my vacuum still build

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dougyethanol
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my vacuum still build

Post by dougyethanol » Thu Aug 15, 2019 1:49 am

I have been working on a vacuum setup, Its like learning to distill all over again. Great power savings can be achieved as you need less heat to boil ethanol with minute power to obtain vacuum. Its a work in progress, i have a working model but needs more work. I will post pics and updates as i work on it.
i luv makin booz.

dougyethanol
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Re: my vacuum still build

Post by dougyethanol » Thu Aug 15, 2019 2:45 am

20190705_164651.jpg
my receiving vessel.
Its a stainless steel pet food bowl with outer edge cut off with a large rubber o ring from Bunnings(Aussie hardware store) to seal it.
one brass fitting is the fluid in line, the other is the vacuum inlet which gets charged before distillation.
i luv makin booz.

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Re: my vacuum still build

Post by dougyethanol » Thu Aug 15, 2019 3:09 am

My boiler vessel. I have been running it in an oil bath which is good for lower concentrations of ethanol.
20190618_103227.jpg
Its smaller than receiving vessel, less vacuum instability achieved this way.
i luv makin booz.

decoy
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Re: my vacuum still build

Post by decoy » Thu Aug 15, 2019 4:05 am

NICE.. good to see more peeps stepping outside the box.
someone on here made a vacuum still some years ago, if you have not done a search yet..

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Re: my vacuum still build

Post by MtRainier » Thu Aug 15, 2019 4:32 am

Do you have to worry about flammable ethanol vapor making it into the vacuum pump?

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Re: my vacuum still build

Post by OtisT » Thu Aug 15, 2019 7:10 am

MtRainier wrote:
Thu Aug 15, 2019 4:32 am
Do you have to worry about flammable ethanol vapor making it into the vacuum pump?
Yes. On vacuum systems I see an additional condenser for drying the air before it goes to the pump. It needs to be a powerful condenser because the velocity of that vapor can be fast.

On my small vacuum rig the condenser was not big enough and was quickly overpowered when the pump was activated and causing a boil, so I had to shut the pump off. My still had a small leak which meant I could only distill for 20 minutes before needing to vacuum again. My workaround was a PITA, but it was safe and it worked. I would distill until I lost enough vacuum that I could not boil at or below my target temp. I would then shutdown power and let the boiler cool to about 20 degrees below my target temp then I would vacuum again just until I made the charge boil then I would stop the pump and start distilling all over again. I have plans to build a new dedicated vacuum rig with no leaks, or slower leaks, but time had not allowed for that yet.

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Re: my vacuum still build

Post by dougyethanol » Thu Aug 15, 2019 5:08 pm

Otis has touched on a very important part of vac still. Leaks! When it is sealed well, runs smoothly.
Once the system is put under vacuum and you have no leaks, there is no need to run vac pump during distillation.
The way i checked mine for leaks, being glass, was to vac it and turn off valve, disconnect from pump and throw it in swimming pool and if there is a leak it would be clearly visible.
The other way is to vac it and leave it over night, if its still under vac in morning, all good.
i luv makin booz.

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Re: my vacuum still build

Post by OtisT » Thu Aug 15, 2019 7:22 pm

Dougyethanol, I did locate some leaking by putting my system under pressure (not vacuum). Rather than submerging though, I used a little soapy water on the joints and looked/listened for the bubbles. My still is stainless and copper, so no way to see inside for leaks.

I found that locating vacuum leaks is extremely difficult. Using liquid on the joints don’t work because I can’t see or hear inside. The best I could do was to put the system under vacuum then monitor the gauge for a drop in vacuum. I would tighten and/or reseat each joint one at a time to see if that fixed the leak. I was able to improve the stills ability to hold vacuum, but I never got it not make a perfect seal long term. It was not originally designed as a vacuum still, so my next one will be built specifically for vacuum with less and better joints and valves.

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Re: my vacuum still build

Post by dougyethanol » Fri Aug 16, 2019 1:53 am

In the first picture you will see there is no joint to tighten, the oring at top is about 1/2 inch thick, which is sandwiched between steel bowl and glass.
The seal only happens when vacuum is applied, its the same at boiler end. If any leak happens lids release and boil instantly disappears, i boil at approx 50celcius.
i luv makin booz.

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Re: my vacuum still build

Post by bcgold » Sat Aug 17, 2019 7:48 am

This nomograpgh maybe of interest to those using vacuum for distilling spirits, the graph makes temperature corrections for barometric pressure and elevation.

