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Operation Manual of Supercritical Fluid Fractionation Unit

Operation Manual of Supercritical Fluid Fractionation Device

Preparation before starting

  • First, check whether the power supply and three phases are intact. (220V/60HZ)
  • Add 30% ethylene glycol + 70% pure water to the water tank in the refrigerator. (Chloride ion content <25mg/L), and connect the cooling water pipe with the CO2 pump head.
  • The pressure of the CO2 gas cylinder is guaranteed to be 5-6MPa. (It can be heated by an electric heating ring when the room temperature is low)
  • Check whether the pipe joints and the connection parts are firm.
  • Add deionized ionized water to each heated water tank, not too full, 2-3cm away from the cover.

Start-up operation sequence

  1. 1Turn on the power, turn on the power switch, the three-phase power indicator lights are on, indicating that the power is normally connected.
  2. Turn on the power of the refrigeration unit and start cooling after a delay of a few minutes. The upper and lower limits of the refrigeration temperature have been set without adjustment and are automatically controlled.
  3. Start heating, turn on the heating switch of the fractionation tower and separation kettle, and set the temperature required by the process. (The water consumption of the jacket should be replenished in time when adding water for the first time)
  4. While starting refrigeration, open the valve of the CO2 gas cylinder. By opening valve 2, the CO2 in the CO2 gas cylinder enters the purifier, cold coil, and storage tank, and the CO2 is liquefied. Liquid CO2 enters the bottom of the sedimentation tank or the upper interface of the sedimentation tank through the CO2 pump, valve 4, and heat exchanger. (Imported process selection)
  5. CO2 supercharging: The CO2 outlet protection pressure has been set at 30MPa and the raw material pump protection pressure has been set at 30MPa when the device leaves the factory. Under normal circumstances, it does not need to be set again.
  6. The working frequency (ie flow range) of the CO2 pump should generally be between 12 and 26 Hz, depending on the process conditions.
  7. Open valve 4 CO2 enters the bottom of the fractionation tower (upper or lower end of the sedimentation tank, process selection), open valves 10 and 12 (close the valves 9 and 11 at this time). CO2 and raw materials enter the separation kettle Ⅰ for separation. Open valve 13 and the solute CO2 enters the separation kettle II for separation again; open valve 15 and circulate the CO2 circuit. Adjust the back pressure valve 12 to control the outlet pressure of the fractionation tower, adjust the valve 13 to control the outlet pressure of the separation kettle I, and adjust valve 15 to control the pressure of the separation kettle II (general process valve 15 does not need to be adjusted and is normally open).
  8. When the pressure and temperature parameters of the CO2 cycle of the fractionation tower, separation kettle I, and separation kettle II are stable and similar to the requirements of the process parameters, the liquid feedstock is started. (Oily substance)
  9. The raw materials are refined and fractionated. The raw materials enter the upper, middle, and lower inlets of the fractionation tower through the raw material pump. The valves 5, 6, 7, and 8 are used to select the raw material imports according to the process conditions.
  10. The refined material is collected in the separation kettle I. If the quality requirements are not met, the separation collector can be selected for the collection, and then the reflux pump is used to enter the top of the fractionation tower to refine and fractionate again.
  11. Valve 3 is a venting valve for the fractionation tower. Valve 9 is a degassing valve of the fractionating tower, valve 11 is a degassing valve of the fractionating tower and separation kettle Ⅰ, and valves 14 and 16 are the bleed valves of the separation kettle Ⅰ and II, respectively.

Matters needing attention and troubleshooting:

1. This device is a high-pressure mobile device. Those who are not familiar with the flow of this system shall not operate it, and shall not leave their posts during high-pressure operations. If an abnormal situation occurs, it should be shut down in time and the power supply should be turned off to check.

2. Refrigeration unit: see the instruction manual for details.

3. For the operation and maintenance of the CO2 high-pressure pump, raw material pump and return pump, please refer to the instruction manual.

CO2 fluid system

(1) When the CO2 pump is running, check whether the pump head has cooling water circulation and whether the plunger cooling is normal. (Bring your own water tank and micro water pump)

(2) When the CO2 pump starts to pressurize, wait for the CO2 to liquefy in the cold box and start working. At the same time, open the pump head vent valve to vent.

Heating and temperature control system

  • It is necessary to check whether the three-phase power supply is correct when starting up, and it is forbidden to run without phase.
  • Check the water level of each heated water tank every time it is turned on (each shift), and replenish it in time when it is not enough (due to high-temperature evaporation), otherwise, it will burn out the electric heating tube and the water pump. At the same time, it is necessary to check whether the three-phase pump motor rotates normally, especially if it has not been turned on for a long time, to prevent the scale from jamming the rotating shaft and burning the motor.