HOME HYDROGENATION This is not an article on how to hydrogenate your home. For that information you would want to consult alt.elemental.architecture, alt.explosions,die.die.die, etc. I am speaking within a very narrowly defined range here. This outlines a specific type of catalytic hydrogenation: the one I know about...don't extrapolate any of this info toward broader chemical theory if yaKnowhatImean. Coincidentally, this process can be utilized in the manufacture of drugs like Methamphetamine and other home remedies. Hydrogenation is a chemical process which involves introducing elemental hydrogen gas to a liquid solution containing a catalyst. The catalyst latches onto the H atoms then gives them up, to bond with the molecules in solution. ~ Elements of Hydrogenation~ CATALYST- The catalyst consists of a metal in powder form which has been sifted into a buffer like Carbon, it is all very fine powder, black and nasty, shouldn't be inhaled and gets all over everything if you're not careful, leaving your fingerprints for all to see. Catalysts come in different concentrations. For example: 10% Palladium on Carbon would be 90% carbon and 10% Palladium by mass, and is expressed: <10% Pd/C>. This procedure describes the use of Pd/C as the catalyst. Other catalysts are used in hydrogenation but I am unfamiliar with them. The catalyst is always settled and filtered out after the process, it is then washed with distilled water, dried, and is reusable up to around 20 times. With this in mind, it's not too expensive. HYDROGEN GAS- The hydrogen is supplied from a pressure tank. A fresh Hydrogen tank contains extreme pressure. For this reason, a pressure regulater is required , fitting a simple valve to the tank is potentially catastrophic. Even pressuring a Parr shaker requires a regulated or low pressure feed. A regulator for a cutting torch is the obvious and best choice. You have to use the regulator and gauge set from the oxygen side of the torch set-up, since it is designed for high pressures. Once you have used a regulator and hoses for hydrogen, NEVER use them for anything else, hydrogen is absorbed into materials and this limits their safe usage with other gases. Smaller gas containers can be obtained from scientific supply houses, they are referred to as 'those little tank things' or 'watchamacallits' and may require different hook-ups. I am unfamiliar with these, but I'm sure it's all worked out. Hydrogen gas is easy to produce yourself, but I have no experience or recommendations in this area. I guess everyone knows that Hindenburgers are char-broiled, or is at least familiar with ledZeppellin album covers...hydrogen is very flammable, doggone explosive, even. POPEYE perceives hydrogen line configurations as two types: fixed hose or detatchable hose. Fixed hose configuration: Exhaust valve->exhaust hose | Reaction vessel<->Hose<->T fitting<->T-fitting <-Regulater <-H tank | psi gauge Detatchable hose configuration: -> exhaust hose / Reaction vessel<->T-fitting<->valve<->quick connect \ | <-hose <-regulater<-H tank psi gauge IMPORTANT: OTHER THAN THE REGULATOR, THERE ARE NO BRASS FITTINGS ALLOWED HERE. THIS PREVENTS PRODUCTION OF WIERD CUPRIC TOXINS..Stainless or specialized plastic, teflon, etc. must be utilized. Hose must be psi rated and neoprene is best. PRESSURE REACTION VESSEL- Where the gas and liquid get together with the catalyst. It must be able to contain (for our purposes) 60 psi, capable of a gas supply hose connection, and an access opening at least the size of a quarter; silver dollar or larger is better, any opening larger than 4" and I would do alot of dry run pressure testing before using, to make sure it will hold. Stainless Steel is the only thing I would use. It's a snob thing. Examples of SS containers which are easily converted: Stove top milk steamer devices as used in home Cappicinno synthesis as well as some types of stove top expresso makers. There are as many varieties of these as there are Yuppies. They have cool little SS valves already configured in. Soda fountain equipment. For larger batches, or mandatory life sentence quantities, the refillable containers that soda fountain syrup comes in are excellent (they're about 6 gals), also the tank on the CO2 maker. These systems are phasing out right now commercially and components are surplus everywhere. Can also be ripped off from the little fenced in area behind the local convenience store. Glass is used commonly, but I don't like it. There is no advantage in transparancy for this application. You have to be able to wire or clamp a stopper and design a hose barb that won't pop out and guess at the psi capacity. There is Sci-glass spec'ed for this. Chemical resistent polymer constructed pump garden sprayers aren't bad and almost ready to go like they are. Come in all