Li+、Na+、K+、SO42--H2O体系相图在MVR蒸发过程的应用研究

doi:10.19964/j.issn.1006-4990.2020-0533

Abstract

Abstract:

In industry,the by-product of extracting lithium from ore to produce lithium carbonate is the sodium sulfate pow-der.In order to solve the current problem of lithium sulfate and sodium sulfate eutectic during MVR evaporation,the following measures were taken：Firstly,combining with the actual sample data of MVR production process,the phase diagram of Li⁺,Na⁺,K⁺,SO₄^2- -H₂O system was theoretically analyzed,and the existence of lithium sulfate and sodium sulfate eutectic com-plex salts in the evaporation process of MVR was proved and comprehensively analyzed by chemical analyzed means of flame photometer,atomic absorption spectrophotometer and XRD.Secondly,combining with the MVR equipment structure and pro-duction process,a solution to the problem of excessive lithium impurities in sodium sulfate production caused by lithium sul-fate and sodium sulfate eutectic was put forward.

Key words: sodium sulfate, MVR crystallizer, lithium sulfate, cocrystallization

CLC Number:

TQ131.1

Cite this article

Tian Haiying,Zhou Fu,Xu Chuan,Tu Mingjiang,Zhong Zhaozi,Liao Shiying,Li Shihong. Application research of Li⁺,Na⁺,K⁺,SO₄^2--H₂O system phase diagram in MVR evaporation process[J]. Inorganic Chemicals Industry, 2021, 53(8): 75-78.

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Figures/Tables 10

Fig.1

Sampling point identification and MVR evaporation flow chart of sodium sulfate"

Fig.1

Table 1

Data of sodium sulfate MVR evaporating crystal slurry"

编号	平衡液相组分质量分数/%				平衡固相组分质量分数/%
编号	Li₂SO₄	Na₂SO₄	K₂SO₄	H₂O	Li₂SO₄	Na₂SO₄	K₂SO₄
1	7.46	18.54	1.83	70.85	32.50	62.47	5.03
2	7.91	21.95	2.05	68.07	30.19	64.87	4.94
3	7.62	19.67	2.17	69.49	31.49	62.85	5.67
4	7.92	22.87	2.06	69.77	29.43	65.74	4.83
5	8.03	20.81	1.81	68.41	31.76	63.72	4.52
6	7.81	22.64	4.71	68.72	27.59	61.90	10.51
7	6.83	19.64	2.10	68.90	29.25	65.08	5.67
8	7.17	21.94	1.91	68.05	28.28	66.95	4.77
9	8.04	21.15	2.52	73.87	30.93	62.95	6.12
10	7.62	18.08	2.39	68.33	32.97	60.51	6.52
11	8.03	19.72	2.42	68.76	32.35	61.49	6.16
12	7.93	18.92	2.81	70.11	32.57	60.14	7.29
13	8.44	20.94	2.90	66.29	31.89	61.19	6.92
14	7.75	19.32	3.00	69.75	31.51	60.79	7.70
15	7.41	19.78	2.78	70.02	30.28	62.54	7.18
16	6.99	19.55	2.54	70.19	29.47	63.76	6.77
17	7.99	15.32	2.06	71.47	37.77	56.08	6.15
18	8.01	18.64	1.96	71.14	33.85	60.92	5.24
19	6.32	22.69	2.21	65.86	25.00	69.47	5.53
20	6.72	21.35	2.44	65.92	27.13	66.66	6.22
21	7.86	17.91	2.71	68.39	33.54	59.15	7.31
22	7.51	22.46	2.65	64.12	28.28	65.42	6.30
23	7.49	20.21	3.85	68.17	29.31	61.19	9.50
24	7.61	19.15	3.10	72.28	31.22	60.75	8.03
25	8.10	23.73	3.16	66.78	28.46	64.53	7.02
26	7.41	19.47	3.59	73.59	29.95	60.90	9.16
27	7.17	24.09	3.70	66.75	25.48	66.22	8.30
28	7.94	23.68	3.48	68.75	27.91	64.37	7.72
29	6.76	24.95	2.82	67.82	24.28	69.33	6.39
30	7.58	25.59	3.09	67.33	25.84	67.50	6.66
31	7.17	25.32	3.38	68.41	24.81	67.81	7.39
32	6.66	27.10	4.27	67.40	21.97	69.15	8.88

