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Recovering Solvent When Making Oil

FeloniousPunk

Well-Known Member
Hi All,

Here in Canada, solvents are hard to come by. My preference is food grade ethyl alcohol.

It is very expensive up here, if you can get it. A friend priced a 40 ounce bottle of Alcool at $97. That is probably the high end, I have seen the same stuff in other parts of the country for $65. Even at $20 a litre, a case (16L) would run you $320. That's a LOT of money for something I'm just going to evaporate off.

So here is my question, are there any good alcohol recovery systems? I am waiting to hear back from the government about a permit to purchase, so this is still in the research stage.

Any thoughts or experiences would be greatly appreciated.

FP. :peace:
 

Old Salt

Member of the Month: Apr 2019
A distiller will allow you to do this. I'd use a pressure cooker as my kettle, with a condenser replacing the pressure control weight. If you want to produce your own ethanol, use a reflux column.

A rosin press will allow you to perform extractions without the recurrent cost of alcohol. Supplies for the press cost about $2 / oz.
 

Bush Doctor 77

Well-Known Member
Get stove top still. That's what I use. I use IPA for extraction, and recover my solvent with a still. What surprised me: you can't get the gas temp in the still above the boiling point of your solvent, no matter how high you turn up the heat, and when the IPA has all been evaporated off, the gas temp in the still will drop, and you will start to get a strong marijuana smell. I then decarb the extract in an oven @ 220F.
 

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Old Salt

Member of the Month: Apr 2019
Get stove top still. That's what I use. I use IPA for extraction, and recover my solvent with a still. What surprised me: you can't get the gas temp in the still above the boiling point of your solvent, no matter how high you turn up the heat, and when the IPA has all been evaporated off, the gas temp in the still will drop, and you will start to get a strong marijuana smell. I then decarb the extract in an oven @ 220F.
That will do it. Brewhaus America also sells stills. When you get down to 2-3 cups, pour the remainder in a pyrex dish. put about 10-12 mm of cooking oil in the bottom of the kettle and finish the distillation. The oil serves to transfer the heat to the pyrex dish.
 

Bush Doctor 77

Well-Known Member
That will do it. Brewhaus America also sells stills. When you get down to 2-3 cups, pour the remainder in a pyrex dish. put about 10-12 mm of cooking oil in the bottom of the kettle and finish the distillation. The oil serves to transfer the heat to the pyrex dish.
I don't use any oil. When the IPA is totally gone, temp drops in the top of the still, and it starts smoking(the process is fairly odorless until this point), I pour it into a Pyrex dish, and it goes into the oven @ 220F. I stir it as long as it bubbles, and when the bubbles stop, it is decarbed. You can use it on joints, in coffee, vaping, drop on your tongue, cooking just like that, or add it to your oil, if you like. My next extraction, I will refreeze the extract for 2 days after extraction to solidify some waxes. I will then vacuum filter it to try to remove that wax. Then to the still, and decarb.
 

FeloniousPunk

Well-Known Member
I don't use any oil. When the IPA is totally gone, temp drops in the top of the still, and it starts smoking(the process is fairly odorless until this point), I pour it into a Pyrex dish, and it goes into the oven @ 220F. I stir it as long as it bubbles, and when the bubbles stop, it is decarbed. You can use it on joints, in coffee, vaping, drop on your tongue, cooking just like that, or add it to your oil, if you like. My next extraction, I will refreeze the extract for 2 days after extraction to solidify some waxes. I will then vacuum filter it to try to remove that wax. Then to the still, and decarb.
Hi Bush Doctor 77,

I believe the bubbles you see in the oven is the last of the alcohol boiling off. The oil isn't pure until all the bubbles are gone. I use ethyl alcohol so that if there is any alcohol I didn't get out it is safe to consume.

There is no visible way to tell when the decarb is complete.

FP. :peace:
 

FeloniousPunk

Well-Known Member
A distiller will allow you to do this. I'd use a pressure cooker as my kettle, with a condenser replacing the pressure control weight. If you want to produce your own ethanol, use a reflux column.

