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ethanol extraction and stability

HWY36

Member
Is it possible to have a stable, shatter like product using an ethanol extraction or will it always be somewhat sappy?

I've been researching c-bleach. Is there an application where for it where the final product is stable? Seems the high temps required would leave me with an unstable product. Is there a way to use it with lower temps?

Regards all
 

WaterFarmFan

Active member
Veteran
Is it possible to have a stable, shatter like product using an ethanol extraction or will it always be somewhat sappy?

Not sure on the other, but you absolutely can make hard shatter using ethanol. You will need to use vacuum purging to get this consistency, as applying heat with a double boiler will cause decarbing, which will produce a runnier product. If you starting material is older it could already have decarbed with time, and if that is the case, it will be a bit sappy even with vaccuum purge.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Is it possible to have a stable, shatter like product using an ethanol extraction or will it always be somewhat sappy?

I've been researching c-bleach. Is there an application where for it where the final product is stable? Seems the high temps required would leave me with an unstable product. Is there a way to use it with lower temps?

Regards all

You can make ethanol shatter.

Recover using vacuum at low temperatures.
 

coldcanna

Active member
Veteran
Low temps for the win. Our lab was having problems with everything going to sap, lowered the recovery temps and shit is like glass now.
 

HWY36

Member
Low temps for the win. Our lab was having problems with everything going to sap, lowered the recovery temps and shit is like glass now.

How low? I guess recovering (or evaporating) ethanol at low temps under vac would be no problem. My concern is that using c-bleach, it either won't filter properly or work at all at lower temps. The instructions say to heat to 176F.

BTW, love the quotes
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
GW, if I used c-beads or magSil in a BHO column would it give me a lighter colored product?

I haven't tried that, but I predict not.

Any of ya'll other readers have any experience with that?
 

AK Extracts

New member
Low temps for the win. Our lab was having problems with everything going to sap, lowered the recovery temps and shit is like glass now.

I'm having the same issue with sappy attempts at shatter. I'm extracting at -45C, cold filtering, and recovering at 38C under full vacuum. With a few attempts in the Cascade vacuum oven, I'm usually getting sappy sometimes partially crystallized gunk. What recovery temp would you recommend for my roto water bath? Any other pointers? Much appreciated.
 

WaterFarmFan

Active member
Veteran
I'm having the same issue with sappy attempts at shatter. I'm extracting at -45C, cold filtering, and recovering at 38C under full vacuum. With a few attempts in the Cascade vacuum oven, I'm usually getting sappy sometimes partially crystallized gunk. What recovery temp would you recommend for my roto water bath? Any other pointers? Much appreciated.

Just curious. What is the consistency of your extract when taken from the rotovap? Thin or thick syrup? What temps on your vacuum oven?
 

AK Extracts

New member
Just curious. What is the consistency of your extract when taken from the rotovap? Thin or thick syrup? What temps on your vacuum oven?

The consistency is thick, I'd compare it to room temperature honey or slightly thinner as it does move. To get it out of the collection bulb we put a heat blanket on the glass and let it drip out overnight.

We've tried a few different temp regimes, as low as 85F (stepping up to 95F) for 5 days and as high as 120F for 3 days. We've only done 4 runs through the oven, so we are just getting started, but are more or less stumbling around in the dark it seems. One run it muffined and we made something resembling honeycomb, that didn't end up being very stable and was somewhat sticky. The other 3 runs we got some extremely sticky crystallized sap that was a medium amber. Any suggestions would be welcome, thanks.
 

Thcvhunter

Well-known member
Veteran
Ive been wondering this for a while.
Thanks for clearing that up.

Good to see ya posting Grey Wolf
 

WaterFarmFan

Active member
Veteran
The consistency is thick, I'd compare it to room temperature honey or slightly thinner as it does move. To get it out of the collection bulb we put a heat blanket on the glass and let it drip out overnight.

We've tried a few different temp regimes, as low as 85F (stepping up to 95F) for 5 days and as high as 120F for 3 days. We've only done 4 runs through the oven, so we are just getting started, but are more or less stumbling around in the dark it seems. One run it muffined and we made something resembling honeycomb, that didn't end up being very stable and was somewhat sticky. The other 3 runs we got some extremely sticky crystallized sap that was a medium amber. Any suggestions would be welcome, thanks.

I think that it is difficult to gauge how long to keep extract in your distillation apparatus. Too long and it is difficult to remove and too little and it is very messy to purge. Those oven purge times are WAY too long IMHO. The deeper the vacuum and quicker that you get to 120F to 125F, the shorter your purge time will be.

Are you stirring or mixing your slabs in the oven? If so, then this can be causing your extract to wax up. Also, how old is the material that you are running? Is it certified free of any pesticides?
 

AK Extracts

New member
You can make ethanol shatter.

Recover using vacuum at low temperatures.

