Rhodium (Chief Bee)
07-22-02 13:55
No 335751
      DIY Catalytic Hydrogenation Apparatus w/ shaker  Bookmark   

../rhodium/chemistry /equipment/hydrogenation.bomb.html
 
 
 
 
    flipper
(Hive Bee)
07-23-02 11:37
No 336099
      You now I love you  Bookmark   

It's beautiful. Thanks Rhodium laugh
 
 
 
 
    sYnThOmAtIc
(Hive Addict)
07-24-02 05:30
No 336354
      I would suppose pvc would make a suitable ...  Bookmark   

I would suppose pvc would make a suitable replacement for the desktop styled apparatus detailed which parr offers? I'd hate to pressurize glass to 50-100psi and have it explode throwing glass and chemicals everywhere.

Also I have seen lately at the hardware store next to pvc cement teflon fiber cement. I bought some and dipped a galvanized pipe in it and it coated it well. It is actually adhered to the metal and does not slide off like teflon tape. I am thinking a 2" galvanized pipe with end capps can be assembeld and have this stuff shaken inside and dried and reapeated seeral times to provide a cheap and functional teflon coat. It says it can be used at pressures up to 2000psi and temps 280c.
 
 
 
 
    epistemologicide
(Hive Bee)
07-25-02 05:55
No 336810
      hailz to you brother  Bookmark   

this will enable me to study and acend some other contrivances of the mind that is your department, all TO SAVE THE PLANET.

hailz and fucking support!!laugh

thank you cheif.

hatred of ontological wastes, and the marathon!!!!
i cook to save the planet!!
 
 
 
 
    SaintCyril
(Hive Bee)
07-25-02 07:15
No 336827
      Try quartz glass  Bookmark   

If you look hard, or happen to know a gas blower, or welder with a hydrogen torch, you could get/make yourself a quartz glass container, maybe if you looked real hard you could find a threaded quatz glass flask which could handle and explosion inside, and just about anything else you can throw at it.  This is what I would do, additionally if you had the treaded glass flask and threaded hose, couldn't you skip over the entire wing-nut/hold down the stopper thing. 

If you were going to use PVC, you might want to look into getting CPVC which can hold higher pressure and is stronger, if you search around you can pind CPVC end caps with and attachment to a regular copper, or steel pipe, there are all sorts of other valves, and attachments also sold for CPVC. 

Anyhow,
Cy

We are the people that your parents warned you about.
 
 
 
 
    flipper
(Hive Bee)
07-25-02 11:51
No 336902
      The big Hydrogen container.  Bookmark   

The big Hydrogen container. How much bigger is the hydrogen container then the reaction-vessel.
Can you have a 10 liter reaction-vessel with a 20 liter container. 
 
 
 
 
    flipper
(Hive Bee)
07-27-02 01:07
No 337496
      This is a very very good read  Bookmark   

It's everything you wanna now about the parr shaking hydrogenator. And the accesoires like special heating or cooling mantels and stuff.

Read this by clicking this link. It's a PDF (http://www.parrinst.com/doc_library/members/3900MB.pdf)

I have still a question. When SWIM wants to do a reaction bigger then say 5 Liters Is a shaking hydrogenator the first option? There isn't a Parr shaker bigger then 2 Liters. There is however a 2 gallon stirred parr hydrogenator. I really wanna have an answer on this question. cool
 
 
 
 
    epistemologicide
(Hive Bee)
07-27-02 04:05
No 337537
      5 litre nom prob  Bookmark   

check the specafications of the step by step adams catalyts guide(rhrodiums site imb zip file called large scale production via hydrogen) that gives you the size and more

hatred of ontological wastes, and the marathon!!!!
i cook to save the planet!!
 