sizes, psi rated. Very economical, I always worry about polymers in the presence of benzene, diethyl ether, etc., but haven't actually had any bad experiences. Polymer gasoline containers are also used, but hose connection takes some doing...not preferred. SHAKER- The Pressure Reaction Vessel is fastened to this mechanical device...imagine a paint shaker...the paint can is your pressure reaction vessel...that's it. There are as many home hydrogenator designs as there are ambitious speedfreaks. Some are brilliant, others are pretty damn funny, still others are unintended amateur militia ordinance or automatic 911 dialers. In deciding on, or tweaking out your own shaker device, there are a few things you should know. As mentioned, the contents of your reaction vessel are a liquid solution, which is flammable, and a solid catalyst in powder form. The catalyst is wha-chaCall PYROGLYPHIC (SP), implying potentially EXPLOSIVE. Into this you are preparing to pump in HYDROGEN and fucking shake it ?!! Proper understanding of handling the catalyst is required. The catalyst is dangerous when dry and floating around in the air like dust, especially around oxygen...see grain elevater explosions-Texas City Disaster. Keeping the catalyst wet throughout the entire procedure is key to survival. This is also why the Pressure reaction Martini is 'shaken not stirred' (kudos jamesBond). Those of you who have utilized mechanical or magnetic stirs, know that the liquid occasionally sloshes up pretty high on the inside of the vessel, the catalyst could easily slosh up there, dry out, then dust...you know the rest. With an effective shaker, the whole inside of the vessel is constantly washed with solution so this cannot happen. Therefore,this is the minimum level of activity required to prevent incident. Shakers also create the most desirable exposure of catalyst surface area to the gas, increasing efficiency and uniformity of the reaction. Here are some approaches to shaker devices Straightforward approach-go out and buy a paint shaker then design a reaction vessel to fit it. (fixed or detachable hose config.) Bizarre approach- The Milwaukee Skateboard-> You will need: A variable speed SAWZALL, a skateboard, a C-clamp, four 1x4's 12" long, A workbench with a sturdy vice, electricity. Place the body of a Sawzall in a vice so that it is parallel to the bench and turned sideways, put two blades in the Sawzall by stacking them (short blades). C-clamp the blade tips to the stern of the skateboard which rides on the benchtop. Nail the 1x4's together so as to imitate two lengths of angle iron each a foot long. Lay the wooden angle pieces on the bench on the port and starboard sides of the skateboard and parallel and not so snugly so as to prevent travel. Tack them to the bench. You now have a little bobsledTunnel sortaThing for the skateboard to run back and forth within. Attach the reaction vessel (a cylinder) to the skateboard by laying down on it's side and duct taping it on. Set the sawzall speed then use the trigger lock. (detachable hose config.) The aerobic approach- Fasten a rope to the pressure vessel, hang it from the ceiling, shake it back & forth by hand on the dangle...tiring, need partner for shift work, not recommended. (fixed or detachable hose config.) The high dollar approach- Buy a Parr shaker. For about three grand. I held onto one of these for an ex-partner/friend who took a mandatory retirement in Folsum for 3 to 5...and had some occasion to try it out. They're bullet proof, precision machined, over built. These are designed for mini-yield experimentation, not production. The model I'm familiar with had a meager 1L capacity yet weighed approx 200 lbs. and took up 42"x27" of floor space. The bottle clamp was not tweakable to greater capacity...the motor was NOT sparkless, the exhaust valve seat was way too small and clogged with catalyst every single time. Before returning it to the owner, I had to change all the bolts from carbon to stainless myself, after minimal acidic exposure rusted them out. Totally unimpressed...not POPEYE approved. (fixed hose config.) POPEYE's bathtub Sailorman approach: I thought this one up myself, it is fairly intuitive so I'm sure others have too. Buy a bunch of those suction cup rubber mats and stick them on the sides and bottom of a bathtub. Fill the tub. After pressuring the reaction vessel, detach the hose, orient the cylindrical vessel horizontally, float it, then spin it, rocking end to end slightly. POPEYE recommends this method because if there are any leaks, they are evident from bubbles in tub. (detachable hose config.) ~Standard hydrogenation methodology~ 1. First combine ingredients of reaction mixture in safe container. 2. In a seperate beaker, carefully add dry catalyst, them moisten with a non-reactive solvent, Hexane is common. 