Sciencemadness Discussion Board

Making high-purity Ammonium Chloride with household cleaning products (?)

Cosaco - 23-7-2019 at 05:57

I would like to obtain food grade ammonium chloride, salammoniac. Ammonium chloride is used as an additive in industrial bakery, and is an essential ingredient of salmiakki, a Scandinavian salty licorice sweet.

However, and for several reasons, buying this product online is more expensive than it should be (in addition to having a high price on many of the pages I look at, it costs me more the ship than the product) or has a too long shipping time.

:.

I have planned to manufacture high quality ammonium chloride with household cleaning products: hydrochloric acid and ammonia.

There is a main problem with this: additives and perfumes.
I cannot manufacture ammonium chloride by directly mixing the two products, since it could poison me in its consumption, due to the presence of cleaning additives.

To avoid this I have thought of two production paths:

1. Purify ammonia and cleaning hydrochloric acid, before using them in the manufacture of ammonium chloride. (I don't know how to do it and maybe I don't have the right equipment).

2. Or, build a kind of gas bell and collect the ammonium chloride formed by the mixture of vapors of hydrochloric acid and ammonia, and then recrystallize it several times.

.:

I would opt for the second way:

The idea is to place a grid or cloth on a large glass, and inside this glass put two glasses or smaller containers.
Each small container would have, respectively, cleaning ammonia and cleaning hydrochloric acid.

The vapors of these two products would rise and mix, perhaps precipitating and nucleating in the cloth.

Once the fabric has enough ammonium chloride, I would scrape the crystals present and disolve them to try to eliminate any harmful component or perfume trapped in them.

I would repeat the dissolution and crystallization process several times so that most of these impurities are volatilized and it is safe to put the product in my mouth.

...

Will this way work?
It is recommendable?

[Edited on 23-7-2019 by Cosaco]

AJKOER - 23-7-2019 at 06:56

Step 1: Buy at a discount store, Epsom Salts (a hydrate of MgSO4, that is of high purity as people add it to their bath, which could expose them to heavy metals, if the product is not of high purity). Also get a good deal on cleaning solutions of ammonia water (generally impure but not important) and food grade NaCl.

Step 2: Coat the inside of a large vessel with moist MgSO4 and insert a smaller vessel containing the NH3 (aq) to which you add NaCl to help with the release of gaseous ammonia. I have used a aluminum foil boat loaded with NaCl for insertion in the aqueous ammonia, where the Al dissolution was exothermic (in my selected ammonia cleaning product) assisting with the release of NH3. Seal the larger vessel to prevent the loss of NH3. In time, a surface reaction on the walls of the larger vessel:

MgSO4.xH2O + 2 NH3 (g) + 2 H2O = Mg(OH)2 (s) + (NH4)2SO4 (aq) + xH2O

Step 3: Collect and mix the targeted products with NaCl and water. Proceed to freeze out the Na2SO4 keeping the ammonium sulfate in excess to limit a sodium impurity:

(NH4)2SO4 (aq) + 2 NaCl (aq) = 2 NH4Cl (aq) + Na2SO4 (aq)

You are left with aqueous NH4Cl and possibly some excess (NH4)2SO4. One could use CaCl2 to remove the sulfate as CaSO4. Heat the dried salt to sublimation and collect for very high purity NH4Cl.
-------------------------------------------------------------------

My experience with this process is that it slow and I should have employed much more ammonia water to produce a good yield on the ammonium salt of interest.
-----------------------------------------

A variation of the above would be to treat aqueous MgSO4 with NaCl (in excess) and freeze out the Na2SO4.10H2O. This leaves aqueous MgCl2 which can be cooled again to obtain crystals of MgCl2(H2O)x. Use the collected crystals to paste onto the inner walls of the ammonia reaction chamber.

[Edited on 23-7-2019 by AJKOER]

draculic acid69 - 25-7-2019 at 02:46

I would dump aluminium foil into HCL and lead the vapours thru water then just boil the nh3 and lead the gas thru that.clean NH4cl solution.

DraconicAcid - 25-7-2019 at 02:56

Quote: Originally posted by draculic acid69  
I would dump aluminium foil into HCL and lead the vapours thru water then just boil the nh3 and lead the gas thru that.clean NH4cl solution.


Dumping aluminum foil into the HCl gives you hydrogen gas, which is not useful for this reaction.

hissingnoise - 25-7-2019 at 03:18

Quote:

I have planned to manufacture high quality ammonium chloride with household cleaning products: hydrochloric acid and ammonia.

Crude NH4Cl can easily be purified by sublimation!

[Edited on 25-7-2019 by hissingnoise]

[Edited on 25-7-2019 by hissingnoise]

Metacelsus - 25-7-2019 at 03:34

Quote: Originally posted by hissingnoise  
Quote:

I have planned to manufacture high quality ammonium chloride with household cleaning products: hydrochloric acid and ammonia.

This is a very fraught process as unless strictly stoichiometric quantities are used various chloramines will also be formed...

Crude NH4Cl can easily be purified by sublimation!

[edit] The trichloramine is a very sensitive, highly explosive yellow oil!
[Edited on 25-7-2019 by hissingnoise]


Do you have a citation for the chloramine production? I would think it should be a simple acid-base reaction. Chloramines would require an oxidizer somewhere.

hissingnoise - 25-7-2019 at 03:43

Thanks for the correction, Meta ─ I mistakenly had hypochlorite in mind...

But I'm 'fully' awake now.

I'll edit it out...

AJKOER - 28-7-2019 at 09:48

Theoretically, one could shake together a mix of NH3, Cl2 (from household chlorine bleach, NaOCl, plus acidic cleaners, like NaHSO4) and dilute H2O2 to create very dilute aqueous NH4Cl.

Chemistry:

Cl2 + H2O = HCl + HOCl

HOCl + H2O2 = HCl + H2O + O2 (g)

2 NH3 + 2 HCl = 2 NH4Cl
----------------------------------
Net: Cl2 + H2O2 + 2 NH3 = 2 NH4Cl + H2O + O2 (g)

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

In place of H2O2, one could try using Fe interacting with first chlorine and upon completion add ammonia. Heat to sublime out the NH4Cl. A quick take on the chemistry:

Cl2 + H2O = HCl + HOCl

Fe --> Fe(ll) + 2 e-

Fe(ll) --> Fe(lll) + e-

e- + HOCl ----> •ClOH-

•ClOH- --> •Cl + OH- (pH < 5) (See cited sources at https://www.sciencemadness.org/whisper/viewthread.php?tid=15... )

•Cl + •Cl = Cl2

•Cl + Cl- = •Cl2-
......

So, in acidic chlorine water, the corresponding fenton-type reaction of ferrous with hypochlorous acid could be:

Fe(ll) + HOCl + H+ --> Fe(lll) + 1/2 Cl2 + H2O

and, the reaction cycles in a closed system forming ferric chloride. At conclusion, adding aqueous NH3 results in NH4Cl, which on heating can be separated out.

[Edited on 28-7-2019 by AJKOER]

rockyit98 - 28-7-2019 at 10:16

you want to eat this right?:)
best and only one is Solvay process(https://en.wikipedia.org/wiki/Solvay_process)
use table salt ,bakers ammonia (Ammonium bicarbonate) from a food shop, and that it.
i made this a couple of time.
cool salt water and add bakers ammonia, sodium bicarbonate will settle out. filter the solution.and let it evaporate.
bakers ammonia is much cheap like 1$ a pound.if it harder to find look shops in the China town.
hay on the plus side you also have baking soda as side product.;)