313.15 K四元体系Na+//  S   O   4   2 -    ，  C   O   3   2 -    ，  N   O   3   -    -H2O固液相平衡研究

doi:10.11949/j.issn.0438-1157.20181517

摘要/Abstract

摘要：

采用等温溶解法研究313.15 K下四元体系Na⁺// $S O 4 2 -$ , $C O 3 2 -$ , $N O 3 -$ -H₂O的固液相平衡关系。测定了平衡溶液的溶解度数据及物理性质数据，包括密度、黏度、折射率。根据实验数据，绘制了相应的干盐相图、水图及物理性质-组成图。实验结果表明：313.15 K下，此四元体系相图包括两个共饱和点，六条单变曲线以及五个单盐结晶区域(分别为NaNO₃，Na₂SO₄，Na₂CO₃·H₂O, Bur(Na₂CO₃·2Na₂SO₄)，Da(NaNO₃·Na₂SO₄·H₂O))，其中Bur的结晶区域最大，最容易从混合溶液中结晶析出。实验中的物理性质(黏度、密度、折射率)随J(Na₂SO₄)的变化呈现相似性规律。该体系中存在复盐碱芒硝Bur(Na₂CO₃·2Na₂SO₄)、钠硝矾Da(NaNO₃·Na₂SO₄·H₂O)，结晶水合物(Na₂CO₃·H₂O)，没有固溶体存在，故该体系是一个复杂的共饱和型。实验所获数据和结论对煤化工过程产生的高盐废水结晶析盐工艺开发及实现资源梯级综合利用具有重要意义。

关键词: 硫酸钠, 相平衡, 四元体系, 物理性质

Abstract:

An experimental study on phase equilibria of the system Na⁺// $S O 4 2 -$ , $C O 3 2 -$ , $N O 3 -$ -H₂O at 313.15K was done by the method of isothermal solution saturation. The solubility and physical properties (ρ, η, n _D) of the equilibrium quaternary system were measured, and the corresponding phase diagram, water diagram and physical property (ρ, η, n _D) diagram were obtained based on the data measured. The results show that: the phase diagram of Na⁺// $S O 4 2 -$ ， $C O 3 2 -$ ， $N O 3 -$ -H₂O at 313.15 K consists of two invariant points, six univariant curves, and five crystallization regions which are NaNO₃，Na₂SO₄，Na₂CO₃·H₂O, Bur(Na₂CO₃·2Na₂SO₄),and Da(NaNO₃·Na₂SO₄·H₂O), respectively. The Bur crystallization field occupies the largest part, which indicates it is easier to crystallize in the mixing solution. All the physical properties (ρ, η, n _D) change regularly with J(Na₂SO₄) composition. Bur(Na₂CO₃·2Na₂SO₄), Da(NaNO₃·Na₂SO₄·H₂O) and crystalline hydrate (Na₂CO₃·H₂O) are proven to co-exist in the quaternary system, whereas no solid solution is found in the temperature range investigated, which means the reciprocal quaternary system is a complex eutectic type. The data and conclusions obtained from the experiment are of great significance for the development of crystallization salt separation process of high salt wastewater produced by coal chemical process and the realization of comprehensive utilization of resources.

Key words: Na₂SO₄, phase equilibria, quaternary system, physical properties

中图分类号:

O 642

任永胜, 曹晶, 于冰洁. 313.15 K四元体系Na⁺// $S O 4 2 -$ ， $C O 3 2 -$ ， $N O 3 -$ -H₂O固液相平衡研究[J]. 化工学报, 2019, 70(6): 2102-2109.

Yongsheng REN, Jing CAO, Bingjie YU. Solid-liquid equilibria of quaternary system Na ⁺// $S O 4 2 -$ , $C O 3 2 -$ , $N O 3 -$ -H₂O at 313.15 K[J]. CIESC Journal, 2019, 70(6): 2102-2109.

