Chemical Industry and Engineering Progress ›› 2021, Vol. 40 ›› Issue (10): 5678-5691.DOI: 10.16085/j.issn.1000-6613.2020-2203
• Fine chemicals • Previous Articles Next Articles
WANG Ben1(), WANG Chao1, YIN Jinhua2()
Received:
2020-11-04
Revised:
2020-12-22
Online:
2021-10-25
Published:
2021-10-10
Contact:
YIN Jinhua
通讯作者:
尹进华
作者简介:
王犇(1970—),男,博士,副教授,硕士生导师,研究方向为安全科学、化工过程强化。E-mail:基金资助:
CLC Number:
WANG Ben, WANG Chao, YIN Jinhua. Continuous-flow diazotization of methyl anthranilate in microreactor system[J]. Chemical Industry and Engineering Progress, 2021, 40(10): 5678-5691.
王犇, 王超, 尹进华. 微反应器内邻氨基苯甲酸甲酯的连续重氮化工艺[J]. 化工进展, 2021, 40(10): 5678-5691.
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URL: https://hgjz.cip.com.cn/EN/10.16085/j.issn.1000-6613.2020-2203
水平 | 因素 | |||
---|---|---|---|---|
A | B | C | D | |
-1 | 1∶1.0 | 1∶2.4 | 25℃ | 30s |
0 | 1∶1.1 | 1∶2.6 | 35℃ | 40s |
1 | 1∶1.2 | 1∶2.8 | 45℃ | 50s |
水平 | 因素 | |||
---|---|---|---|---|
A | B | C | D | |
-1 | 1∶1.0 | 1∶2.4 | 25℃ | 30s |
0 | 1∶1.1 | 1∶2.6 | 35℃ | 40s |
1 | 1∶1.2 | 1∶2.8 | 45℃ | 50s |
水平 | 因素 | |||
---|---|---|---|---|
A | B | C | D | |
-1 | 1∶1.2 | 1∶2.8 | 5℃ | 10min |
0 | 1∶1.3 | 1∶3.0 | 15℃ | 15min |
1 | 1∶1.4 | 1∶3.2 | 25℃ | 20min |
水平 | 因素 | |||
---|---|---|---|---|
A | B | C | D | |
-1 | 1∶1.2 | 1∶2.8 | 5℃ | 10min |
0 | 1∶1.3 | 1∶3.0 | 15℃ | 15min |
1 | 1∶1.4 | 1∶3.2 | 25℃ | 20min |
编号 | 因素编码值 | 连续收率/% | 半间歇收率/% | |||||
---|---|---|---|---|---|---|---|---|
A | B | C | D | 实测 | 预测 | 实测 | 预测 | |
1 | 0 | 0 | 0 | 0 | 90.7 | 90.40 | 80.5 | 80.44 |
2 | -11 | 0 | -11 | 0 | 82.5 | 82.66 | 68.5 | 68.11 |
3 | -11 | 1 | 0 | 0 | 87.8 | 87.58 | 78.0 | 77.98 |
4 | 1 | -11 | 0 | 0 | 88.4 | 87.88 | 78.2 | 78.08 |
5 | 0 | 0 | -11 | -11 | 75.6 | 74.77 | 62.4 | 62.92 |
6 | 0 | 0 | 1 | 1 | 84.3 | 84.40 | 71.7 | 71.05 |
7 | -11 | -11 | 0 | 0 | 83.2 | 82.95 | 71.1 | 71.25 |
8 | -11 | 0 | 0 | 1 | 86.8 | 86.68 | 76.2 | 76.20 |
9 | 0 | 0 | 0 | 0 | 90.0 | 90.40 | 80.1 | 80.44 |
10 | -11 | 0 | 1 | 0 | 83.9 | 84.23 | 69.8 | 69.65 |
11 | 0 | 1 | 1 | 0 | 88.2 | 88.21 | 76.7 | 77.10 |
12 | 0 | -11 | 0 | -11 | 79.2 | 79.51 | 73.4 | 72.98 |
13 | 1 | 0 | -11 | 0 | 85.5 | 85.39 | 69.8 | 69.80 |
