Building a Hydrogenator for Newbees

[Cept]

Where would construction of a hydrogenator(couple liters max) capable of reducing phenylalanine at approx. 90psi begin? Stainless Steel everything, hydrogen inlet, strong mechanical stirring and how? Is a ground neccesary/static dangers? Any info treasured.
   It is dangerous for people to experiment with this who have not had hands-on experience.

[Cept]

Find a stainless fire extinguisher and clean it out. if it has not the nozzle/adapter to facilitate hydrogen introduction then you'll just have to go to the local gas shop and find the right shit.
   why will stainless steel resist oxidation or reduction under intense pressures? UTFSE! that's why! remember VSEPR. remember sammy jenkis.
   Oh i know, but i'm having fun sitting here talking to you.
   maybe shaking could replace mechanical stirring? crazy but maybe just doable.
   I can Remember all those dreams, nonstop 24-hour-wackers and my sore fucking arm. didn't mind then, don't mind now. silliness is manually stirring a 10lb oxone epoxidation with a stick wrapped in teflon and that goddamn gallon of denatured stink...it's interesting even if it's only dreams right?
  but something stands out in my mind, something about a hollow stirbar to max out the surface area in contact, no sticks here.
   don't worry y'all, we'll figure it out...
smile you fuck! i'm out into the world to integrate, have a nice day bees.

[jimwig]

stainless soda containers - the type used for on-site mixing of syrup and CO2 - are available. (Found six or seven behind a home made beer brew store)

They have some OTC thread already on top. And they will probably do the PSI you mentioned. More info is on line.

Let me know your thoughts and/or results. JW

[MnkyBoy78]

There are still a few home brewing online supply houses that have 5.5 gal kegs you speak of for ~20 USD.  I'd recommend you purchase all new o-rings for them though.  They are pressure tested/rated at 120 psi.  (These kegs used to be soda kegs, but when Pepsi switched over to bags of syrup they got rid off millions of these kegs)

I dont recommend the small kegs (~ 1 gallon sized ones).  These are not rated for nearly as high of pressure and are not double lined w/ a vacume barier in between like the old soda kegs.

[Cept]

So lemme get this straight; stainless steel seems to be an acceptable vessel material when reducing/hydrogenating? Or are there limitations i.e. will it oxidize or would chemicals oxidize, me no knoweth. Was thinking about all sorts of hydrogenation lately maybee-not.

I maybe not checked out the DUPONT performance Finish plant the other day, hopefully lookin for a jobby job. Was looking into that internal teflon bake-job tank coating concept on a propane tank internal.  Those fuckers! Wouldn't even let me in, or take an App, some security issue from a fat donut eating (he really was!) fuck, ooh if i could get a job there, i'd make it okay... anyhow...

i went and picked up a Carlo Rossi wine-jug, not forgetting to get fucking hammered off the lovely 10% grapejuice contained within. I won't try and remember names of posts cuz i've read far too many lately and they are blurring into a confusion (not incomprehensible confusion to alleviate your concern), but i've been downloading shittons of stuff on all the alphabet letters here..building a comp for the grandkids yah know! and much thoughts dedicated to The Rossi, maybe KRZ (masterplan) or whoever mentioned it could be set up to take some pressure...i dunno ...maybe 30...maybe 90...psi ob...thinkin oic acid of amph?

maybe someone found 300 grams of phenylalanine on his doorstep in a cradle one day and is dying to reduce it...maybe not.

maybe somneone snatched a bottle of labgrade nickel sulfate hexahydrate (hexa? i think so, i'm so sleepy, no stihzel lately), and is waiting to fuck with all sorts of U-Cats, maybe the STP Urish-W6 (i think it tis, shady some wise bee said twas kinda hard) maybe hoping aluminum foil is useable in place of aluminum grains

maybe just get into all sorts of hydrogenation of PhenylALanine hopefully with nickel cats at slight pressures, although some other wise bee shot down some shit at Rhodiums site the other day, and i didn't know how to feel cuz he seemed accurate, probly pertained to low pressure hydrogenation of eph and phenAL.