A rosin press will allow you to perform extractions without the recurrent cost of alcohol. Supplies for the press cost about $2 / oz.
Hi Old Salt,

I know very little about rosin presses. My uneducated opinion is that distilling with alcohol if more efficient. Is this true? I know that solvents return about 10 to 15%. So an ounce of bud should return 3 to 4.5 grams of oil. Are resin presses as efficient?

FP. :peace:
 

Bush Doctor 77

Well-Known Member
Hi Bush Doctor 77,

I believe the bubbles you see in the oven is the last of the alcohol boiling off. The oil isn't pure until all the bubbles are gone. I use ethyl alcohol so that if there is any alcohol I didn't get out it is safe to consume.

There is no visible way to tell when the decarb is complete.

FP. :peace:
The alcohol is gone when the temperature in the vessel drops, because there are no more vapors(alcohol steam). The bubbles from decarb are carbon dioxide that comes off 40-50 degrees F above the boiling point of alcohol. It's like you can't have liquid water above 212F at sea level. By definition, when no more CO2(bubbles) are coming off, it's decarbed.
 

Old Salt

Member of the Month: Apr 2019
Hi Old Salt,

I know very little about rosin presses. My uneducated opinion is that distilling with alcohol if more efficient. Is this true? I know that solvents return about 10 to 15%. So an ounce of bud should return 3 to 4.5 grams of oil. Are resin presses as efficient?

FP. :peace:
Just like solvents, your yield is dependent on the quality of your source material. My last press of 105 gm (3.75oz) Crown Royale yielded 14.79 gm of rosin for a yield of 14.1%. I have had presses over 18%. My lowest yield of 7.9% was with Nightingale. Others in Gandpa Tokin's rosin thread routinely get over 20% with different strains.

Timewise,it took 2 hours to press, about 2hrs to collect the rosin from the parchment, and 2 hrs to decarb, mix with oil and put into capsules.


Rosin Press and Tools


These Were my Worst Results


Making Rosin Capsules
 

FeloniousPunk

Well-Known Member
The alcohol is gone when the temperature in the vessel drops, because there are no more vapors(alcohol steam). The bubbles from decarb are carbon dioxide that comes off 40-50 degrees F above the boiling point of alcohol. It's like you can't have liquid water above 212F at sea level. By definition, when no more CO2(bubbles) are coming off, it's decarbed.
Hi Bush Doctor 77,

Thank you for the explanation. I still don't get how the CO2 bubbles relate to dropping the acid atom (THCA to THC).

FP. :peace:
 

Bush Doctor 77

Well-Known Member
Hi Bush Doctor 77,

Thank you for the explanation. I still don't get how the CO2 bubbles relate to dropping the acid atom (THCA to THC).

FP. :peace:
"Scientifically speaking, Decarboxylation is a chemical reaction that removes a carboxyl group and releases carbon dioxide (CO2)." That's where the bubbles come from.
 

The Bard

Well-Known Member
Hey there!

Fellow Canadian here, going through the exact same process. @Old Salt has been a huge help, and as I write this, I am making my own high-proof alcohol solvent. I purchased a water distiller from amazon Canada, and am currently running regular vodka through it. The nice feature on the distiller I got is that it also has a thermostat on it. I have it set at 180F as Old Salt suggested. The distiller cycles on and off to hold that temp, and uses air-cooling fans to condense the alcohol fumes.

I started with a bit over 2 liters of vodka, and have reclaimed about 600 mL. The hydrometer I got is showing 80-85% alcohol, or 160-170 proof, which I am pretty happy with. The rest of the starting liquid is in the base of the still, and is showing less than 15% alcohol remaining, so I am getting near the end of the process.

I will be freezing the alcohol and the cannabis (I already decarbed it). Tomorrow I will mix the two and freeze again for a few minutes. Shake and strain. I'll then distill the infused alcohol again, and try to recover most of it. The leftover "oil" from the cannabis will remain in the bottom of the distiller, and I'll evaporate the remainder of the water/alcohol off. It is actually kind of fun, safe, and I feel a lot better than using ISO.

A big thank you to @Old Salt for all the advice he gave me a couple of weeks ago.
 

Bush Doctor 77

Well-Known Member
Hey there!