Image

manu de hanoi
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Re: my vacuum still build

Post by manu de hanoi » Thu Aug 29, 2019 4:49 am

dougyethanol wrote:
Thu Aug 15, 2019 1:49 am
I have been working on a vacuum setup, Its like learning to distill all over again. Great power savings can be achieved as you need less heat to boil ethanol with minute power to obtain vacuum. Its a work in progress, i have a working model but needs more work. I will post pics and updates as i work on it.
unfortunately heat up energy (2.57 J/g.K) isnt that much compared to boiling off energy(841j/g) , so the energy savings arent that much

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Re: my vacuum still build

Post by LWTCS » Thu Aug 29, 2019 1:26 pm

manu de hanoi wrote:
Thu Aug 29, 2019 4:49 am
dougyethanol wrote:
Thu Aug 15, 2019 1:49 am
I have been working on a vacuum setup, Its like learning to distill all over again. Great power savings can be achieved as you need less heat to boil ethanol with minute power to obtain vacuum. Its a work in progress, i have a working model but needs more work. I will post pics and updates as i work on it.
unfortunately heat up energy (2.57 J/g.K) isnt that much compared to boiling off energy(841j/g) , so the energy savings arent that much

Not to mention, you don't get any of the other benefits that heat provides to more traditional distiing for our purposes.
For example:
Maliard reaction
Esterfication.
Trample the injured and hurdle the dead.

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Re: my vacuum still build

Post by dougyethanol » Thu Nov 28, 2019 12:07 am

Thanks for replies.
manu, i run a 2200 watt still(no vacuum) and the vacuum still at around 400 watts on max(pwm/temp controlled). i havent converted my results to j/g.k as that is a bit beyond me. I get high 30s degrees celcius where i live, i can boil without any heat added at all so that would have to be a saving. I do take your point though, the evaporation does have a cooling effect. Boiling off energy(841j/g), is that at atmospheric pressure?
lwtcs, i had to google those terms and from what i read it seems that is in regards to flavour such as rums? I make neutral and fuel. Actually i do make the occasional rum at 2200 watts unthrottled. Pretty sure thats what you were talking about.
i luv makin booz.

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Re: my vacuum still build

Post by OtisT » Thu Nov 28, 2019 7:52 am

I was using mine for essential oil extraction. The lower temp boiling point is good for making oils because excessive heat will degrade some types of oil. Saving a few pennies on energy was not a factor for me at all.

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Re: my vacuum still build

Post by Tinkerzone » Sat Nov 30, 2019 7:28 pm

OtisT wrote:
Thu Aug 15, 2019 7:22 pm
I found that locating vacuum leaks is extremely difficult.
An easy method of locating vacuum leaks is to use length of flexible tubing as a stethoscope. Even smaller leaks (not bubble leaks) are detectable if hearing is good. As a safety precautions, do not insert tube into ear channel, sudden higher pressure may damage sensitive inner ear.

Vac Distillation has definitely advantages however it may change flavors of product drastically.

Vacuum is sure handy for degassing, transfers and drying dessicant. If sucked substance is condensing, volatile and/or damaging to the pump, cold trap made out of mason jar in suction line is a must. If degassing, assure that container holding degassed fluid is full to the maximum to prevent accumulation of potentially explosive energy if container gives.

Cheers
Tinkerzone

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Re: my vacuum still build

Post by OtisT » Sat Nov 30, 2019 11:57 pm

Tinkerzone wrote:
Sat Nov 30, 2019 7:28 pm
Vacuum is sure handy for degassing, transfers and drying dessicant. If sucked substance is condensing, volatile and/or damaging to the pump, cold trap made out of mason jar in suction line is a must.
I don’t think I will be using a mason jar for my vacuum system. That sounds too damn dangerous. Kaboom!

I have a 1/6 bbl keg I previously tested as a vacuum reservoir and I will likely use it again when I build my next vacuum still.

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Re: my vacuum still build

Post by Tinkerzone » Sun Dec 01, 2019 5:29 pm

No do not use mason jar for a boiler or any part of the still, too dangerous.

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Re: my vacuum still build

Post by cayars » Thu Dec 05, 2019 12:52 pm

I'm just curious what your use of the vac still is going to be. Is it for essential oils and the like?
It's not for spirit production is it?

I'm not a member of the "glass police" and won't condemn this. But I'll point out that 99 out of 100 mason jars might work for this or other similar uses for a while before failing when run smartly but why take chances? When they break or crack it could be a "yawn" moment or an "oh shit" moment depending on the safety of your setup and use. If you want to use glass, order some lab grade glass made for this purpose at the very least.

