CIESC Journal ›› 2024, Vol. 75 ›› Issue (12): 4780-4792.DOI: 10.11949/0438-1157.20240617
• Energy and environmental engineering • Previous Articles Next Articles
Zhongliang XIAO1(), Yubo XIA1, Liubin SONG1(
), Youtao XIANG1, Tingting ZHAO1, Jing LUO1, Yuanjia LIU1, Penghui DENG1, Qunxuan YAN2(
)
Received:
2024-06-04
Revised:
2024-08-16
Online:
2025-01-03
Published:
2024-12-25
Contact:
Liubin SONG, Qunxuan YAN
肖忠良1(), 夏宇博1, 宋刘斌1(
), 向优涛1, 赵亭亭1, 罗静1, 刘远佳1, 邓鹏辉1, 颜群轩2(
)
通讯作者:
宋刘斌,颜群轩
作者简介:
肖忠良(1964—),男,博士,教授,xiaozhongliang@163.com
基金资助:
CLC Number:
Zhongliang XIAO, Yubo XIA, Liubin SONG, Youtao XIANG, Tingting ZHAO, Jing LUO, Yuanjia LIU, Penghui DENG, Qunxuan YAN. Synergistic leaching process of waste LiFePO4 with phosphoric acid-tartaric acid system[J]. CIESC Journal, 2024, 75(12): 4780-4792.
肖忠良, 夏宇博, 宋刘斌, 向优涛, 赵亭亭, 罗静, 刘远佳, 邓鹏辉, 颜群轩. 磷酸-酒石酸体系协同浸出废旧磷酸铁锂工艺[J]. 化工学报, 2024, 75(12): 4780-4792.
药品名称 | 分子式 | 规格 | 厂家 |
---|---|---|---|
磷酸 | H3PO4 | AR | 国药集团有限公司 |
酒石酸 | C4H6O6 | AR | 国药集团有限公司 |
碳酸锂 | Li2CO3 | 电池级 | 上海麦克林生化科技股份有限公司 |
氧化铁 | Fe2O3 | AR | 上海麦克林生化科技股份有限公司 |
Table 1 Experimental reagents
药品名称 | 分子式 | 规格 | 厂家 |
---|---|---|---|
磷酸 | H3PO4 | AR | 国药集团有限公司 |
酒石酸 | C4H6O6 | AR | 国药集团有限公司 |
碳酸锂 | Li2CO3 | 电池级 | 上海麦克林生化科技股份有限公司 |
氧化铁 | Fe2O3 | AR | 上海麦克林生化科技股份有限公司 |
仪器名称 | 型号 | 生产厂家 |
---|---|---|
恒速电动搅拌器 | JJ-1B | 西城新瑞仪器厂 |
集热式恒温加热磁力 搅拌器 | DF-101S | 上海力辰邦西仪器科技公司 |
管式炉 | HLG-X-16 | 洛阳恒立窑炉有限公司 |
X射线衍射分析仪 | D8 Advance | 德国Bruker公司 |
电感耦合等离子体发生光谱仪 | ARCOS | 德国SPECTRO公司 |
Table 2 Experimental equipments
仪器名称 | 型号 | 生产厂家 |
---|---|---|
恒速电动搅拌器 | JJ-1B | 西城新瑞仪器厂 |
集热式恒温加热磁力 搅拌器 | DF-101S | 上海力辰邦西仪器科技公司 |
管式炉 | HLG-X-16 | 洛阳恒立窑炉有限公司 |
X射线衍射分析仪 | D8 Advance | 德国Bruker公司 |
电感耦合等离子体发生光谱仪 | ARCOS | 德国SPECTRO公司 |
Element | Composition/% |
---|---|
Li | 3.62 |
Fe | 28.06 |
Al | 0.72 |
P | 16.28 |
Table 3 Chemical element composition of iron-lithium powder
Element | Composition/% |
---|---|
Li | 3.62 |
Fe | 28.06 |
Al | 0.72 |
P | 16.28 |
实验 序号 | 搅拌速度/(r/min) | 磷酸浓度/(mol/L) | 酒石酸浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 200 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 89.60 | 88.78 |
2 | 300 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 92.58 | 95.33 |
3 | 400 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 92.59 | 96.34 |
4 | 500 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 94.83 | 96.67 |
5 | 600 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 93.14 | 97.34 |
6 | 700 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 91.27 | 93.00 |
Table 4 Effect of stirring speed on leaching rate of Li and Fe
实验 序号 | 搅拌速度/(r/min) | 磷酸浓度/(mol/L) | 酒石酸浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 200 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 89.60 | 88.78 |
2 | 300 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 92.58 | 95.33 |
