Aluminium amalgam (Al/Hg) summary

[ACAB]

I need the dry solvent later for salting out the sulfat and because i recover most of my solvents, i dry them very hard. It should only be a comparison of what little things I sometimes pay attention to in relation to the purchase of the aluminum foil.

 

[WillD]

You can dry the extract after. If we take benzene, then after azeotropic distillation, the remaining water is evaporated together with benzene

 

[ACAB]

Which synthesis are you now exactly talking about?
For extraction I use petroleum ether, dry this with MgSO4 and evaporate it. Then I use my dried solvents for salting out.
Which distillation are you talking about? I once used a process where I did a distillation before alkalinization and got all the solvents and almost all the water out. The reason for this was to get the water-soluble impurities out so that they would not be in the product later during steam distillation.

 

[WillD]

Try with benzene or its homologs. And the final product is better crystallized into acetone than in any other (if acetone prevails)

 

[ACAB]

You don't answer my questions or give reasons for your advice, I don't even have a clue what you are writing about, the next one says I should use red water to rinse the filters, so why should I care?

 

[mixxxman]

just a quick question guys.
when i did my amalgam ( hgcl2 + AL)
i mixed my products together and it was alright, i saw the grey color and the small bubbles coming.
after waiting more the production of h2 was a lot !
when the reaction looked down, i was planning to wash my amalgam of the mercury salt.
after have washed a couple of time it, i had my precursor ( nitro group/-- (P2NP disolved in iso alcohol) with GAAK. and nothing !!!

if someone can help me.
cause i was thinking maybe, the AL.HG was reacting. and after the rush of h2, the amalgam became down.
should i, maybe wash it, at the beginning when the small bubble and the grey color start ?
thank you so much for your help.
cause this step is not very clear for me
thank you

 

[G.Patton]

What of the concentration of P2NP in IPA did you use? Have you tried to warm the reaction mixture?

 

[mixxxman]

i don't really remember the proportion of the mixture. sorry...
but was a nice ratio. ( at the limit to be saturated)
i think it came from because i maybe was waiting to long after the reaction of the amalgam to do that.
is it a problem if i don't wash the hg.al from the mercury salt before to do a hydrogenization to a amine.
i know some people, they just mix everything together...
but is not really my point of view.... i like when it's clear and perfect !
is it possible, my amalgam was down cause i maybe wach to much ? or leave it a bit too long with my solvants ( to react and creat h2)
thank you guys for your messages.. i am feeling less alone with all of these questions.

 

[diogenes]

In my experience it is best to start the reaction when the amalgamation is started. Wait for a `sizzling` sound of the amalgam (Al + HgCl2 + water) and for all the Al coming to the top and small bubbles appearing. When all 3 signs are together 1.sizzling sound 2. Al coming to the surface floating 3. small bubbles, then drain the water immediately and add your reaction mixture (10g P2NP + 100ml IPA + 50ml glacial acetic acid). You will see a very stormy reaction immediately. Cool to some degree, but not overly, let it run as long us it is above 40 degree C. The better you get the beginning of when all 3 signs are together the better. I tried to wash it once and it still worked, but I think first better to try without washing as you will get rid of the Mercury later anyway. I hope this helps.

 

[G.Patton]

Approximately same that I told u @Pennywise

 

[ACAB]

Yes, like my older route, but without cooling.

 

[ASheSChem]

For the amalgam i have two neck on my balloon...
I ordered glass stoppers, but the delivery is endless...

noob question...
can I use a cork stopper?
"the french touch"

 

[ACAB]

I do not close the flask at all, I just let the hydrogen escape and then simply do not smoke in time
Why do you want to close the flask?

 

[ASheSChem]

since they say to put an allhin condenser... i didn't find it logical to leave the other neck open

 

[ACAB]

I see, the next step, I use an adapter for a thermometer, in this step it is important to keep an eye on the temperature, otherwise close it with "the french touch"
Otherwise, you could still make a hole in the cork with a small 6 or 7 drill bit and push the thermometer through that hole. This should also work.

 

[mixxxman]

thank you for your answer.
it is why i was maybe thinking about this possibility. and why i was scared to wash my amalgam cause.. maybe the al.hg will react with the H2O... and i will lose my reaction...

so, it's sound the easiest way without a washing, to don't hurt my amalgam.... but i am a bit worried to keep this mercury salt in my product...

-someone has some idea ?

for example, i was thinking to tryto take the mercury metal at the bottom, when i will make my mix alkalin with NAOH.
but is it possible to get some mercury dissolved the solvents i used (water, organic solvent, DCM,...)
because i really try and want to have to safest product at the end.

anyone, reuse this mercury to do a other amalgam ?
cause honestly... it's pretty hard to get !

thank you guys

 

[MadHatter]

Mercury is easy to get. Just buy mercury switches from ebay. You'll get like 200 from China for 10 Euro.
Mercury Nitrate is hard to get, but easy to make from mercury and nitric acid.

 

[Mclssmxxl]

A bit unrelated but does anybody know if galium salts form amalgams, if so which? Or do i need elemental galium?

 

[ASheSChem]

you need mercury

 

[Mclssmxxl]

Do you know for sure gallium does not work? I was looking to explore less toxic materials.