Author Topic: 50 gal. Reaction/ Distillation Vessel Construction  (Read 6483 times)

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alchemy_bee

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50 gal. Reaction/ Distillation Vessel Construction
« on: May 27, 2002, 08:30:00 PM »
The objective is to describe the construction of a multipurpose vessel that can act as both a reaction vessel - with cooling and heating capabilities and which can also act as a distillation setup with simple, vacuum and fractional arrangements.

Below is a graphic illustrating the draft idea.



For the main vessel a large 55 gallon stainless steal drum. The inside to be sanded and polished with an orbital polisher and compound. The top to be cut off and in its place a washer-like ring of stainless steel welded into place that has an internal diameter equal to that of the drum, and an external, several inches greater allowing for a ledge to which a top could be bolted into place. Holes drilled in for bolts.

For the top, a disk of stainless steal equal to the external diameter of the ledge, holes drilled to match the ledge. Two access holes are cut respectively allowing for over head stirring and the larger hole for a condenser or column depending on the setup. Additional bolt-holes drilled around these access holes. Appropriate gaskets to be put in place where necessary.

The condenser, column, connecting joints all to be fabricated from stainless steal parts and some tricky welding.

For cooling and heating of the vessel; An acetylene torch is passed across copper piping to white hot. After piping has cooled it is annealed (temper removed) to allow for forming. Piping is formed half-round and to be welded to the exterior and under part of the vessel in a coil network that would allow for adjusting. Adjustments would allow for where and how high along the outside of the vessel heat is applied (as heat is only needed to the height of the material being heated in the vessel for distillation). Glass insulation is provided around the coiling when heating. The coils are arranged into sections that intersect at in and out line manifolds. Circulating the heating and cooling fluids is a jet pump.

For cooling purposes a large tank of salted ice water could be arranged. Alternately for heating purposes, a 15 gallon stainless steal tank could be constructed to heat cooking oil by propane flame. A thermostat and flame controller could be coupled to the tank from a restaurant style gas powered deep fryer.

Questions:

Is the circulating oil heating scheme viable? Using the coils for circulating cooling fluid is highly desirable. If a sole direct flame heating is desirable -  could the heated oil be circulated and additionally - direct flame could be applied under the vessel under the bottom coils? Its the purpose of oil heating to allow for smooth, even heating.

For the over head stirring motor, it is desirable to be able to stir during a vacuumated distillation - does anyone know of a device that would allow for throughput shaft into a highly vacuumated system? This sealed device should also be used when refluxing flammable liquids.






lugh

  • Guest
Vacuum
« Reply #1 on: May 27, 2002, 10:06:00 PM »
Some of your ideas are good, but a mere drum isn't going to hold much vacuum  :(  For starters, you might want to study alcohol fuel production, literature should be available in a local libary  :)  Once you understand that, you'll be more ready for more advanced construction projects  :)

alchemy_bee

  • Guest
Lugh: Thanks for the post.
« Reply #2 on: May 27, 2002, 10:39:00 PM »
Lugh: Thanks for the post.



but a mere drum isn't going to hold much vacuum



Do you mean it cant maintain a vacuum or physically cant support a vacuum? Appropriate gaskets would be used and the bolts would be of a heavy gauge and could be tightened considerably with long wrenches. Additionally id guess that all seams could be greased over to assure a seal. If the structure couldn't support a high vacuum - well, one that could would be used.



For starters, you might want to study alcohol fuel production, literature should be available in a local library



With intention for starting some informative discussion in this thread can you expand on this? What aspect of fuel production would be helpful to look at when considering a project like this?




alchemy_bee

  • Guest
make it all custom
« Reply #3 on: May 27, 2002, 10:51:00 PM »
Hammer: Ideally this setup would function to distill product oils, that is to say a vacuum of 1 micron(mm/hg) would be lovly.

For a application of this size though, a simple water aspriator or even a nice Welch 1200 vacuum pump wouldnt cut it. Although what vacuum source would fit this monster is for another thread entierly.

My only reservation about using thicker steal in the construction is that the heat transfer would be depleated. This could be solved by using more direct means of heating though.



RoundBottom

  • Guest
cooling and heating circulators
« Reply #4 on: May 27, 2002, 11:18:00 PM »
why are the heating coils on the outside?  wouldn't it be better to have them on the inside, and keep the manifolds on the outside?  this would require them to be SS, of course. 

another idea would be to have a separate set of coils for cooling liquid. 

i learned a thing or two from charlie dontcha know.

alchemy_bee

  • Guest
RoundBottom: That's a great idea to have the ...
« Reply #5 on: May 28, 2002, 12:35:00 AM »
RoundBottom: That's a great idea to have the coils on the inside! That would certainly solve the heat transfer problem if thicker steal was chosen for the construction material. Is that the a more valid option for heating and cooling?