14 | 1 | 0 | 0 | -11 | 82.3 | 82.94 | 76.9 | 77.19 |
15 | 1 | 1 | 0 | 0 | 90.2 | 89.72 | 80.4 | 80.12 |
16 | 0 | 1 | 0 | 1 | 90.1 | 90.01 | 80.6 | 80.86 |
17 | -11 | 0 | 0 | -11 | 79.7 | 79.81 | 72.3 | 72.55 |
18 | 0 | 1 | 0 | -11 | 82.5 | 82.99 | 77.4 | 77.26 |
19 | 0 | 0 | -11 | 1 | 89.0 | 88.98 | 74.5 | 74.87 |
20 | 1 | 0 | 1 | 0 | 88.5 | 88.56 | 77.0 | 77.23 |
21 | 0 | 0 | 0 | 0 | 90.9 | 90.40 | 80.1 | 80.44 |
22 | 0 | -11 | -11 | 0 | 82.1 | 82.61 | 68.2 | 68.09 |
23 | 0 | -11 | 0 | 1 | 87.3 | 87.03 | 76.4 | 76.38 |
24 | 0 | 0 | 0 | 0 | 90.1 | 90.40 | 80.7 | 80.44 |
25 | 0 | 0 | 1 | -11 | 84.8 | 84.08 | 76.5 | 76.00 |
26 | 0 | -11 | 1 | 0 | 84.1 | 84.33 | 69.9 | 70.42 |
27 | 0 | 0 | 0 | 0 | 90.3 | 90.40 | 80.8 | 80.44 |
28 | 0 | 1 | -11 | 0 | 84.9 | 85.19 | 70.4 | 70.17 |
29 | 1 | 0 | 0 | 1 | 90.2 | 90.61 | 80.5 | 80.54 |
编号 | 因素编码值 | 连续收率/% | 半间歇收率/% | |||||
---|---|---|---|---|---|---|---|---|
A | B | C | D | 实测 | 预测 | 实测 | 预测 | |
1 | 0 | 0 | 0 | 0 | 90.7 | 90.40 | 80.5 | 80.44 |
2 | -11 | 0 | -11 | 0 | 82.5 | 82.66 | 68.5 | 68.11 |
3 | -11 | 1 | 0 | 0 | 87.8 | 87.58 | 78.0 | 77.98 |
4 | 1 | -11 | 0 | 0 | 88.4 | 87.88 | 78.2 | 78.08 |
5 | 0 | 0 | -11 | -11 | 75.6 | 74.77 | 62.4 | 62.92 |
6 | 0 | 0 | 1 | 1 | 84.3 | 84.40 | 71.7 | 71.05 |
7 | -11 | -11 | 0 | 0 | 83.2 | 82.95 | 71.1 | 71.25 |
8 | -11 | 0 | 0 | 1 | 86.8 | 86.68 | 76.2 | 76.20 |
9 | 0 | 0 | 0 | 0 | 90.0 | 90.40 | 80.1 | 80.44 |
10 | -11 | 0 | 1 | 0 | 83.9 | 84.23 | 69.8 | 69.65 |
11 | 0 | 1 | 1 | 0 | 88.2 | 88.21 | 76.7 | 77.10 |
12 | 0 | -11 | 0 | -11 | 79.2 | 79.51 | 73.4 | 72.98 |
13 | 1 | 0 | -11 | 0 | 85.5 | 85.39 | 69.8 | 69.80 |
14 | 1 | 0 | 0 | -11 | 82.3 | 82.94 | 76.9 | 77.19 |
15 | 1 | 1 | 0 | 0 | 90.2 | 89.72 | 80.4 | 80.12 |
16 | 0 | 1 | 0 | 1 | 90.1 | 90.01 | 80.6 | 80.86 |
17 | -11 | 0 | 0 | -11 | 79.7 | 79.81 | 72.3 | 72.55 |
18 | 0 | 1 | 0 | -11 | 82.5 | 82.99 | 77.4 | 77.26 |
19 | 0 | 0 | -11 | 1 | 89.0 | 88.98 | 74.5 | 74.87 |
20 | 1 | 0 | 1 | 0 | 88.5 | 88.56 | 77.0 | 77.23 |
21 | 0 | 0 | 0 | 0 | 90.9 | 90.40 | 80.1 | 80.44 |
22 | 0 | -11 | -11 | 0 | 82.1 | 82.61 | 68.2 | 68.09 |
23 | 0 | -11 | 0 | 1 | 87.3 | 87.03 | 76.4 | 76.38 |
24 | 0 | 0 | 0 | 0 | 90.1 | 90.40 | 80.7 | 80.44 |