Fellow Canadian here, going through the exact same process. @Old Salt has been a huge help, and as I write this, I am making my own high-proof alcohol solvent. I purchased a water distiller from amazon Canada, and am currently running regular vodka through it. The nice feature on the distiller I got is that it also has a thermostat on it. I have it set at 180F as Old Salt suggested. The distiller cycles on and off to hold that temp, and uses air-cooling fans to condense the alcohol fumes.

I started with a bit over 2 liters of vodka, and have reclaimed about 600 mL. The hydrometer I got is showing 80-85% alcohol, or 160-170 proof, which I am pretty happy with. The rest of the starting liquid is in the base of the still, and is showing less than 15% alcohol remaining, so I am getting near the end of the process.

I will be freezing the alcohol and the cannabis (I already decarbed it). Tomorrow I will mix the two and freeze again for a few minutes. Shake and strain. I'll then distill the infused alcohol again, and try to recover most of it. The leftover "oil" from the cannabis will remain in the bottom of the distiller, and I'll evaporate the remainder of the water/alcohol off. It is actually kind of fun, safe, and I feel a lot better than using ISO.

A big thank you to @Old Salt for all the advice he gave me a couple of weeks ago.
Why is it better than using IPA? Why decarb before extraction? Read about Rick Simpson Oil. Mr. Simpson pretty much settled on using IPA for his process, as far as I can find out. BTW, as I understand it, ethyl alcohol has an affinity for water, and the presence of any water(it will pull H2O from the air)in the extraction process with increase chlorophyll in your final product, which is not desirable. When all your alcohol is gone from your still, the temperature in the space above the residue(water) left in the still will drop below 180F, as there will be no more alcohol left to produce vapor. After some time, if left on the heat source, it will slowly rise to 212F, and never above, until all your water is gone. While you run the still, as long as there is any alcohol left in the still, you cannot raise the temp in the top of the still above 180F. Just as the temp in the top of the still can't go above the boiling point of water as long as there is steam present, it can't go above 180F if there is alcohol steam present. That's why I know that when it goes into the oven for decarb at 220-230, it is impossible for any IPA to be present. It could never go above 180F, if it were. Try to raise the boiling point of water above 212F. Can't.

This all assumes sea level, in an open system. Phase changes(ice>water>steam) have basically two controls. temperature and pressure.
 
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Old Salt

Member of the Month: Apr 2019
IPA or IsoPropyl Alcohol or isopropanol is hygroscopic, just like ethanol. The reason Rick Simpson used naptha and alcohols other than ethanol was due to ethanol at a high enough concentration is not available to the public here in Nova Scotia. The closest you can get is 151 proof rum (75% ethanol) at $1.00/oz. Naptha and most alcohols other than ethanol are poisonous and were used by Rick Simpson as a last resort. He was very careful to fully evaporate whatever he was using as a solvent at the time.

I'm in Nova Scotia, less than 100 miles from where Rick originally made his RSO.
 

Bush Doctor 77

Well-Known Member
Ethyl alcohol is also a poison.
He was very careful to fully evaporate whatever he was using as a solvent at the time.

I'm in Nova Scotia, less than 100 miles from where Rick originally made his RSO.
Must be a challenge to grow there. Can't be more careful than raising it above 180F. Can't be any IPA left at 220-230F, as IPA undergoes a phase change at 180F and becomes vapor. If you're concerned about residual alcohol of any type, put a flame to it. Ethyl alcohol is also toxic.
 

Old Salt

Member of the Month: Apr 2019
Ethyl alcohol is also a poison.
True, but it's also the alcohol many of us drink. LD50 = 8.5gm/Kg

Methanol is much worse. The Chief Bosun's Mate on my first ship went camping with two of his friends. They accidentally drank methanol. One of his friends died, the other was blinded, and the Chief is now called Wiggy, as he lost ALL of his hair. LD50 = 1.187gm/Kg

I haven't heard of what isopropanol does to you, probably because it's either too dangerous, or doesn't get you drunk. LD50 = 3.6 gm/kg

Naptha will kill you. LD50 varies with composition. The cyclohexane component has an LD50 of 0.6gm/Kg

If I were to use a liquid solvent, it would be ethanol. Its effects are known to most adults, and is relatively safe. It's also not too difficult to make your own. Been there, done that, got the t-shirt.

Pressing rosin is much safer than any of the solvents above.
 

