XeonTheMGPony
International Hazard
Posts: 1636
Registered: 5-1-2016
Member Is Offline
Mood: No Mood
|
|
SO3 Succes with basic set up!
http://www.sciencemadness.org/talk/viewthread.php?tid=65358#...
http://www.sciencemadness.org/member_publications/SO3_and_ol... < What I based this off of.
http://www.sciencemadness.org/talk/viewthread.php?tid=4409 < Long discussion on Ortho / Meta Phosphoric acid and uses
I used the Phosphoric acid method.
I re-distilled a large batch of sulfuric acid to concentrate it and clean it, this usually leaved about a 50Ml or more of tailings.
Once the distillation flask had cooled I loaded in a test tube 50ml of phosphoric acid and heated slowly till it was at read heat then put my torch at
full till the test tube was a solid faint red glow.
I allowed this to cool to the point it was pourable then added it slowly to the H2SO4 tailings. Immediately a fog appeared but stayed with in the
flask.
I assembled a short path distillation set up then wrapped a part in a damp paper rag, and slowly heated the distillation flask, the mantle surface
temp was 450c distillate came off much cooler.
Seems this reaction is very forgiving of proportions as I mostly eye balled things yet got good smooth results! So long as the Phosphoric is heated to
max dryness (Dull red glow for at least a minute.
On dismantling (Out side after it all cooled) I got the tell tale fuming and when doused with water the residue hissed and popped
Next run I will give more quantitative details but for now I wanted to show how available this really is!
   
[Edited on 28-8-2017 by XeonTheMGPony]
|
|
|
elementcollector1
International Hazard
Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline
Mood: Molten
|
|
Interesting! If you want to try making sulfur chlorides, this might provide a good path to thionyl chloride, an extremely useful drying agent.
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
|
|
|
clearly_not_atara
International Hazard
Posts: 2692
Registered: 3-11-2013
Member Is Offline
Mood: Big
|
|
I don't know how this could possibly make thionyl chloride. Sulfur would have to be reduced by something, plus SOCl2 is more dehydrating than HPO3.
However, I do think that if you can make SO3, you can also make ClSO3H by adding HCl (g), and chlorosulfonic acid can be distilled and used to make
tosyl chloride among other things.
|
|
|
Metacelsus
International Hazard
Posts: 2531
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
|
|
clearly_not_atara: The process for thionyl chloride involves reacting SO3 and SCl2.
XeonTheMGPony: nice job!
|
|
|
XeonTheMGPony
International Hazard
Posts: 1636
Registered: 5-1-2016
Member Is Offline
Mood: No Mood
|
|
Thanks! I Forgot to mention this was 24/40 and the vacuum take off was wrapped with damp cotton as a scrubber. The black plug that is seen was put on
for the cool down to keep air out of it as it was some what humid.
The receiving flask is 100ml of 98% H2SO4 that was put in the freezer for 20min
Need to buy some bottles of drain cleaner acid to distill! will repeat with the tailings again! as they are most certainly 98% by then! Reason I leave
them is they have crystal contaminants present but this did not seem to interfere in the least with the reaction!
Atm my use of the SO3 is to make concentrated sulfuric acid Once I have the rest at 99% I want to ampule several 5ml to 10ml of SO3 for when needed
that'd be when doing the above will be viable, but looks very promising given how well a ruffly eye balled amount worked!
[Edited on 29-8-2017 by XeonTheMGPony]
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
