Sciencemadness Discussion Board

Ammonium permanganate preparation

madscientist - 20-5-2002 at 18:32

Ammonium permanganate, contrary to popular belief, is actually a relatively stable compound (although not a stable explosive). Preparing NH4MnO4 requires a solution of HMnO4 (it can't exist on its own). The simplist way to prepare a solution of HMnO4 is to add Mn2O7 to water. This route is dangerous because of the involvement of Mn2O7, a dangerously explosive oily liquid. I have designed an alternative process for preparing an aqueous HMnO4 solution.

(COOH)2 + KMnO4 --> KOOCCOOH + HMnO4

That is the reaction that I used to prepare the HMnO4. I tried two experiments.

1) I heated 200mL of water to 90C. I was planning on cooling the solution to around 0C after the reaction, so that I could filter out virtually all of the KOOCCOOH formed. I then added 10g KMnO4 to the solution. I added 6g (COOH)2 to the solution; fierce fizzling began. HMnO4 gas wasn't being given off; it has a strong odor and color, which wasn't observed. I believe the H3O+ ion was being oxidized by the MnO4- ion, causing (COO-)2 ions to decompose. Anyways, I ended up dumping the solution down the drain.

2) I decided that since in experiment #1 the H3O+ ion was being oxidized, causing the decomposition of the (COO-)2 ion, I would use far lower temperatures this time. I took 200mL of water at the temperature of 10C, and added 5g KMnO4. I then added 3g (COOH)2. There was a slight amount of fizzling. I continued to cool the contents of the beaker until the temperature was at 5C; then I filtered the contents of the beaker. The filtered liquid, an *intense* purple aqueous solution of HMnO4, did not fizzle (because of the absence of the (COO-)2 ion). I then added 20mL of 10% NH4OH solution (I wanted to make sure that all of the HMnO4 was fully reacted) while keeping the beaker in an ice bath. The temperature rose about 5C despite the ice bath. As of right now, I am waiting for the water to evaporate off. More news on this experiment later.

[Edited on 21-5-2002 by madscientist]

madscientist - 21-5-2002 at 16:03

A problem with preparing ammonium permanganate in aqueous solution has just occured to me. The NH4MnO4 will slowly decompose into NH3, H2O, and Mn3O4.

NH4MnO4 + H2O --> [NH4+] + [MnO4-] + H2O

[NH4+] + [MnO4-] + H2O --> NH3(g) + [MnO4-] + [H3O+]

12[MnO4-] + 12[H3O+] --> 4Mn3O4 + 13O2 + 6H2O

And, obviously, reaction of the NH4MnO4 with the Mn3O4 will occur...

Precipitation of Mn3O4 from the solution of NH4MnO4, from experiment #2 (referring to the above post) has already been observed.

madscientist - 22-5-2002 at 17:40

Well, the reactions posted in the post directly above have spelt the end of the ammonium permanganate I had prepared, which was in solution. There is now nothing but a precipitate of Mn3O4 resting on the bottom of the beaker, and the faint scent of ammonia.

I have, however, thought of an idea for extracting the ammonium permanganate from solution. In ice, since it is a solid, the particles inside have very restricted movement. Therefore, the ammonium permanganate in a frozen aqueous solution will not be decomposing. Ice slowly sublimes. Therefore, if a solution of ammonium permanganate is frozen, and left frozen, eventually all of the H2O will be gone, leaving pure NH4MnO4 crystals.

[Edited on 23-5-2002 by madscientist]

This sounds like a job for...

Polverone - 27-5-2002 at 11:55

...Vacuum Sublimation Man! Seriously, unless you want to wait months for the results of your experiment, you're going to have to sublime the ice under vacuum. It may not even be necessary to keep the ice frozen the whole time. Add your ice, pump air out, and slowly raise the temperature. If the liquid water is removed almost as fast as it appears, you shouldn't have to worry too much about decomposition.

madscientist - 14-6-2002 at 13:11

Here's a way of preparing high-purity NH4MnO4 that has been tested, and works. Simply mix a stoichemical amount of ammonium oxalate and potassium permanganate; dump it in a small amount of water in a jar, and allow the NH4MnO4 crystals to form on the sides of the container. I recommend using a lid with a small punched in it. The crystals are spiny, and are obviously a dark violet color; they however are not as intensely violet as potassium permanganate. This is how it works:

(COONH4)2 + 2H2O --> (COO)2[-2] + 2NH3 + 2H3O[+1]

The ammonia evaporates out of solution.

