-------------------------------------------------------------------------------
Simulator

LaBTop your answerwas a litlle-bit difficult to swallow,I apreciate your concern
about my safety,I realy do,but after reading back what I have written till now,I
can't see what is so differend compared to the regulars on this board. First of
all,its my friends problem and I only have offered him some help by looking
around on the Net if there should be a expert who will give him some advice to
solve HIS problem. You are right about my education in chemistry,I am a
sculpturer. But in this caseis it "the cripple who helps the blind",I have a
computer but not the necessary "flight hours" and my friend ... well he has
other means of support and a bike. So now you know some backgrounds.....and
maybe you will stop to bite me. About the methode my friend explained to me the
following.

If he should make that product he would use a low-pressure S.S autoclave with
1/4 space for the Hydrogen gas,a mixer motor on top and the shaft made leakproof
by a mechanical seal to stand 5,0 bar pressure and approx. 0,5 bar vacuum In a
large fridge he should cool the (big) steel cilinder MeNH2 liquid gas,he should
lift the cilinder with a(takel zoals gebruikt in garages) in a near horizontal
position just till above the fridge. With a flex.s.s hose is the cilinder
conected to the autoclave,between the sealing and the lift he would make a scale
(ulster)to be able to weight te amount of gas he should use.

He think to know that he should use:
1.500 ml PMK (MDP2P)
1.000 ml MeOH
1.100 ml MeNH2 (liquid gas)
10 gr Platinum IV oxide (Adamscatalyst)

When those chemicals are in the autoclave he will evacuate the autoclav to a
vacuum of approx. 0,5 bar to get rid of the oxygen. Then he should open the
Hydrogen bottle for a short moment till approx.1,0 bar,and then evacuate a
second time to be absolute sure all the oxygen is out.

He should then start the mixer motor( brush-less type in case of a Hydrogen
leakage) and then he should open the Hydrogen to approx.3,5 bar. By adjusting
the pressure between 2,5 and 4,0 bar he could keep the temp. around 50 C and
never higher than 60 C. After ca 2 hours the temp will possibly go down,to
control the uptake of the Hydrogen gas he should close the bottle and watch for
a periode of 10 minutes if the pressure in the autoclave gets lower in that case
open up the bottle for a view minutes more and otherwise the reactie is stopt
and could he after a couple of hours drain the autoclave. He should use a
Buchner filter on a vacuum bottle with Whatman no 401 filtering paper,he expect
that other type of filters makes this filtering of the Platinum powder a endless
job He would then destill.(open without vacuum)the MeOH,the MeNH2 and the water
out. Change the reciever bowl and by approx.150-160 C at 20mm/Hg the oil will
come over with a 90% yield(depends on the MDP2P) For making the cristals he is
very oldfashioned and thinks with 1 ltr oil in 7/8 ltr cold (4.0 C) Ether and
HCL bubbles out of the steel flash to make approx.1.1 kg.

And all this is not possible with the aq.MeNH2 40%w/w and even with the MeNH2 on
MeOH base he expect there will be no result (but maybe the last fact hase to do
with a wrong calculation of the amount/percentage

-------------------------------------------------------------------------------

     LaBTop
     Member 
   posted 05-15-99 09:27 PM

Now we know each other, let's start cooking!

Ingredients:
1800 ml 98% MDP2P (PMK)
1200 ml 98% Methanol
1200 ml 99% MeNH2 liquid gas=..... gram
24 gram PlatinumIV oxide

Switch your vacuumpump on, connected by valve to the system.
First you mix the PtOIV with the PMK, because this can not burn!
Then you fill this mix in your clean and vacuumed hydrogynator,
with the help of a deep SS- funnel with a valve under it, welded
on top of your hydrogynator. Fill the funnel and let suck in, but
not totally, close valve and fill funnel again, etc. Let no air come
in.Then you fill the MeNH2 through your SS flex.hose,preferable
also with a valve inbetween (Valves are a necessary safety
precaution for pressure-BOMBs!: they tend to become BOMBs when
oxygen comes to the reaction....) Do not forget to vacuum the SS
hose up till the gascylinder also, before you let MeNH2 in.
As the last you fill the Methanol through your SS funnel.
You close all valves, except the valve to the H2 cylinder ( suck the
SS pipe to the H2 cyl. also vacuum!
Stop your vacuumpump ( after closing its valve!).
Now you warm up the hydrogynator to 50-55 C and keep it there.
Open the H2 gas valve and bring the whole thing to 3,5 atm.
Not higher or lower!Keep there!
NOW you start the mixer and not earlier!Or poisonous byproducts
will be formed and influence the reaction badly.
Let react for 30 minutes.
During this time the temp. will rise 5 to 9 degrees Celsius. As soon
as the temp. drops 3 to 5 degrees the reaction has ended.(30min.)
Take the pressure off and suck by means of your vacuum the last
H2 gas out and then let clean air in the system.
Now you tap off your raw base ,in a metal bucket, it's hot you know,
filter it and distill it, make crystals.(Re-use your PtOIV!)Yes, 1:1,1.

A good extra read is " Home Hydrogenation" by Popeye. You can find this on
Rhodium's site on the Lycaeum. He gives a lot of small details which you surely
should read.