3. Introduce 1/3rd reaction mixture to catalyst 'paste', stir briskly, quickly transfer to pressure vessel. Repeat. Repeat. Pressure vessel should never exceed 2/3rds full to allow for sloshAbout. 4. Seal pressure container, afix hydrogen feed line, and pressurize container to 40psi. Now realign valves and release the pressure into a safe exhaust. This is called 'purging', and is done three times. 5. Now pressurize to 60psi, cut off H feed then shake (or spin) 6. Continuously monitor the pressure gauge and when the pressure within the vessel falls below 20psi, repressurize to 60psi. When uptake of hydrogen ceases (after 3x's is average) reacton is finished. 7. Remove pressure vessel from shaker and orient in a vertical position, let rest about 15 minutes, then slowly release pressure into safe exhaust...it is not unusual for the contents of the container to aerosol out with the gas resulting in loss of product and temper, for this reason, POPEYE recommends you design a simple liquid trap (aspirator) which is afixed along the exhaust line at this point. ->exhaust HOSE->->->-> ->->->exhaust | | v ^ _|_|_ \ / \ / <-two holed rubber stopper GLASS BOTTLE G LA S S B O T T L E G L A S S B O T T L E G L A S S B O T T L E G L A S S B O T T L E Troubleshooting: The hydrogen is not being taken up. Not using enough catalyst, check recipe. Catalyst is old or no good. Your recipe is no good or you've goofed the chemistry. Have you cut off hydrogen feed b-4 shaking as mentioned in step 5? Your psi gauge is malfunctioning or is fouled with catalyst. Line or valve is fouled with catalyst. The hydrogen is endlessly being taken up. You have a leak! Filtering Catalyst From Reaction Mixture Methanol is used as a solvent/carrier in this description...appropriate substitution where necessary. Combine contents of aspirator and pressure container into a glass vessel which can be stoppered. Rinse containers with methanol and add. The holding vessel should then be filled to the top with methanol to purge the air and prevent any wierd oxidation catastrophes, then stoppered. Let sit for halfAday until Pd/C settles out. Carefully suction out the reaction mixture without disturbing Pd/C sedimentation. To increase yield, refill container with methanol and repeat last step. Now, filter solution until it is free of catalyst, adding more methanol to carry solution through filtercake as necessary. Vaccuum or distill off Methanol leaving product. Wash catalyst w/ distilled H2O and air dry for re-use. *final disclaimer* I am not 'in the business', I have grown weary of 'the business' and worrying about the cops. It is interesting to note that the existence of one is very much dependent upon the health of the other. You would do good to avoid both. If you think about it, that is where the real value of this Newsgroup lies. -Peace -POPEYE ----------------------------------------------------------------------------- Subject: the holy hydrogenator Combine 100 gms L-ephedrine and 890 mls. glacial Acetic Acid in a 5L ehrlemeyer on a stir plate and begin stirring. Slowly add 66.56mls Sulphuric Acid at a rate which will keep the temperature below 71C. In a pressure container, a paste is made up of 65 gms. Pd/C and enough glacial acetic to moisten, the contents of the ehrlemeyer are then added. The container is sealed and heat blanketed so that the temperature can be held at 38C. The dieties are called upon, the sacred valves are gently fondled, and a holy purge is brought about. The vessel is annointed with the most elemental of all gasses. Now the sacramental hydrogenation ceremony is carried forth. The straining of the catalyst shall follow and all that was before, will be no longer, and in its place shall be born anew, and it is good, and it is freebased, so that the primordial elements and acids be torn asunder that they shall be cast aside. And the oil is extracted, and the oil is acidified, and from the oil shall the pure white crystals emerge. And it was done. Yea, though it was done in ancient times, it did come to pass. And those who witnessed, were heard to say, "These are not the promised yields!" and doubt was cast even upon the virtue of the chosen few crystals which came about amidst a gnashing of teeth, wringing of hands and a great burning of the eyes. And lo, the time did pass, until one day, he who did cometh from the sea, though he be not a fisher of Men, but a Half Blind Sailor, turned to his brethren in the holy land of INTERNET and cried out, "Hear me, Ye ministers of the Elements, have my sins and faltering ways wrought these fallow fields of hollow crystal, or was I led astray by false scripture unto a fool's quest, wherein no man could but cast his ephedrine into the sea and harvest only wind. What say Ye?...for I know not where to lay my faith, or place