25 | 0 | 0 | 1 | -11 | 84.8 | 84.08 | 76.5 | 76.00 |
26 | 0 | -11 | 1 | 0 | 84.1 | 84.33 | 69.9 | 70.42 |
27 | 0 | 0 | 0 | 0 | 90.3 | 90.40 | 80.8 | 80.44 |
28 | 0 | 1 | -11 | 0 | 84.9 | 85.19 | 70.4 | 70.17 |
29 | 1 | 0 | 0 | 1 | 90.2 | 90.61 | 80.5 | 80.54 |
来源 | 平方和和 | 自由度 | 均方 | F值 | P值 |
---|---|---|---|---|---|
模型 | 446.06 | 14 | 31.86 | 111.65 | <0.0001 |
A | 37.45 | 1 | 37.45 | 131.25 | <0.0001 |
B | 31.36 | 1 | 31.36 | 109.91 | <0.0001 |
C | 16.80 | 1 | 16.80 | 58.89 | <0.0001 |
D | 158.41 | 1 | 158.41 | 555.14 | <0.0001 |
AB | 1.96 | 1 | 1.96 | 6.87 | 0.0201 |
AC | 0.64 | 1 | 0.64 | 2.24 | 0.1564 |
AD | 0.16 | 1 | 0.16 | 0.56 | 0.4664 |
BC | 0.42 | 1 | 0.42 | 1.48 | 0.2438 |
BD | 0.063 | 1 | 0.063 | 0.22 | 0.6470 |
CD | 48.30 | 1 | 48.30 | 169.27 | <0.0001 |
A2 | 17.04 | 1 | 17.04 | 59.72 | <0.0001 |
B2 | 19.77 | 1 | 19.77 | 69.28 | <0.0001 |
C2 | 82.71 | 1 | 82.71 | 289.84 | <0.0001 |
D2 | 92.23 | 1 | 92.23 | 323.22 | <0.0001 |
残差 | 3.99 | 14 | 0.27 | ||
失拟误差 | 3.39 | 10 | 0.34 | 2.26 | 0.2240 |
纯误差 | 0.60 | 4 | 0.15 | ||
总误差 | 450.02 | 28 | |||
标准偏差 | 0.53 | 预测系数R | 0.9545 | ||
确定系数R2 | 0.9911 | 变异系数 | 0.62% | ||
调整系数R | 0.9822 | 精密度 | 41.234 |
来源 | 平方和和 | 自由度 | 均方 | F值 | P值 |
---|---|---|---|---|---|
模型 | 446.06 | 14 | 31.86 | 111.65 | <0.0001 |
A | 37.45 | 1 | 37.45 | 131.25 | <0.0001 |
B | 31.36 | 1 | 31.36 | 109.91 | <0.0001 |
C | 16.80 | 1 | 16.80 | 58.89 | <0.0001 |
D | 158.41 | 1 | 158.41 | 555.14 | <0.0001 |
AB | 1.96 | 1 | 1.96 | 6.87 | 0.0201 |
AC | 0.64 | 1 | 0.64 | 2.24 | 0.1564 |
AD | 0.16 | 1 | 0.16 | 0.56 | 0.4664 |
BC | 0.42 | 1 | 0.42 | 1.48 | 0.2438 |
BD | 0.063 | 1 | 0.063 | 0.22 | 0.6470 |
CD | 48.30 | 1 | 48.30 | 169.27 | <0.0001 |
A2 | 17.04 | 1 | 17.04 | 59.72 | <0.0001 |
B2 | 19.77 | 1 | 19.77 | 69.28 | <0.0001 |
C2 | 82.71 | 1 | 82.71 | 289.84 | <0.0001 |
D2 | 92.23 | 1 | 92.23 | 323.22 | <0.0001 |
残差 | 3.99 | 14 | 0.27 | ||
失拟误差 | 3.39 | 10 | 0.34 | 2.26 | 0.2240 |
纯误差 | 0.60 | 4 | 0.15 | ||
总误差 | 450.02 | 28 | |||
标准偏差 | 0.53 | 预测系数R | 0.9545 | ||
确定系数R2 | 0.9911 | 变异系数 | 0.62% | ||
调整系数R | 0.9822 | 精密度 | 41.234 |
来源 | 平方和 | 自由度 | 均方 | F值 | P值 |
---|---|---|---|---|---|
模型 | 661.71 | 14 | 47.26 | 239.50 | <0.0001 |