KMnO4 --(H2O)--> K[+1] + MnO4[-1]

MnO4[-1] + H3O[+1] --> HMnO4 + H2O

The HMnO4 evaporates out of solution.

HMnO4 + NH3 --> NH4MnO4

The ammonium permanganate crystals form in the air, some crystalizing on the sides of the container, given a starting point for more ammonium permanganate crystals to add on to the starting crystal.

vulture - 15-6-2002 at 10:20

So mixing ammonia and potassium permanganate and then adding sulfuric acid (to the solution!) should also work?

madscientist - 15-6-2002 at 10:46

I would think it would; but not nearly as well as the method I posted previously. :)

PHILOU Zrealone - 16-8-2002 at 08:57

Oxalic acid can be mesured via permanganatimetry (KMnO4 in basic or acidic media)!
Again oxalic (you seem to like oxalic, oxamide, nitroxamide, .... ;) ) is a reducer and KMnO4 is an oxydiser...oxydoreduction will occure always freeing CO2 and leaving MnO2 (brown)!
2KMnO4 + 3HO2C-CO2H --> K2CO3 + 5CO2 + 2MnO2 + 3H2O

If you want permanganate of NH4; use a salt of ammonium that can't be oxydised like NH4 sulfate, NH4 phosphate, NH4 nitrate (there is a risk of detonation here), NH4 perchlorate (here too).The idea is to find a salt of K (KX) that is less soluble than KMnO4 and NH4 brother (NH4X); then the reaction will go easy!

PH Z

rikkitikkitavi - 17-8-2002 at 12:02

hmm
KMnO4(aq)+NH4ClO4 (aq)=>

KClO4 (s) + NH4MnO4 (aq)

it relies on the fact that KClO4 is less soluble than the other possible compounds. It s is somewhat soluble in cold water though, but the contaminants
NH4ClO4 and KMnO4 would probably not be a problem..

/rickard

IodineForLunch - 31-8-2002 at 15:19

Hmm, Rickard's method sounds good to me. If you want all of your ammonium permagnanate to be in solution, you're going to have to perform the reaction in at least a liter of water. Otherwise, the ammonium permanganate, which is not very soluble at all (8 g per 100 ml at 15 degrees), will precipitate out along wtih the potassium perchlorate, and how the hell do you separate those two, if they're a solid mixture?

Rickard, it's not somewhat soluble in cold water at all. At 1 degree celsius, 1 gram of KClO4 will dissolve in 100 ml of water - hardly a critical amount.

Maybe you could take the solid mixture of NH4MnO4 and KClO4, and dissolve it in alcohol. KClO4 is practically insoluble in alcohol, but I'm guessing that NH4MnO4 is (anyone care to clarify that?).

Either way, I would certainly like to prepare this compound.

David Hansen

Not Rickard...

Ramiel - 31-8-2002 at 21:47

:mad: ...it's Rikkitikkitavi.

Pretty awesome book from what I can remember (all of 15 years ago) :D

PHILOU Zrealone - 9-9-2002 at 15:32

Fusion of MnO2 + KOH + KNO3 --> dark green managanates K2MnO4
Manganates are stable in strongly alkaline solution but disproportionate in neutral or acidic conditions into permanganates!
3K2MnO4 + 2H2SO4 --> 2KMnO4 + MnO2 + 2H2O + 2K2SO4
2K2MnO4 + 2H2O --> 2KMnO4 + 2KOH + H2
Oxydation in aqueous solution of Mn(2+) salts by strong oxydiser like NaBiO3 or PbO2 also forms permanganates!

So based on those datas!
It seems a good idea to try to fuse:
MnO2 with Ca(OH)2 and Ca(NO3)2 or Ba(OH)2 and Ba(NO3)2 to get CaMnO4 and BaMnO4.

The later upon treatment with H2SO4 should leave...
3CaMnO4 (solution)+ 2H2SO4 (diluted) --> Ca(MnO4)2 + MnO2 + 2H2O + 2CaSO4
finally Ca(MnO4)2 + H2SO4 --> CaSO4 + 2 HMnO4
CaSO4 is quite unsoluble (plaster), MnO2 is unsoluble too; thus it would be quite easy to dissolve NH4OH in the filtrated solution to get...NH4MnO4!
Thadaaahhh!