Table 1

Table 2

Data of sodium sulfate MVR evaporated slurry"

编号	平衡液相组分质量分数/%				平衡固相组分质量分数/%
编号	Li₂SO₄	Na₂SO₄	K₂SO₄	H₂O	Li₂SO₄	Na₂SO₄	K₂SO₄
1	3.84	22.28	1.18	68.16	17.58	78.99	3.43
2	3.10	23.91	0.84	69.03	14.01	83.59	2.40
3	3.53	21.16	1.13	70.61	17.11	79.44	3.45
4	3.37	24.39	1.13	66.34	14.69	82.21	3.10
5	3.91	19.97	1.37	70.33	19.34	76.39	4.27
6	3.19	22.50	1.38	68.93	14.87	81.07	4.07
7	4.06	23.92	1.74	68.37	17.16	78.20	4.64
8	3.53	21.03	1.48	72.38	17.03	78.47	4.50
9	3.20	24.51	0.93	69.79	14.08	83.34	2.58
10	4.07	21.03	1.73	69.65	18.99	75.93	5.09
11	4.30	23.74	1.84	69.68	18.06	77.06	4.88
12	4.74	24.74	2.00	70.42	18.85	76.13	5.01
13	4.05	27.04	1.42	69.16	15.65	80.87	3.47
14	4.85	27.45	2.14	65.98	17.67	77.42	4.92
15	3.78	28.22	1.67	67.69	14.17	81.88	3.95
16	3.66	30.22	1.53	66.87	13.05	83.50	3.45
17	3.29	34.76	1.42	66.15	10.59	86.53	2.88
18	3.31	29.81	1.43	67.86	12.12	84.57	3.31
19	3.33	28.75	1.48	70.47	12.57	83.90	3.53
20	3.60	30.69	1.58	68.04	12.70	83.79	3.51
21	3.81	28.81	1.77	68.06	14.00	81.90	4.11
22	3.86	27.39	1.66	67.51	14.79	81.19	4.02
23	3.84	27.57	1.73	67.29	14.61	81.22	4.17
24	4.22	28.28	2.01	67.38	15.40	79.95	4.64
25	4.73	27.75	2.05	66.82	17.20	78.09	4.70
26	4.00	28.22	1.97	66.10	14.78	80.62	4.60
27	3.75	27.63	1.62	68.23	14.34	81.75	3.91
28	3.94	27.42	1.94	68.01	14.95	80.40	4.65
29	3.58	28.04	1.69	69.08	13.60	82.34	4.06
30	3.72	27.22	1.03	68.76	14.64	82.82	2.55
31	4.29	29.27	2.85	67.79	14.92	78.82	6.26
32	4.37	28.32	2.17	67.76	15.81	79.23	4.96

Table 2

Table 3

Data of sodium sulfate MVR evaporative centrifuge mother liquor"

