High pressure hydrogenation reactor operation precautions

January 07, 2021

1. Before turning on the console current switch, first turn the stirring switch and the speed control heating switch to zero.

2. Rinse the inner wall of the autoclave, stir and join the surface with distilled water before feeding. After washing the joint surface, wipe it with cotton or silk cloth, and then slowly close the upper cover to avoid hitting the joint surface.

3. When screwing up, be sure to check the number and use a torque wrench to form a cross-shaped symmetry to avoid uneven force. Do not twist the screw in place at one time, and gradually tighten the force symmetrically.

4. After the screw is tightened, first vacuum the pump with a mechanical pump, then repeatedly pass nitrogen gas two to four times, drain the air in the kettle, then vacuum, pass hydrogen, stir, heat up, and operate normally.

5. After the reaction was completed, the stirring was stopped, the residual hydrogen in the kettle was exhausted, nitrogen gas was introduced, the air was vented, and the screw was unscrewed for sampling.

The 6.5L hydrogenation reactor is not resistant to strong acid, and strong acid such as hydrochloric acid, sulfuric acid or nitric acid is prohibited in the reaction solution.

7. In the vicinity of the hydrogenation reactor, the operation of generating sparks is prohibited, and the operation of wearing nail shoes is prohibited.

Experience: Detailed steps and methods for high pressure catalytic hydrogenation

1, washing kettle

2, open the kettle to put the substrate

3. Close the kettle, the palladium/carbon catalyst dissolved in the solvent is added to the kettle through the funnel feeding device, the feeding device is removed, the hydrogen copper tube is connected, and the air inlet and the air outlet are closed.

4, close the pressure reducing valve, all open the hydrogen cylinder main valve

5, adjust the pressure reducing valve to 18 atmospheres

6. Open the air inlet, adjust the pressure in the kettle to about 5 kg, close the air inlet, open the air outlet, adjust the pressure in the kettle to about 2 kg, close the air outlet; open the air inlet again, adjust the pressure inside the kettle. 5 kg or so, close the air inlet, keep it for about 15 minutes, see if there is any change in the kettle pressure, check the air tightness of the kettle; open the air outlet, adjust the pressure inside the kettle to 2 kg, close the air outlet; open the air inlet again. Adjust the pressure to hydrogenation pressure (about 15 kg), turn on the stirring, and slightly increase the temperature inside the kettle. Because the reaction temperature rises after the exotherm, the jacket cooling water should be used to adjust the temperature, and the temperature and pressure changes are recorded at intervals until the pressure No longer change. (In the hydrogenation process, hydrogen should be continuously added. The specific additional procedure is: the pressure is reduced from 15 to 10, the intake valve is opened to adjust the pressure in the kettle to 15 kg again, the intake valve is closed, and the record is added. Amount of hydrogen)

7. After the reaction is completed, close the main valve of the hydrogen cylinder, open the outlet valve of the kettle, adjust the pressure in the kettle to about 3 kg, close the outlet valve, open the intake valve, close the intake valve, open the outlet valve, and adjust the pressure inside the kettle. At about 3 kg, close the air outlet valve until the pressure value of the pressure reducing valve is safe and remove the air intake.

8. Connect the discharge device and open the intake valve to hydraulically pump out the material inside.



( Source: China Pharmaceutical Network )

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