Vacuum Trap Or Cold Trap?

go go kid said:

does your distillation collom have a vacumme take off point?

Click to expand...

I'm still trying to get one and a vigreux distillation column in 24/40. I have a PO box and many of the places won't ship here as they use Purolator or FedEx so I got fed up and gave up for a bit. Hard to contact the actual shipper to find out which they use so I can use the addy for the drop-off point with my name at the top and go pick it up. I'm using amazon . ca for most of my shopping for stuff like this. Got most of what I need but could also use another condenser for faster straight distillation.

Naphtha is hard on seals. It's a silicon seal on my countertop distiller that works fine for ethanol and ISO but seems to absorb the naphtha then swell up and blow the seal. My 12L pot still had the same problem with its silicon seals for the outlet and thermometer seal so I made gaskets with automotive gasket paper and that fixed that up.

I have a good aerator pump for my dugout and it can be used as a vac pump but I'm concerned about naphtha wrecking its diaphragms so will need to make sure I have some sort of absorbent in the tubing leading to it or get a pump that won't be affected and already spent more money on stuff like this than I originally planned to.

I'll get it all together eventually.

OldMedUser said:

I'm still trying to get one and a vigreux distillation column in 24/40. I have a PO box and many of the places won't ship here as they use Purolator or FedEx so I got fed up and gave up for a bit. Hard to contact the actual shipper to find out which they use so I can use the addy for the drop-off point with my name at the top and go pick it up. I'm using amazon . ca for most of my shopping for stuff like this. Got most of what I need but could also use another condenser for faster straight distillation.

Naphtha is hard on seals. It's a silicon seal on my countertop distiller that works fine for ethanol and ISO but seems to absorb the naphtha then swell up and blow the seal. My 12L pot still had the same problem with its silicon seals for the outlet and thermometer seal so I made gaskets with automotive gasket paper and that fixed that up.

I have a good aerator pump for my dugout and it can be used as a vac pump but I'm concerned about naphtha wrecking its diaphragms so will need to make sure I have some sort of absorbent in the tubing leading to it or get a pump that won't be affected and already spent more money on stuff like this than I originally planned to.

I'll get it all together eventually.

Click to expand...

have you thaught about rubbing dow corning chemical resistant vacumme grease around and over any seals or rubber parts? its chemicly resistant and should stop the naptha attacking the seal material, it will at least give them a longer lifespan. just a thaught
vasaline may well do the same thing too, just a dam sight cheaper

go go kid said:

have you thaught about rubbing dow corning chemical resistant vacumme grease around and over any seals or rubber parts? its chemicly resistant and should stop the naptha attacking the seal material, it will at least give them a longer lifespan. just a thaught
vasaline may well do the same thing too, just a dam sight cheaper

Click to expand...

I got a fresh tube of Dupont Molykote just a few months ago but getting it to cover the seals and hold is pretty doubtful. It has silicon and other stuff in it too so some could also just wash off and end up in my cannabis oil and I'd be tossing that out. I should probably mix a weighed little bit with naphtha in a clean weighed little beaker then set it on heat for a while then cool and pour off most of the naphtha, evap any remainder and see if any grease was lost. If not then it might work OK.

Vaseline is made from petroleum so would easily dissolve into naphtha so that's out. That 150g tube of Molykote was $75 with the shipping. Got it for the seals on the RO system I haven't set up yet.

yeah, my dow corning was $60 a 150 g tube without shipping , it aint cheap, but you get whjat you pay for.
yes, thats a great idea to see if any grease gets lost , i dont remember any warning on it, but its a long time ago and it wasnt for cannabis oils. cant find it right off, but its around someware.
shit, forgot about the patroleum part of the vasaline. need sleep, not thinking strait lol insomnia, who needs it

go go kid said:

need sleep, not thinking strait lol insomnia, who needs it

Click to expand...

I just had one of my 'nap attacks' myself. Always feel like crap for a while after and should probably just go to bed as I have to get up for 7am to make a doctor's appt by 9:30 and it's 9:15pm now. But then I'd be awake by 4am and that's way too f'n early.

I used to have horrible insomnia until a small stroke about 7 years back but I don't recommend it as a cure.