编号	平衡液相组分质量分数/%				平衡固相组分质量分数/%
编号	Li₂SO₄	Na₂SO₄	K₂SO₄	H₂O	Li₂SO₄	Na₂SO₄	K₂SO₄
1	3.19	24.71	0.91	69.11	13.93	83.56	2.51
2	3.66	18.78	0.11	70.98	20.03	79.59	0.38
3	3.80	22.67	1.56	69.14	17.01	78.57	4.42
4	3.28	25.25	1.27	70.76	13.88	82.73	3.39
5	4.35	25.19	1.96	68.47	17.36	77.70	4.94
6	4.18	25.37	1.26	68.98	17.00	79.76	3.24
7	3.33	28.12	1.72	69.14	12.71	83.15	4.14
8	3.50	29.01	1.49	68.43	13.03	83.47	3.50
9	3.40	27.28	2.88	69.36	12.90	80.19	6.91
10	3.98	29.61	1.88	66.91	14.16	81.62	4.22
11	3.92	28.30	1.71	67.50	14.58	81.41	4.01
12	4.83	27.40	1.99	66.49	17.71	77.69	4.60
13	4.15	26.68	1.83	67.06	15.99	79.55	4.46
14	3.58	27.64	17.03	61.32	10.02	59.87	30.11
15	4.18	27.52	1.90	68.91	15.66	79.83	4.50

Table 3

Fig.2

Phase diagram of Li2SO4-Na2SO4-K2SO4-H2O and MVR evaporation process data enlarged by 2 times"

Fig.2

Table 4

Solid A composition detection of crystal slurry"

编号	各组分质量分数/%				n（Li⁺）/ n（SO₄^2-）	n（Na⁺）/ n（SO₄^2-）	n（K⁺）/ n（SO₄^2-）
编号	Li⁺	Na⁺	K⁺	SO₄^2-	n（Li⁺）/ n（SO₄^2-）	n（Na⁺）/ n（SO₄^2-）	n（K⁺）/ n（SO₄^2-）
1	2.73	21.80	5.15	58.49	0.64	1.56	0.22
2	2.17	24.12	4.71	59.07	0.51	1.70	0.20
3	2.09	22.73	4.60	59.10	0.48	1.61	0.19
4	1.03	26.34	1.74	55.14	0.26	1.99	0.08
5	1.63	26.99	3.55	66.96	0.34	1.68	0.13
6	1.18	27.29	2.32	62.60	0.26	1.82	0.09

Table 4

Fig.3

XRD pattern of Solid A"

Fig.3

Table 5

Composition of original solution g/L"

成分	质量浓度	成分	质量浓度
Li₂O	8.24	K⁺	4.20
SO₄^2-	190.60	Na⁺	82.50

Table 5

Table 6

Experimental condition and results of dissolution of eutectic substances dissolved at 25 ℃ for 30 min"

编号	原液体积/mL	共晶料体积/mL	V（原液）/ V（共晶料）	冲洗后母液 ρ（Li₂O）/(g·L^-1)	冲洗后固体 w（Li₂O）/%
1	341	1 900	0.18	25.05	0.45
2	341	1 900	0.18	25.24	0.72
3	741	1 500	0.49	23.10	0.09
4	741	1 500	0.49	22.50	0.08
5	1 100	1 700	0.65	20.06	0.09
6	1 100	1 700	0.65	20.54	0.09

Table 6

Fig.4

XRD pattern of solid substances after dissolution reaction"

Fig.4

References 6

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[2]	陈贵娥, 张志刚. 电池级碳酸锂的生产及其应用实践研究[J]. 世界有色金属, 2019(2):155,157.
[3]	彭建忠. 国内碳酸锂生产工艺和效益分析[J]. 盐科学与化工, 2019, 48(10):18-21.
[4]	任志峰. 我国元明粉市场纵览[J]. 日用化学品科学, 2007(10):1-4,8.
[5]	刘长岩, 秦佳政. 盐化工技术在锂行业的应用[J]. 盐业与化工, 2016, 45(3):1-3.
[6]	Liu Y, Guo Y, Yu X, et al. Solid-liquid metastable phase equili-bria in the five-component system(Li+Na+K+Cl+SO₄+H₂O) at 308.15 K[J]. Journal of Chemical & Engineering Data, 2014, 59(5):1685-1691. doi: 10.1021/je500140e

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Application research of Li⁺,Na⁺,K⁺,SO₄^2--H₂O system phase diagram in MVR evaporation process

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Application research of Li⁺,Na⁺,K⁺,SO₄^2--H₂O system phase diagram in MVR evaporation process