You can heat to make pressure, be careful about how much solvent you are letting go.The goal is to modify the solubility slowly. The Best way I have found is thermocycling in a pressure reactor. I do this for bulk crystal production.
12 Likes
How much solvent I am letting go? Meaning how much I evaporate off before putting in a vessel? I put it in pretty liquidy where you can still pour with minimal sticking to the side of the vessel. I sealed it and threw it on heat to build pressure. I am currently still heating and at about 60psi. It had been on the heat over night. Should I be moving it into the freezer now?? Or taking off heat and leaving room temp?
The amount of solvent is related to how much material you wish to crystallize.Start with an excess of solvent, remove it until your solution is super saturated. I recrystalize from pentane, I usually set my controller to cool to 0c then ramp up to 20c, burp, then re -cycle . You are watching for crystals to crash on the cold side of the swing, then melt on the hot side. This cycles the solution to the optimal saturation. This method allows for large crystals to be formed due to the fact that all the small crystals will go back into solution while the large ones will remain as seeds.
33 Likes
Ohh I see so itās a cycle of cooling and heating, repeat etcā¦ getting to 0c then to 20c and then repeating? How long do you stay at temperature intervals while cycling?
4 Likes
About an hour each way.
11 Likes
Thank you for your help I will post reaults ASAP! So I assume temps are more important than pressure when growing? Or a combination of both? If you added nitrogen or co2 what pressures are you looking to achieve when crashing diamonds
1 Like
How do you go about purging the pentane out after recrystallization?
1 Like
The shape of the Isobutane molecule makes it harder to release its bond tho?
Is there a need to fuss with the ramping speed of the chiller/heater in this model? 0Ā°-20Ā° at what ever pace the heater pushes? And by ācold sideā do you mean the top vs the bottom where the fluid enters the jacket?
1 Like
Crush the crystals, vac oven. The crystals will get wet looking and begin to melt. Thatās where I stop. Hold under hard vacuum and sweep with argon. Let cool under hard vaccum.
3 Likes
The reactor cycles from 0c to 20c in 60 min in a slow gradient. Pressure is then lowered by a few psi. The gradient now goes 20c back to 0c in 60 min. The cycle is repeated until your satisfyed with the results.
6 Likes
Im curently running the tek and im halfway trough the 72hr crashing process in dry ice /iso bath and i was wondering when is the right time and how much solvent should i leave in the jars for optimal result. I see thca blooming everywhere in the jars .i have 6x 250 ml mason jars filled to the brim 48hr before now its at 3/4, used 1/10 ratio to 3 half pound of material so 500ml of mother liqor per 1/2
So i donāt need a blast proof freezer ?
Iāve been able to achieve that as you explain. With a thick layer of Terps that seems as it is very wax/fat infested to make it that thick.
1 Like
what did you do with the fatty terp layer? I would assume it wouldnāt be the best for consumption at that point, however might just be like dabbing non-waxed extracts
Iām curious about the final step as well. So once the terp fraction is done purging in the oven, you then take the frozen thca jar, pour the warm purged terp fraction in the frozen thca jar, than place back in the oven and pull a vacuum? For how long and to what psi? Can you elaborate on this final phase please.
1 Like
From what I understand you place the jar in the freezer with the solvent in it right out of the honey pot. Correct me if I am wrong but the white layer that forms in the freezer are fats and waxes. The point of this is to further refine you solution to help the thca crash out easier. The actual thca formation occurs when you do the heating and cooling process once it is in a sealed jar or pressure vessel.
*this info could be wrong as I am still in the beginning process of this tek. Will update once I have completed my trial run.
2 Likes
The white layer at the bottom are thca blooms forming not fats and waxes. That is the crashing phase youāre talking about. Read the directions thoroughly and you will see what Iām referring to. 
5 Likes
Iām in Phx,AZ. 1086 elevation.
1 Like
Ok then how long do we keep the THC portion in the fridge, I was curious about same part but this didnāt answer the part we confused about is when to put that in freezer or what to do with while terp in oven