(Chem) Adding water to Ethanol Extract at end of distillation.

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OGCraiggles

OGCraiggles

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So. I am a rookie at this, I soaked material that was fresh fresh. So after distilling most of it I have water and oil.


If I had a 190 proof ethanol solution and distilled 95% of it off and added say 400 ml of water to 100 ml of my ethanol solution. Would the massive dilution of the ethanol force the oil out of solution and then allow me to use a separatory funnel to drain off the water/alcohol solution? Or would it still be bound to the ethanol solution even if diluted 5:1 with water:ethanol thus leaving me with a big headache?
 
tobh

tobh

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The relevant compounds are captured by the alcohol at this point. You won't separate them without evaporation, preferably under vacuum.
 
OGCraiggles

OGCraiggles

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So. What I can do is add a little bit of water so that when I boil off all the alcohol and, I wont immediately start to burn the extract and can just use my funnel to drain off the water. Correct?

I have a problem with regulating temp with my setup, so its hard to perfectly tell when I cross the threshold.
 
detroitjoe

detroitjoe

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You have a problem regulating temps?

Don't blow up your parents house.
They worked hard for it
 
tobh

tobh

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So. What I can do is add a little bit of water so that when I boil off all the alcohol and, I wont immediately start to burn the extract and can just use my funnel to drain off the water. Correct?

I have a problem with regulating temp with my setup, so its hard to perfectly tell when I cross the threshold.
i don't quite understand your setup. I've assuming you have a full vacuum distillation lab setup. Further I don't understand your end goals. What are you trying to achieve?

The oils you've extracted from the plant material become incredibly viscous in alcohol (any solvent -- they're weak oils). What are you trying to gain from adding water?

I suspect you're trying to make RSO, in which case you distill down to a thick viscous point, and it's done.
 
Eskander

Eskander

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This sounds like a hot plate boil off job not an evaporator.

You ultimately want oil that is free of water and ethanol right? You pretty much just need to heat it to a boil it until the bubbles stop. Put a thermometer in there and don’t let it get above 100C if you just want to dry it. Take it up a bit higher to decarb it if you want.

As joe says, don’t blow yourself up. You are boiling a flabable liquid which means you have fuel, oxygen and a heat source in the same place. No open flames and aggressive ventilation are required to do this safely.

-Eskander
 
OLDSILVERTIP

OLDSILVERTIP

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This sounds like a hot plate boil off job not an evaporator.

You ultimately want oil that is free of water and ethanol right? You pretty much just need to heat it to a boil it until the bubbles stop. Put a thermometer in there and don’t let it get above 100C if you just want to dry it. Take it up a bit higher to decarb it if you want.

As joe says, don’t blow yourself up. You are boiling a flabable liquid which means you have fuel, oxygen and a heat source in the same place. No open flames and aggressive ventilation are required to do this safely.

-Eskander
hot plate outside to be on safe side,if makin RSO ,think of the way shiners do it outside, have ran a few stills back in the day,never in an enclosed space.
 
OGCraiggles

OGCraiggles

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yeah. Hot plate with side arm flask and vinyl tubing. With things legalized in new york this year I had a few people drop a massive amount of their harvest trims and low grade nug on me and I'm slowly building a setup to make carts, What I am currently trying to do is recoup the ethanol even if it is not as efficient as I would like it to be by Routing the tubing into a 1000 ml flask inside an ice bath. Yes I understand the risks. That's not what I'm here for. I was just curious if massive dilution would force apart the bonds between the last bit of alcohol and oil. Mantles are hundreds of dollars so I am not ready to cross that line yet and buy a real distillation setup on top of that. So I am trying to use gear I already had.

I am just reaching the point where I am trying to clean it up and pull out all the chlorophyll using different methods. Doing a small trial batch right now to test the end result considering I am not using hexane to polish. I am having a hard time trying to find it locally. So for now I was just curious about the dilution thing since I could not find anything about it online. I appreciate all of your advice.

But its looking like I'm just going to have to cross the line and buy a vacuum distillation setup and some hexane. Currently trying to polish with the light naphta and salt water method because I pulled a ton of chlorophyll. (I soaked 2 oz in freezer with cold ethanol for 24 hr) and regretting letting it extract that long.
 
Eskander

Eskander

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yeah. Hot plate with side arm flask and vinyl tubing. With things legalized in new york this year I had a few people drop a massive amount of their harvest trims and low grade nug on me and I'm slowly building a setup to make carts, What I am currently trying to do is recoup the ethanol even if it is not as efficient as I would like it to be by Routing the tubing into a 1000 ml flask inside an ice bath. Yes I understand the risks. That's not what I'm here for. I was just curious if massive dilution would force apart the bonds between the last bit of alcohol and oil. Mantles are hundreds of dollars so I am not ready to cross that line yet and buy a real distillation setup on top of that. So I am trying to use gear I already had.

I am just reaching the point where I am trying to clean it up and pull out all the chlorophyll using different methods. Doing a small trial batch right now to test the end result considering I am not using hexane to polish. I am having a hard time trying to find it locally. So for now I was just curious about the dilution thing since I could not find anything about it online. I appreciate all of your advice.