Hi Gray Wolf. How low would you recommend? We are recovering at 38C currently. Should I be recovering all (or as close to all as I can get it) of the ethanol in the rotovap and getting a thick oil, or am I better off leaving a little bit of ethanol in there when making shatter. Any ethanol remaining will be purged off in the vacuum oven of course. Thanks
 

AK Extracts

New member
I think that it is difficult to gauge how long to keep extract in your distillation apparatus. Too long and it is difficult to remove and too little and it is very messy to purge. Those oven purge times are WAY too long IMHO. The deeper the vacuum and quicker that you get to 120F to 125F, the shorter your purge time will be.

Are you stirring or mixing your slabs in the oven? If so, then this can be causing your extract to wax up. Also, how old is the material that you are running? Is it certified free of any pesticides?

I agree that those oven times are way too long and much longer than we anticipated. We just left it in there because nothing was happening and we hoped more time would improve the result, which it did not.

We aren't stirring, we just poured the oil in the trays and checked them everyday hoping they'd harden up.

Yes the material is certified pesticide free and was about a month old (had been stored in a freezer).

Based on what I'm reading, I think perhaps we are too hot in our ethanol recovery (38C) and perhaps we are recovering too much ethanol, thus the very thick oil. Even 20ml of ethanol in a 300gram batch of oil significantly reduces the viscosity. Is there some logic in leaving a little of the ethanol in there when making shatter?

Are you recommending purging at 120-125F and then reducing temps, or keep them about the same? Thanks
 

c03rcion

New member
You can totally make shatter/glass with ethanol extraction. I have made very glass-like shatter that tested on my hplc at 86% thca.

Is your starting material decarbed?

Is your oil getting decarbed somewhere along the process--whats the temperature of your ethanol during extraction, what is the rotovap water bath temp set to?

Purging in the vacuum oven at 38 C is fine.

Is there water in your oil? Is the oil agitated somehow during the purge phase?
 

AK Extracts

New member
You can totally make shatter/glass with ethanol extraction. I have made very glass-like shatter that tested on my hplc at 86% thca.

Is your starting material decarbed?

Is your oil getting decarbed somewhere along the process--whats the temperature of your ethanol during extraction, what is the rotovap water bath temp set to?

Purging in the vacuum oven at 38 C is fine.

Is there water in your oil? Is the oil agitated somehow during the purge phase?

Hi c03rcion, thanks for the reply.

No, the starting material is not decarbed. Our oil commonly tests at 1 or 2% THC and 70-80% THCA indicating we are not decarbing anywhere in the process. After the first few sticky runs we tried decarbing a sample just to see what it would do. The answer: not much.

We are extracting at -45C, so no chance of decarb there. Then it gets cold filtered and straight into the rotovap. The rotovap water bath is 38C, which I'm thinking may be too high. What temp would you recommend?

I don't believe there is any water in our oil, or very, very little.

We don't agitate the oil in the oven, we just poured the oil into trays. It spread out and then just gets stickier and sticker. Do you purge at 38C the entire time, or do you change the temps?

Many thanks
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Hi Gray Wolf. How low would you recommend? We are recovering at 38C currently. Should I be recovering all (or as close to all as I can get it) of the ethanol in the rotovap and getting a thick oil, or am I better off leaving a little bit of ethanol in there when making shatter. Any ethanol remaining will be purged off in the vacuum oven of course. Thanks


Here is our procedure:

PROCEDURE

In this experiment, the rotary evaporator is being used to distill ethanol out of winterized, filtered butane hash oil (BHO).

1. Add 500 ml of BHO/ethanol mixture to the evaporating flask. Note that greater volumes may be appropriate in situations where a larger flask is used but care should be taken as to avoid filling the flask over half full.

2. Lock the flask into place on the rotary valve and lower the unit into the warming bath.

3. Set the temperature of the bath to 25ºC.

4. Set the rotation of the flask at 160 rpm. Note that faster speeds may be achievable in a larger flask but operators noticed that higher rotational speeds in the 1 L flask resulted in excessive bumping.

5. Set the initial vacuum level to 80 mbar to begin the process. Increase the vacuum over the course of the distillation as follows.

a. 0-1 min: Pull down for atmospheric pressure to 80 mbar.

b. 1-5 min: Hold at 80 mbar.

c. 5-10 min: Reduce pressure to 60 mbar, hold. At 10 min, about 50 ml of ethanol should have been reclaimed.

d. 10-15 min: Reduce pressure 40 mbar, hold. At 15 min, about 100 ml of ethanol should have been reclaimed.

e. 15-45 min. Reduce pressure to 20 mbar, hold. Vacuum does not exceed 20 mbar but will remain on constantly at this point. At 45 min, about 450 ml of ethanol should have been reclaimed. Note that it is important to leave some ethanol behind so as to be able to easily remove the remaining material from the evaporation flask.

f. The material is collected, spread on PTFE sheets, and placed in the vacuum oven to complete final purge.

RESULTS

Once a pressure of 20 mbar has been achieved, ethanol is recovered at a rate of 11.6 ml/min. This can vary slightly due to the density of the product ie. Ratio of BHO to ethanol. Faster distillation rates are achievable at higher temperatures but more supervision is required to minimize bumping. Furthermore, qualitative evaluations suggest that higher operational temperatures resulted in a somewhat degraded final product. Cold temperature distillations are possible as well but result in increased distillation time and no noticeable improvement in final product.

