煤化工高盐废水复分解法制备硫酸钾实验研究

Abstract

Abstract:

The process of methanol and light hydrocarbon production in coal chemical plant produces a large amount of waste-water and the high salt wastewater can be obtained by reverse osmosis,nanofiltration membrane concentration and reduction treatment.Potassium sulfate was prepared from high salt wastewater by two-step conversion（double decomposition） after being concentrated to saturate sodium sulfate.In the first step,aphthitalite was prepared by adding potassium chloride to concent-rated wastewater.Sodium chloride was obtained by evaporating part of water from the mother liquor and the mother liquor was concentrated by adding sodium sulfate,also the mother liquor was recycled.In the second step,potassium sulfate was prepared from aphthitalite by adding potassium chloride.The effects of concentration ratio,potassium chloride dosage and amount of evaporation water on the purity and yield of aphthitalite were investigated and the influence of the dosage of potassium chloride and water on the purity and yield of potassium sulphate were determined.The optimum conditions for the preparation of potassium sulfate from high-salt wastewater were concluded as follows：In the process of preparing aphthitalite,the concentration ratio of high salt wastewater was 4.35 times,the addition of potassium chloride was 84.25 g,and the amount of water evaporation was 100 g based on 500 g concentrated wastewater.In the process of preparing potassium sulfate,the dosage of aphthitalite and water were 153.08 g and 322.06 g based on 100 g potassium chloride,respectively.The mass frac-tion of K₂O and Cl ^- in potassium sulphate were 52.96% and 1.09%,respectively,which was in line with the requirements of premium grade in the standard of agricultural potassium sulfate（GB/T 20406—2017）.After the mother liquor was recycled for 3 times in the preparation process of aphthitalite,TOC has little effect on the purity and has an effect on the whiteness of aphthitalite.The mother liquor K was produced by the preparation of potassium sulfate by aphthitalite and potassium chloride,and the mother liquor K″ was obtained by adding sodium sulfate to the mother liquor K.The composition of mother liquor K″ was basically consistent with that of mother liquor F produced by concentrated waste water to prepare aphthitalite,which verified the feasibility of the circulating process route.

Key words: high-salt wastewater in coal chemical industry, potassium sulfate, aphthitalite, sodium sulfate

CLC Number:

X703

Chen Xia,Bai Fengxia,Shi Yapeng,Dong Sicheng,Liao Enxin,Li Ying,Miao Shulan. Experimental research of preparation of potassium sulfate from high-salt wastewater in coal chemical industry by double decomposition method[J]. Inorganic Chemicals Industry, 2019, 51(6): 57-61.

Figures/Tables 12

References 19

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项目	w（Na⁺）/ %	w（SO₄^2-）/ %	w（K⁺）/ %	w（Cl^-）/ %	w（NO₃^-）/ %	w（H₂O）/ %	w（TOC）/ （mg·kg^-1）	COD/ （mg·kg^-1）	pH
高盐废水	1.64	2.56	0.08	0.63	0.14	—	346.00	700	10
4.35倍率浓缩废水	7.36	11.59	0.31	2.58	0.86	77.30	1 341.85	—	—
硝酸钠折算成氯化钠后浓缩废水	7.51	11.59	0.31	3.30	—	77.29	—	—	—

项目	w（Na⁺）/ %	w（SO₄^2-）/ %	w（K⁺）/ %	w（Cl^-）/ %	w（NO₃^-）/ %	w（H₂O）/ %
母液F	8.86	2.84	4.53	14.26	1.74	67.77
硝酸钠折算成氯化钠母液F	9.30	3.91	6.98	17.82	0.00	61.99

蒸发次数	模拟值				实际值				TOC/（mg·kg^-1）		白度/%
蒸发次数	m（NaCl）/ g	w（NaCl）/ %	m（Gla）/ g	w（Gla）/ %	m（NaCl）/ g	w（NaCl）/ %	m（Gla）/ g	w（Gla）/ %	NaCl	Gla	NaCl	Gla
1	63.71	96.75	12.40	97.55	63.45	96.41	12.14	97.30	527.32	3 445	68.9	67.5
2	45.76	96.10	9.87	97.11	45.23	96.64	9.85	96.85	650.45	4 620	63.4	64.1
3	36.54	95.65	7.81	96.75	36.55	95.48	7.54	96.21	691.23	5 100	59.3	60.3

m（加水）/ g	硫酸钾		m（加水）/ g	硫酸钾
m（加水）/ g	w（K₂O）/%	w（Cl^-）/%	m（加水）/ g	w（K₂O）/%	w（Cl^-）/%
284.90	51.55	1.96	334.45	52.98	0.95
297.29	51.97	1.66	346.84	53.04	0.85
309.68	52.51	1.53	359.22	53.09	0.82
322.06	52.96	1.09

项目	m（母液K″）/g	w（Gla）/%	Gla产率/%
模拟值	364.21	97.65	76.81
实际值	368.88	97.20	76.01

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Experimental research of preparation of potassium sulfate from high-salt wastewater in coal chemical industry by double decomposition method

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母液	w（Na⁺）/%	w（K⁺）/%	w（Cl^-）/%	w（SO₄^2-）/%	w（H₂O）/%
F	9.30	6.98	17.82	3.91	61.99
K″	9.26	7.02	17.75	3.82	62.06