PH Z
:cool:

vulture - 10-9-2002 at 06:37

Nice idea. It seems that MnO4- salts with 2+ or 3+ metals are much stronger oxidizers than KMnO4, is this correct?

PHILOU Zrealone - 13-9-2002 at 07:40

Rectification:
Not stronger oxydisers but higher in oxygen contain (active oxygen %)!

PH Z

Ammonium permangante

chloric1 - 8-10-2003 at 17:41

Here is another thought. what about oxidizing fusion using MnO2, NaOH, + a little NaClO3 or PbO2 then converting this to sodium permanganate; then after adding strong ammonia, you could bubble CO2 or add dry ice until you get a sparingly soluble NaHCO3 precipitate?
I have seen various Patent literature that uses the Solvay process to make ammonium compounds

chloric1 - 8-10-2003 at 17:44

...but then again this ammoniation followed by carbonation is based on the principle that the ammonium salt desired is VERY soluble in which case the permanganate might not be. IF that did not work you could always make barium permanganate and use ammonium sulfate solution.

Axt - 18-10-2004 at 08:44

As per pm request,

The ammonium permanganate vid I have <a href="http://geocities.com/roguemovies7/">here</a> shows the result of the following synth:

20 grams of potassium permanganate is dissolved into 200ml of boiling water, to this mix is added 250g of ammonium nitrate and allowed to dissolve. The solution is poured off into another beaker to leave any undissolved or decomposed products in the bottom. Chill the solution to 10°C to precipitate the NH4MnO4, the solution can be poured off to retrieve the reddish-purple crystals. Place the product onto absorbent paper and leave to dry at room temperature.

So I just used a great excess of ammonium salt to drive the precipitate into being the ammonium permanganate. The precip will initially be granular, if cooled further it will be needles, you want the granular stuff not the needles.

Drop test of this stuff gives 15-20cm (ETN=30-35 PETN=40-45) so pretty sensitive, and low powered(1700m/s), therefore novelty purposes only!

Theoretic - 19-10-2004 at 05:36

PHILOU Zrealone, disproportionation of manganates will not give hydrogen.

mark - 23-10-2004 at 16:16

Axt
Is it possible to use Ammonium sulphate in your reaction? Due to this new anti-terror crap I no longer have accesses to NH4NO3. Your reaction seems to be as follows:

KMnO4 + NH4NO3 à NH3MnO4 + KNO3

My proposed reaction is:

KMnO4 + NH3SO4 à NH3MnO4 + KSO4

Does this seam feasible?

(I hope I am not breaking any forum rules)

neutrino - 23-10-2004 at 16:47

You mean:

KMnO<sub>4</sub> + (NH<sub>4</sub>;)<sub>2</sub>SO<sub>4</sub> -> NH<sub>4</sub>MnO<sub>4</sub> + K<sub>2</sub>SO<sub>4</sub>

Sounds possible to me.

The_Davster - 23-10-2004 at 21:55

I think the reaction is possible, however extraction will be a problem because potassium sulfate has a lower solubility than potassium nitrate, and thus when cooling potassium sulfate may also crystalize out in addition to the ammonium permanganate.

neutrino - 24-10-2004 at 05:25

K<sub>2</sub>SO<sub>4</sub> = 11g/100g H<sub>2</sub>O @ 20*C

NH<sub>4</sub>MnO<sub>4</sub> = 0.8g/100g @ 15*C

It shouldn't be too hard to separate them.

Axt - 24-10-2004 at 12:05

Quote:
Originally posted by neutrino
NH<sub>4</sub>MnO<sub>4</sub> = 0.8g/100g @ 15*C


Sure that aint 8.0g! The problem is more in that KMnO4 is less soluble, therefore it really has to be driven towards the ammonium salt with excess AN. Using 250g AN to get 10g AP, not good.

I think PATR gives a synth using (NH4)2SO4. But AN looked the better option to me, for the reason RC (<--bad acronym dude! :P) mentioned, as well as AN's higher solubility.

[Edited on 24-10-2004 by Axt]

The_Davster - 24-10-2004 at 12:13

Yeah, I realized that Axt a couple months ago. I f I could go back and change it I would make it something less kewl and not have the acronym of a suicide bomber:(

neutrino - 25-10-2004 at 16:19

It says 0.8 quite clearly in my pdf of Lange's 15th.