But its looking like I'm just going to have to cross the line and buy a vacuum distillation setup and some hexane. Currently trying to polish with the light naphta and salt water method because I pulled a ton of chlorophyll. (I soaked 2 oz in freezer with cold ethanol for 24 hr) and regretting letting it extract that long.

So I have just about every piece of gear in my home lab to do extraction with hexane. Understand that I’m talking about a fume containment that vents outside along with a full face respirator in case of splashes. I can do all of my handling and rotovaping in the containment. It is not a solvent to use lightly. You have essentially all the same dangers involved from using butane with additional issues of toxicity and a significantly harder purge.

The one thing I still need to set up is venting pipes for my vacuum pumps so they don’t blow off inside. And yes pumps plural because you need very light vacuum to run filter and recovery but a harder vacuum to do purge. Even with all my ventilation precautions, I’ll still be doing all the open handling at -25F to reduce the vapor pressure and give a better fire safety margin.

I strongly suggest that given where you are in your journey that you stick with QWET and an easy To use recovery tool like the extract craft. You can always sell it if you move onto a rotovap. If you stick with your simple distillation then running vapor through a copper tubing coil with a fan across it will do ok. Particularly outside given the temps this time of year. It will take a long damn time to get your ethanol boiled off though but you will probably get back a decent percentage.

You can dry the ethanol back to 200 proof by adding anhydrous magnesium sulfate until it swirls around like a snow globe and then filtering it out. You can recover the mgso4 by baking it if you feel like. It is cheap though and if you just let the residual ethanol evaporate off, it is jus epsom salt so you can put it on your plants.


You are looking at something with a mantle for heating… You know that a short path distillation is not for solvent recovery right?

-Eskander
 
OGCraiggles

OGCraiggles

4
1
So I have just about every piece of gear in my home lab to do extraction with hexane. Understand that I’m talking about a fume containment that vents outside along with a full face respirator in case of splashes. I can do all of my handling and rotovaping in the containment. It is not a solvent to use lightly. You have essentially all the same dangers involved from using butane with additional issues of toxicity and a significantly harder purge.

The one thing I still need to set up is venting pipes for my vacuum pumps so they don’t blow off inside. And yes pumps plural because you need very light vacuum to run filter and recovery but a harder vacuum to do purge. Even with all my ventilation precautions, I’ll still be doing all the open handling at -25F to reduce the vapor pressure and give a better fire safety margin.

I strongly suggest that given where you are in your journey that you stick with QWET and an easy To use recovery tool like the extract craft. You can always sell it if you move onto a rotovap. If you stick with your simple distillation then running vapor through a copper tubing coil with a fan across it will do ok. Particularly outside given the temps this time of year. It will take a long damn time to get your ethanol boiled off though but you will probably get back a decent percentage.

You can dry the ethanol back to 200 proof by adding anhydrous magnesium sulfate until it swirls around like a snow globe and then filtering it out. You can recover the mgso4 by baking it if you feel like. It is cheap though and if you just let the residual ethanol evaporate off, it is jus epsom salt so you can put it on your plants.


You are looking at something with a mantle for heating… You know that a short path distillation is not for solvent recovery right?

-Eskander
Wish I had the education you have on this matter. Chem's always been a passion but never offered 15 years ago when I was in school. I am sold on that piece of EQ but for $600, in your opinion, couldn't I build a distillation setup with a mantle for half of that price? Do you have any resources I can read about doing this? I tend to over research things and I'm having problems making a decision a source of glassware that is bang4buck since there are so many options out there. I was even looking on purchasing through alibaba. This is $100 for a 1000 / 500ml and I have a $500 lab vac pump. I'd just need the mantle and more stands.

Please tell me if I'm incorrect on this.
 
Lab
Eskander

Eskander

116
43
Wish I had the education you have on this matter. Chem's always been a passion but never offered 15 years ago when I was in school. I am sold on that piece of EQ but for $600, in your opinion, couldn't I build a distillation setup with a mantle for half of that price? Do you have any resources I can read about doing this? I tend to over research things and I'm having problems making a decision a source of glassware that is bang4buck since there are so many options out there. I was even looking on purchasing through alibaba. This is $100 for a 1000 / 500ml and I have a $500 lab vac pump. I'd just need the mantle and more stands.

Please tell me if I'm incorrect on this.
You can certainly do a traditional distillation set up for ethanol recovery. It will be slower for sure but with a magnetic stirrer/hotplate you might see decent rates of recovery.

What you show is for refluxing which really has no place in what we are doing. It is for separating things with very similar boiling points and we don't have that issue. Plus if you used that with any real vacuum you would loose a lot of ethanol out the vacuum pump because the vapor cooling capacity of the water jacket just isn't high enough. Where you see people using systems that look like kinda this with a mantle, it is short path distillation and that is not for solvent recovery, it is for refining decarbed oil into a pure THC isolate.

https://www.amazon.com/VEVOR-Distillation-Apparatus-Max-450°CShort-Glassware/dp/B07LG18MR4/ref=sr_1_3?crid=3OO6CK29UBZ35&keywords=short+path+distillation+kit&qid=1651235563&sprefix=short+path+distillation+kit%2Caps%2C46&sr=8-3

-Eskander
 

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