硝酸铁和磷酸共沉淀法制备电池级磷酸铁工艺研究

doi:10.19964/j.issn.1006-4990.2022-0548

Abstract

Abstract:

By using ferric nitrate and phosphoric acid as raw materials，the co-precipitation method was used to prepare the battery grade ferric phosphate.The effects of reaction temperature，reactant concentration，feeding proportion and reaction time on the yield and particle size of ferric phosphate were studied，and the optimal process conditions were obtained through orthogonal optimization：the solution concentration of Fe（NO₃）₃ was 1.1 mol/L，the feed ratio of phosphoric acid to ferric nitrate was 1.1，the reaction temperature was 90 ℃，and the reaction time was 8 h.The prepared iron phosphate was characterized by scanning electron microscopy（SEM），laser particle size analyzer，X-ray diffractometer（XRD） and TG-DTA.The analysis results showed that the obtained ferrophosphate dihydrate was monoclinic crystal with high purity and secondary particle size D₅₀ of 2.41 μm，which met the requirements of battery grade ferrophosphate.The performance of LiFePO₄/C prepared by the precursor system of iron phosphate was good.The initial discharge specific capacity of the battery composed of iron phosphate as cathode materials were 143.9，136.8 and 131.4 mA·h/g at 0.05C，0.1C and 1C，respectively.

Key words: ferric nitrate, ferric phosphate, co-precipitation method, lithium iron phosphate, orthogonal experiment

CLC Number:

TQ138.1

WANG Zihan, LI Jun, CHEN Ming, ZHOU Qingyu. Study on preparation of battery grade ferric phosphate by co-precipitation of ferric nitrate and phosphoric acid[J]. Inorganic Chemicals Industry, 2023, 55(7): 51-57.

Figures/Tables 15

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水平	因素
水平	A 反应温度/℃	B 反应物浓度/ （mol·L^-1）	C 投料比	D 反应时间/h
1	80	0.2	1.1	8
2	85	0.5	1.3	9
3	90	0.8	1.5	10
4	95	1.1	1.7	11

实验	实验因素					二次粒径/μm
实验	A	B	C	D	空白实验	二次粒径/μm
1	1	1	1	1	1	4.23
2	1	2	2	2	2	12.2
3	1	3	3	3	3	9.12
4	1	4	4	4	4	2.52
5	2	1	2	4	3	5.95
6	2	2	1	3	4	6.98
7	2	3	4	2	1	9.23
8	2	4	3	1	2	3.86
9	3	1	3	2	4	2.88
10	3	2	4	1	3	2.58
11	3	3	1	4	2	2.87
12	3	4	2	3	1	3.01
13	4	1	4	3	2	3.83
14	4	2	3	4	1	9.06
15	4	3	2	1	4	10.7
16	4	4	1	2	3	2.56
K₁	28.07	16.89	16.64	21.37	25.53
K₂	26.02	30.82	31.86	26.87	22.76
K₃	11.34	31.92	24.92	22.94	20.21
K₄	26.15	11.95	18.16	20.40	23.08
k₁	7.02	4.22	4.16	5.34	6.38
k₂	6.51	7.71	7.97	6.72	5.69
k₃	2.84	7.98	6.23	5.74	5.05
k₄	6.54	2.99	4.54	5.10	5.77
R	4.18	4.99	3.81	1.62	1.33

方差来源	偏差平方和	自由度	方差	F值	F_α	显著性
A	41.67	3	13.89	3.90	F_0.005（1，9）=13.61	*
B	75.03	3	25.01	7.02	F_0.05（1，9）=5.12	**
C	36.50	3	12.17	3.42	F_0.10（1，9）=3.36	*
D	6.09	3	2.03	0.57
误差	10.69	3	3.56
总和	169.98	15

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Study on preparation of battery grade ferric phosphate by co-precipitation of ferric nitrate and phosphoric acid

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