碱法回收湿法磷酸萃余渣中五氧化二磷的研究

doi:10.19964/j.issn.1006-4990.2020-0459

Abstract

Abstract:

Phosphoric acid is an important chemical raw material.At present,the method of producing phosphoric acid and phosphate mainly adopts wet-process,but wet-process phosphoric acid contains a large amount of impurities.In the process of purifying wet-process phosphoric acid by solvent extraction,a large amount of metal ion impurities precipitate in the form of insoluble phosphate precipitate,and the problem of recycling of insoluble P₂O₅ has received widespread attention.Alkaline hydrolysis process was used and single factor experiment was designed,the effect of liquid-solid ratio,n（Na₂O）/n（P₂O₅）,reac-tion temperature and reaction time on the wet-process phosphoric acid extraction residue（insoluble metal phosphate） deco-mposition were inspected,and a suitable range of reaction condition was selected.On this basis,the optimal reaction conditions were obtained through quadratic regression orthogonal experiments.The results showed that the optimum conditions were con-firmed as following：liquid-solid ratio was 30 mL/g, n（Na₂O）/n（P₂O₅）was 3.31,reaction temperature was 82 ℃ and reactiontime was 4.05 h.Under optimum conditions,the recovery rate of P₂O₅ could reach 92.48%.The reaction lye could be further used as raw material for the production of trisodium phosphate.In this study,a reasonable scheme for purifying phosphoric acid extraction residue was obtained,and related parameters were given,which provided guidance for the practical applica-tion of this program.It was of great significance for the utilization of extraction residue and environmental protection.

Key words: wet-process phosphoric acid, extraction residue, phosphorus recovery

CLC Number:

TQ126.35

Zhang Yaotao,Li Jun,Chen Ming,Zheng Zhuochao. Study on the recovery of phosphorus pentoxide from wet-process phosphoric acid extraction residue by alkaline process[J]. Inorganic Chemicals Industry, 2021, 53(7): 86-91.

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References 15

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规范变量	自然变量
规范变量	X₁ n（Na₂O）/n（P₂O₅）	X₂ 反应温度/℃	X₃ 反应时间/h
上星号臂+1.215	3.400	85.000	4.500
上水平1	3.382	84.115	4.411
零水平0	3.300	80.000	4.000
下水平-1	3.217	75.884	3.588
下星号臂-1.215	3.200	75.000	3.500

化合物	溶度积	化合物	溶度积
AlPO₄	6.4×10^-19	Al（OH）₃	1.9×10^-33
FePO₄·2H₂O	9.91×10^-16	Fe（OH）₃	2.79×10^-39
Mg₃（PO₄）₂	6.31×10^-26	Fe（OH）₂	4.87×10^-17
CaHPO₄	1×10^-7	Mg（OH）₂	5.61×10^-12
Ca₃（PO₄）₂	2×10^-29	Ca（OH）₂	5.5×10^-6

编号	X₁	X₂	X₃	X₁X₂	X₁X₃	X₂X₃	X₁²	X₂²	X₃²	实验结果/%	计算值/%
1	-1	-1	-1	244.198	11.546	272.275	10.356	5 758.533	12.874	88.11	88.00
2	-1	-1	1	244.198	14.198	334.805	10.356	5 758.533	19.466	90.01	90.06
3	-1	1	-1	270.682	11.546	301.805	10.356	7 075.333	12.874	90.52	90.61
4	-1	1	1	270.682	14.198	371.115	10.356	7 075.333	19.466	91.14	90.92
5	1	-1	-1	256.643	12.135	272.275	11.438	5 758.533	12.874	89.36	89.63
6	1	-1	1	256.643	14.921	334.805	11.438	5 758.533	19.466	90.71	90.66
7	1	1	-1	284.477	12.135	301.805	11.438	7 075.333	12.874	91.12	91.13
8	1	1	1	284.477	14.921	371.115	11.438	7 075.333	19.466	90.26	90.41
9	-1.215	0	0	256.000	12.800	320.000	10.240	6 400.000	16.000	90.22	90.48
10	1.215	0	0	272.000	13.600	320.000	11.560	6 400.000	16.000	91.46	91.17
11	0	-1.215	0	247.500	13.200	300.000	10.890	5 625.000	16.000	90.04	89.97
12	0	1.215	0	280.500	13.200	340.000	10.890	7 225.000	16.000	91.37	91.40
13	0	0	-1.215	264.000	11.550	280.000	10.890	6 400.000	12.250	90.68	90.53
14	0	0	1.215	264.000	14.850	360.000	10.890	6 400.000	20.250	91.23	91.34
15	0	0	0	264.000	13.200	320.000	10.890	6 400.000	16.000	91.38	91.43

项目	回归系数	标准误差	t值	P值	下限 95%	上限 95%
截距	-12.197 0	2.307 4	-5.286 1	0.003 2	-18.128 4	-6.265 7
x₁	5.005 5	1.290 1	3.879 9	0.011 6	1.689 2	8.321 8
x₂	0.086 9	0.015 9	5.478 2	0.002 8	0.046 1	0.127 6
x₃	0.623 6	0.123 3	5.058 7	0.003 9	0.306 7	0.940 5
x₁x₂	-0.008 3	0.002 9	-2.861 6	0.035 3	-0.015 7	-0.000 8
x₁x₃	-0.075 8	0.029 1	-2.606 2	0.047 9	-0.150 5	-0.001 0
x₂x₃	-0.002 6	0.000 6	-4.478 4	0.006 5	-0.004 1	-0.001 1
x₁²	-0.607 2	0.191 6	-3.169 8	0.024 8	-1.099 6	-0.114 8
x₂²	-0.000 3	0.000 1	-3.841 1	0.012 1	-0.000 5	-0.000 1
x₃²	-0.019 9	0.007 8	-2.563 0	0.050 5	-0.039 9	0.000 1

项目	自由度	离差平方和	均方	F值	显著性
回归分析	9	0.001 1	0.000 1	16.211 5	0.003 4
残差	5	0.000 0	0.000 0
总计	14	0.001 1

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Study on the recovery of phosphorus pentoxide from wet-process phosphoric acid extraction residue by alkaline process

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