The operation of parallel high-pressure reactors must strictly follow safety regulations, and the following are the key operating steps:
1、 Preparation before operation
1. Equipment Joint Inspection
Synchronously inspect the bodies, sealing surfaces, mixing devices, and pipeline connections of multiple reaction vessels to confirm that there are no cracks or corrosion.
Verify that all safety valves, pressure gauges, and rupture discs of the kettle are within their valid period and functioning properly.
Ensure reliable grounding of the electrical system (heater, motor) and no risk of leakage.
2. Material and Environmental Preparation
The feeding amount of each kettle should not exceed 3/4 of the volume to avoid reaction expansion and overpressure. It is strictly prohibited to mix strong acids or corrosive substances.
The laboratory needs to be equipped with explosion-proof devices and fire extinguishing equipment, and operators should wear anti-static clothing.
2、 Loading and sealing
1. Synchronous loading
Feed according to the principle of "liquid first, solid second", and add the solid after crushing. Liquid materials are vacuum injected under nitrogen protection.
Rinse the sealing surface with mother liquor before capping to ensure no residue.
2. Sealing and airtightness testing
Use a torque wrench to tighten the bolts step by step in diagonal order, and the torque should meet the equipment specifications.
Simultaneously introduce nitrogen gas and gradually increase the pressure (to 105% of the working pressure), maintain the pressure for 30 minutes to detect multiple kettle leaks. Disable oxygen or hydrogen testing.
3、 Reaction process control
1. Inert and hydrogen gas introduction
Synchronize vacuuming → fill with nitrogen, replace 2-4 times until the oxygen content meets the standard.
When introducing hydrogen gas, the pressure needs to be gradually increased (with each increase ≤ 20% of the working pressure).
2. Parameter monitoring
Heating rate ≤ 80 ℃/h, to avoid cracking of the kettle due to thermal stress.
Real time recording of pressure, temperature, and stirring speed of each kettle, and immediate shutdown if any abnormalities are found.
When the temperature is above 60 ℃, cooling water needs to be supplied to the magnetic stirring water jacket.
4、 End of reaction and post-processing
1. Safe pressure relief
Slowly release hydrogen until the pressure is less than 0.15 MPa, and then replace residual hydrogen with nitrogen.
2. Cooling and Cleaning
Turn off the heating and let it cool naturally to room temperature. Do not rapidly cool down.
Before opening the lid, confirm that the pressure is reset to zero, thoroughly clean the kettle body and sealing surface, and inspect vulnerable parts such as the stirring blade.
5、 Key Attention
1. Personnel configuration: At least two people are required to operate, one of whom must have experience in high-pressure reactors.
2. Prohibited items: Overloading/overheating operation, sudden changes in temperature (temperature difference>110 ℃), and individual operation are strictly prohibited.
3. Maintenance requirements: Regularly verify safety accessories and conduct annual inspections according to pressure vessel specifications.
Note: Parallel operations need to ensure consistency in the parameters of each reactor. It is recommended to use a central control system to synchronously monitor the status of multiple reactors.