By the way:
KMnO<sub>4</sub> = 6.34g/100g H<sub>2</sub>O

Axt - 25-10-2004 at 17:31

It says 7.9 @ 15°C in CRC. One of them has it wrong.

0.8's a typo I reckon! If that were the case you wouldnt need an excess of AN, as it would precip immediately.

[Edited on 26-10-2004 by Axt]

The_Davster - 25-10-2004 at 18:27

I had a go at ammonium permanganate yesterday. I used Axt's procedure except 10x less.
Everything was the same as in Axt's procedure untill the cooling step. I was on this site, lost track of time and when I went to the freezer to check on the cooling of the beaker it was a slurry as some of the water had begun to freeze. I poured/scraped this slurry into the filter paper and let it sit there melting. Soon I received a nice ammount of purple crystals. I ended up leaving the filtration for a day accidently because I was busy with other things. I come back to it today, everything has dried out, and the bottom of the filter paper is incredibly brittle and darkened. This ended up contaminating the product sugnificantly.

The low VoD Axt mentioned is obvious, even the combustion of the product seems quite...unenergetic

Axt - 28-10-2004 at 13:54

What did the crystals look like, If you went as far to freeze it I think it less then pure. While it isn't terribly interesting it should at least pop into a cloud of MnO2.

You really want to get it as it first starts to precipitate, which isnt easy since you cant see into the dark purple solution.

The_Davster - 28-10-2004 at 16:32

The crystals are a very dark purple, however not as dark as potassium permanganate. The ammonium permanganate is in the form of a very fine powder with no discernable crystal shape and some longer crystals. About a 2:1 ratio of powder:crystals.
I get the cloud of MnO2 upon ignition and after ignition there is no unflamable residue other than the manganese dioxide. However the combustion does spread some unburned ammonium permanganate over a smal area, I know that this is ammonium permanganate and not some potassium permanganate impurities because they still are flamable.

I forgot to mention earlier, but after filtering but before letting the crystals sit in the damp filter for days, I did wash the crystalls with a small ammount of water just above freezing. This would have removed any ammonium nitrate impurities and hopefully some potassium permanganate impurities( I know I would have lost some ammonium permanganate this way).

mark - 29-10-2004 at 17:59

I have just prepared what I think is NH4MnO4, I used Axt Procedure accept 10x less and Ammonium sulphate instead Ammonium nitrate. I boiled some water and added to the beaker with KmnO4 in it at 90 degrees I added the ammonium sulphate. At 50 degrees I realised I didn’t do the pouring step. Which I then did, I chilled down the mixture and filtered it this is now drying. I also filtered the undissolved stuff and it’s all drying now. I’ll tell you later if it works or not.

Edit

Also is NH4MnO4 soulable in acetone?

[Edited on 30-10-2004 by mark]

mark - 30-10-2004 at 18:29

I made another batch yesterday as well using the proper method with pouring. I poured it into the beaker when it was at 70 degrees. After drying it the burn tests using a propane torch failed miserably. It only decomposed and now explosion or flame or anything was seen. It seems NH4NO3 is the best way to go.

KMnO4

Blackout - 6-1-2005 at 16:08

Sorry to bring back an old post but...

2 MnSO4 + 5 PbO2 + 3 H2SO4 => 2 HMnO4 + 5 PbSO4 + 2 H2O

Then:
HMnO4 + KCl => KMnO4 + HCl

Could it be possible?

mark - 6-1-2005 at 17:37

KMnO4 reacts with HCl to give chlorine.

K9 - 15-2-2005 at 08:31

Sorry to dig up an old thread for the second time, but I just made some and after drying for one day the powder/crystals are quite dark. The drying product also caused the filter paper to start disintegrating. My question is just how long should it be before it's completely dry. I did a little burn test last night and it crackled as it burned and I assume this is from retaining moisture.

EDIT: Ok scratch that, it's dried out. Goes up quickly with a little puff.

[Edited on 15-2-2005 by K9]

chemoleo - 15-2-2005 at 18:58

It might be a good idea to rinse the crystalline material on the filter paper with cold ethanol or acetone (more the latter as it is oxidised), which can be dried faster than with water. However, test it with a small amount first, you may know about the experiment of KMnO4 and glycerin which spontaneously ignites, ethanol is an alcohol too.
Although - my personal guess would be that there won't be a problem as long as it is cold.
But try it first, under supervision.

