Was curious if anyone else is using heptane with TiBA in their conversion method? My collogues and I have been at it for around 10-11 months and are having some success, but still having issues with moisture creating D8 at up to 8% in our final product. Also with that, our D9 has never been above 85%… usually total THC is at roughly 88-92%
We have tried drying our solvent with molecular sieves as well as magnesium sulfate but still seeing smoke when introducing the catalyst inside the reactor when it makes contact with the heptane and CBD solution.
We clean the reactor, with heptane, seal it properly, then run it under vacuum for at least 8 hours.
We have tried three methods of adding the CBD to the reactor.
Melting the CBD, opening a port on the reactor and pouring it inside.
-Our thought process here is melting the CBD would take out any of the moisture content inside, if there is any there. But we also realize that breaking the seal of the dried reactor and pouring it in there is not the best of ideas
Melt the CBD, and pour it into the reactor, seal it up, and leave it under vacuum for 8 hours.
The thought here is the same with melting the CBD and hoping to bake out any moisture in it. The problem here, is as soon as its in the cold reactor, it crystalized and took a long time for the CBD to dissolve into the solvent the next workday.
Add the CBD Isolate into the reactor, seal it up, and leave it under vacuum for 8 hours.
We did this hoping that if there was any moisture in the CBD, the vacuum would be able to draw it out.
We do realize with the last two methods, we should add the CBD , but also turn on our temperature controller, and set it to a temp, below the vaporizing point of CBD, to hopefully pull the moisture out as well.
We do observe the D8 forming around hours 5-6 in the reaction while there is still CBD. CBD is usually fully converted by hour 10.
So sorry for the confusion, we are using vacuum to help dry the system to make sure no moisture gets in. Before we start the process, we turn the vacuum off and flood the system with inert gas, creating pressure up to 4PSI. We have a bubbler going to insure we always have positive pressure in the reactor while running the reaction.
We have SP 43C and the reaction temp is usually at ~45C.
To neutralize we quench in this method and order
IPA
Glacial Acetic Acid (3:1 Mol Tiba)
H2O saturated by Sodium Bicarbonate
PH Neutral Water, for as many times until the solution coming out, is the same PH going in, plus no more smell of IPA.
I recommend dissolving your CBD in heptane prior to the reaction. You can then dry that solution and sparge it. 4a zeolite works well for the drying process.
Also it should be pointed out that when you dry a solution of CBD in Heptane with Zeolite or any other drying agent you will invariably leave a small fraction of a percent of water in your solution. Feel free to dry your solution and then dry it again with a fresh batch of drying agent. With ennough successive applications of an appropriate drying agent you will remove almost all of the latent humidity thats causing your d8 production.
We did dissolve CBD into our heptane, but when adding it into our vessel while adding the drying agent, the CBD crashed out inside the vessel after sitting for 24hours.
Do you have a suggestion on how to dissolve the CBD into heptane, so it wont crash out? We currently run a 3:1 Heptane:CBD.
We are introducing TiBA through a 16g 36" cannula needle via positive pressure at around 4PSI. But at the same time, heptane vapor is pushing against the other end of the Cannula, from the reactor
We have added the TiBA in 4 aliquots and we have added all the TiBA in one large aliquot and neither of those have produced different results.
So far @ennui remarks make most sense cbd issolate is wet and needs to be dried drying dissolved in a solvent is best personally don t like molsieves for the job and prefure dehydration salts
As for solvent cbd ratio I run 1:5 minimum 1:8 max
Administration of tiba I do slowely with a knf lab pump takes in total about 2 hours
Molsieves I place occasionally in the reaction vessel and still not convinced it makes sense
The accitic acid quench on ipa is comon
Althoug as additional wash I use
Hydrogenperoxide 30%
Your 8 appears either deu to wet conditions or /and a imperfect quench
Before and after distillation can give proof of your quench if your vacuum is deep
We currently use a GC to test our results periodically throughout the run, and the GC shows D8 while the conversion is happening. So its safe to say that our 8 is pre-quench during the reaction.
Do you think there is a better dehydration salt than Mag Sulf?
The Mini Dia pump from KNF? or which one do you use if you don’t mind me asking.
Also, the Hydrogenperoxide, is 30% solution or are we adding 1mol of Hydrogenperoxide to 1mol of tiba.
We have thought about this, but we have no means of adding heat to our drying vessel. Is there a good system for this? Otherwise we would have to use our primary reactor, but how do we then separate the dehydration salt before use?
Inert gas should be running thru a dri rite tube so gas is bone dry. When you dry your reactor under vacuum your jacket should be at least at 90C. The vacuum should not be static, you should have a slight bleed of dry inert gas sweeping the reactor…that mass transfer will whisk moisture from your glass into your pump. Much more effective than a static vacuum with no bleed. When done drying, you need to cool down the jacket with dry inert gas flowing.
We do run our inert gas through a column of mol sieves, then through a dri rite column into the reactor.
That is a good idea to run heat, while the vacuum is running and having gas sweep the reactor. We will implement that on our next run. Thank You very much.
A other detail
Pulling vacuum on vessels is great
IF THEY DO NOT LEAK
Especially the bottom drain when pulling from the top
For if they do leak all you are doing is pulling treu a humid air stream refreshed by the minute
Reason I like working with argon overpressure and heat on the jacket
Since my botom drain on the janky chineese glass reactor leaks under vacuum not for liquids thou then it s fine
If your CBD is crashing out after 24 hours in the vessel with your drying agent then you will either need to dillute your solution more or remove your solution from the vessel prior to the crash.
Have you been sparging your CBD solution prior to the reaction?