 
 
 
    flipper
(Hive Bee)
07-27-02 12:21
No 337680
      The hydrogen container  Bookmark   

Is it really necessairy to have a container between the H2 tank and the reaction vessel?
How big must it bee in comparison to the reaction vessel. laugh

 
 
 
 
    terbium
(Old P2P Cook)
07-27-02 19:44
No 337759
      Hydrogen ballast tank.  Bookmark   

Is it really necessairy to have a container between the H2 tank and the reaction vessel?
It is not necessary but it is very helpfull to have this ballast. This tank is filled with hydrogen from the high pressure supply tank and then the high pressure supply tank is closed. By observing the pressure drop in the ballast tank as the hydrogen is consummed one can follow the course of the hydrogenation.

How big must it bee in comparison to the reaction vessel.
There is no hard rule. One can do one's own estimation. Say one had a 500 ml reaction vessel that was going to be used to produce MDMA via low pressure (2-3 atmosphere, 15-30 psig) hydrogenation. So, in this 500 ml reaction vessel one would put around 300 ml of reaction mixture containing perhaps 35 grams (0.2 mole) of MDP2P (plus methylamine and catalyst with methanol solvent). To hydrogenate this 0.2 mole of imine will require 0.2 mole of H2 or 4.5 liters of H2 at STP. So if the ballast tank is 1 liter (plus the 0.2 liter of head space in the reaction vessel) there is 1.2 liter of gas space and if the pressure is allowed to drop 1 atmosphere (15 psi) each time before the ballast tank is repressurized from the high pressure tank then the ballast tank will need to be refilled 3 times to provide the 4.5 liters of hydrogen.
 
 
 
 
    terbium
(Old P2P Cook)
07-27-02 23:16
No 337818
      Big ballast tank.  Bookmark   

The only negative that I can think of at the moment to using the bigger ballast tank is the larger volume that (in the case of a hydrogenation) needs to be purged with argon and then with hydrogen prior to the reaction and then vented and purged again after the reaction.
 
 
 
 
    terbium
(Old P2P Cook)
07-27-02 23:49
No 337826
      Vacuum seems a possibility.  Bookmark   

The upper explosive concentration of hydrogen in air is 75% hydrogen. So if you can pump out better than 75% of the air and refill with hydrogen then this should be safe. Even safer would be to do both - pump the air down to 1/4 atmosphere, refill with argon and then pump down to 1/4 atmosphere again before refilling with hydrogen.

I suggest 1/4 atmosphere instead of high vacuum because I am assuming that the reaction mixture will be in the hydrogenator when this is  being done and if one pulls a high vacuum than the solvent will start to boil and bump.

 
 
 
 
    Beaker
(Stranger)
07-27-02 23:49
No 337827
      Vacuum Purging  Bookmark   

I was always taught that using vacuum to purge oxygen before hydrogenating is actually the preferred procedure. However, this is probably not a good idea if you have methylamine or something similar in your reaction mixture, and there may be an explosion risk depending on what your vacuum source is. However, when you finish the hydrogenation and have highly flammable reduced catalyst in the reactor, it is safer to add argon or nitrogen back into the flask when you purge, regardless of whether you use vacuum or not. Also, you usually evacuate, fill, and purge 3x with hydrogen in the beginning, and 3x with nitrogen or argon at the end.
 
 
 
 
    java
(Newbee)
07-28-02 00:56
No 337840
      Ref: Hydrogenation  Bookmark   

Swin always vacumed all the air out of the reaction just until you see bubbles in your solvent in the hydrogenation bottle or glass vessel being used, then purged and vacumed out three times using Argon. After a few accidents with the palladium igniting  with my solvent(methanol) Iswin decided to use a heavier gas, argon instead of nitrogen.

After all the hydrogen is taken up  i usually allow allthe hydrogen remaining in vessel to flow out through wn escape hose leading to the outside .  A small sub tank is best in case of  an emergency you only have enough to load your reaction  vessel three to four times.

NOTE: always have argon flowing into your glass hydrogenation vessel when introducing your catalyst,with any hose about half ways so it doesn't blow your catalyst up in the air. Then flood it with your solvent being used  just enough to wet all of your catalyst , after  you can remove the hose that's inside the chanber and fill your vessel to the desired volume , but never fill  your glass vessel,always leave 1-2 inches clearence. 
 