dreamt of Fucking up a RP-I2 using dirty (pink) stufdafuf and wack ratios cuz of greed (common prob with stihzelheads), get this!: 110g Stuf, 140g Dine (via geez's mucho primo pretty shiny slow-noogen-style 7%, and 30g RP (FUCKING THIRTY!!! OMG!(hearing half-a-pint in my head saying "BUT NOBODY IS GETTIN MY RED PHOS, NOBODY!!! HAHAAHA", well, mine went back to him cuz he loves it! maybe me too.)

maybe up all night, maybe not, maybe used time released WWs and gots beautious stihzels on the skihzel-undrizheler (unwetter? haha), yield is probly good, went nuts on ratio this time: 12grams Ephdasufdadrinedafuf (hehe), 14grams Dine, 8grams Redphos. 7grams water, and a few more grams at 3 hours, twas done in 4.5 hours maybee-not and stihzel pictorials seem to indicate full conversion (no pinwheelios and much nice straightened stealth bombers (or should i say Stihzelth bombers(heheahah)))

maybe wondering how to make sodium metabisulfite into sodium sulfite to do the hydriotic (or hydriodic?) via Dine and Water.

maybe about to puke from the copper stink from the cheap copper condenser from home depot, cheap though.

maybe too concerned with xtracting hydrocodone syrup and hyping it up

maybe too worried i'll forget to research the orgasm chemical, if there is one.

maybe too worried that 'shadow people' are coming from midcook vapor phosphine lovelove,

and most off all the maybee-not really eye-burning hateful benzyl chloride that methinks will go to benzaldehyde via DMSO and sodium bicarbonate? just cannot take the halogens anymore...mehates them...i'll have to let you go now, it's been 5 days and she's callin, but for what it's worth i could have went to the kitchen 5 minutes ago, i just prefer to sit and talk to my friends...

have nice day cept

ps: you may disect this post and classify into proper forums.

pps: or just delete if it annoys you. byebye.

oh yes and thinking of electromagnetic vibrating 'holey' contraption for replacement of mechanical stirring and facilitating construction of the newbee hydrogenator thanks to organikum,. cuz he's the best.

[foxy2]

dreamt of Fucking up a RP-I2

From the looks of that post you must have had a successful one.  LOL.


maybe KRZ (masterplan)

If I recall correctly KRZ himself admitted that he was bullshiting about the "masterplan".  I think scrapeing is probably a better idea than blowing yourself up with a master bomb of phenylalanine.

[Rhodium]

Yes, "the master plan" is bogus. There has been only one article published ever on the one-step reduction of an aliphatic carboxylic acid to a methyl group, and that uses Et₃SiH and B(C₆F₅)₃ - nothing for hobby chemists. The article in question can be read here:

Post 194986

(Rhodium: "First published direct reduction of COOH to CH3", Serious Chemistry)

[Snakebyte]

I would like to construct a low pressure hydrogenator for producing MDMA from ketone.  I searched everything(i think) on the subject but i still have a few questions for bees who have knowledge of it. I would also like to state that I have no previous experience with hydrogenating anything, but I have worked with high pressure cylinders with oxy-aceteline welding tanks.
1. Since it will only be pressurized to about 35psi (Ritter says works damn well), will a plastic or polypropalene vessel work as well as stainless steel? I have my eye on one of those plastic 7L pesticide sprayers.

2. Will magnetic stirring be good enough?

3. At that pressure and capacity will evacuating the vessel and purging with hydrogen be safe enough or should one purge with argon first?

[terbium]

1. Since it will only be pressurized to about 35psi (Ritter says works damn well), will a plastic or polypropalene vessel work as well as stainless steel?
You don't need any pressure above atmosphere. With Adams catalyst at one atmosphere the reaction will procede rapidly. You can use an erlenmyer flask as the reaction vessel.

2. Will magnetic stirring be good enough?
Yes, or with flexible rubber tubing for your gas connections, you can even shake by hand.

3. At that pressure and capacity will evacuating the vessel and purging with hydrogen be safe enough or should one purge with argon first?
It is certainly much safer to purge with argon both before and after. This is especially true when one is engaged in an activity where you don't want to risk attracting any attention.