3 | 400 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 92.59 | 96.34 |
4 | 500 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 94.83 | 96.67 |
5 | 600 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 93.14 | 97.34 |
6 | 700 | 2.90 | 1.33 | 5∶1 | 70 | 5 | 91.27 | 93.00 |
实验 序号 | 磷酸 浓度/(mol/L) | 搅拌 速度/(r/min) | 酒石酸 浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 1.74 | 500 | 1.33 | 5∶1 | 70 | 5 | 88.93 | 85.38 |
2 | 2.32 | 500 | 1.33 | 5∶1 | 70 | 5 | 94.55 | 94.32 |
3 | 2.90 | 500 | 1.33 | 5∶1 | 70 | 5 | 96.34 | 96.48 |
4 | 3.48 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.97 | 94.44 |
5 | 4.06 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.12 | 94.35 |
6 | 4.64 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.61 | 74.15 |
Table 5 Effect of H3PO4 concentration on leaching rate of Li and Fe
实验 序号 | 磷酸 浓度/(mol/L) | 搅拌 速度/(r/min) | 酒石酸 浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 1.74 | 500 | 1.33 | 5∶1 | 70 | 5 | 88.93 | 85.38 |
2 | 2.32 | 500 | 1.33 | 5∶1 | 70 | 5 | 94.55 | 94.32 |
3 | 2.90 | 500 | 1.33 | 5∶1 | 70 | 5 | 96.34 | 96.48 |
4 | 3.48 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.97 | 94.44 |
5 | 4.06 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.12 | 94.35 |
6 | 4.64 | 500 | 1.33 | 5∶1 | 70 | 5 | 95.61 | 74.15 |
实验 序号 | 酒石酸 浓度/(mol/L) | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 0.53 | 500 | 2.90 | 5∶1 | 70 | 5 | 93.21 | 24.94 |
2 | 0.80 | 500 | 2.90 | 5∶1 | 70 | 5 | 93.45 | 52.04 |
3 | 1.06 | 500 | 2.90 | 5∶1 | 70 | 5 | 94.03 | 81.83 |
4 | 1.33 | 500 | 2.90 | 5∶1 | 70 | 5 | 95.11 | 97.08 |
5 | 1.60 | 500 | 2.90 | 5∶1 | 70 | 5 | 95.11 | 94.44 |
6 | 1.86 | 500 | 2.90 | 5∶1 | 70 | 5 | 94.53 | 93.79 |
Table 6 Effect of tartaric acid concentration on leaching rate of Li and Fe
实验 序号 | 酒石酸 浓度/(mol/L) | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 液固比/(ml/g) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 0.53 | 500 | 2.90 | 5∶1 | 70 | 5 | 93.21 | 24.94 |
2 | 0.80 | 500 | 2.90 | 5∶1 | 70 | 5 | 93.45 | 52.04 |
3 | 1.06 | 500 | 2.90 | 5∶1 | 70 | 5 | 94.03 | 81.83 |
4 | 1.33 | 500 | 2.90 | 5∶1 | 70 | 5 | 95.11 | 97.08 |
5 | 1.60 | 500 | 2.90 | 5∶1 | 70 | 5 | 95.11 | 94.44 |
6 | 1.86 | 500 | 2.90 | 5∶1 | 70 | 5 | 94.53 | 93.79 |
实验 序号 | 温度/℃ | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 液固比/(ml/g) | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 40 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 88.91 | 84.26 |
2 | 50 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 93.71 | 90.03 |
3 | 60 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 94.45 | 97.99 |
4 | 70 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 95.76 | 99.20 |
5 | 80 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 95.15 | 94.49 |
6 | 90 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 94.43 | 92.78 |