my trust. Is this a travesty of the cheministry, a fuming trial of Meth oozala's children..or have I but mine ownself to blame for worshipping not even at the high school alter of the organics and handling the Glass of Ware not in the traditions of the elders, but like a tamer of scooters who shuns his own somnabulistic ritual. You may testify by E-Mail or before the flock. When you plant ice You're gonna harvest wind -Half Blind Sailor ----------------------------------------------------------------------------- Subject: Home hydrogenation-precusors Date: 1995/07/19 My anonymous Net Pal asked me to post this for information purposes only. -oLIVEoIL *standard disclaimer* It should be obvious that I am not a chemist. Merely a chemHacker experienced in certain chemical processes/techniques. This describes illegal activity, this is posted cross-eyed and double blind anonymous, I could be making this up, I have already been publicly denounced, don't try this in Tupperware... I have hereby disclaimed, you have been warned....be careful in realTime, remember to keep your mouth shut. All responses expounding ethical and/or moral pretences will be mutilated for entertainment purposes and your addressing circulated amongst low-life scooter-trash. *disclaimer over* Whenever I've purchased supplies from commercial distributers, I forged a Purchase Order (using a different boxy bold font for the PO number, so it looks like automatic consecutive printing) fake company (related to purchase) fake address on a fictitious street, space for phone number left blank (sorry not hookedUp yet). A PO facillitates filling the order and the lack of one is a red flag indicating that you are not a business in the legitimate taxpaying sense. Since we all have computers, formatting a PO is worth the trouble. Supplying a PO also helps you to tell the difference between clerks who may need info just to fill out in-house paperwork for banal reasons, and nosey, brainwashed, gung-ho, bootlicking, snitchPrick targetheads who will invariably ask for verification or ID. If the Bullshit on the PO ain't good enough, fuck'em, walk out. And while you're at it, tell them that a legitimate businessperson, such as yourself, has no interest in being shitlisted with Jack-booted government thugs just because a bunch of slimy dope fiends can't control themselves and everybody else refuses to mind their own fucking business. POPEYE never slinks out like a common criminal. In the interest of bandwidth preservation, I will not belabor common sense variables such as flagrant display of auto liscence plates, paying with personal checks, stomping in on DocMartins clad in raunchy crankOil stinking leathers with your Jolly Roger headband and studded chain mail riding gloves, taking direct routes to/from suppliers and labs and/or customers, selling 1/4 grams directly from a fully stocked lab out in the garage of your family home, a virtually endless list of possible no-brainer fumbles that will cost you everything. Pd/C catalyst: Purchasing- I will leave it up to others to decide just how "watched" we all are, but will say that I have purchased 100 gm bottles Pd/C from chem supply houses without being asked to sign anything or produce ID, that may have been the 90's, organic memory is partially chemErased, could be different now, call and ask, use a pay phone. Stealing/Bribing- Since POPEYE actually IS a common criminal, behold: petroChem plants and many oil refineries use this in cracking towers by the ton. It comes in bags like concrete in bulk. Plants have security against industrial sabotage and politico-terrorist corporate paranoid delusional contingencies so it's best to hit railroad cars en route (obviously while they are stopped somewhere) or bribe truck drivers or plant workers to steal it for you. Good product can be much more persuasive than money, since these folks are well paid but overworked. Hydrogen Gas: As mentioned this can be acquired at chem supply houses but I don't know if you must sign for it or if they put little bugs or homing devices or detonators in them, or follow you home in a helicopter. A well stocked welding supply house. It is used in specialized welding, glass blowing, neon sign art, sci glass and any application that requires a totally clean burn but not extreme temperature. Whether you are leasing a tank from the supplier, or purchasing one, you will be required to register it. This is a theft discouraging thing that all welding supply houses engage in. A letterhead may suffice. POPEYE is a Biker and always knows lots of welders, I had someone get one for me, on pay or barter, when I was into this sort of thing. Stealing/bribing-too much trouble to steal, never steal something you can't run with, huh? Who me? What hydrogen tank? Give Me Liberty or Give Me Meth -POPEYE