 
 
 
    java
(Newbee)
07-28-02 02:41
No 337871
      Ref: Hydrogenation  Bookmark   

Max,.......as long as the empty space that you plan to introduce your solvent and catalyst into has been vacummed and purged, as noted , you can turn on that stopcock and introduce your prepared material with the catalyst already included . I guess its because of difficulty of opening and closing the  vessel that you ask this question,  I see no problem in doing it the way you suggest .  In swin experience with Parr  hydrogenators  I  always used the two liter borosilicate bottle with the plastic coating for safety  and the hydrogenation was done as few times to process the 2k  of product namely methamphetamine ,. Swin considered going to a larger unit but as someone pointed out  its as big as it gets for a shaker.   It appears the larger units  are more expensive and  one can process  as much of a large quantities using the two lt. bottle .  Swim processed 2k of meth in 2-3 hours in the chlorephedrine  to meth  reaction using palladium on charcoal in methanol.
 
 
 
 
    hest
(Hive Addict)
07-28-02 13:44
No 338043
      For the tank 5L to one 500mL flask works good (it ...  Bookmark   

For the tank 5L to one 500mL flask works good (it the setup on my parr) I newer have to refill under a reaction, but the presuredrop is big enough to predict how ling the reaction has run.
I newer purg with argon, evac with waterpump is fine.
I only purge (with hydrogen) when im' using H2 at atm. presure (evac, H2 in, evac H2 in)
I don't think you need tha small container, but iff something shit happend's a 5l tank with 6bar is much more fun than a 15L tank with 200barsmile
 
 
 
 
    bartleby
(Stranger)
09-15-02 11:12
No 356502
      possible off the shelf pressure vessel  Bookmark   

Perhaps one of these pressure vessels could be used with minimal modification in a shaker type setup.  They come in both stainless and PVC.  Just a thought.  http://www.hcti.com/vessels/index.htm
 
 
 
 
    ClearLight
(Hive Addict)
09-17-02 01:55
No 357119
      reaction vessels...  Bookmark   


 Good three liter with the clamp will handle everything... they appear on auction sites now and then... you can use the lid with joint clamps on the connectors... 60 psi is ok...
  stirring or shaking will work, rememeber glass balls to increase agitation...

Infinite Radiant Light - THKRA
 
 
 
 
    dwarfer
(Hive Addict)
09-17-02 02:13
No 357124
      easy pressurized PVC hydrogenator  Bookmark   

September 16, 2002

A PVC pipe hydrogenator,
with autogenous H2 production via Al,
and with “shaker” features,
and self regulated pressure,
can be built by anyone who knows how
to wield a hack saw and solvent glue.

(This would exclude Gluefingers Mc Osmium,
I regret to note.)
[Note that the mods have been instructed
to not respond to such insults,
as they are to set a higher standard than this..”:<) ]

Anyway, here’s the quick and dirty:
details available if needed,
though the elaboration of the construct
is not rocket science...

The device is shaped like a capitol
N <like that there: yeah..

The left UP arm (of the N )
has a poppet valve set at 70 PSI t the top,
and the upper end is removable for addition of AL and base or acid. 
(An automatic pressure regulating NaOH “dripper”
has been conceived,
although the size of the Al will determine the rate of production of H2,
so it has not been fabricated..)

The DOWN middle arm (of the N ) delivers
the produced H2 to the right “reaction vessel”. 
The middle arm of the mechanism
can be a smaller size if wanted.
The middle arm should be fitted with a PVC “one way valve” ,
located near the BOTTOM
before intersecting the UP section. 
(This can be eliminated if you are careful,
but WTF: they are cheap..)

The UP arm has a removable threaded end piece
with a 60 PSI poppet valve fitted.