Table 7 Effect of reaction temperature on leaching rate of Li and Fe
实验 序号 | 温度/℃ | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 液固比/(ml/g) | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 40 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 88.91 | 84.26 |
2 | 50 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 93.71 | 90.03 |
3 | 60 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 94.45 | 97.99 |
4 | 70 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 95.76 | 99.20 |
5 | 80 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 95.15 | 94.49 |
6 | 90 | 500 | 2.90 | 1.33 | 5∶1 | 5 | 94.43 | 92.78 |
实验 序号 | 液固比/(ml/g) | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 3∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 83.92 | 77.84 |
2 | 4∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 92.01 | 90.71 |
3 | 5∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 94.00 | 97.39 |
4 | 6∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 97.52 | 98.87 |
5 | 8∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 96.53 | 97.71 |
6 | 10∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 92.23 | 86.51 |
Table 8 Effect of liquid-solid ratio on leaching rate of Li and Fe
实验 序号 | 液固比/(ml/g) | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 温度/℃ | 时间/h | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 3∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 83.92 | 77.84 |
2 | 4∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 92.01 | 90.71 |
3 | 5∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 94.00 | 97.39 |
4 | 6∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 97.52 | 98.87 |
5 | 8∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 96.53 | 97.71 |
6 | 10∶1 | 500 | 2.90 | 1.33 | 70 | 5 | 92.23 | 86.51 |
实验 序号 | 时间/h | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 温度/℃ | 液固比/(ml/g) | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 2 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 86.65 | 86.69 |
2 | 3 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 91.03 | 91.39 |
3 | 4 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 94.92 | 96.83 |
4 | 5 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 97.88 | 98.47 |
5 | 6 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 98.08 | 97.43 |
6 | 7 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 97.69 | 97.29 |
Table 9 Effect of reaction time on leaching rate of Li and Fe
实验 序号 | 时间/h | 搅拌 速度/(r/min) | 磷酸 浓度/(mol/L) | 酒石酸 浓度/(mol/L) | 温度/℃ | 液固比/(ml/g) | Li 浸出率/% | Fe 浸出率/% |
---|---|---|---|---|---|---|---|---|
1 | 2 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 86.65 | 86.69 |
2 | 3 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 91.03 | 91.39 |
3 | 4 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 94.92 | 96.83 |
