A complete operation of high pressure reactor includes assembly, hydrogenation, sampling, hydrogen discharging and disassembly five processes:
I. Assembly
1. Check whether there is inflammable and explosive substances in and out of the reactor; or whether there exists substances not good for ventilation and please move away if there is.
2. Check whether the valves and reactor inside are clean; please clean up if not.
3. Turn off all the valves (except venting valve) and begin to feed medium. Close the tank cover after medium feeding (Note: please rotate the nuts with uniform force and tighten screws according to diagonal order to avoid air leakage).
4. Turn off the venting valve.
II. Check Tightness
Turn off all the valves and close the tank cover (Note: please rotate the nuts with uniform force and tighten screws according to diagonal order to avoid air leakage). Turn on the gas inlet valve to fill nitrogen in until the pressure reaches to 1MPa, then turn off the gas inlet valve and check pressure changes to make sure whether there is air leakage.
III. Hydrogenation
1. Check whether all the valves are tightened.
2. Place the venting flexible pipe towards a open place with good ventilation.
3. Tighten the top hydrogen pressure loading valve (note its thread is reversed) and nitrogen pressure valve, then check whether there is air leakage with soap-suds. (please tighten again if there is air leakage).
4. Vacuum pump out the air above liquid level at venting port.
5. Open the gas inlet valve and nitrogen pressure loading valve to fill nitrogen in. After the inner tank pressure reaches to 0.2MPa, turn off the nitrogen pressure loading valve and gas inlet valve for 2mins to check whether the pressure shown on piezometer is reducing and whether there is air leakage at tank cover by listening the sound of valve. If there is no leakage, turn on the venting valve slowly and discharge the pressure to 0.01MPa, then turn off the venting valve.
6. Repeat the operations in step 5.
7. Open the gas inlet valve and hydrogen pressure loading valve to fill hydrogen in to the pressure needed, then turn off the gas inlet valve and hydrogen pressure loading valve. Adjust the other parameters to the states needed.
IV. Sampling Control
1. Check whether all the parameters are normal each half an hour and need to supplement hydrogen if the pressure is reduced.
2. Hydrogen in hydrogen gas cylinder cannot be all discharged. Need to change to new cylinder with ensuring there is certain pressure in the old one (P≈0.01Mpa).
3. Sampling: turn on the venting valve slowly and set the inner tank pressure as 0.2MPa, then turn off the venting valve. Turn on sampling valve slowly and turn it off until there is reaction solution coming out. Sampling process can be done in this moment then clean the sampling port to ensure no inflammable residuals.
V. Hydrogen Discharging
Making sure the reaction is finished and discharge hydrogen slowly and thoroughly (note to turn off the venting valve once there is pressure inside, to avoid oxygen entering in). Turn on gas inlet valve to fill nitrogen in and turn the valve off when pressure reaches to 0.2MPa, then turn on the venting valve slowly to discharge the gas mixture inside and re-fill nitrogen when it is almost done. Repeat such gas changing for three times and pump out the gas above liquid level with vacuum pump; turn on the venting valve and sampling valve, then discharge medium from the bottom valve (note: as there is inflammable substances like Pa/c and RaneyNi inside, so it is forbidden to spill out of the vessel), if there is spilling, use wet towel to dip immediately, then put into bucket with water in; destroy it with a little dilute acid and turn off the bottom valve immediately once the medium discharging finished.
VI. Disassembly
Clean the reactor immediately after discharging mediums. Follow below steps before the cleaning:
1. Add the reaction solvent into reactor from the venting valve; after cleaning most of the residuals, fill water to the half space of reactor and mix for 10mins, then can open the tank cover at this time and clean the inner wall.
2. The tank cover and sampling valve must be cleaned; fill some nitrogen if there is water in the tank.
3. If the reactor will not be used for a period, it is better to add clean ethanol to the 70% volume of reactor for soaking; screws can be not tightened.