Note that the relief holes on this poppet valve
have been shrouded with a piece of rubber
and hose clamp, sealing them. 
The escape area thus is restricted
to the clearance between the poppet stem
and it’s containment hole. 
(Otherwise, it lets off too much pressure when it unseats. )

In use, the left UP arm  (of the N ) is grasped in a vice
(after wrapping with a towel..),
the reduction liquor and contents
are added to the right hand arm,
wherein they are contained
because of the one way valve referenced 2 paragraphs up..

The base is added to the Al
(or acid, preferentially just because
you are having (one would presume)
an acidic process JUST over to the right,
and who wants a mix if it overflows???)
[truth is, if you leave plenty of headspace
(like 50 %) no problems should be realized
with the base...) <<so far....
and quick like a bunny
 you screw on the end piece,
and wait to see the pressure go up
in the vertical pipe on the right. 

OOPS: did I forget to mention a pressure gauge
on the right hand vertical??  Bad me.

First couple of burps
probably is purging atmosphere,
but after that,
put a balloon over the relief valves
so you can have a floater to give the Kiddees...



Vibration: 

Obtain a variable speed (via rheostat)
water bed vibrator:
you know: the kind you put a quarter in in cheap motels..   If you do not have cheap motels in your vicinity,
a water bed store should be able to fix you up
for under $50.


Attach it to the right hand vertical
near the bottom with plenty of polyfoam layers
(pipe insulation), and U clips,
and carefully   dial in
your preferred vibratory attunement.

Some placement experiments will be needed: 
 control of the amplitude of the vibrations
may be necessary,
by placement of extension boards
from the workbench. 
You can shake the crap out of the tube in this manner..

 I’ve never had a problem
with any signs of PVC cracking,
but I’ve been reasonably judicious.
(about 2" to 3" peak to peak...)

dwarfer
 
 
 
 
    Organikum
(Hive Bee)
09-17-02 16:03
No 357290
      PVC and ketones  Bookmark   

As far as I remember ketones dissolve PVC. Thus MEK is used for dissolving and welding PVC.

This may not be from interest if you plan to hydrogenate a benzylalcohol like pseudo and E, but when you work with P2P or MDP2P which are ketones you should think twice.

Every better junkjard gives you professional high pressurizable vessels. Take a SS one, or coat an usual one with plastic. There are special coatings easy available - not very cheap but worth the penny. Teflon coating is not always best or needed anyway. Think perhaps for a "bottle in the bottle" design", outer vessel steel, inner vessel glass or plastic, pressurized in whole. Letting steel balls bounce around inside the reaction is not t he best idea I ever heard of. Take something like teflon(coated) balls, or other usable plastic. Metal on metal   gives sparks. I would prefer not to force my guardian angel....

If you don´t get something able to hold more than 200psi you should cancel the project. 60psi is farting.

ORGY

~ Love is the law, love under will. ~
 
 
 
 
    dwarfer
(Hive Addict)
09-19-02 01:30
No 357836
      re-fart re-tort  Bookmark   

laugh

The whole durn thing could be replicated
in any pipe you care to specify, with it's
pressure rating.

The "down" arm could maybe be a smaller pipe of
the same material to give the flexibility it would need to enable the vibrator to be effective.

I know pop-off and re-seat valves are available for up to
about 500 PSI.  The left hand H2 generator can be of any size, so H2 production is not limited.

I have TWO variable speed water bed swing weight
vibrators, and attaching both would probably do it,
given the experience I've had with watching the effect
on a 2" steel pipe 4' long.  The frequencies as they
interact are both interesting and powerful.

I've not MADE one of these SS ones,
 so THIS IS a fart..

blushcrazyblush

dwarfer
 
 
 
 
    Organikum
(Hive Bee)
09-19-02 05:14
No 357944
      You ruin your ingeneous layout....  Bookmark   


You ruin your ingeneous layout, Dwarf by sticking on the lousy PVC. So there is no microwave irridating necessary it is preferable to use this old steel, stainless if by hand, or coated with a resistant plastic paint.
And please tell me seriously what you think about the "vessel in vessel" concept. Please?