4 | 5 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 97.88 | 98.47 |
5 | 6 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 98.08 | 97.43 |
6 | 7 | 500 | 2.90 | 1.33 | 70 | 6∶1 | 97.69 | 97.29 |
Factors | Code value | ||
---|---|---|---|
-1 | 0 | 1 | |
A: H3PO4/(mol/L) | 2 | 3 | 4 |
B: Tartaric acid/(mol/L) | 0.8 | 1.3 | 1.8 |
C: L/S/(ml/g) | 4∶1 | 7∶1 | 10∶1 |
D: Temperature/℃ | 40 | 65 | 90 |
Table 10 Box-Behnken experimental factor level
Factors | Code value | ||
---|---|---|---|
-1 | 0 | 1 | |
A: H3PO4/(mol/L) | 2 | 3 | 4 |
B: Tartaric acid/(mol/L) | 0.8 | 1.3 | 1.8 |
C: L/S/(ml/g) | 4∶1 | 7∶1 | 10∶1 |
D: Temperature/℃ | 40 | 65 | 90 |
Run | H3PO4 concentration/(mol/L) | Tartaric acid concentration /(mol/L) | Liquid/Solid ratios/(ml/g) | Leaching temperature /℃ | Leaching rate of Li/% | Leaching rate of Fe/% |
---|---|---|---|---|---|---|
1 | 0 | 1 | 0 | 1 | 83.38 | 85.78 |
2 | 0 | 0 | 0 | 0 | 97.08 | 98.03 |
3 | -1 | -1 | 0 | 0 | 75.33 | 63.17 |
4 | -1 | 0 | 1 | 0 | 63.06 | 62.65 |
5 | -1 | 0 | 0 | 1 | 72.45 | 70.76 |
6 | 0 | 0 | 0 | 0 | 97.41 | 97.48 |
7 | 1 | 0 | 0 | 1 | 80.24 | 80.87 |
8 | 1 | -1 | 0 | 0 | 76.08 | 71.25 |
9 | 0 | 1 | 0 | -1 | 84.37 | 75.74 |
10 | 1 | 0 | 1 | 0 | 64.95 | 70.24 |
11 | 0 | -1 | 0 | -1 | 80.78 | 65.75 |
12 | 0 | 0 | 0 | 0 | 97.63 | 98.21 |
13 | -1 | 0 | -1 | 0 | 68.94 | 74.24 |
14 | 0 | 1 | -1 | 0 | 77.45 | 85.15 |
15 | 0 | -1 | 0 | 1 | 84.98 | 69.54 |
16 | 0 | 0 | 1 | 1 | 75.45 | 68.25 |
17 | 1 | 0 | -1 | 0 | 75.3 | 81.53 |
18 | -1 | 1 | 0 | 0 | 72.45 | 77.47 |
19 | 0 | 0 | 1 | -1 | 67.26 | 69.36 |
20 | 1 | 1 | 0 | 0 | 78.9 | 83.18 |
21 | 0 | 0 | -1 | 1 | 78.93 | 87.32 |
22 | 0 | 1 | 1 | 0 | 72.78 | 71.3 |
23 | -1 | 0 | 0 | -1 | 72.75 | 67.56 |
24 | 0 | 0 | -1 | -1 | 82.38 | 73.69 |
25 | 1 | 0 | 0 | -1 | 72.88 | 71.24 |
26 | 0 | -1 | 1 | 0 | 70.28 | 64.27 |
27 | 0 | -1 | -1 | 0 | 81.05 | 72.53 |
Table 11 BBD experimental design for Li and Fe leaching rate
Run | H3PO4 concentration/(mol/L) | Tartaric acid concentration /(mol/L) | Liquid/Solid ratios/(ml/g) | Leaching temperature /℃ | Leaching rate of Li/% | Leaching rate of Fe/% |
---|---|---|---|---|---|---|
1 | 0 | 1 | 0 | 1 | 83.38 | 85.78 |
2 | 0 | 0 | 0 | 0 | 97.08 | 98.03 |
3 | -1 | -1 | 0 | 0 | 75.33 | 63.17 |
4 | -1 | 0 | 1 | 0 | 63.06 | 62.65 |
5 | -1 | 0 | 0 | 1 | 72.45 | 70.76 |
6 | 0 | 0 | 0 | 0 | 97.41 | 97.48 |
7 | 1 | 0 | 0 | 1 | 80.24 | 80.87 |
8 | 1 | -1 | 0 | 0 | 76.08 | 71.25 |
9 | 0 | 1 | 0 | -1 | 84.37 | 75.74 |
10 | 1 | 0 | 1 | 0 | 64.95 | 70.24 |
11 | 0 | -1 | 0 | -1 | 80.78 | 65.75 |
12 | 0 | 0 | 0 | 0 | 97.63 | 98.21 |
13 | -1 | 0 | -1 | 0 | 68.94 | 74.24 |
14 | 0 | 1 | -1 | 0 | 77.45 | 85.15 |
15 | 0 | -1 | 0 | 1 | 84.98 | 69.54 |
16 | 0 | 0 | 1 | 1 | 75.45 | 68.25 |
17 | 1 | 0 | -1 | 0 | 75.3 | 81.53 |
18 | -1 | 1 | 0 | 0 | 72.45 | 77.47 |
