固定床反应器连续催化加氢（脱苄基）
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固定床反应器连续催化加氢（湖北）
反应体系中各物质的热力学参数见表 1。
项目 | 数值 | 单位 | 备注 |
硝基原料浓度（初始） | 100g/500mL | - | - |
硝基原料浓度（换算后） | 0.6191 | mol/L | 摩尔质量323g/mol |
固定床体积 | 5 | mL | - |
液相流速（初始） | 0.45 | mL/min | - |
液相流速（换算后） | 7.5×10⁻⁶ | L/s | 换算过程：0.45×1L÷1000mL×1min÷60s |
摩尔流量 | 4.644×10⁻⁶ | mol/s | 物质的量/时间 |
硝基苯反应焓变 | ≈550 | kJ/mol | 根据文献，∆fGθm = ∆fHθm - T∆fSθm = - 54.815×10³ J/mol |
转化率 | 100% | - | - |
放热速率 | 2.554 | J/s | 计算过程：550000J/mol×4.644×10⁻⁶ mol/s |
单位体积放热速率 | 510 | W/L | 计算过程：2.55 J/s÷0.005L |
液相295nm,流动相甲醇，1mL/min | ||||||||||
产物出峰位置，3.907 min 原料出峰位置，3.292min 5.324%; 5.033min 92.496% | ||||||||||
注：浓度0.5M代表摩尔浓度；5V代表底物与溶剂体积比 | ||||||||||
EA作溶剂 | ||||||||||
项目 | 液相mL/min | 气相mL/min | 温度/℃ | 压力/MPa | 溶剂/浓度 | 3.062min | 3.907min | 4.870min | 5.033min | 转化率 |
杂质 | 产物 | 杂质 | 原料 | |||||||
1 | 1 | 30 | 60 | 1 | EA/0.1M | 3.05% | 96.44% | / | 0% | 100% |
2 | 1 | 30 | 60 | 1.5 | EA/0.1M | 5.26% | 93.63% | / | 0% | 100% |
3 | 1 | 30 | 60 | 2 | EA/0.1M | 2.33% | 96.79% | / | 0% | 100% |
4 | 1.2 | 30 | 60 | 1 | EA/0.1M | 5.83% | 92.81% | / | 0% | 100% |
5 | 1.5 | 40 | 60 | 1 | EA/0.1M | 5.61% | 93.19% | / | 0% | 100% |
6 | 1.8 | 50 | 60 | 1 | EA/0.1M | 5.08% | 90.74% | / | 3% | 97% |
7 | 1.5 | 40 | 60 | 1 | EA/0.2M | 9.51% | 88.88% | / | 0% | 100% |
8 | 1.8 | 50 | 60 | 1 | EA/0.2M | 9.12% | 85.40% | / | 1.46% | 98% |
9 | 0.5 | 30 | 60 | 1.5 | EA/5V | 8.46% | 91.33% | / | 0% | 100% |
10 | 0.7 | 30 | 60 | 1.5 | EA/5V | 8.37% | 91.22% | / | 0% | 100% |
11 | 1 | 30 | 60 | 1.5 | EA/5V | 8.01% | 88.98% | / | 2.40% | 98% |
液相295nm,流动相甲醇，1mL/min | |||||||||||
产物出峰位置，3.907 min 原料出峰位置，3.292min 5.324%; 5.033min 92.496% | |||||||||||
注：浓度0.5M代表摩尔浓度；5V代表底物与溶剂体积比 | |||||||||||
EA作溶剂 | |||||||||||
项目 | 液相mL/min | 气相mL/min | 温度/℃ | 压力/MPa | 溶剂/浓度 | 3.062min | 3.907min | 4.870min | 5.033min | 转化率 | 时间 |
杂质 | 产物 | 杂质 | 原料 | ||||||||
1 | 0.7 | 30 | 60 | 1.5 | EA/5V | 2.33% | 93.78% | / | 0.00% | 1 | |
2 | 0.7 | 30 | 60 | 1.5 | EA/5V | 3.80% | 93.92% | / | 0% | 2 | |
3 | 0.7 | 30 | 60 | 1.5 | EA/5V | 7.85% | 91.06% | / | 0% | 3 | |
4 | 0.7 | 30 | 60 | 1.5 | EA/5V | 6.12% | 79.79% | / | 12.24% | 87% | 4h，原料反应不完全 |
5 | 0.7 | 30 | 60 | 2.5 | EA/5V | 8.29% | 82.75% | / | 7.94% | 92.00% | 5h |
