Operating procedures and steps of the laboratory hydrogenation reactor.

Operating procedures and steps of the laboratory hydrogenation reactor.

1. Check whether there are flammable and explosive items inside and outside the kettle, and whether there are items not conducive to air circulation present; if so, please remove them.

2. Check whether the valves and kettle are clean; if not, please wash them.

3. Close all valves (except the exhaust valve) and start feeding. After feeding, cover the kettle lid (Note: Apply even force when rotating the nut and make sure the two screws on the diagonal are tightened to each other to prevent air leakage after tightening).

4、Close the exhaust valve.

5、Close all valves and cover the kettle cover (Note: When rotating the screw cap, apply even force to ensure that the two diagonal screws are tightened to each other to prevent gas leakage after tightening); open the inlet valve and pass nitrogen to 1MPa, close the inlet valve and observe the pressure change to confirm whether the device is leaking gas.

6, on the hydrogen pressure reducing valve door (note that the fillet of the hydrogen pressure valve is anti-filament), nitrogen pressure valve, on good, with soapy water to check whether the air leakage (such as air leakage, please re-up).

7. extract the air from the liquid surface with vacuum at the exhaust port.

8, open the inlet valve of the kettle, open the pressure reducing valve, fill the nitrogen, make the inner kettle pressure (P=0.2Mpa), then close the nitrogen pressure reducing valve, close the inlet valve, keep it for about 2 minutes, see if the pressure gauge pressure drops, in addition, look down the first side to hear if the valve and kettle cover are leaking, if not, slowly open the exhaust valve, drain the pressure inside to 0.01Mpa, then close the exhaust valve.

9、Open the inlet valve, open the hydrogen pressure reducing valve, fill the hydrogen to the required pressure, close the inlet valve, close the hydrogen pressure reducing valve, and then debug other parameters to the required state to make it react.

10、Every half an hour, observe whether the data is normal, if the pressure decreases, the hydrogen must be replenished again.

11、Slowly open the exhaust valve, set the pressure in the kettle to 0.2Mpa, close the exhaust valve, slowly open the sampling valve until the reaction liquid comes out, close the sampling valve, take a sample, then clean the sampling port, and do not let flammable materials remain.

12、After confirming the reaction is over, slowly discharge hydrogen to the end (note that there is a little pressure inside to close the exhaust valve to avoid oxygen entering), open the inlet valve, flush in nitrogen to 0.2Mpa to close the inlet valve, then slowly open the exhaust valve to release the mixed gas inside, will be exhausted when re-entering nitrogen, so after three times of gas exchange, use the vacuum pump to pump out the gas on the liquid surface, open the exhaust valve, sampling valve, and start to discharge from the (Note, because there is oxygen-prone spontaneous combustion of substances such as Pa/c, RaneyNi, so do not spill outside the container), if spilled, please immediately dip it out with a wet towel, put it into a bucket with water, and then use a small amount of dilute acid to destroy it, close the bottom valve immediately after the discharge.

13、The laboratory hydrogenation reactor should be cleaned immediately after the material is released.