The Bard

Well-Known Member
Why is it better than using IPA? Why decarb before extraction? Read about Rick Simpson Oil. Mr. Simpson pretty much settled on using IPA for his process, as far as I can find out. BTW, as I understand it, ethyl alcohol has an affinity for water, and the presence of any water(it will pull H2O from the air)in the extraction process with increase chlorophyll in your final product, which is not desirable. When all your alcohol is gone from your still, the temperature in the space above the residue(water) left in the still will drop below 180F, as there will be no more alcohol left to produce vapor. After some time, if left on the heat source, it will slowly rise to 212F, and never above, until all your water is gone. While you run the still, as long as there is any alcohol left in the still, you cannot raise the temp in the top of the still above 180F. Just as the temp in the top of the still can't go above the boiling point of water as long as there is steam present, it can't go above 180F if there is alcohol steam present. That's why I know that when it goes into the oven for decarb at 220-230, it is impossible for any IPA to be present. It could never go above 180F, if it were. Try to raise the boiling point of water above 212F. Can't.

This all assumes sea level, in an open system. Phase changes(ice>water>steam) have basically two controls. temperature and pressure.
@Old Salt has already eloquently answered a number of your questions. I'll just add a couple of comments, starting with the fact that I am definitely no expert or experienced with the process. I am in the midst of my first attempt at an alcohol extraction.

Since I am ultimately going through this process to make meds for Mrs. Bard, it seems counter-intuitive to me to use a toxic material if it can be avoided. Yes, I understand that the toxicity can be reduced and even eliminated through complete evaporation/distillation. However, I have also read anecdotal feedback from members here who have had their oil tested, and found traces of ISO/IPA remaining. So let's just say that it is a personal choice on my part not to use a poisonous ingredient in my recipe. If that sounds a bit irrational, so be it.

Yes chlorophyll and other undesirable elements of the plant are water-soluble. This is why I am trying to reduce the amount of water in the solvent as much as possible, through "pre-distillation" to increase the proof-level. The easier/more elegant solution would be to use Everclear (190 proof, 95% alcohol, only 5% water) but it is not available in Canada. So I am trying to "make my own" Everclear.

In addition, by freezing both the buds and the alcohol before mixing, my understanding is that locks up the water-soluble elements in ice within the plant. If there is very little water in liquid form, the chlorophyll should be immobile, and removed with the spent buds during filtration.

I decarb before the infusion stage because the temperature and duration of the subsequent distillation/purification step is insufficient to complete the decarb process. I decarb sous vide, both for odour control and temperature stability.

Finally, I like the thermostat feature on the distiller that I got. By setting it to 180F (just a bit higher than the boiling point of alcohol), basically I am getting a pretty pure alcohol distillate, leaving most of the water behind. By the time I finished my DIY Everyclear yesterday, the distillate was 86% alcohol, according to my hydrometer. The leftover water was about 10-15% alcohol. So I think I got most of the good stuff. Basically, at 180F, when the still stopped producing any output, I knew that most of the alcohol had been extracted, with relatively little water vapour along the way.

As I mentioned, I don't have much experience with this process (I have been using infused olive or coconut oil previously), but the ideas above emerged as I was doing my research.

Any comments or corrections to what I have shared would be great!

Thanks.
 

Bush Doctor 77

Well-Known Member
True, but it's also the alcohol many of us drink. LD50 = 8.5gm/Kg

Methanol is much worse. The Chief Bosun's Mate on my first ship went camping with two of his friends. They accidentally drank methanol. One of his friends died, the other was blinded, and the Chief is now called Wiggy, as he lost ALL of his hair. LD50 = 1.187gm/Kg

I haven't heard of what isopropanol does to you, probably because it's either too dangerous, or doesn't get you drunk. LD50 = 3.6 gm/kg

Naptha will kill you. LD50 varies with composition. The cyclohexane component has an LD50 of 0.6gm/Kg

If I were to use a liquid solvent, it would be ethanol. Its effects are known to most adults, and is relatively safe. It's also not too difficult to make your own. Been there, done that, got the t-shirt.

Pressing rosin is much safer than any of the solvents above.
Pressing rosin leaves you with a product that still has to be decarbed, to get full potential. Fine if you smoke it, but less than optimum for edibles in it's raw stage.
 
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