6 | 0.7 | 30 | 80 | 3 | EA/5V | 7.63% | 91.16% | / | 0.36% | 99.00% | 6h |
7 | 0.7 | 30 | 80 | 3 | EA/5V | 7.67% | 91.02% | / | 0.37% | 99.00% | 6.5h |
8 | 0.7 | 30 | 80 | 2.5 | EA/5V | 8.41% | 90.49% | / | 0.00% | 100.00% | 8h |
9 | 0.7 | 30 | 80 | 2.5 | EA/5V | 0.00% | 100.00% | 9h | |||
液相295nm,流动相甲醇，1mL/min | |||||||||||
产物出峰位置，3.907 min 原料出峰位置，3.292min 5.324%; 5.033min 92.496% | |||||||||||
注：浓度0.5M代表摩尔浓度；5V代表底物与溶剂体积比 | |||||||||||
二甲苯作溶剂 | |||||||||||
项目 | 液相mL/min | 气相mL/min | 温度/℃ | 压力/MPa | 溶剂/浓度 | 3.062min | 3.907min | 4.870min | 5.033min | 转化率 | |
杂质 | 产物 | 杂质 | 原料 | ||||||||
1 | 1 | 30 | 60 | 1 | 0.2M | 0% | 96.87% | 1.48% | 0% | 100% | |
2 | 1.2 | 30 | 60 | 1 | 0.2M | 2.25% | 88.40% | 7.64% | 0% | 100% | |
3 | 1.4 | 40 | 60 | 1 | 0.2M | 0% | 95.54% | 3.74% | 0% | 100% | |
4 | 1.4 | 50 | 80 | 1 | 0.2M | 1.33% | 88.74% | 9.60% | 0% | 100% | |
5 | 0.5 | 30 | 60 | 1 | 5V | 2.04% | 91.84% | 4.50% | 0% | 100% | |
6 | 0.5 | 30 | 60 | 2 | 5V | 5.20% | 88.05% | 6.23% | 0% | 100% | |
7 | 0.5 | 50 | 60 | 2 | 5V | 4.75% | 89.73% | 5.52% | 0% | 100% | |
液相295nm,流动相甲醇，1mL/min | |||||||||||
产物出峰位置，3.907 min 原料出峰位置，3.292min 5.324%; 5.033min 92.496% | |||||||||||
注：浓度0.5M代表摩尔浓度；5V代表底物与溶剂体积比 | |||||||||||
EA 作溶剂 | |||||||||||
项目 | 液相mL/min | 气相mL/min | 温度/℃ | 压力/MPa | 溶剂/浓度 | 3.062min | 3.907min | 6.72min | 5.033min | 转化率 | 时间 |
杂质 | 产物 | 杂质 | 原料 | ||||||||
1 | 0.45 | 21 | 60 | 1.5 | EA/5V | 14.23% | 84.09% | / | 0% | 100.00% | 1h |
2 | 0.45 | 21 | 60 | 1.5 | EA/5V | 11.48% | 87.32% | / | 0% | 100.00% | 2h |
3 | 0.45 | 21 | 60 | 1.5 | EA/5V | 8.05% | 91.32% | / | 0% | 100.00% | 3h |
4 | 0.45 | 21 | 60 | 1.5 | EA/5V | 11.02% | 88.70% | / | 0% | 100.00% | 4h |
5 | 0.45 | 21 | 60 | 1.5 | EA/5V | 10.79% | 86.87% | / | 0% | 100.00% | 5h |
6 | 0.45 | 21 | 80 | 1.5 | EA/5V | 6.14% | 92.98% | / | 0% | 100.00% | 6h |
7 | 0.45 | 21 | 80 | 1.5 | EA/5V | 10.45% | 89.24% | / | 0% | 100.00% | 7h |
8 | 0.45 | 21 | 80 | 1.5 | EA/5V | 9.56% | 90.33% | / | 0% | 100.00% | 9h |
9 | 0.45 | 21 | 80 | 1.5 | EA/5V | 11.70% | 88.76% | 3.95% | 97.00% | 11h | |
总结：经实验对比分析可知，相较于 0.7 mL/min 的流速，0.45 mL/min 流速下反应系统压力更为稳定，后续无需依据反应实际状况提升反应系统压力。然而，在长时间运行过程中，催化剂会在底部被压实成粉末，从而阻塞氢气流通通道。运行 6 小时后，每两小时需对底部进行一次处理。因此，在工业化生产中，需添加惰性瓷球以避免此类情况的发生。
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