19 | 0 | 0 | 1 | -1 | 67.26 | 69.36 |
20 | 1 | 1 | 0 | 0 | 78.9 | 83.18 |
21 | 0 | 0 | -1 | 1 | 78.93 | 87.32 |
22 | 0 | 1 | 1 | 0 | 72.78 | 71.3 |
23 | -1 | 0 | 0 | -1 | 72.75 | 67.56 |
24 | 0 | 0 | -1 | -1 | 82.38 | 73.69 |
25 | 1 | 0 | 0 | -1 | 72.88 | 71.24 |
26 | 0 | -1 | 1 | 0 | 70.28 | 64.27 |
27 | 0 | -1 | -1 | 0 | 81.05 | 72.53 |
Source | Sum of Squares | Degree of freedom(df) | Mean Square | F | P-value Prob>F | |
---|---|---|---|---|---|---|
Model | 2097.05 | 14 | 149.79 | 156.62 | <0.0001 | Significant |
A-H3PO4 | 45.51 | 1 | 45.51 | 118.05 | <0.0001 | |
B-Tartaric acid | 0.0574 | 1 | 0.0574 | 340.48 | 0.7773 | |
C-L/S ratios | 210.59 | 1 | 210.59 | 306.26 | <0.0001 | |
D-Temperature | 18.78 | 1 | 18.78 | 100.51 | 0.0002 | |
AB | 8.12 | 1 | 8.12 | 1.10 | 0.0049 | |
AC | 5.00 | 1 | 5.00 | 0.0177 | 0.0194 | |
AD | 14.67 | 1 | 14.67 | 8.12 | 0.0006 | |
BC | 9.30 | 1 | 9.30 | 6.14 | 0.0031 | |
BD | 6.73 | 1 | 6.73 | 7.67 | 0.0086 | |
CD | 33.87 | 1 | 33.87 | 42.68 | <0.0001 | |
A2 | 1206.07 | 1 | 1206.07 | 723.00 | <0.0001 | |
B2 | 259.24 | 1 | 259.50 | 579.92 | <0.0001 | |
C2 | 1117.53 | 1 | 1117.53 | 638.00 | <0.0001 | |
D2 | 278.24 | 1 | 278.24 | 570.96 | <0.0001 | |
Residual | 8.23 | 12 | 0.6860 | |||
Lack of Fit | 8.08 | 10 | 0.8079 | 10.54 | 0.0897 | Not significant |
Pure error | 0.1533 | 2 | 0.0766 | |||
Cor total | 2105.28 | 26 | ||||
Adeq precision | 55.9368 | |||||
R2 | 0.9961 | |||||
Adjusted R2 | 0.9915 | |||||
Predicted R2 | 0.9777 | |||||
C.V./% | 1.06 |
Table 12 Variance analysis of BBD model for Li leaching rate
Source | Sum of Squares | Degree of freedom(df) | Mean Square | F | P-value Prob>F | |
---|---|---|---|---|---|---|
Model | 2097.05 | 14 | 149.79 | 156.62 | <0.0001 | Significant |
A-H3PO4 | 45.51 | 1 | 45.51 | 118.05 | <0.0001 | |
B-Tartaric acid | 0.0574 | 1 | 0.0574 | 340.48 | 0.7773 | |
C-L/S ratios | 210.59 | 1 | 210.59 | 306.26 | <0.0001 | |
D-Temperature | 18.78 | 1 | 18.78 | 100.51 | 0.0002 | |
AB | 8.12 | 1 | 8.12 | 1.10 | 0.0049 | |
AC | 5.00 | 1 | 5.00 | 0.0177 | 0.0194 | |
AD | 14.67 | 1 | 14.67 | 8.12 | 0.0006 | |
BC | 9.30 | 1 | 9.30 | 6.14 | 0.0031 | |
BD | 6.73 | 1 | 6.73 | 7.67 | 0.0086 | |
CD | 33.87 | 1 | 33.87 | 42.68 | <0.0001 | |
A2 | 1206.07 | 1 | 1206.07 | 723.00 | <0.0001 | |
B2 | 259.24 | 1 | 259.50 | 579.92 | <0.0001 | |
C2 | 1117.53 | 1 | 1117.53 | 638.00 | <0.0001 | |
D2 | 278.24 | 1 | 278.24 | 570.96 | <0.0001 | |
Residual | 8.23 | 12 | 0.6860 | |||
Lack of Fit | 8.08 | 10 | 0.8079 | 10.54 | 0.0897 | Not significant |
Pure error | 0.1533 | 2 | 0.0766 | |||
Cor total | 2105.28 | 26 | ||||
Adeq precision | 55.9368 | |||||
R2 | 0.9961 | |||||
Adjusted R2 | 0.9915 | |||||
Predicted R2 | 0.9777 | |||||
C.V./% | 1.06 |
Source | Sum of Squares | Degee of freedom(df) | Mean Square | F | P-value Prob>F | |
---|---|---|---|---|---|---|
