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Complete operating procedures for autoclave reactions

Release date: 2019-01-11 14:19:24 Visits: 1067

The operation procedure of the complete high-pressure reactor can be divided into the following six processes:

(1) Installation

1. Check whether there are flammable and explosive materials inside and outside the kettle, and whether there are any items that are not conducive to air circulation. If so, remove them;

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

3. Close all valves (except the exhaust valve) and start feeding. After feeding, cover the lid of the kettle (Note: Apply force evenly when rotating the nut to ensure that the two diagonal screws are tightened to prevent leakage after tightening) ;

4. Close the exhaust valve.

(2) Check the air tightness of the device

Close all valves and cover the lid of the kettle (note: apply the force evenly when rotating the nut to ensure that the two diagonal screws are tightened with each other to prevent air leakage after tightening); open the inlet valve and pass nitrogen to 1MPa to close the inlet Valve, observe the pressure changes, and confirm whether the device leaks air!

(Three) hydrogenation

1. Check whether each valve is closed tightly;

2. Point the exhaust hose to an open and airy place;

3. Put on the hydrogen pressure reducing valve (note that the silk port of the hydrogen pressure valve is anti-filament) and nitrogen pressure valve, and check if there is air leak with soapy water after it is installed (if it leaks, please re-enter it);

4. Vacuum the air on the liquid surface at the exhaust port;

5. Open the inlet valve of the kettle, open the nitrogen pressure reducing valve, and fill it with nitrogen to make the pressure in the inner kettle (P = 0.2Mpa), close the nitrogen pressure reducing valve, close the inlet valve, and keep it for about 2 minutes, see the pressure gauge pressure Whether to descend, and listen to the valve and kettle cover for leaks. If not, slowly open the exhaust valve and close the exhaust valve when the pressure inside is discharged to 0.01Mpa.

6. Repeat step 5 again.

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

(4) Control sampling:

1. Every half an hour, observe whether the data is normal. If the pressure decreases, you must replenish hydrogen;

2. The hydrogen in the hydrogen cylinder cannot be exhausted. When a certain pressure (P≈0.01Mpa) must be ensured, the new bottle should be discarded and replaced;

3. Sampling. Open the exhaust valve slowly and set the pressure in the kettle to 0.2Mpa, close the exhaust valve, slowly open the sampling valve until the reaction liquid emerges, close the sampling valve, take a sample, and then clean the sampling port to prevent flammable materials from remaining.

(5) Hydrogen leakage:

After confirming that the reaction is over, slowly discharge the hydrogen gas to the end (note that the exhaust valve is closed when there is a slight pressure to prevent oxygen from entering), open the intake valve, flush the nitrogen to 0.2Mpa to close the intake valve, and then slowly open the exhaust valve. Release the mixed gas inside, and re-enter the nitrogen gas as soon as possible. After three gas exchanges, use a vacuum pump to extract the gas on the liquid surface, open the exhaust valve and sampling valve, and start discharging from the bottom valve (note that because of oxygen Spontaneous combustion materials such as Pa / c, RaneyNi, so do not spill it on the container), if leaked, immediately dip it out with a wet towel, put it in a bucket with water, and then destroy it with a small amount of dilute acid After the material is discharged, close the bottom valve immediately.

(VI) Unloading

The finished kettle should be cleaned immediately, and the following steps should be performed before cleaning:

1. Charge the reaction solvent into the kettle from the exhaust valve. After cleaning most of the residue, pour in half of the kettle and stir for 10 minutes. Then you can open the kettle lid and clean the inner wall of the kettle

2. During cleaning, the lid and sampling valve of the kettle must be cleaned. At the same time, if there is water in the reactor, the nitrogen gas is slightly charged;

3. For the reactor that is not used temporarily, it is better to soak the reactor with 70% volume of absolute anhydrous ethanol to immerse it, without tightening the screws.
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