图/表 7

表1 不同单变曲线阶段饱和溶液的配制方案

Table 1 Preparation of solutions corresponding to different sections of isotherm

Ternary system	Initial point	Solid phase	Additive
Na₂SO₄-NaNO₃-H₂O	E	NaNO₃+NaNO₃·Na₂SO₄·H₂O	NaCl
Na₂SO₄-NaNO₃-H₂O	F	Na₂SO₄+NaNO₃·Na₂SO₄·H₂O	NaCl
Na₂CO₃-Na₂SO₄-H₂O	H	Na₂SO₄ + Na₂CO₃·2Na₂SO₄	NaNO₃
	L	Na₂CO₃ + Na₂CO₃·2Na₂SO₄	NaNO₃
Na₂CO₃-NaNO₃-H₂O	G	Na₂CO₃ + NaNO₃	Na₂SO₄

表2 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时固液相平衡数据①

Table 2 Solid-liquid equilibrium of quaternary system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

No.	Composition of solution, w(b)×100			J?necke index of dry salt/(g/100 g S)				平衡固相^②
No.	Na₂SO₄	Na₂CO₃	NaNO₃	J(Na₂SO₄)	J(Na₂CO₃)	J(NaNO₃)	J(H₂O)	平衡固相^②
1,E	2.47	0.00	48.91	4.81	0.00	95.19	94.63	N + NS
2	2.49	2.44	46.48	4.83	4.74	90.42	94.52	N + NS
3	2.54	4.93	42.94	5.04	9.77	85.18	98.39	N + NS
4	2.42	7.36	41.69	4.70	14.30	81.00	94.28	N + NS
5,Q	2.38	8.26	40.05	4.70	16.30	79.01	97.29	N + NS + C
6,F	7.76	0.00	36.07	17.70	0.00	82.30	128.20	S + NS
7	7.09	2.79	34.93	15.83	6.22	77.95	123.14	S + NS
8	5.30	5.24	33.96	11.91	11.78	76.31	124.67	S + NS + CS
9,G	0.00	9.06	40.70	0.00	18.21	81.79	100.98	N + C
10,Q	2.37	8.74	39.29	4.69	17.35	77.96	98.41	N + C + CS
11,H	20.85	13.35	0.00	60.97	39.03	0.00	192.39	S + CS
12	18.79	13.17	3.29	53.31	37.36	9.33	183.68	S + CS
13	16.98	12.87	6.48	46.74	35.42	17.84	175.25	S + CS
14	15.46	10.98	9.25	43.32	30.76	25.92	180.16	S + CS
15	13.74	10.28	12.40	37.72	28.24	34.04	174.62	S + CS
16	12.60	9.01	15.48	33.96	24.30	41.74	169.57	S + CS
17	11.53	8.18	17.74	30.79	21.84	47.37	167.08	S + CS
18	10.19	7.76	20.90	26.23	19.98	53.79	157.32	S + CS
19	9.24	7.55	22.72	23.39	19.11	57.50	153.11	S + CS
20	6.45	7.18	28.27	15.39	17.14	67.47	138.68	S + CS
21	5.64	7.10	30.29	13.11	16.51	70.39	132.36	S + CS
22,S	3.81	6.64	32.60	8.85	15.41	75.74	132.29	S + CS + NS
23,L	5.12	29.71	0.00	14.69	85.31	0.00	187.18	C + CS
24	5.07	27.88	3.54	14.14	76.19	9.67	173.34	C + CS
25	4.96	25.81	6.31	13.38	69.62	17.01	169.70	C + CS
26	4.58	23.61	9.52	12.15	62.60	25.25	165.09	C + CS
27	4.50	21.82	12.47	11.61	56.25	32.14	157.78	C + CS
28	4.00	19.90	15.25	10.22	50.83	38.95	155.44	C + CS
29	3.50	18.58	18.35	8.66	45.96	45.38	147.31	C + CS
30	3.15	17.21	20.63	7.69	41.99	50.32	143.95	C + CS
31	2.84	15.92	23.55	6.72	37.62	55.66	136.33	C + CS
32	2.61	14.60	26.20	6.01	33.64	60.35	130.34	C + CS
33	2.42	13.48	28.61	5.44	30.29	64.27	124.66	C + CS
34	2.32	11.52	32.91	4.96	24.64	70.40	113.90	C + CS
35,Q	2.37	8.74	39.29	4.69	17.35	77.96	98.41	N + C + CS

表2 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时固液相平衡数据①

Table 2 Solid-liquid equilibrium of quaternary system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