For me only one way is left to go, after I insulted my HIVE-ZEN master, the fabulous Dwarf.

Mikado.
äh, no,

yep: HARAKIRI

sniff, sniff
ORGY


~ Love is the law, love under will. ~
 
 
 
 
    jimwig
(Stranger)
09-20-02 02:44
No 358309
      looks good tastes good  Bookmark   

glad i didn't step in it

been considering the stainless steel soft drink containers.
anyone know how to test them for pressure without drawing blood?


just read that the containers have  a maximum of 7 bar which i interpolate as being around 101.5 psi and seeing how the commercial par containers don't go over 65 psi i rectum this will work.

the construction on the kegs is such that the more pressure is generated inside the tighter the lids are held in place. catchy,eh? of course the limit is probably the gasket???

don't recall any welds anywhere
.
 anywho these are around for as little as $20 or so. the beer makers seem to love them. that's where i got the dozen or so i have - out of a dumpster behind one of xxxx's best home brewers supply when they went out of business last year.

Lucky and keep on diving.....

 
 
 
 
    Osmium
(Stoni's sexual toy)
09-20-02 04:00
No 358346
      > anyone know how to test them for pressure ...  Bookmark   

> anyone know how to test them for pressure without drawing blood?

Fill them with water and take cover.


I'm not fat just horizontally disproportionate.
 
 
 
 
    jimwig
(Newbee)
09-22-02 22:20
No 359172
      hey i did that to my cat once  Bookmark   

her eyes became as to digital sensors
her rectum as to very low pressure relief valve
and her howl as to the ends of the earth

WATER? - where the hell is your sense of adventure.


and when she got back to the planet - her tailed hairless and smoking - she barely whispered - "may I have another?"
 
 
 
 
    Organikum
(Hive Bee)
09-22-02 23:08
No 359198
      stainless steel soft drink containers  Bookmark   


Yes JIMWIG, so often mentioned so easy to get and very safe. Seems to be too easy - the hard way is prefered crazy.

In europe the KEGs are rated at 12atm aka 170psi, more exact the one I just have looked this up is thus labeled.
Law for the european community says that the burst pressure of such containers has to be min. 8x the rating. So burst pressure is >90atm aka 1300psi. Enough headspace I might say. Yes and the containers have to be made in such a way they will never explode shrapnels flying around, but they will break open in a controlled way. Therefore a weakest point is defined.

But I told thus before - did JIMWIGS cat listen?
Has Schrödinger found his cat?

ORGY

~ Love is the law, love under will. ~
 
 
 
 
    bartleby
(Stranger)
09-23-02 08:21
No 359399
      hydrogenation vessel  Bookmark   

The stainless steel soda kegs are rated for a maximum working pressure of 130 psi (stamped right on the hatch)and there is a spring loaded pressure relief valve on top that will blow if the pressure gets too high.  Swib has seen these kegs in 3,5, and 10 gallon sizes.  There is a welded seam on them - very smooth though and barely noticeable.  The gauge of the steel is light which makes swib wonder about how much of a vacuum they'll take.  The hatch, connectors, and pressure relief valve have O-rings on them that are made of a rubber-like material called Buna-N.  I'm not sure if this material will withstand the catalytic hydrogenation environment, but the O-rings look to be generic and can easily be replaced with something more suitable.  Also, the quick disconnects are available in stainless steel but most of the brewing shops only carry the plastic ones.  Connections to the disconnects are either 1/4" flared or barbed. 
 
 
 
 
    Chicken
(Stranger)
09-23-02 17:46
No 359509
      Automotive NOS tank  Bookmark   

Automotive NOS tanks work very well as the ballast in this size.  NOS tanks are offered in a variety of cylinder sizes such as 10Lb, 15Lb, and a largew 50Lb if you look hard enough.  These tanks are mad eof ver thick metal and have been tested to 8 bar in this application with no problems.