Chemtech KD6 Cannabinoid Distilling

KD-6 Cannabinoid Distilling SOP Number

51002

Revision Number

0

Revision Date

April 21, 2022 To provide a procedure for cannabinoid distilling on the Chemtech Services, Inc. Mini-5 and KD-6 distillation system.

This procedure applies to both the glass and stainless steel versions of the Chemtech Services, Inc. Mini-5 and KD-6 distillation systems.

Purpose Scope Referenced Documents

52001 KD-6 Cleaning

Materials and Equipment

Appropriate PPE

Definitions

Turbo Pump: turbomolecular pump (Leybold Turbovac 90i or Pfeiffer HiPace 60P) Vacuum Pump: rotary vane vacuum pump (Leybold D8B) Turbo Valve: right-angle valve between the turbo pump and the system Vacuum Bypass Valve: right-angle valve between the vacuum pump and the system Bleed Valve: KF-16 needle valve

Prior to engaging in any of the procedures outlined below, operators must have an understanding of all steps and wear appropriate PPE.

Cannabinoid Distilling Start Up Procedure 1. Turn on the circulators and set the temperatures according to Table 1 below.

Table 1: Cannabinoid Distilling Circulator Temperatures

Circulator Feed

Temperature (°C) 100°C

Residue

130-140°C

Evaporator

150-180°C

Condenser

100°C

Cold Trap

-50°C

Notes Hotter residue temperatures can be utilized for material prone to “freezing up” in the non-jacketed sections or in an environment that is very cold that may cause “freezing” in the non-jacketed sections.

Mini units – set the residue circulator to the same temperature as the feed.

The evaporator temperature is dependent on vacuum level and feed rate, hence the wide range of temperatures. Systems with liquid nitrogen cold traps can achieve deeper vacuum levels which allows for a lower evaporator temperature. A typical evaporator temperature setting is 170°C at a vacuum level of approximately 2.0x10-2 Torr with a feed rate determined by the desired separation.

Set the cold trap circulator to its lowest allowable temperature set point and run it as cold as possible.

2. Start the wiper motor when the evaporator circulator reaches 50°C and set it to half-speed according to Table 2.

NOTE: There is a risk of deforming the PTFE wiper rollers if the wiper motor is not started before the evaporator circulator reaches 100°C. Table 2: Wiper Motor Speeds

Unit Type Stainless Steel Glass

Half-Speed 200rpm 125-150rpm Page 1 of 4

Run Speed 400rpm 250-300rpm

3. Sample may be added to the feed tank when the feed circulator reaches the set point temperature. Stir the sample to ensure uniform temperature.

4. When the cold trap circulator reaches -30°C or lower, start the vacuum pump with the vacuum bypass valve open and the turbo valve closed: a. Open the bleed valve. b. Turn on the vacuum pump. c. Close the bleed valve.

NOTE: These steps prevent any potential shock from the vacuum to the glass of the system.

5. When the vacuum reaches 3.9x10-1 Torr or lower, turn on the turbo pump by either using the switch mounted on the turbo pump or the disconnect handle on the control panel. Monitor the three indicator lights on the turbo pump for any errors using Figure 1 from the Leybold Turbovac manual below. If a warning or fault is present, shut off the turbo and remedy the root cause. When the green light on the side of the turbo pump has changed from blinking to solid, slowly open the turbo valve and close the vacuum bypass valve.

Figure 1: Leybold Turbo pump indicator lights.

Cannabinoid Distilling Procedure 1. Increase the wiper motor speed to run speed according to Table 2 above.

2. When all set point temperatures are achieved and vacuum level reaches approximately 2.0x10-2 Torr or lower, turn on the feed motor to start feeding the sample. As a starting point, set the feed motor speed to 100rpm.

Remove the feed tank stopper.

3. Increase the feed rate while maintaining a vacuum level below 5.0x10-2 Torr, but preferably below 2.0x10-2 Torr.

4. Adjust the feed rate and/or evaporator temperature as necessary to achieve the observed separation.

5. If the residue material is very thick, increase the residue circulator temperature to 140-150°C. 6. If applicable, start the discharge pumps: a. Allow the sight glass to accumulate approximately 300mL of material. b. For systems outfitted with check valves on the outlets of the discharge pumps, no priming is necessary.

Open the valves below the sight glass, if applicable, and turn on the discharge pumps.

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NOTE: If the check valve was left with material inside from a wet shut down, then it may have “frozen open.” Simply heat gun the check valve so the highly viscous material can liquify and the spring in the check valve can close the check valve to create a vacuum seal. c. For systems without check valves: i. Allow the sight glass to fill to approximately 300mL prior to priming the pump. ii. Heat gun any non-jacketed sections containing cold oil from previous runs. iii. Turn on the discharge pump. iv. Plug the end of the gooseneck with a gloved finger. v. Slowly open the valve with the red handle beneath the sight glass. The vacuum will evacuate the air left in the gooseneck and the pump until the pump “catches” and starts to discharge the fluid. d. If a cleaning cycle was not run after terpene stripping and prior to cannabinoid distilling, collect the first 100 to 500mL of distillate and recycle it back into the feed tank. This will allow any mixed oil remaining in the system to be flushed out. e. Adjust the discharge pump feed rate as necessary.

NOTE: The discharge pump will always out-pace the fluid flow coming into the sight glass. The sight glass will appear empty, but as long as there is a constant flow of fluid entering the gears of the discharge pump, then the combination of the moving gears lubricated by fluid will create a vacuum seal. f. Allow the discharge pumps to continuously discharge fluid into the preferred collection vessel.

Cannabinoid Distilling Shut Down Procedure 1. When distillation is complete, plug the feed tank with the stopper, then turn off the feed motor.

NOTE: Always plug the feed tank BEFORE the tank empties completely to prevent air from aspirating into the system, damaging the turbo pump.

2. For units fitted with discharge pumps, close the valve under the sight glass, if applicable, and shut off the residue and distillate pumps.

3. Close the turbo valve.

4. Turn off the turbo pump.

NOTE: Do not turn off the main vacuum until the blinking green light on the turbo pump has stopped.

5. Adjust the circulator temperatures according to Table 3 below.

Table 3: Cannabinoid Distilling Shut Down Circulator Temperatures

Circulator Feed Residue Evaporator

Temperature (°C) 50°C 50°C 50°C

Notes

Condenser

25°C

Cold Trap

-50°C

Lowering the condenser circulator temperature will help cool down the evaporator body faster. Additionally, a fan can be pointed at the evaporator body.

Set the cold trap circulator to its lowest allowable temperature set point and run it as cold as possible.

6. When the blinking green light on the turbo pump has stopped, shut off the vacuum pump.

7. When the evaporator temperature drops below 100°C, turn off the wiper motor and all circulators.

8. Continue on to a cleaning run, if necessary. The cleaning procedure can be found in the reference document 52001 KD-6 Cleaning.

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Disclaimer Consult the acceptability of the above procedure against local codes. The customer takes part in the above outlined procedure at their own risk. Chemtech Services, Inc. assumes no liability for any damage to or loss of property.

Revision History Revision 0

Date April 21, 2022

Changes Initial Release

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