Chongqing Jingzhi Pharmaceutical has customized a 2L hydrogenation stainless steel high-pressure vessel and delivered it for use

Operating procedures for high-pressure reactors

1. Connect

Firstly, connect the high-pressure reactor and the high-pressure reactor controller through a circuit, and connect the heater to the high-pressure reactor controller.

When tightening the main bolt, do not exceed the specified tightening torque to prevent the sealing surface from being crushed or accelerated wear. tighten

When using bolts, they must be tightened diagonally. The screws should not be twisted into place at once, but should be tightened gradually and symmetrically in multiple steps, using force

Be uniform and do not allow the kettle lid to tilt to one side to achieve good sealing effect.

2. Check the mixer and heating system

(1) Open controlceremonyBefore the current switch, the mixing switch and the speed regulating heating switch should be activated firstwaitAdjust to zero.

(2) Turn on the power. Slowly adjust and observe whether the temperature inside the kettle displayed on the instrument rises normally and whether the mixer rotates normally. (Note that after starting the mixer, wait for a moment before starting to slowly rotate until it reaches the set speed.)

3．checkairtightsex

(1) First, connect the hydrogen pipe to the inlet to ensure a tight connection.

(2) To supply hydrogen gas, first turn on the knob of the hydrogen gas cylinder. At this time, the knob of the pressure reducing valve is in the closed or loosened state

When the high pressure gauge displays a certain value, open the pressure reducing valve knob and turn it clockwise until the low pressure gauge reaches the required pressure,

Observe the pressure gauge on the high-pressure vessel,Conduct an air tightness test on the entire system, using soap water, listening, touching, and other methods to find leaks,

And tighten it under pressure, but the pressure should not exceed 0.1MPa. After all processing is completed, raise the pressure to the reaction site

Pressure is required. Observe the pressure gauge for 1 hour, and a pressure drop of ≤ 0.05MPa is considered qualified.

(Note: When connecting the hydrogen gas pipe and the intake valve, align the small head of the small nut in the intake valve with the intake port, and slightly exceed the hydrogen gas pipe.)

Remove the small nut and tighten the outer nut. ）

4．add ingredients

Add reactants and introduce hydrogen gas，Open the air outlet and wait for the air inside the kettle to be completely expelledClose the air inlet and outlet.

5．Pressurized displacement

（1）Close the pressure reducing valve and open the main valve of the hydrogen cylinder.

（2）Adjust the pressure reducing valve toResponse requiredatmospheric pressure.

（3）Open the air intake,Control the hydrogen inlet valve to slowly increase the pressure to 0.5 MPa,Maintain for about 15 minutes and check if the kettle pressure is maintained

Change, inspect the airtightness of the kettle;Open the exhaust valve of the high-pressure reactor and exhaust until the pressure drops to around 0.1 MPa,

Close the exhaust valve, then increase the pressure to 0.5MPa and exhaust using the same method. Repeat this process three times in total.

6．Heating and Boosting

Heating and boosting must be done slowly. Turn on the stirring and slightly increase the temperature inside the kettle, as the reaction temperature rises after releasing heat

Use jacket cooling water to regulate the temperature, and record the changes in temperature and pressure at intervals until the pressure no longer changes.

During the hydrogenation process, hydrogen gas should be continuously replenished, and the specific replenishment procedure is: reduce the pressure from 15 to 10, and then

Adjust the pressure inside the kettle to 15 kilograms through the intake valve, close the intake valve, and record the amount of hydrogen added.

7. Stop the reaction

After the reaction is completed,Close the main valve of the hydrogen cylinder,Stop heatingCool down and release high-pressure gas from the kettle to reduce the pressure

At atmospheric pressure,At this point, it is necessary to cool down to 50℃belowThen loosen and remove the bolts symmetrically and evenly. During the process of removing the cover

Pay special attention to protecting the sealing surface. After each operation, the residue on the kettle body and lid should be removed, and any residue on the high-pressure kettle should be removed

There is a sealing surface that should be cleaned regularly and kept dry. It is not allowed to use hard or soft materials with rough surfaces for cleaning.

The mixer needs to be removed and cleaned.Some waste catalysts can oxidize and ignite, so they need to be properly disposed of.