	23.26	20.73	0.00	56.01	52.87	47.13	0.00	127.32	Bis + Li-Car
8	1.3263	1.4362	22.68	20.53	3.48	53.31	48.57	43.98	7.45	114.20	Bis + Li-Car
9, F₁	1.3329	1.4411	22.54	19.83	4.64	52.99	47.95	42.18	9.87	112.77	Bis + Li-Car + Tac
10	1.3340	1.4409	23.04	17.42	4.30	55.24	51.47	38.92	9.61	123.35	Li-Car + Tac
11	1.3368	1.4419	24.51	16.84	4.18	54.47	53.83	36.99	9.18	119.66	Li-Car + Tac
12	1.3268	1.4421	30.25	12.30	4.34	53.11	64.52	26.23	9.25	113.25	Li-Car + Tac
13, B	1.3081	1.4399	36.91	9.16	0.00	53.93	80.12	19.88	0.00	117.04	Li-Car + LC
14	1.3366	1.4420	35.73	9.34	2.76	52.17	74.70	19.54	5.76	109.06	Li-Car + LC
15, F₂	1.3353	1.4434	35.30	8.94	4.29	51.47	72.75	18.41	8.84	106.08	Li-Car + LC + Tac
16	1.3217	1.4451	35.34	8.68	5.41	50.57	71.49	17.57	10.94	102.30	LC + Tac
17	1.3294	1.4468	34.70	8.25	6.79	50.26	69.76	16.58	13.66	101.05	LC + Tac
18	1.3578	1.4480	33.69	7.02	9.52	49.77	67.07	13.97	18.96	99.07	LC + Tac
19	1.3354	1.4471	32.23	5.37	11.78	50.62	65.28	10.87	23.85	102.52	LC + Tac
20	1.3197	1.4411	29.84	4.49	12.67	53.00	63.48	9.55	26.97	112.75	LC + Tac
21	1.3751	1.4558	30.15	3.56	19.04	47.25	57.16	6.74	36.10	89.60	LC + Tac
22	1.3852	1.4558	29.40	2.21	21.33	47.06	55.53	4.18	40.29	88.90	LC + Tac
23	1.4294	1.4679	28.51	2.01	27.00	42.48	49.56	3.49	46.95	73.86	LC + Tac
24, F₃	1.4198	1.4660	25.44	1.73	29.83	43.00	44.62	3.04	52.34	75.43	LC + Tac + Sin
25, C	1.4100	1.4702	27.78	0.00	30.76	41.46	47.45	0.00	52.55	70.80	LC + Sin
26, D	1.4770	1.5076	0.00	3.26	54.31	42.43	0.00	5.66	94.34	73.70	Tac + Sin
27	1.4743	1.4824	4.26	3.16	49.47	43.11	7.49	5.55	86.96	75.77	Tac + Sin
28	1.4720	1.4912	8.33	2.68	46.20	42.79	14.56	4.69	80.75	74.78	Tac + Sin
29	1.4537	1.4680	13.93	2.44	39.11	44.52	25.11	4.39	70.50	80.24	Tac + Sin
30	1.4451	1.4670	19.40	2.51	34.29	43.80	34.52	4.46	61.02	77.95	Tac + Sin
31	1.4489	1.4689	22.74	1.96	33.22	42.08	39.26	3.38	57.36	72.66	Tac + Sin

编号	J(B)/(g/100 g)				平衡固相	编号	J(B)/(g/100 g)				平衡固相
编号	LiCl	MgCl₂	CaCl₂	H₂O	平衡固相	编号	LiCl	MgCl₂	CaCl₂	H₂O	平衡固相
1	56.70	43.30	0.00	130.06	Bis+Li-Car	22	77.61	16.37	6.02	108.45	LiCl·H₂O+Li-Car
2	55.80	42.77	1.43	129.13	Bis+Li-Car	23	76.53	16.29	7.18	107.82	LiCl·H₂O+Li-Car
3	54.90	42.26	2.84	128.20	Bis+Li-Car	24	75.99	16.26	7.75	107.51	LiCl·H₂O+Li-Car
4	54.00	41.77	4.23	127.28	Bis+Li-Car	25	75.23	16.21	8.56	107.07	LiCl·H₂O+Li-Car
5	53.10	41.29	5.61	126.36	Bis+Li-Car	26	74.66	16.18	9.16	106.74	LiCl·H₂O+Li-Car+Tac
6	51.41	40.42	8.17	124.63	Bis+Li-Car+Tac	27	74.22	14.12	11.66	105.06	LiCl·H₂O+Tac
7	0.00	51.64	48.36	122.17	Bis+Tac	28	68.83	9.33	21.84	98.37	LiCl·H₂O+Tac
8	10.61	49.54	39.85	125.18	Bis+Tac	29	62.22	7.05	30.73	92.28	LiCl·H₂O+Tac
9	21.61	47.73	30.66	127.42	Bis+Tac	30	55.96	5.63	38.41	86.53	LiCl·H₂O+Tac
10	27.15	46.79	26.06	128.09	Bis+Tac	31	55.28	0.00	44.72	79.56	LiCl·H₂O+Sin
11	32.65	45.75	21.60	128.36	Bis+Tac	32	53.61	2.32	44.07	81.08	LiCl·H₂O+Sin
12	38.03	44.58	17.39	128.15	Bis+Tac	33	51.76	4.83	43.41	82.40	LiCl·H₂O+Sin+Tac
13	43.20	43.22	13.58	127.39	Bis+Tac	34	0.00	14.95	85.05	83.22	Sin+Tac
14	60.56	30.16	9.28	119.05	Li-Car+Tac	35	7.28	13.98	78.74	85.92	Sin+Tac
15	67.45	23.02	9.53	113.65	Li-Car+Tac	36	14.85	12.77	72.38	87.61	Sin+Tac
16	70.51	20.04	9.45	110.89	Li-Car+Tac	37	22.49	11.43	66.08	88.42	Sin+Tac
17	83.20	16.80	0.00	111.59	LiCl·H₂O+Li-Car	38	29.98	9.99	60.03	88.41	Sin+Tac
18	82.06	16.70	1.24	110.96	LiCl·H₂O+Li-Car	39	37.14	8.50	54.36	87.61	Sin+Tac
19	80.94	16.61	2.45	110.33	LiCl·H₂O+Li-Car	40	43.75	6.97	49.28	86.01	Sin+Tac
20	79.82	16.53	3.65	109.70	LiCl·H₂O+Li-Car	41	49.62	5.45	44.93	83.62	Sin+Tac
21	78.71	16.44	4.85	109.07	LiCl·H₂O+Li-Car

Phase equilibria and calculation of quaternary system LiCl+MgCl₂+CaCl₂+H₂O at 323.2 K

四元体系LiCl+MgCl₂+CaCl₂+H₂O 323.2 K相平衡研究及计算

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