If you are going to skip any argon purge then skip the one at the beginning. The Platinum oxide will sink to the bottom, under the solvent and not be any hazard until it has been reduced. Just be certain to purge well with hydrogen to remove the air. After the reduction is complete then the platinum oxide has been converted to highly active and pyrophoric platinum black so this is when an argon purge is most important.

I have posted here before about atmospheric pressure hydrogenation of P2P-methylimine to methamphetamine using Adams catalyst in an erlenmyer flask hydrogenation vessel.

[Snakebyte]

Thanx for the good info Terb.  Do u know if Adams catalyst is watched in Canada?  I checked my chem supplier and its not on their list.  Anyone know where to aquire some?  Also, what about Urushibara catalysts talked about on Rhodiums site?

[terbium]

Better to make your own Adams' catalyst. Adams' catalyst can be made from platinum metal. You also need concentrated hydrochloric and nitric acids to convert the platinum metal into chloroplatinic acid. You then precipitate the chloroplatinic acid with ammonium chloride to form ammonium chloroplatinate and fuse the ammonium chloroplatinate with (molten) sodium nitrate. The sodium nitrate is melted in a ceramic dish using a propane torch and a thermocouple is handy for monitoring the temperature. The procedure that I used to use is from Vogel, 3rd Ed.

[jemma_jamerson]

than the process of making adams catalyst

from

Large scale meth production via catalytic hydrogenation
(zipped word doc)

at rhodiums, if your a hobby chemist, bee carefull with things like adams catalyst,

terb did you ever read that process, it look fucking dangerous.

[terbium]

terb did you ever read that process, it look fucking dangerous.
I just now glanced at it. It seems about right though the author is misinformed about the dangers of handling Adams' catalyst. Adams' catalyst (PtO2) is not pyrophoric and does not require any special handling precautions. It is only after the catalyst has been reduced to platinum black that it becomes capable of starting fires. WHich part seemed dangerous?

[zero_nrg]

I think these could be interesting homemade hydrogenation vessels and they come in SS

http://www.hcti.com/vessels/index.htm

I have a question for those familiar with hydrogenations:  It has been suggested that using SS soda kegs as hydrogenators would be a good idea, but is it dangerous to have a vessel that has a volume that is far greater than that of the reactants?  If yes, do you just compensate with more solvent? I seem to recall reading somewhere that it is dangerous to have catalysts such as platinum black get splashed somewhere in the hydrogenator where it then dries because of insuffincient shaking or stirring.  Also, with pro hydrogenators (Parr etc) how do they prevent catalyst from getting splashed up into the lines that supply the hydrogen? -zero

[terbium]

I think these could be interesting homemade hydrogenation vessels and they come in SS http://www.hcti.com/vessels/index.htm
The are badly proportioned - too long and narrow. I guess they would work but it will be more of an effort to get good contact between the liquid and hydrogen. Besides, catalytic hydrogenation of MDP2Pmethylimine proceeds rapidly at atmospheric pressure.



I have a question for those familiar with hydrogenations:  It has been suggested that using SS soda kegs as hydrogenators would be a good idea, but is it dangerous to have a vessel that has a volume that is far greater than that of the reactants?
It will make purging the vessel with inert gas and hydrogen much more time consuming. And, you will loose more product on the walls of the vessel.

If yes, do you just compensate with more solvent?
No, you should compensate with a smaller vessel.

I seem to recall reading somewhere that it is dangerous to have catalysts such as platinum black get splashed somewhere in the hydrogenator where it then dries because of insuffincient shaking or stirring.
It only becomes a problem when the catalyst comes into contact with a combustible mixture of air and solvent or air and hydrogen. This is why you should flush the hydrogenator with argon after the reaction is complete and then wash down the walls with solvent or water as soon as it is opened.

Also, with pro hydrogenators (Parr etc) how do they prevent catalyst from getting splashed up into the lines that supply the hydrogen? -zero
Up into the supply line? Hmm, don't stir so hard?