The unit is easy to clean and dismantle but it can be difficult to remove all of the material once distillation is complete. This is an issue that all rotary evaporators have however and it should not be held against this piece of equipment in particular. As a result, it is up to the operator to make sure that the consistency of the final product is appropriate for their final purpose.

Manually refilling the collection task is easy but somewhat time consuming as the operator has to take care to bring the vacuum down slowly when starting a new batch. Continuous operation is possible with additional equipment and is most likely the missing piece in terms of integrating this equipment into a production setting.
 

c03rcion

New member
Hi c03rcion, thanks for the reply.

No, the starting material is not decarbed. Our oil commonly tests at 1 or 2% THC and 70-80% THCA indicating we are not decarbing anywhere in the process. After the first few sticky runs we tried decarbing a sample just to see what it would do. The answer: not much.

We are extracting at -45C, so no chance of decarb there. Then it gets cold filtered and straight into the rotovap. The rotovap water bath is 38C, which I'm thinking may be too high. What temp would you recommend?

I don't believe there is any water in our oil, or very, very little.

We don't agitate the oil in the oven, we just poured the oil into trays. It spread out and then just gets stickier and sticker. Do you purge at 38C the entire time, or do you change the temps?

Many thanks

Yes I kept the temperature constant during the oven purge.

Is there water in your ethanol? Has it been recycled many times?
 

AK Extracts

New member
Here is our procedure:

PROCEDURE

In this experiment, the rotary evaporator is being used to distill ethanol out of winterized, filtered butane hash oil (BHO).

1. Add 500 ml of BHO/ethanol mixture to the evaporating flask. Note that greater volumes may be appropriate in situations where a larger flask is used but care should be taken as to avoid filling the flask over half full.

2. Lock the flask into place on the rotary valve and lower the unit into the warming bath.

3. Set the temperature of the bath to 25ºC.

4. Set the rotation of the flask at 160 rpm. Note that faster speeds may be achievable in a larger flask but operators noticed that higher rotational speeds in the 1 L flask resulted in excessive bumping.

5. Set the initial vacuum level to 80 mbar to begin the process. Increase the vacuum over the course of the distillation as follows.

a. 0-1 min: Pull down for atmospheric pressure to 80 mbar.

b. 1-5 min: Hold at 80 mbar.

c. 5-10 min: Reduce pressure to 60 mbar, hold. At 10 min, about 50 ml of ethanol should have been reclaimed.

d. 10-15 min: Reduce pressure 40 mbar, hold. At 15 min, about 100 ml of ethanol should have been reclaimed.

e. 15-45 min. Reduce pressure to 20 mbar, hold. Vacuum does not exceed 20 mbar but will remain on constantly at this point. At 45 min, about 450 ml of ethanol should have been reclaimed. Note that it is important to leave some ethanol behind so as to be able to easily remove the remaining material from the evaporation flask.

f. The material is collected, spread on PTFE sheets, and placed in the vacuum oven to complete final purge.

RESULTS

Once a pressure of 20 mbar has been achieved, ethanol is recovered at a rate of 11.6 ml/min. This can vary slightly due to the density of the product ie. Ratio of BHO to ethanol. Faster distillation rates are achievable at higher temperatures but more supervision is required to minimize bumping. Furthermore, qualitative evaluations suggest that higher operational temperatures resulted in a somewhat degraded final product. Cold temperature distillations are possible as well but result in increased distillation time and no noticeable improvement in final product.

The unit is easy to clean and dismantle but it can be difficult to remove all of the material once distillation is complete. This is an issue that all rotary evaporators have however and it should not be held against this piece of equipment in particular. As a result, it is up to the operator to make sure that the consistency of the final product is appropriate for their final purpose.

Manually refilling the collection task is easy but somewhat time consuming as the operator has to take care to bring the vacuum down slowly when starting a new batch. Continuous operation is possible with additional equipment and is most likely the missing piece in terms of integrating this equipment into a production setting.

Thanks Gray Wolf. We'll try leaving some ethanol in and see how that goes. It would be easier to get out of the bulb and work with that's for sure.

On your vacuum pressures, you mentioned vacuums under 100mbar. We are recovering ethanol under full vacuum, at 700mb up to 760mbar, recovering about 5 liters/hour in a 20 liter system.

The more I read, the more it sounds like our water bath temps were just way too high. We had the bath at 38C and it sounds like around 25C might be the way to go for oil that will become shatter. We aren't getting significant decarboxylation, but it must affect the shatter stability somehow. It could be a number of factors, but it sounds like this is the most likely. Appreciate the feedback. Been following your posts for awhile.
 

AK Extracts

New member
Yes I kept the temperature constant during the oven purge.

Is there water in your ethanol? Has it been recycled many times?

No, we regenerate the ethanol every round and test with a hydrometer. We are at 200 proof.

What do you think about a 38C water bath? It makes for quick evaporation, especially under full vacuum, but I'm reading that it can make ethanol extracted shatter unstable.
 
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