No.	Composition of solution, w(b)×100			J?necke index of dry salt/(g/100 g S)				平衡固相^②
No.	Na₂SO₄	Na₂CO₃	NaNO₃	J(Na₂SO₄)	J(Na₂CO₃)	J(NaNO₃)	J(H₂O)	平衡固相^②
1,E	2.47	0.00	48.91	4.81	0.00	95.19	94.63	N + NS
2	2.49	2.44	46.48	4.83	4.74	90.42	94.52	N + NS
3	2.54	4.93	42.94	5.04	9.77	85.18	98.39	N + NS
4	2.42	7.36	41.69	4.70	14.30	81.00	94.28	N + NS
5,Q	2.38	8.26	40.05	4.70	16.30	79.01	97.29	N + NS + C
6,F	7.76	0.00	36.07	17.70	0.00	82.30	128.20	S + NS
7	7.09	2.79	34.93	15.83	6.22	77.95	123.14	S + NS
8	5.30	5.24	33.96	11.91	11.78	76.31	124.67	S + NS + CS
9,G	0.00	9.06	40.70	0.00	18.21	81.79	100.98	N + C
10,Q	2.37	8.74	39.29	4.69	17.35	77.96	98.41	N + C + CS
11,H	20.85	13.35	0.00	60.97	39.03	0.00	192.39	S + CS
12	18.79	13.17	3.29	53.31	37.36	9.33	183.68	S + CS
13	16.98	12.87	6.48	46.74	35.42	17.84	175.25	S + CS
14	15.46	10.98	9.25	43.32	30.76	25.92	180.16	S + CS
15	13.74	10.28	12.40	37.72	28.24	34.04	174.62	S + CS
16	12.60	9.01	15.48	33.96	24.30	41.74	169.57	S + CS
17	11.53	8.18	17.74	30.79	21.84	47.37	167.08	S + CS
18	10.19	7.76	20.90	26.23	19.98	53.79	157.32	S + CS
19	9.24	7.55	22.72	23.39	19.11	57.50	153.11	S + CS
20	6.45	7.18	28.27	15.39	17.14	67.47	138.68	S + CS
21	5.64	7.10	30.29	13.11	16.51	70.39	132.36	S + CS
22,S	3.81	6.64	32.60	8.85	15.41	75.74	132.29	S + CS + NS
23,L	5.12	29.71	0.00	14.69	85.31	0.00	187.18	C + CS
24	5.07	27.88	3.54	14.14	76.19	9.67	173.34	C + CS
25	4.96	25.81	6.31	13.38	69.62	17.01	169.70	C + CS
26	4.58	23.61	9.52	12.15	62.60	25.25	165.09	C + CS
27	4.50	21.82	12.47	11.61	56.25	32.14	157.78	C + CS
28	4.00	19.90	15.25	10.22	50.83	38.95	155.44	C + CS
29	3.50	18.58	18.35	8.66	45.96	45.38	147.31	C + CS
30	3.15	17.21	20.63	7.69	41.99	50.32	143.95	C + CS
31	2.84	15.92	23.55	6.72	37.62	55.66	136.33	C + CS
32	2.61	14.60	26.20	6.01	33.64	60.35	130.34	C + CS
33	2.42	13.48	28.61	5.44	30.29	64.27	124.66	C + CS
34	2.32	11.52	32.91	4.96	24.64	70.40	113.90	C + CS
35,Q	2.37	8.74	39.29	4.69	17.35	77.96	98.41	N + C + CS

图1 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时干盐图

Fig.1 Dry-salt phase diagram of system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

图2 共饱和点Q和S的XRD谱图

Fig.2 XRD pattern of invariant point Q(a) and S(b)

图3 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时水图

Fig.3 Water-content diagram of system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

图4 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O) 在313.15 K时物理性质-组成图

Fig.4 Physical properties as function of J (Na2SO4) composition in quaternary system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

表3 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时平衡液相物理性质

Table 3 Physical properties of quaternary system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

