有机溶剂浸取湿法磷酸脱氟渣制备磷酸的研究

doi:10.19964/j.issn.1006-4990.2021-0654

Abstract

Abstract:

The fluoride residue is a solid waste produced in the chemical defluorination process of wet-process phosphoric acid.The effects of leaching time，temperature and liquid-solid ratio on the leaching ratio of P₂O₅ and F and the phosphor-fluorine ratio［m（P₂O₅）/m（F）］ were studied by using methanol，ethanol and acetone to leach the fluoride residue for recycling phosphoric acid.The suitable leaching conditions were obtained.After the leaching solution was evaporated and concentrated to recover the leaching agent，the concentrated solution all could meet the requirements of the m（P₂O₅）/m（F） of wet-process phosphoric acid for producing feed-grade calcium hydrogen phosphate.Considering the cost of the leaching solvents，the leaching ratio of P₂O₅and m（P₂O₅）/m（F），methanol was selected as the optimal leaching solvent，and the leaching conditions of methanol was optimized by response surface methodology.Under the optimized conditions，the leaching ratio of P₂O₅ was 97.13%，and the m（P₂O₅）/m（F） of the leaching solution was 51.62.After 5 cycles of solvent recovery and leaching，recovered methanol still had good leaching effect on the fluoride residue.

Key words: wet-process phosphoric acid, fluoride residue, leaching, response surface methodology

CLC Number:

X705

FU Ziqi, ZHANG Cheng, SHENG Yong, JI Lijun. Study on preparation of phosphoric acid by leaching fluoride residue from wet-process phosphoric acid with organic solvents[J]. Inorganic Chemicals Industry, 2022, 54(7): 129-134.

Figures/Tables 12

Fig.1

Table 1

Fig.2

Fig.3

Fig.4

Fig.5

Fig.6

Table 2

Results of leaching solution before andafter concentration"

浸取剂	$φ P$ /%	$φ F$ /%	浓缩	w（P₂O₅）/ %	w（F）/ %	m（P₂O₅）/ m（F）
甲醇	97.72	3.56	前	6.83	0.138	49.41
甲醇	97.72	3.56	后	50.69	0.161	314.84
乙醇	70.63	0.25	前	5.97	0.012	506.16
乙醇	70.63	0.25	后	50.30	0.027	1 862.96
丙酮	63.99	0.33	前	4.52	0.013	349.68
丙酮	63.99	0.33	后	40.79	0.046	886.74

Table 2

Table 3

Table 4

Results of response surface test"

序号	A	B	C	$φ P$ /%	m（P₂O₅）/ m（F）
1	-1	0	1	90.57	48.03
2	-1	1	0	86.93	51.22
3	-1	-1	0	84.32	50.13
4	-1	0	-1	81.79	60.04
5	0	0	0	89.91	49.11
6	0	0	0	89.33	48.23
7	0	-1	1	96.20	49.36
8	0	0	0	89.52	48.02
9	0	0	0	89.58	49.25
10	0	1	-1	82.03	62.53
11	0	1	1	97.76	49.45
12	0	-1	-1	80.80	60.36
13	0	0	0	89.65	49.03
14	1	-1	0	94.97	32.87
15	1	0	1	98.55	34.62
16	1	1	0	96.05	35.38
17	1	0	-1	84.31	40.05

Table 4

Table 5

Fig.7

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w（P₂O₅）	w（F^-）	w（SiF₆^2-）	w（SiO₂）	w（SO₄^2-）	w（Na₂O）
20.03	11.15	10.90	17.57	7.98	5.16
w（CaO）	w（MgO）	w（Al₂O₃）	w（Fe₂O₃）	w（H₂O）
1.63	1.78	1.36	0.45	20.57

变量	自由度	平方和	均方	F值	p值	显著性
A	1	544.83	544.83	525.31	<0.000 1	**
B	1	5.02	5.02	4.84	0.063 6
C	1	215.49	215.49	207.77	<0.000 1	**
AB	1	0.902 5	0.902 5	0.870 2	0.382 0
AC	1	10.82	10.82	10.44	0.014 4	*
BC	1	1.08	1.08	1.04	0.341 2
A²	1	267.72	267.72	258.13	<0.000 1	**
B²	1	13.13	13.13	12.66	0.009 2	**
C²	1	102.38	102.38	98.71	<0.000 1	**
模型	9	1 142.6	126.96	122.41	<0.000 1	**
残差	7	7.26	1.04
失拟项	3	6.00	2.00	6.36	0.053 0
纯误差	4	1.26	0.314 7
总离差	16	1 149.87

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Study on preparation of phosphoric acid by leaching fluoride residue from wet-process phosphoric acid with organic solvents

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