Author Topic: DIY Catalytic Hydrogenation Apparatus w/ shaker  (Read 5600 times)

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flipper

  • Guest
You now I love you
« Reply #1 on: July 23, 2002, 11:37:00 AM »
It's beautiful. Thanks Rhodium  ;D

sYnThOmAtIc

  • Guest
I would suppose pvc would make a suitable ...
« Reply #2 on: July 24, 2002, 05:30:00 AM »
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

  • Guest
hailz to you brother
« Reply #3 on: July 25, 2002, 05:55:00 AM »
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!! ;D

thank you cheif.

hatred of ontological wastes, and the marathon!!!!
i cook to save the planet!!

SaintCyril

  • Guest
Try quartz glass
« Reply #4 on: July 25, 2002, 07:15:00 AM »
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

  • Guest
The big Hydrogen container.
« Reply #5 on: July 25, 2002, 11:51:00 AM »
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

  • Guest
This is a very very good read
« Reply #6 on: July 27, 2002, 01:07:00 AM »
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.  8)

epistemologicide

  • Guest
5 litre nom prob
« Reply #7 on: July 27, 2002, 04:05:00 AM »
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

  • Guest
The hydrogen container
« Reply #8 on: July 27, 2002, 12:21:00 PM »
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.  ;D


terbium

  • Guest
Hydrogen ballast tank.
« Reply #9 on: July 27, 2002, 07:44:00 PM »
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

  • Guest
Big ballast tank.
« Reply #10 on: July 27, 2002, 11:16:00 PM »
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

  • Guest
Vacuum seems a possibility.
« Reply #11 on: July 27, 2002, 11:49:00 PM »
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

  • Guest
Vacuum Purging
« Reply #12 on: July 27, 2002, 11:49:00 PM »
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

  • Guest
Ref: Hydrogenation
« Reply #13 on: July 28, 2002, 12:56:00 AM »
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

  • Guest
Ref: Hydrogenation
« Reply #14 on: July 28, 2002, 02:41:00 AM »
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

  • Guest
For the tank 5L to one 500mL flask works good (it ...
« Reply #15 on: July 28, 2002, 01:44:00 PM »
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 200bar :)

bartleby

  • Guest
possible off the shelf pressure vessel
« Reply #16 on: September 15, 2002, 11:12:00 AM »
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

  • Guest
reaction vessels...
« Reply #17 on: September 17, 2002, 01:55:00 AM »

 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

  • Guest
easy pressurized PVC hydrogenator
« Reply #18 on: September 17, 2002, 02:13:00 AM »
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
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...) <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

  • Guest
PVC and ketones
« Reply #19 on: September 17, 2002, 04:03:00 PM »
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. ~