Author Topic: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)  (Read 123 times)

solidstone

  • Subordinate Wasp
  • ***
  • Posts: 102
Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« on: March 02, 2011, 06:56:14 PM »
Recently I've been playing with Gallium a bit, as well as using a pressure cooker to distill liquor, meanwhile researching a host of hydrogenation reactions.

It is apparent that with 1-2 atmospheres a lot can be accomplished although pushing the pressure far higher than this is ideal for both reaction rates and more dynamic chemical manipulations.

I've been looking at a lot of the larger hydrogenators, and they seem uncannily similiar to a pressure cooker or an autoclave, with the addition of gas inlets, a mechanical stirrer, and in some cases a vacuum pump.

I've been playing around with palladium salts in the lab (working on mastering the Heck reaction), however a lot of them require a pressure reactor and my university does not have it in their budget to provide me with a fancy parr shaker, so on comes the engineering challenge.  Time to make my own.

The biggest question is how much pressure can I pump into one of these steal or aluminum pressure vessels before it bursts.  They have a safety valve, but that’s easily nixed.  It appears to have a gauge that reads to 2 atm albeit theres a caution sign on that end of the gauge.  I’d wager it can take a good deal more than is intended for simple steam cookery and sterilization.

The model I have identified as looking the most structurally sound for this investigation is the Wisconsin all American 910 (10.5 quart).  However this is aluminum which could prove problematic with my proposed gallium route to pressurizing with hydrogen.  I may look into pressurizing from a tank, but while I’m still enjoying the novelty of gallium, I’ll stay away from aluminum.

Another interesting candidate is a 12L stainless steel autoclave used for dentistry and tattooing.  The question again is how much pressure can it take.

I will be ordering one in a few days, if there are any recommendations, please feel free to advise.

Once I get the autoclave, I’ll play with the max pressure, simple modifications, and then start working on some stress tests.  Concurrently I’ll likely play with lower pressure reactions in the typical range, and try investigate my proposed scheme of pressurizing via an Al/Ga hydrolysis reaction.

I hope to end with a sectioned pressure reactor that can replace the need for pipe bombs, fire extinguishers and glass bottle, that have been recommended to me, but that lack certain safety assurances, not to mention do not address the concern of scale!
Anyone competent enough to crunch some theoretical numbers on suspected pressure resistance, or who want to participate in a lateral investigation with me… by all means it is encouraged.

If there is already a comprehensive guide or an easier (but not ghetto) solution, my ears are open.

Regards,

Stone
« Last Edit: March 02, 2011, 07:14:41 PM by solidstone »

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« Reply #1 on: March 02, 2011, 09:44:23 PM »
I believe someone over at sciencemadness had made their own autoclave, you may want to look into that a bit, as the pressure he reached was much more than 20 PSI, if I remember correctly.

I honestly would not feel safe about having the pressure cooker go over 20 PSI, however if it is an all american, which has metal-to-metal seals, the temperature may not be an issue. I know my pressure cooker should not exceed 20 PSI - but that might be because of temperature and the rubber seal...

Not to sure, but I don't think it is safe - perhaps you could contact them and they might have some information on it?
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Wizard X

  • Lord of the Realms
  • Foundress Queen
  • *****
  • Posts: 1,224
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« Reply #2 on: March 03, 2011, 03:10:28 AM »
Parr hydrogenation apparatus.

http://www.erowid.org/archive/rhodium/pdf/safe-parr.pdf


Parr shaker type hydrogenators provide compact and easily operated systems for treating chemicals with hydrogen in the presence of a catalyst at pressures up to 5 atmospheres (60 psig) and temperatures to 80ºC. They are used primarily for synthesizing or modifying organic compounds by catalytic hydrogenation, reduction or condensation, but they are equally suitable for any other laboratory procedure in which a liquid and gas must be mixed vigorously in a glass  reactor at pressures up to 5 atm.

http://www.parrinst.com/default.cfm?page_id=309
http://www.parrinst.com/doc_library/members/Parr_4500-Catalog_v11.02.pdf
« Last Edit: March 03, 2011, 03:13:57 AM by Wizard X »
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

solidstone

  • Subordinate Wasp
  • ***
  • Posts: 102
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker
« Reply #3 on: March 03, 2011, 03:12:34 AM »
look up 12 L tattooing autoclave on an auction site...  the american pressure cookers can take 30 no question, but I think the stainless steal autoclave will easily take that and much more.  2 atmospheres should be more than sufficient for most palladium reductions and thats easily accomplished with minimal tweaking.
15 psi~1 atm  fyi

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« Reply #4 on: March 03, 2011, 03:18:48 AM »
Generally, as you mentioned earlier, the dental autoclaves can take more pressure and heat. They are used for faster sterilization...

Also don't forget to look around surplus places at other schools, perhaps. I have seen autoclaves there, and you might even get lucky and find a working/fixable parr shaker - I have seen many expensive and crazy things at surplus places that appear in just fine condition and probably work.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

overunity33

  • Subordinate Wasp
  • ***
  • Posts: 218
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« Reply #5 on: March 03, 2011, 03:49:54 AM »
somebody on scimadness had a signature: friends dont let friends build autoclaves (hydrogenators).  Buying a surplus one would be a good idea but they actually are looked at the same way as pill presses by the alphabet soup.

solidstone

  • Subordinate Wasp
  • ***
  • Posts: 102
Re: Experimental: Hydrogenation apparatus (modified autoclave or pressure cooker)
« Reply #6 on: March 03, 2011, 04:08:06 AM »
probably wise words overunity, but the autoclaves look almost identical to the bulk parr reactors, even dug through the specs of both to make sure.  The hardest bit would be ensuring theres an inert gas line to bleed in.  I'm proceeding with lots of caution, especially since I'm proposing too work with hydrogen gas.

I'm playing with this as well http://www.sciencedaily.com/releases/2009/06/090623120833.htm.  I have alot of the original data (as I know someone on the original research team).  Honestly hoping that will make lower pressures a reality for these sorts of reductions, but its hard to know at this point.

Regardless, I am going to do a lot of tests before I even consider testing it with hydrogen, and if I do get to the stage were I feel I must test it for a pd catalyzed reaction I will make sure I stay at a far distance and can quench any potential take off reactions before opening the chamber