1 材料与方法
1.1 试验材料
1.2 试验设备
1.3 试验方法
1.3.1 材料预处理
1.3.2 提取工艺
1.3.3 单因素试验
1.3.4 响应面试验
表1 响应面试验因素及编码水平 |
| 变量 | 代码 | 编码水平 | ||
|---|---|---|---|---|
| -1 | 0 | 1 | ||
| NaOH浓度/(g/L) | A | 1.5 | 1.8 | 2.1 |
| 料液比/(g/mL) | B | 10 | 20 | 30 |
| 碱解温度/℃ | C | 40 | 50 | 60 |
| 碱解时间/min | D | 120 | 150 | 180 |
1.4 数据分析
2 结果与分析
2.1 单因素试验
2.1.1 NaOH浓度对IDF提取率的影响
2.1.2 料液比对IDF提取率的影响
2.1.3 碱解温度对IDF提取率的影响
2.1.4 碱解时间对IDF提取率的影响
2.2 响应面试验
表2 Box-Behnken Design试验设计与结果 |
| 运行 | NaOH浓度(A)/(g/L) | 料液比(B)/ (g/mL) | 碱解温度(C)/℃ | 碱解时间(D)/min | 提取率(Y)/% |
|---|---|---|---|---|---|
| 1 | 1 | 0 | 0 | -1 | 72.233 |
| 2 | 0 | -1 | -1 | 0 | 70.750 |
| 3 | 1 | 0 | 1 | 0 | 66.450 |
| 4 | 0 | 0 | 0 | 0 | 81.465 |
| 5 | 0 | 0 | 1 | 1 | 66.100 |
| 6 | 0 | 0 | 1 | -1 | 75.170 |
| 7 | 0 | 0 | 0 | 0 | 81.840 |
| 8 | 1 | -1 | 0 | 0 | 70.170 |
| 9 | -1 | 0 | 0 | -1 | 73.250 |
| 10 | 0 | 0 | 0 | 0 | 82.160 |
| 11 | -1 | 0 | 1 | 0 | 63.320 |
| 12 | 0 | 0 | 0 | 0 | 82.560 |
| 13 | 0 | 1 | 0 | 1 | 74.050 |
| 14 | 0 | 0 | 0 | 0 | 81.520 |
| 15 | 0 | 1 | -1 | 0 | 70.320 |
| 16 | 0 | 1 | 1 | 0 | 67.100 |
| 17 | -1 | -1 | 0 | 0 | 71.170 |
| 18 | 0 | -1 | 0 | -1 | 76.440 |
| 19 | 1 | 0 | -1 | 0 | 69.590 |
| 20 | 1 | 0 | 0 | 1 | 72.900 |
| 21 | 0 | -1 | 1 | 0 | 69.950 |
| 22 | -1 | 0 | -1 | 0 | 65.640 |
| 23 | -1 | 0 | 0 | 1 | 67.670 |
| 24 | 0 | -1 | 0 | 1 | 72.567 |
| 25 | 1 | 1 | 0 | 0 | 72.350 |
| 26 | 0 | 0 | -1 | -1 | 70.230 |
| 27 | -1 | 1 | 0 | 0 | 65.650 |
| 28 | 0 | 1 | 0 | -1 | 73.900 |
| 29 | 0 | 0 | -1 | 1 | 74.320 |
表3 响应面试验方差分析 |
| 方差来源 | 平方和 | 自由度 | 均方 | F值 | P值 | 显著性 |
|---|---|---|---|---|---|---|
| 模型 | 813.73 | 14 | 58.12 | 191.39 | <0.000 1 | 显著 |
| 浓度(A) | 24.06 | 1 | 24.06 | 79.24 | <0.000 1 | |
| 料液比(B) | 4.91 | 1 | 4.91 | 16.17 | 0.001 3 | |
| 温度(C) | 13.57 | 1 | 13.57 | 44.68 | <0.000 1 | |
| 时间(D) | 15.45 | 1 | 15.45 | 50.87 | <0.000 1 | |
| AB | 14.82 | 1 | 14.82 | 48.81 | <0.000 1 | |
| AC | 0.168 1 | 1 | 0.168 1 | 0.553 5 | 0.469 2 | |
| AD | 9.76 | 1 | 9.76 | 32.13 | <0.000 1 | |
| BC | 1.46 | 1 | 1.46 | 4.82 | 0.045 5 | |
| BD | 4.05 | 1 | 4.05 | 13.32 | 0.002 6 | |
| CD | 43.30 | 1 | 43.30 | 142.57 | <0.000 1 | |
| A2 | 377.21 | 1 | 377.21 | 1 242.10 | <0.000 1 | |
| B2 | 138.62 | 1 | 138.62 | 456.45 | <0.000 1 | |
| C2 | 395.39 | 1 | 395.39 | 1 301.97 | <0.000 1 | |
| D2 | 51.63 | 1 | 51.63 | 170.00 | <0.000 1 | |
| 残差 | 4.25 | 14 | 0.303 7 | |||
| 失拟项 | 3.41 | 10 | 0.341 2 | 1.62 | 0.338 7 | 不显著 |
| 纯误差 | 0.840 0 | 4 | 0.210 0 | |||
| 校正总和 | 817.98 | 28 | ||||
| 标准差 | 0.551 1 | R 2 | 0.994 8 | |||
| 均值 | 72.44 | Adjusted R 2 | 0.989 6 | |||
| 变异系数 | 0.760 7 | Predicted R 2 | 0.974 4 | |||
| Adeq Precision | 44.678 8 | |||||