臭氧氧化法去除氟硅酸中氯的工艺研究

doi:10.19964/j.issn.1006-4990.2024-0618

Abstract

Abstract:

The by-product fluosilicic acid produced by the wet-process phosphoric acid production contains various impurities such as chlorine.The presence of these impurities not only affects the purity of fluosilicic acid and the quality of subsequent products，but also causes corrosion to the production equipment and pollutes the environment.In this paper，the single-factor method was used to conduct an experimental study on the removal of chlorine from fluosilicic acid solution by ozone oxidation.The effects of ozone flow rate，fluosilicic acid content，reaction time，and reaction temperature on the removal of chloride ions from fluosilicic acid solution by ozone oxidation were analyzed.In order to more accurately determine the parameters for ozone chloride removal，based on the results of the single-factor experiments，three factors that had a significant impact on the chloride removal rate were selected，including reaction time，reaction temperature，and fluosilicic acid content.The Box-Behnken（BBD） method in Design-Expert 13 was used to design a 3-factor 3-level experimental scheme for response surface experiments.The results showed that the optimal conditions for ozone to remove chlorine from fluosilicic acid were：ozone flow rate of 48 g/h，reaction temperature of 45 ℃，reaction time of 4 h，and fluosilicic acid content of 36.00%.Under the best experimental conditions，the chlorine removal rate was 96.85%，and the fluoride loss rate was 3.29%.This study could provide new ideas for removing chlorine from fluosilicic acid.

Key words: ozone oxidation, fluorosilicic acid, dechlorination, fluorine

CLC Number:

TQ124.4

CHEN Yi, LI Tianxiang, LIU Songlin, SUI Yanfeng, LI Baiyu, ZHU Jing. Study on removal process of chlorine from fluorosilicic acid by ozonidation[J]. Inorganic Chemicals Industry, 2025, 57(12): 56-62.

Figures/Tables 11

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Table 1

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Table 5

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References 19

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水平	因素
水平	A/h	B/℃	C/%
-1	3	25	16.00
0	4	35	26.00
1	5	45	36.00

编号	A/h	B/℃	C/%	氯去除率/%	氟损失率/%
1	4	45	36.00	98.79	10.80
2	4	35	26.00	76.73	9.63
3	5	25	26.00	63.71	12.01
4	4	35	26.00	76.73	9.63
5	3	25	26.00	47.50	7.30
6	5	45	26.00	97.55	20.35
7	3	35	16.00	58.43	10.93
8	5	35	36.00	83.09	14.45
9	4	35	26.00	73.47	11.01
10	3	45	26.00	92.20	18.76
11	4	45	16.00	84.33	19.02
12	4	35	26.00	74.05	10.98
13	4	25	36.00	54.56	7.84
14	4	25	16.00	49.32	7.56
15	5	35	16.00	70.77	17.78
16	3	35	36.00	62.93	9.83
17	4	35	26.00	75.34	11.21

方差来源	平方和	自由度	均方	F	P	显著性
相关系数（R²） 0.993 5
模型	3 832.07	9	425.79	118.96	<0.000 1	极显著
A	365.31	1	365.31	102.06	<0.000 1	极显著
B	3 111.82	1	3 111.82	869.40	<0.000 1	极显著
C	166.71	1	166.71	46.58	0.000 2	极显著
AB	29.48	1	29.48	8.24	0.024 0	显著
AC	15.29	1	15.29	4.27	0.077 6
BC	21.25	1	21.25	5.94	0.045 0	显著
A²	9.28	1	9.28	2.59	0.151 4
B²	8.98	1	8.98	2.51	0.157 2
C²	104.19	1	104.19	29.11	0.001 0	极显著
残差	25.05	7	3.58
失拟项	16.06	3	5.35	2.38	0.210 5	不显著
纯误差	9.00	4	2.25
总离差	3 857.13	16

方差来源	平方和	自由度	均方	F	P	显著性
相关系数（R²） 0.961 1
模型	271.86	9	30.21	19.21	0.000 4	极显著
A	39.47	1	39.47	25.10	0.001 5	极显著
B	146.38	1	146.38	93.09	<0.000 1	极显著
C	19.13	1	19.13	12.16	0.010 2	显著
AB	2.43	1	2.43	1.55	0.253 5
AC	1.24	1	1.24	0.79	0.403 4
BC	18.06	1	18.06	11.49	0.011 6	显著
A²	38.60	1	38.60	24.55	0.001 6	极显著
B²	4.96	1	4.96	3.15	0.119 0
C²	0.31	1	0.31	0.20	0.669 4
残差	11.01	7	1.57
失拟项	8.50	3	2.83	4.52	0.089 6	不显著
纯误差	2.51	4	0.63
总离差	282.87	16

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Inorganic Acid-Base-Salt Committee of CIESC

Study on removal process of chlorine from fluorosilicic acid by ozonidation

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