Affixing total covering coiling to the outside would be a far easier task than doing the same on the inside and it would provide heat/cooling to every surface- however it would be less efficient as its indirect.

It would be difficult to have the entire vessel coiled on the inside - opposite my diagram. However you may not need to weld the coiling to the inner surface as its a direct means of heating/cooling, and simply have the outside of the vessel insulated.

If the coiling was kept on the outside, and additionally a run of coiling was placed inside and the entier vessel was insulated this may perhaps provide a good cooling and heating setup?

What would be the benefits of having coils on the inside and outside? Is there some other heating/cooling scheme that would work?



pandemonium

  • Guest
Internal Heat exchangers
« Reply #6 on: May 28, 2002, 12:52:00 AM »
as in ss tubings within the vessel itself are the standard in the industry. KIckass work Alchemy, still absorbing it...

If you can find one, an industrial steam kettle, used in hospitals and military institutions would be something adaptable, though It might not suit this need. I hear Colonel Sanders even deep fries under pressure, those things mentioned just to muse the old designer bent. Nice to see here, very nice.

Instant Karma's gonna get you, gonna knock ya right in the head

BenWiFFen

  • Guest
Swimming pool filters
« Reply #7 on: May 28, 2002, 02:06:00 AM »
Someone knowing i'm a collecter of relics gave me a comercial size pool filter. It's about 1/4" thick S/S with a dommed top convex bottem. The top has a  bolted flang. It also is tapped with a PSI gage and some plugs. How would copper tubing bee?

Give me libreum or give me Meth

ClearLight

  • Guest
s.s.
« Reply #8 on: May 28, 2002, 02:13:00 AM »

  Just go around to the local ag/dairy/food processing plants in your area and ask if they have any "scrap" stainless or surplus stuff they can liquidate...talk to the yard guy to get you to the foreman to get you to the plant engineer...they always have shit they'd be glad to have you haul away for them.. afof got a complete 30 foot distillation and another reverse osmosis membrane set up for free!



Infinite Radiant Light - THKRA

alchemy_bee

  • Guest
A used steam kettel might be somthing to ...
« Reply #9 on: May 28, 2002, 02:18:00 AM »
A used steam kettel might be somthing to consider, what the heck are they and how/what are they used for? They sure lookin interesting!



What is their basic contruction? How would they stand up to high vacuum?



dchef

  • Guest
what the heck are they and how/what are they used ...
« Reply #10 on: May 28, 2002, 02:28:00 AM »
what the heck are they and how/what are they used for? They sure lookin interesting!
______________________________________________________

 Looks like you have found a setup for brewing beer, like the ones used at micro-brewerys. There's a couple of nice ones around here where you can get a good dinner and ripped off of the brew of the week. Oh yeah
:)

Meth, it does a body good

Bwiti

  • Guest
Inert Coating On Inside
« Reply #11 on: May 28, 2002, 03:39:00 PM »
What could be used as an inert coating for the inside of the vessel? I can't find anything useful as far as teflon mixures goes, but what about pottery glaze? If it can stand-up to the heat of a kiln, then it'll work fine in any type of chemistry "experiment". I was thinking about making a 5000ml flask from a piece of steel pipe with a huge diameter, sand the inside, then apply the glaze. After the glaze dries, heat the outside of the vessel with something like a propane torch to cure the glaze.....But, the steel might expand too much and shatter the glaze. Ahhhh, fuck it, I wanna learn glass blowing. 8)

Love my country, fear my government.

alchemy_bee

  • Guest
Bwiti: You definitely cannot glaze the inside of ...
« Reply #12 on: May 28, 2002, 05:29:00 PM »
Bwiti: You definitely cannot glaze the inside of a metal container with pottery glaze. The expansion rate is to different. Additionaly you can't cure pottery glaze with a torch either - a proper kiln has different settings depending on the glaze that is used (red roka, roqu, etc.) and must cool down gradually.

You can however enamel some metals with glass powder. This is done in jewelry making usually on metals that have resistance to oxidation at high temps. Usually on silver, sometimes on copper - even gold, a holding agent is spread on the piece, and glass power is dusted on, the piece is then placed into a furnace at around 1500f until glowing hot and when the molten glass is smooth over the piece. At this temp the holding agent which also acts as an anti-oxidizer burns off and the glass is enameled onto the surface of the metal.

I think you might also reconsider teflon. There are many grades of "Teflon" which is a brand name for a line of coatings produced by DuPont, anyways, in this product line there are like 5 or 6 different formulas with different properties; FEP, PFA, PTFE etc. and are ideal for coating metal and have superb heat and chemical resistance depending on the formula. 3M also manufactures a big line of coatings, off hand Kel-F (PolyChloroTriFluoroEthylene) offers good acid resisitance.