No.^①	J(Na₂SO₄)	Viscosity $× 10 - 3$ /(Pa·s)^②	Refractive index	Density/(g·cm^?3)
1,E	4.81	2.2861	1.39229	1.4258
2	4.83	2.6218	1.39407	1.4290
3	5.04	3.0358	1.39539	1.4351
4	4.70	3.4904	1.39720	1.4415
5,Q	4.70	3.6338	1.39801	1.4414
6,F	17.70	1.9106	1.38343	1.3569
7	15.83	2.2850	1.38656	1.3754
8	11.91	2.5782	1.38871	1.3824
9,G	0.00	3.5211	1.39744	1.4351
10,Q	4.69	3.8538	1.39813	1.4456
11,H	60.97	4.2930	1.38712	1.3470
12	53.31	4.0326	1.38700	1.3406
13	46.74	3.9056	1.38719	1.3508
14	43.32	3.2815	1.38495	1.3369
15	37.72	3.0421	1.38340	1.3372
16	33.96	2.7706	1.38308	1.3345
17	30.79	2.7511	1.38407	1.3538
18	26.23	2.7164	1.38460	1.3596
19	23.39	2.6785	1.38520	1.3655
20	15.39	2.6085	1.38704	1.3771
21	13.11	2.7023	1.38807	1.3864
22,S	8.85	2.8018	1.38994	1.3953
23,L	14.69	7.6458	1.39776	1.3754
24	14.14	7.2336	1.39757	1.3790
25	13.38	6.4775	1.39598	1.3815
26	12.15	5.7420	1.39545	1.3787
27	11.61	5.3353	1.39517	1.3802
28	10.22	4.8954	1.39353	1.3821
29	8.66	4.6353	1.39414	1.3837
30	7.69	4.3998	1.39422	1.3881
31	6.72	4.1579	1.39454	1.3923
32	6.01	4.0156	1.39471	1.3979
33	5.44	3.8859	1.39479	1.4042
34	4.96	3.7780	1.39516	1.4123
35,Q	4.69	3.7191	1.39568	1.4191

表3 四元体系(Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O)在313.15 K时平衡液相物理性质

Table 3 Physical properties of quaternary system Na+// S O 4 2 - ， C O 3 2 - ， N O 3 - -H2O at 313.15 K

No.^①	J(Na₂SO₄)	Viscosity $× 10 - 3$ /(Pa·s)^②	Refractive index	Density/(g·cm^?3)
1,E	4.81	2.2861	1.39229	1.4258
2	4.83	2.6218	1.39407	1.4290
3	5.04	3.0358	1.39539	1.4351
4	4.70	3.4904	1.39720	1.4415
5,Q	4.70	3.6338	1.39801	1.4414
6,F	17.70	1.9106	1.38343	1.3569
7	15.83	2.2850	1.38656	1.3754
8	11.91	2.5782	1.38871	1.3824
9,G	0.00	3.5211	1.39744	1.4351
10,Q	4.69	3.8538	1.39813	1.4456
11,H	60.97	4.2930	1.38712	1.3470
12	53.31	4.0326	1.38700	1.3406
13	46.74	3.9056	1.38719	1.3508
14	43.32	3.2815	1.38495	1.3369
15	37.72	3.0421	1.38340	1.3372
16	33.96	2.7706	1.38308	1.3345
17	30.79	2.7511	1.38407	1.3538
18	26.23	2.7164	1.38460	1.3596
19	23.39	2.6785	1.38520	1.3655
20	15.39	2.6085	1.38704	1.3771
21	13.11	2.7023	1.38807	1.3864
22,S	8.85	2.8018	1.38994	1.3953
23,L	14.69	7.6458	1.39776	1.3754
24	14.14	7.2336	1.39757	1.3790
25	13.38	6.4775	1.39598	1.3815
26	12.15	5.7420	1.39545	1.3787
27	11.61	5.3353	1.39517	1.3802
28	10.22	4.8954	1.39353	1.3821
29	8.66	4.6353	1.39414	1.3837
30	7.69	4.3998	1.39422	1.3881
31	6.72	4.1579	1.39454	1.3923
32	6.01	4.0156	1.39471	1.3979
33	5.44	3.8859	1.39479	1.4042
34	4.96	3.7780	1.39516	1.4123
35,Q	4.69	3.7191	1.39568	1.4191

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313.15 K四元体系Na⁺// $S O 4 2 -$ ， $C O 3 2 -$ ， $N O 3 -$ -H₂O固液相平衡研究

Solid-liquid equilibria of quaternary system Na ⁺// $S O 4 2 -$ , $C O 3 2 -$ , $N O 3 -$ -H₂O at 313.15 K

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