A | 60.30 | 1 | 60.30 | 305.56 | <0.0001 |
B | 57.64 | 1 | 57.64 | 292.08 | <0.0001 |
C | 64.40 | 1 | 64.40 | 326.35 | <0.0001 |
D | 36.75 | 1 | 36.75 | 186.22 | <0.0001 |
AB | 5.52 | 1 | 5.52 | 27.98 | 0.0001 |
AC | 8.70 | 1 | 8.70 | 44.10 | <0.0001 |
AD | 0.023 | 1 | 0.023 | 0.11 | 0.7406 |
BC | 5.29 | 1 | 5.29 | 26.81 | 0.0001 |
BD | 0.01 | 1 | 0.01 | 0.051 | 0.8251 |
CD | 71.40 | 1 | 71.40 | 361.82 | <0.0001 |
A2 | 23.81 | 1 | 23.81 | 120.64 | <0.0001 |
B2 | 18.00 | 1 | 18.00 | 91.21 | <0.0001 |
C2 | 348.35 | 1 | 348.35 | 1765.20 | <0.0001 |
D2 | 23.50 | 1 | 23.50 | 119.07 | <0.0001 |
残差 | 2.76 | 14 | 0.20 | ||
失拟误差 | 2.33 | 10 | 0.23 | 2.16 | 0.2385 |
纯误差 | 0.43 | 4 | 0.11 | ||
总误差 | 664.47 | 28 | |||
标准偏差 | 0.44 | 预测系数R | 0.9788 | ||
确定系数R2 | 0.9958 | 变异系数 | 0.59% | ||
调整系数R | 0.9917 | 精密度 | 56.170 |
来源 | 平方和 | 自由度 | 均方 | F值 | P值 |
---|---|---|---|---|---|
模型 | 661.71 | 14 | 47.26 | 239.50 | <0.0001 |
A | 60.30 | 1 | 60.30 | 305.56 | <0.0001 |
B | 57.64 | 1 | 57.64 | 292.08 | <0.0001 |
C | 64.40 | 1 | 64.40 | 326.35 | <0.0001 |
D | 36.75 | 1 | 36.75 | 186.22 | <0.0001 |
AB | 5.52 | 1 | 5.52 | 27.98 | 0.0001 |
AC | 8.70 | 1 | 8.70 | 44.10 | <0.0001 |
AD | 0.023 | 1 | 0.023 | 0.11 | 0.7406 |
BC | 5.29 | 1 | 5.29 | 26.81 | 0.0001 |
BD | 0.01 | 1 | 0.01 | 0.051 | 0.8251 |
CD | 71.40 | 1 | 71.40 | 361.82 | <0.0001 |
A2 | 23.81 | 1 | 23.81 | 120.64 | <0.0001 |
B2 | 18.00 | 1 | 18.00 | 91.21 | <0.0001 |
C2 | 348.35 | 1 | 348.35 | 1765.20 | <0.0001 |
D2 | 23.50 | 1 | 23.50 | 119.07 | <0.0001 |
残差 | 2.76 | 14 | 0.20 | ||
失拟误差 | 2.33 | 10 | 0.23 | 2.16 | 0.2385 |
纯误差 | 0.43 | 4 | 0.11 | ||
总误差 | 664.47 | 28 | |||
标准偏差 | 0.44 | 预测系数R | 0.9788 | ||
确定系数R2 | 0.9958 | 变异系数 | 0.59% | ||
调整系数R | 0.9917 | 精密度 | 56.170 |
反应器 | 单位体积换热面积/m2·m-3 | 年产量 /t | 产量放大 方式 | 放大效应 |
---|---|---|---|---|
AFRTM-G1 | 2500 | 25~80 | 数增放大 | 无放大效应 |
AFRTM-G4 | 2500 | 约2000 | — | — |
半间歇反应釜 | 10 | 约1500 | 尺寸放大 | 小试-中试-生产 |
反应器 | 单位体积换热面积/m2·m-3 | 年产量 /t | 产量放大 方式 | 放大效应 |
---|---|---|---|---|
AFRTM-G1 | 2500 | 25~80 | 数增放大 | 无放大效应 |
AFRTM-G4 | 2500 | 约2000 | — | — |
半间歇反应釜 | 10 | 约1500 | 尺寸放大 | 小试-中试-生产 |
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