Need help convert bmk 5449-12-7 to free base A-oil

[Saul]

yes iam now making my first test with 250gr cas 5449-12-7 and phosphoric acid boiling point 150°c
I dont wanna use to much water to solve the pouder becouse the boiling point goes down then.
dont be to greety with the phosphoric acid . the amount off water use to solve the pouder I add extra in phosphoric

1 kg ap 0.5 water 1.2 phorsphor ( so here I use an extra 0.5liter phosphoric )
140 degrees 5 hours with agitator
You have to get 140 degrees at a lower temperature you get dirty oil
(thx to brombeer88)

 

[Saul]

Damn can edit.

Yes, I am now making my first test with 250gr CAS 5449-12-7 and phosphoric acid boiling point 150°c
I don't want to use too much water to solve the powder because the boiling point goes down then.
Don't be too greedy with the phosphoric acid. The amount off water use to solve the powder I add extra in phosphoric

1 kg app 0.5 water 1.2 phosphor 85% strong (so here I use an extra 0.5liter phosphoric)
140 degrees 5 hours with agitator
You have to get 140 degrees, at a lower temperature you get dirty oil
(thanks to brombeer88)

edit

if you use 75% strong phosphor, you need minimum 10% extra to become the same effect
so 1.2liters is then 1.4 liter minimum

 

[btcboss2022]

You need to do it in tor browser.

 

[Saul]

After 2 hours cooking 147°c looking good

open in tor

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/yvzu2lobd7-jpg.6136/?hash=19eaa128fb853103089ca8458b440fd5

 

[Saul]

After more than 4 hours cooking, it looks like this

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/ye7b2svaix-jpg.6138/?hash=28073778566ac037c65c9126ef26b3f0

 

[Saul]

Problem after 6 hours cooking, my metal inox overhead sering tool completely dissolved in acid .
there is nothing left off it . I read here on the forum some guy use it all the time lol .
maybe he believes that himself .
so what to do now with it ?

 

[UWe9o12jkied91d]

I don't think anybody is using stainless to stir conc. acid solutions for more than a few hours lol.In a very broad sense reacting an unsubstituted metal with an acid will react to form the respective salt.
You need either HDPE bar + pallet, or a new identical inox but with PTFE (Teflon) coating or epoxy coating.

 

[Bartholomeus]

@Saul what were the results you obtained from experiment?
On how much BMK powder you started this experiment?
And how much p2p oil you obtained?

 

[Saul]

Thanks for your answer. I think I put my mixing tool too deep in the flask and my heat source was gas
the rod is not damage, it looks only a little black now.
it would be nice if I can connect HDPE bar + pallet to the one I have
to absorb sensitivity of the shaft. My shaft is 6 mm and my mixer also can handle max 6 mm

can I still use the liquid? there are still small pieces of undissolved metal in what at first looks like gold.
the strange thing is that these pieces float to the top in the liquid so in the part of the liquid I need
maybe use a filter or does someone have another suggestion thank you

 

[Saul]

it looked very promising before the metal started to dissolve. I think the result has changed because of this . it's still in the flask until I know if I can solve the problem

 

[UWe9o12jkied91d]

Proceed as normal IMO.If the inox got corroded all that is formed is probably some ferric and ferrous phosphate.Insoluble in water so that is why it's maybe behaving the way you're describing.

 

[Saul]

this is how it looks now. you see the metal peaces in it . a real shame Iam feeling lost off it.

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/hpabfgldva-jpg.6141/?hash=ad1e80fa5ae1796e0eb6cdfa6ac6e97d

 

[btcboss2022]

You only need to discard bottom layer and wash with H2O the oil layer, this oil has a very good color, better than mine ;-) I can't find the way to put my mixture at 140C in large scale, my mixture don't get higher than 120-123C even I put reactor temp at 200C.

 

[G.Patton]

Hi, looks nice. What is the problem to filter or distill it?

 

[Saul]

I don't know what to do with those metal remains floating above. They have changed from gold color to black. Lots of black dots .

 

[G.Patton]

Did you try my suggestions? I'm sure that distillation will help you 100%.

 

[Saul]

your boiling point is now 123°c so even if you give 500°c heat it will not rise. I think you should add some sulfuric acid to raise the boiling point.
boiling temperature of sulfuric acid 96% pure is 320°c

 

[Saul]

Hello smart brain,

this is a stupid question for you, but I'm going to ask it.
So I distill the upper layer only, or everything together?

Edit
all the metal is gone this morning, so maybe it is not needed anymore?

 

[serialz]

Hello,

Use a separation funnel. Keep the top part and distill only that part.

Maybe you can do an additional solvent extraction for the "green" part and then evaporate the solvent and finally distill this additional part. But I'm not sure that the time versus the yield of this last extraction is useful.

 

[Saul]

this morning I decided to do it differently.
I wanted to raise my cooking temperature even more. so I had added 150ml of sulfuric acid 96%. now my liquid boiled over 170°c I let it boil for two and a half hours ( see video )

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/data/video/6/6155-282d1fad0ec5cac405cfb61445dfc330.mp4

this is the same flask from yesterday with the same content

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/rzobp6hnwl-jpg.6156/?hash=74f916dcd865a35218c5a34fd9878307

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/v2qafmtf69-jpg.6157/?hash=74f916dcd865a35218c5a34fd9878307