SoggyCashew said:

No i didnt know about shutting vacuum tube off to stop water mixing, there isnt even a valve anyway between the two. I usually use a tiny pump that came with the setup but this time decided to grab a hvac vacuum pump that pulled way more vacuum. This bigger pump was causing a cold boil in my filtered mixture when i was filtering it. Anyways, I cooked it down till about 10 ml. There were still some water left and I figure I'll let it set. I woke up this morning. The top layer harden up and the bottom layer is water. I don't know if you can tell in the picture. I poked a hole and dumped out the water... Lol what a crappy experience this was!

View attachment 5266978
View attachment 5266979

Click to expand...

Good job recovering! If you want to recover using less heat, you can pour it out in a casserole dish with a cloth dust cover and let the alcohol evaporate away, before sticking it in the freezer to harden and clump the oil the oil, so that the water can be poured off.

Good that you noticed your pump oil color before you wiped out your oil bath pump. The cost of using one in a wet application is frequent oil changes, and the color in your site glass is first warning.

How much moisture was in the plant material that you extracted using QWET? That looks like more than 5% from the azeotropic 190 proof.

As far as protecting the pump, what kind of vessel are you using for the boiling chamber and how is the inlet protected from spray?

To catch liquids, you can install either a cold trap or a desiccant trap, but the desiccant trap would work better for water, unless you want to go to dry ice to cool it.

They are relatively simple to build. The chamber is filled with a desiccant like Mol Sieve 5A and there is an inlet and an outlet for your flow. The inlet usually has a dip tube so that inlet flow starts at the bottom of the desiccant chamber and flows out the top. You also need a screen on top of the desiccant, and a paper filter to catch desiccant dust.

Consider a simple Sporlan inline "Grenade" filter/drier cartridge: https://ph.parker.com/us/17575/en/catch-all-filter-drier......

I built my own filter/drier using sanitary stainless components and a molded zeolite filter insert, typically used in air conditioning to remove water. I based it on Sporlan's replaceable core series. https://ph.parker.com/us/en/replaceable-cores-and-filters-sporlan-series

go go kid said:

he used 95 % everclear, now thats still 5% water, said hed used it b4 and never had problems, but sounds to me like he didnt close vaccume off b4 distilling as the vasc pump oil did the same thing.
now if memory serves, you can distill everclear to 99.9% and then chuck a load of dried sodium chloride at it to get the rest of the azetropic water out of it, leaving you relatively water free alcahol, all alcahol is max 99.5% azeotroopic mixture, so the desecant should get rid of the water and some alcahol. but better then useing 95% everclear.
but i dont think he knows about shutting vacuume tube off to stop water mixing with pump oil. its a closed circuit, the vaccume will stsy for a time, b4 needing to be re vacuumed again

Click to expand...

I know you can salt out Isopropyl, but not sure about ethanol. I'll do some research and get back.

Azeotropic ethanol and water is around 95.5% unless under vacuum. A vacuum pot still will typically reach about 130 proof the first run and I only reached 180 proof with five runs.

I used 5A molecular sieve to save time and move to 190 proof for that experiment, but I also picked up dust from it and required redistillation. It could ostensibly have been done with 0.2 submicron filtration, but I didn't have one at the time.

I was however able to go from 130 proof to 190 proof in one step using a 60" reflux column, and you could ostensibly use mol sieve to reach 200 proof.

The pictures show more water than I've encountered using QWET extraction with 95% ethanol, which is why I'm curious about other possible sources.

go go kid said:

yeah, my dow corning was $60 a 150 g tube without shipping , it aint cheap, but you get whjat you pay for.
yes, thats a great idea to see if any grease gets lost , i dont remember any warning on it, but its a long time ago and it wasnt for cannabis oils. cant find it right off, but its around someware.
shit, forgot about the patroleum part of the vasaline. need sleep, not thinking strait lol insomnia, who needs it

Click to expand...

Not cheap, but it works and it doesn't require a lot of glass ware to pay for a tube.

Fadedawg said:

I know you can salt out Isopropyl, but not sure about ethanol. I'll do some research and get back.

Click to expand...