To make things more interesting- I wonder how permanganates of i.e. formaloxime (H2C=NOH)/methylamine/ethylenediamine will fare. If we assume a final product of Mn2O3, it would mean that per MnO4 moiety, 2.5 oxygens are available for oxidation. With ammonium permanganate, there'd be a slight excess of oxygen. Maybe it could be used to produce a more energetic amine salt.

Ammonium Permanganate

AndersHoveland - 20-12-2011 at 20:42

http://www.youtube.com/watch?v=Bh-maHh0nvU

(NH4)2MnO4 explodes with a copious cloud of dark brownish-purple smoke. The substance is sensitive to friction, and very easily is set off by flame.

It is not entirely chemically stable, and slowly degrades. It can be stored for about 4 months.

The permanganate ion is much more reactive oxidizer than perchlorate, which is why this salt is so sensitive and chemically unstable.

Like ammonium perchlorate, ammonium permanganate is another ammonium salt that is not very soluble (most ammonium salts are very soluble). Unfortunately, potassium permanganate is not very soluble either, so this is not advantageous for making it.


Preparation 1 (the below has not been tested)

Sodium permanganate can be made by dissolving a manganese compound, such as MnCl2 or MnO2 (but do not use potassium permanganate for this procedure), in bleach. The reaction turns purple. Add extra manganese compound to be sure that all the bleach has reacted. After thorough mixing for 30 minutes, a test is to add a little piece of manganese dioxide, which then should not dissolve, indicating all the hypochlorite in the bleach has been reacted.

Separately, mix a small quantity of ammonium sulfate (or ammonium nitrate or ammonium chloride), but only add a small quantity, with some ammonia. Too much ammonium sulfate will make the reaction acidic, which is bad since that will make the permanganate oxidize the ammonia. If you have a pH strip, the ammonia mixture with the ammonium sulfate should be preferably neutral, or slightly basic. Be sure all the ammonium sulfate is dissolved in the ammonia, some extra water might be added to help dissolve it.

Add the second mixture to the first, then lower the temperature to 10degC until purple crystals appear. Use a spoon to scoop out the crystals, then flter out the crystals using coffee filter paper, washing with with a little water. The crystals are ammonium permanganate. Note that no potassium compound can be used in the above preparation, since the potassium permanganate would then solidify out.

If there is trouble crystallizing out the ammonium permanganate, some ammonia (the concentrated type) can be added to the solution, which should help because of the "common ion effect". The solution should not be cooled too long, otherwise sodium sulfate (salt) will begin to solidify out with the ammonium permanganate. Actually, ammonium chloride or ammonium nitrate are better than ammonium sulfate to use in this procedure, because the sodium sulfate is less soluble than sodium chloride.


Preparation 2 (has been tested)

20 grams of potassium permanganate is dissolved into 200ml of boiling water, to this mix is added 250g of ammonium nitrate and allowed to dissolve. The solution is poured off into another beaker to leave any undissolved or decomposed products in the bottom. Chill the solution to 10°C to precipitate the NH4MnO4, the solution can be poured off to retrieve the reddish-purple crystals. Place the product onto absorbent paper and leave to dry at room temperature. Excess ammonium nitrate must be used, otherwise it is difficult to preferentially precipitate out only the ammonium permanganate, since it is not much less soluble than potassium permanganate.


For preparing solutions of permanganic acid:

2 MnSO4 + 5 PbO2 + 3 H2SO4 => 2 HMnO4 + 5 PbSO4 + 2 H2O

The reaction is slow. The lead sulfate solidifies out, then is removed. To the remaining solution, add baking soda to make more alkaline (otherwise HMnO4 is a reactive oxidizer), then add the ammonia. The sodium ions are not as problematic as potassium ions, since the sodium permanganate is much more soluble.

Aqueous solutions of permanganic acid partially decompose when heated to 40degC, and completely decompose if boiled. The solutions slowly degrade at room temperature, especially above 20degC. The decomposition products are hydrated MnO2 and oxygen gas. If the water is allowed to evaporate out, the oxygen that forms from decomposition contains traces of ozone, giving it a distinct odor. The solutions slowly oxidize elemental sulfur after a few days to dilute sulfuric acid.


Alternatively, ammonium sulfate to the barium permanganate would work, the barium sulfate would solidify out and could be separated out, but use plenty of water, since the ammonium permanganate is not very soluble either. the solution will then contain ammonium permanganate, and the water could be evaporated out in a warm dark place. After some evaporation, lowing temperature will help crystallize out product.