You may have a great handle on how to use any glass properly but some dumb smuck might come here to the forums from a Google search, see what you did and try and copy it without the proper knowledge...
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Re: my vacuum still build

Post by Tinkerzone » Wed Dec 11, 2019 9:54 am

Let's cast some light on the subject of mason jars (MJ) in VACUUM service as a part of this thread.
Primary use for MJ is home food preservation and successful process of canning requires certain degree of vacuum to be present in the MJ to inhibit bacteria growth thus they are designed for vacuum conditions just like certain glass labware in laboratory (Buchner flask).
The MJ walls are constructed from heavy annealed glass to handle vacuum and moderate temperature shock. Annealed glass tends to crack as oppose to shattering of tempered glass.
Larger the vessel volume results larger amount of energy accumulated so as a precaution MJ size should be the smallest practical just in case.
If in vac service MJ must not be exposed to thermal shock i.e. hot MJ rapid cold liquid introduction.
As an additional safety layer MJ can be wrapped in elastic envelope such as duct tape to contain fragments from unlikely implosion and/or further their safety by personal protection equipment.
There is a chance that "some dumb smuck" or even HD chemist may reach for a pickle jar in lieu of MJ which is not designed for above mentioned process conditions and problems will follow for sure.
Just saying

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Re: my vacuum still build

Post by OtisT » Wed Dec 11, 2019 11:05 am

Tinkerzone wrote:
Wed Dec 11, 2019 9:54 am
Let's cast some light on the subject of mason jars (MJ) in VACUUM service as a part of this thread.
Primary use for MJ is home food preservation and successful process of canning requires certain degree of vacuum to be present in the MJ to inhibit bacteria growth thus they are designed for vacuum conditions just like certain glass labware in laboratory (Buchner flask).
The MJ walls are constructed from heavy annealed glass to handle vacuum and moderate temperature shock. Annealed glass tends to crack as oppose to shattering of tempered glass.
Larger the vessel volume results larger amount of energy accumulated so as a precaution MJ size should be the smallest practical just in case.
If in vac service MJ must not be exposed to thermal shock i.e. hot MJ rapid cold liquid introduction.
As an additional safety layer MJ can be wrapped in elastic envelope such as duct tape to contain fragments from unlikely implosion and/or further their safety by personal protection equipment.
There is a chance that "some dumb smuck" or even HD chemist may reach for a pickle jar in lieu of MJ which is not designed for above mentioned process conditions and problems will follow for sure.
Just saying
This is very irresponsible.

File this under just my opinion, but I’m going to go out on a limb here to say using a mason jar as a vacuum chamber for distillation purposes is a stupid idea. It’s one thing to talk theory and ask questions, but another thing all together to put this out on a public forum saying it is Ok to use. The potential harm done to someone if a jar implodes can be very serious.

So I’m curious, do you run a vacuum still yourself? Do you know how much vacuum is applied in order to achieve a meaningfully lower boiling point? Have you put a mason jar under that pressure?

Have you seen how fast temp moves when a close system is under moderate vacuum then the pump is activated? All that vapor goes straight from boiler to pump, and heats the shit out of where it collects in a second, including any air traps.

And a jar won’t do shit for keeping air dry in a vacuum still. The vapor shoots past everything and heads straight for the exit (pump)

If you run a vacuum still and can prove me wrong with knowledge from your actual experience, then please share the details and I will apologize sincerely and promptly. Until then, I’m calling BS.

Otis

[EDIT - added info. Mason jars only work for canning with a high vacuum when the jar is full of solids and a liquid (very little to no air.) Gmaw B taught me when canning to fill the jar to the rim or a set level just below the rim, depending of what we were canning, otherwise the glass would implode when it cooled due to the vacuum created by heat loss]
Last edited by OtisT on Wed Dec 11, 2019 7:42 pm, edited 1 time in total.
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Re: my vacuum still build

Post by cayars » Wed Dec 11, 2019 12:07 pm

I wish we could upvote posts.
I was trying to be diplomatic in my post but I think Otis nailed this with his "opinion", and the very to point questions asked and statements maid about what happens in a vacuum still.
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Re: my vacuum still build

Post by Danespirit » Mon Dec 16, 2019 7:16 am

+1 OtisT

I would refrain from using ordinary glass vessels for vacuum distillation..!
The chances of an accident are just too many.
If I ever was to create such a device I'd weld it together from thick-walled stainless steel (copper would just cost a fortune).
Creating such a vessel isn't for the average hobbyist with a TIG torch in the shed.
To be safe we talk welding with purging gas and a bunch of other things crucial for a good AND safe result.
All in all, there is way more to it than a couple of copper pipes and a blow torch from Wall-mart.

Edit: Btw..dougyethanol .....is this "gasket" my eyes see in the first picture a silicone seal from somewhere?

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Re: my vacuum still build

Post by dougyethanol » Mon Jun 15, 2020 12:34 am

Hi guys, i haven't stilled for quite sometime, back into it now.
Alot of good safety tips above and definitely make sure you have a good glass vessel, steel is safer!

Not endorsing it but make up your own mind, that was cheap glass. Laboratories use glass.
Danespirit, you picked up the rubber oring, not ideal and the final setup will not have it.
It is a vacuum vessel nothing is touching it, not even air(gets to be a technical point).
Reading above about implosion, no vacuum, no gas. DONOT use a flame to heat your vessel. DONOT!
i luv makin booz.

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