Nix on the ethanol. Just ISO. Link here for salting out ISO.

yeah that was for iso, i thaught it a better solvent for the OP to use, as you say, 99.5% azeotropic mixture with everclear.
methanol will come down to pureish alcahol, but you cant injest it like everclear.

if you vacumme filtered everclear in enclosed system, tap off at the pump once up to pressure, distilled into a part dessicant filled flask. would you get 99.9% everclear

Isopropyl scares me thats why I use everclear, plus wouldnt i have to vacuum purge to remove all the Isopropyl?

SoggyCashew said:

Isopropyl scares me thats why I use everclear, plus wouldnt i have to vacuum purge to remove all the Isopropyl?

Click to expand...

ISO is not as toxic as you and a lot of others think it is. It's used a hand cleaner, body rub etc so a lot gets inhaled and even absorbed through the skin with normal use. I've never purged other than warming over simmering water and stirring it around. I don't even do that step anymore as I wait and do my decarb on the oil after cooking off the ISO. 250F for 30 min will get all but the smallest amount out so it will be so far beyond any reasonable level of toxicity that you'd have to consume a gallon of the oil and still wouldn't be harmed by any traces of the ISO. The gal of oil is gonna mess you up real bad tho.

You ingest more toxins on a 2 block walk down a busy city street than smoking an oz of the unpurged oil. More likely to be harmed crossing such a street as well.

In other words the risk is so minimal worrying about it takes energy away from the million and one things in life that we really need to be worried about.

go go kid said:

yeah that was for iso, i thaught it a better solvent for the OP to use, as you say, 99.5% azeotropic mixture with everclear.
methanol will come down to pureish alcahol, but you cant injest it like everclear.

if you vacumme filtered everclear in enclosed system, tap off at the pump once up to pressure, distilled into a part dessicant filled flask. would you get 99.9% everclear

Click to expand...

I'm not sure about getting 99.9% ethanol doing that. Not at all sure you need to so as to make oil. A pure hydrocarbon like naphtha or butane makes a cleaner oil a lot easier. I want all those impurities from the plants in my oils anyway as it's going for edibles and there's a lot more medicine in the plant than just THC and CBD.

Methyl hydrate aka methanol aka wood alcohol comes at 99.9 and is about $12/4L. I've used the stuff from the hardware store but distill it before use. Didn't find any residue but prefer ISO if I'm going to use an alcohol to extract with.

from what ive read, just let it sit in a water bath and let it get rid of water that way.
but use iso next time or methanol. i would anyway

Is there a good detailed beginner tutorial on using ISO? I was at the hydroponics store the other day and they had gallons for like $35

this one had the highest number of views.

SoggyCashew said:

Is there a good detailed beginner tutorial on using ISO? I was at the hydroponics store the other day and they had gallons for like $35

Click to expand...

QWISO or Quick Wash ISO is the preferred method of extracting cleaner oil where you freeze everything for a day or more before pouring the ice-cold ISO over your crumbled up bud, swirling for 30 seconds then pouring out and pouring some clean ISO over the pot for another 30 sec then pouring out. I don't try to filter at that time but let the stuff overnight or longer so all the fine particles settle to the bottom then decant into another container like home-made beer or wine to leave all the crud on the bottom. Then I filter through a lab grade filter tho a coffee filter will do. Goes thru fast as there's no fines to plug up the pores in the paper. Barely anything there if you decanted well.

Do a search in here for QWISO and you'll see how easy it is. Even google it. Plenty of videos on UTube if that works better for you.

SoggyCashew said:

Is there a good detailed beginner tutorial on using ISO? I was at the hydroponics store the other day and they had gallons for like $35

Click to expand...

£35 for 5 liters, look around, maybe do an ebay search, you should be able to get it cheeper i think

Ok so the ISO was exactly like how i did the ethanol. I did the quick wash and then i filtered in my Buchner using a 1.0uf filter and a 1/8" diatomaceous earth filter to get waxes and lipids out. After that i used my distiller to get my alcohol back I said the temperature on 174 Fahrenheit. The remaining liquid by then heated it up on my magnetic stir plate until it was an oil.

Is there any videos of a Buckner setup for filtering a very cold fluid. This is where things got screwed up and I got the water in my material.

Thank you for posting the videos, they were very helpful. The only thing is I don't dab that much. I usually use it for edibles so the ISO I would have to fully eliminate, correct?

Here is the Buckner funnel that I bought and here is the Distillerler I bought. Here is the Magnetic hot plate that I bought as well.