Quick question, When trying to bring the pH of an ethanol mixture up prior to distillation, would adding small amounts of sodium bicarbonate work? Would I need to filter the mixture before rotoing it and putting it in the boiling flask?
Yes iT does but My lack of chemistry doessn t know If i should recomend iT
I do iT but If its wise i don t know
@Photon_noir doesn t recomend iT
So what can i say
In the Degumming tread hè talks about it
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O and Yes i would def_enatly filter afterwords_
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I just responded elsewhere about this. Do NOT adjust pH for no particular reason!
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What if for some reason your eho comes out salty, I’m thinking about tossing it out
The etho salty how so ?
You using etho from tequila sunrise ?
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Idk.it just tastes salty it’s odd. I was thinking about redissolve then carbon filter
How about evaporating it all with a moderate reflux ?
I’m having a similar issue in that I tried degumming and now I’m stuck with a low pH.
- I have roughly 70 gallons of etho solution with a pH.
- Used a 50L reactor and added citric acid in batches to start the degumming reaction.
- While the mixture was still swirling, I unloaded them into a bunch of 5 gallon buckets and waited 24 hours for the gums to sink to the bottom of the buckets.
- Tried to filter a couple of buckets over celite 545 and Magnesol but I noticed that the gums were too fine and would pass through when I added more solution.
- I decided to decant the top of the solution while leaving the gummy sediment at the bottom of the buckets. After taking a sample and adding more citric acid, no gums where swirling and the citric acid would sink to the bottom, leaving me to believe that no gums are present.
- Now all that’s left is finding a good way to neutralize the pH.
Options:
A. Perform a liquid-liquid separation. Not sure how to do this properly, can somebody point me in the right direction?
B. I understand from @Photon_noir SOP that I can add small amounts of Magnesium Oxide but I wanted to know if this is still the best way to neutralize.
C. Any other suggested options?
I too was thinking about sodium bicarbonate and I tried doing it with a small sample which yielded A LOT of salt and a milky emulsion from water. This was expected as citric acid with sodium bicarbonate would yield water, carbon dioxide, and salt, if I’m not mistaken.
If you’re wanting to do LLE, you’ll want to take hep/hexane at about 4:1 Alkane to crude. Then mix it together and add water. This will louche out the ethanol. You’ll want to add about 10:1 water to ethanol in the solution and it should all jump to the hep/hex quite easily.
It’s loke y’all are speeding Chinese lol
Then why does everyone scream ph etoh? I never do, and I add di directly to my wash.
I just ordered litmus paper just for this.
Will that get rid of the citric acid? Where does the citric acid bond to in the separation? Will it stay with the ethanol?
Correct me if im wrong:
- Reduce 70 gallons to crude and add 4:1 alkane in my reactor.
- Add water to louche whatever ethanol is left (and the citric acid)
- Drain the water-emulsion-crude/heptane and roto out the heptane?
Would it be more effective to use saline water?
Saline water may indeed work better. Might not, try both ways. Also check the pH of the water and if need be repeat the wash until it’s neutral.
I use saline water but I don’t think it’s necessary.
Doing multiple washes on the alkane+oleo solution will neutralize the pH if you’re doing washes with neutral pH water.
But yeah, rotavap off the majority of the alcohol and then washing the hep/hexane solution with water will neutralize.
A basic wash can be had
- Clean water with some or alot of salt. First pushes.
- Citric acid to swing ph over and get other side of spectrum of what you want to remove. Second pushes.
- Sodium bicarbonate neutralizations and considered your third pushes.
- Bare water to shake up and remove protonated water soluables stuck to glass.
Short answer, yes it’s not needed to do water washes. If water soluble compounds are present the. It’s needed. They will affect your distillation and end product usually over a period of time. Anytime you do a mechanical separation via washes you will be messing with alot of the material itself, a good practice is to neutralize it back to normal.
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I have my litmus paper incoming. I’ll ph test all 6x 5gal buckets of rotovaped etoh and post the results.
All my etoh has had food grade di directly in it.
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Who has spare Tums in their medicine cabinet
The emulsion is due to your production of sodium citrate, a known emulsifying salt… which is why I recommend avoiding using a sodium base (like baking soda) to neutralize citric acid. Also, carbon dioxide (from baking soda) in water forms a new acid: carbonic acid.
Louching yields a milky microemulsion of resin globules in watery ethanol… and you only need a little bit of water in the 190 proof ethanol:resin solution to precipitate all the resin; about 1 part water to 10 parts ethanol:resin solution. You then layer non-polar solvent over this milky aqueous ethanol in a separatory funnel and swirl/shake to get all the cloudiness (resin globules) to dissolve into the non-polar solvent, leaving a clear solution of ethanol, water, citric acid, and a bit of color behind. If the ethanol layer is still cloudy, extract it again with a bit more np solvent. If you are scared you didn’t get all the resin, add a little more water to it to see if it gets cloudy again (chances are it won’t), and extract with a bit more np solvent if it does. The color in the clear ethanol is normal, and it is just pigment you don’t want, anyway, not resin.
You can later wash the np solvent with a bit of fresh or brine water. This will remove any little bit of ethanol or citric acid that may have dissolved in the solvent.
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If your eho is salty, you can dissolve in np solvent like hexane or heptane, as described above, and wash it with water. Remove the water. Evaporate the np solvent.
@Demontrich I don’t know. I only recommend a litmus of EtOH prior to using it to dissolve resin, then after dissolving the resin, if one suspects excess acid in the resin… and that usually only happens when scrubbing or adjusting pH intentionally, neither of which do I recommend.