Just a suggesting - if you look up custom "teflon(or whatever) coating" on the internet there are places that will do just that. Its kinda pricey but they will coat anything ya want. SWIM had a pressure tank for car painting ghetto rigged into a pressure reaction vessle coated with teflon, works like a charm.



alchemy_bee

  • Guest
If 5/32" - 6/32" plate steal was used for the ...
« Reply #13 on: May 28, 2002, 11:19:00 PM »
If 5/32" - 6/32" plate steal was used for the body would there still be need for suport bars or consern over vacuum? I took a stack of computer paper and measured this thickness out just for a visual que. Im working on a revised draft, but im considering that even with steal this thick, a combination of hot-oil/coil heating and direct heating may work.

Also im considering using other metals that conduct heat well for the contruction material - namly copper. Would copper be a more expensive material to work with? Obviously if copper is used the interior would be coated with teflon or like material...



goiterjoe

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how much are you going to end up spending?
« Reply #14 on: May 29, 2002, 12:52:00 AM »
as far as a heating source, you can modify a turkey cooker to heat a kettle fairly easily.  I've seen a few modern day liquor stills set up utilizing this design.

as far as getting the container to distribute heat evenly, you will probably want to get the tank modified to have coiled tubing running through it that you can run hot oil through.  Thick copper tubing would probably work the best.

zed

  • Guest
Vacuume.
« Reply #15 on: May 29, 2002, 02:47:00 AM »
Regarding vacuume source. Theoretically, in a sealed system, high flow is not required. Once a vacuume has been established, distillation and condensation being equal, what is to be evacuated? In practice, of course, all systems leak and condensation is never perfect. But, your vacuume pump might not need to be as robust as you imagine.

Lugh, is correct, regarding the original drum idea. A 55 gallon drum is not likely to survive even a moderate vacuume. Unless, drums are alot stronger than they used to be; a simple aspirator, at normal temps, can collapse a 55 gallon drum, if given a little time.

 

foxy2

  • Guest
autoclave
« Reply #16 on: May 29, 2002, 04:11:00 AM »
A used autoclave might bee ideal.

Not sure what modifications would bee necessary for vacuume work.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety

alchemy_bee

  • Guest
Revised...
« Reply #17 on: May 29, 2002, 04:40:00 AM »
When cooling a vessel of this size, coils have excellent cooling ability as water can be circulated through them very rapidly. A jet pump is desirable for this application.

It is known that as the volume of the material increases, exponentially does the amount of energy needed to bring it to a boil.

In a nearby 15 gallon steel tank (or steam kettle as suggested), oil could be easily heated to 100c-400c from a direct propane flame and circulated rapidly. I believe with some modification a jet pump could be used to circulate the hot oil as well.

In put is needed here; I do not have any experience to draw from when inferring the best heating method. It has been suggested that direct flame heating is needed for something this big. Considering how well forced hot water heats my house, it would be very convenient to use the coiling aforementioned for heating purposes as well. It would also be very easy to integrate a propane burner under the vessel for additional heating.

With a sizable burner under the vessel optimum heating could be achieved, additionally the circulation of hot oil around the vessel would allow for smooth even heating and with insulation material around the entire device - I would think that heating to reflux would be easily obtained.

Below is a graphic illustrating a revised draft incorporating elements suggested in this thread.


Please note i left out the coils in the lower graphic and abridged the coils in the top one simply for easy of drawing, the intended exterior coil configuration is shown in the first post.

The reason for keeping the main coiling on the outside is simply because it would be to difficult to form and affix it to the inside. I think the bottom plate - which has interior coiling and a burner, is the main source of heating/cooling, and the bulk of the exterior coiling just supplies additional heating and cooling value.

Im considering two variations for the bottom - the lower one incorporates a sealed air chamber. You often find air chambers in high end cookware - i think somthing like this would help heat distribution greatly and avoid hot spots if flame heating is to be used. With this scheme there is also heating protection allotted from the copper coiling that is encased in the chamber, this to help absorb and distribute heat into the vessel.



foxy2

  • Guest
heating
« Reply #18 on: May 29, 2002, 07:38:00 PM »
the ideal is to heat with high pressure steam,

Do to the thermodynamics of condenseing steam you ca put ALOT more heat into the vessel with it.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety

goiterjoe

  • Guest
steam jenny
« Reply #19 on: May 29, 2002, 11:42:00 PM »
What about a steam jenny, the steam pressure washer devices?  They can be had for around $1,000.  I've seen a person with 3rd degree burns from one of these devices that malfunctioned on him, so I'm not saying their safe.

is 100C going to be hot enough for your applications?  I doubt it will.  Oil is probably your best bet if your planning on going homemade.

What are you planning on reacting in this anyway?