Model | 2790.57 | 14 | 199.33 | 156.62 | <0.0001 | Significant |
A-H3PO4 | 150.24 | 1 | 150.24 | 118.05 | <0.0001 | |
B-Tartaric acid | 433.32 | 1 | 433.32 | 340.48 | <0.0001 | |
C-L/S ratios | 389.77 | 1 | 389.77 | 306.26 | <0.0001 | |
D-Temperature | 127.92 | 1 | 127.92 | 100.51 | <0.0001 | |
AB | 1.40 | 1 | 1.40 | 1.10 | 0.3142 | |
AC | 0.0225 | 1 | 0.0225 | 0.0177 | 0.8964 | |
AD | 10.34 | 1 | 10.34 | 8.12 | 0.0146 | |
BC | 7.81 | 1 | 7.81 | 6.14 | 0.0291 | |
BD | 9.77 | 1 | 9.77 | 7.67 | 0.0170 | |
CD | 54.32 | 1 | 54.32 | 42.68 | <0.0001 | |
A2 | 920.15 | 1 | 920.15 | 723.00 | <0.0001 | |
B2 | 738.06 | 1 | 738.06 | 579.92 | <0.0001 | |
C2 | 811.97 | 1 | 811.97 | 638.00 | <0.0001 | |
D2 | 726.65 | 1 | 726.65 | 570.96 | <0.0001 | |
Residual | 15.27 | 12 | 1.27 | |||
Lack of Fit | 14.98 | 10 | 1.50 | 10.36 | 0.0912 | Not significant |
Pure error | 0.2893 | 2 | 0.1446 | |||
Cor total | 2805.84 | 26 | ||||
Adeq precision | 41.6701 | |||||
R2 | 0.9946 | |||||
Adjusted R2 | 0.9882 | |||||
Predicted R2 | 0.9690 | |||||
C.V./% | 1.48 |
Table 13 Variance analysis of BBD model for Fe leaching rate
Source | Sum of Squares | Degee of freedom(df) | Mean Square | F | P-value Prob>F | |
---|---|---|---|---|---|---|
Model | 2790.57 | 14 | 199.33 | 156.62 | <0.0001 | Significant |
A-H3PO4 | 150.24 | 1 | 150.24 | 118.05 | <0.0001 | |
B-Tartaric acid | 433.32 | 1 | 433.32 | 340.48 | <0.0001 | |
C-L/S ratios | 389.77 | 1 | 389.77 | 306.26 | <0.0001 | |
D-Temperature | 127.92 | 1 | 127.92 | 100.51 | <0.0001 | |
AB | 1.40 | 1 | 1.40 | 1.10 | 0.3142 | |
AC | 0.0225 | 1 | 0.0225 | 0.0177 | 0.8964 | |
AD | 10.34 | 1 | 10.34 | 8.12 | 0.0146 | |
BC | 7.81 | 1 | 7.81 | 6.14 | 0.0291 | |
BD | 9.77 | 1 | 9.77 | 7.67 | 0.0170 | |
CD | 54.32 | 1 | 54.32 | 42.68 | <0.0001 | |
A2 | 920.15 | 1 | 920.15 | 723.00 | <0.0001 | |
B2 | 738.06 | 1 | 738.06 | 579.92 | <0.0001 | |
C2 | 811.97 | 1 | 811.97 | 638.00 | <0.0001 | |
D2 | 726.65 | 1 | 726.65 | 570.96 | <0.0001 | |
Residual | 15.27 | 12 | 1.27 | |||
Lack of Fit | 14.98 | 10 | 1.50 | 10.36 | 0.0912 | Not significant |
Pure error | 0.2893 | 2 | 0.1446 | |||
Cor total | 2805.84 | 26 | ||||
Adeq precision | 41.6701 | |||||
R2 | 0.9946 | |||||
Adjusted R2 | 0.9882 | |||||
Predicted R2 | 0.9690 | |||||
C.V./% | 1.48 |
Fig.4 (a) Residual diagram of Li response surface model; (b) Residual diagram of Fe response surface model; (c) Distribution diagram of experimental value and predicted value of Li leaching rate; (d) Distribution diagram of experimental value and predicted value of Fe leaching
Fig.5 (a) Three-dimensional response surface diagram of Li leaching rate; (b) Three-dimensional response surface diagram of Fe leaching rate; (c) Two-dimensional contour map of Li leaching rate; (d) Two-dimensional contour map of Fe leaching rate
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