Unfortunately, potassium ferrate K2FeO4, oxidizes ammonia, so ammonium ferrate is not possible.

Toxicity of Ammonium Permanganate

Berrilium - 31-3-2012 at 10:18

I couldn't find any info as to the toxicity of ammonium permanganate, i would think that it isn't toxic at all.

Also, what about TATP?

neptunium - 31-3-2012 at 10:26

its probably because it is way too unstable to even be consider for a toxicity study...

woelen - 31-3-2012 at 10:27

Ammonium permanganate is not especially toxic, not more than the well-known potassium permanganate. But ammonium permanganate is very unstable. How would you want to make this compound? It certainly is not available commercially. The only route I can imagine is through the insanely dangerous Mn2O7.

TATP also is not especially toxic, but it is equally dangerous and even can explode by looking angry at it.

I would say to you: Stay away from these typical K3WL chemicals if you value your limbs.

Vikascoder - 31-3-2012 at 10:35

en.m.wikipedia.org/wiki/Ammonium_permanganate ammonium permanganate is not toxic according to wikipedia are you thinking to detonate with TATP

barley81 - 31-3-2012 at 11:18

Toxicity of potassium permanganate:
http://members.tripod.com/~Prof_Anil_Aggrawal/poiso024.html

It is the permanganate ion that is toxic, not potassium. Ammonium is not toxic either (salmiakki is licorice containing ammonium chloride in amounts up to 8%) If ammonium permanganate indeed is stable, it will be roughly as toxic as potassium permanganate.

Berrilium - 31-3-2012 at 13:51

To answer questions, no I don't intend to use TATP to detonate anything at the moment as it is just not something I would even think of. But I was just wondering as I have made both NH4MnO4 and TATP and was wondering about the dangers that aren't of thought of

As for synthesis of the ammonium permanganate I make it by preparing a saturated solution of ammonium nitrate and water (this is all together 100ml) as I am using fertilizer grade I filter it a few times and then heat it until boiling point and add 6 grams pottasium permanganate. Stir and cool. Works for me. :)


Vikascoder - 31-3-2012 at 19:39

Is ammonium permanganate is sensitive to TATP . Can TATP alone detonate ammonium permanganate

AndersHoveland - 31-3-2012 at 20:31

Ammonium permanganate is considered a fairly sensitive explosive. It can detonate from open flame.

Vikascoder - 1-4-2012 at 00:17

Then it is going to be a nice time now i will try to use it as a booster charge 0.5 gm of mercury fulminate or 0.5 gm of hmtd i will use to detonate ammonium permanganate then if possible try to detonate any other thing.

Ammonium Permanganate

Berrilium - 1-4-2012 at 02:45

I have found that ammonium permanganate is way more stable than people say, I'm not sure if this is due to dampness/impurities but i stried to make a small charge using ammonium permanganate as my primary, it was suppose to be ignited by a christmas light and then detonate.

It did not work, i then proceeded to shoot it with an air rifle to dry dispose of it, it didnt detonate. I poured out the contents and hit it with a hammer. Only then did it detonate... When i burn it it barely burns... all in all it is pretty useless explosive/oxidizer

Vikascoder - 1-4-2012 at 05:04

in your previous post you have mentioned that you have TATP . try detonating ammonium permanganate withTATP and post your results. it is so easy to make so its potential of using it as booster can be developed if it works.

Adas - 1-4-2012 at 11:34

It is very unstable and decomposes. I have made it once and before it dried, most of it decomposed to some crap.

Vikascoder - 4-4-2012 at 00:31

I am thinking to make ammonium permanganate by dissolving diammonium phosphate in water then adding potassium permanganate . Since the solubelity of dipotassium phosphate is very high and of ammonium permanganate is very low it can be easily filtered of. Will this process work

A new method for ammonium permanganate

Vikascoder - 4-4-2012 at 19:17

Hello friends in my country diammonium phosphate is easily available so i thought to prepare ammonium permanganate from it and potassium permanganate . The method is to make saturated solution of diammonium phosphate then add KMnO4 until no more precipitate form . Since the solubelity of di potassium phosphate is very i high as i read on wiki pedia so it will stay in solution and ammonium permanganate can be filtered off easily.

chemrox - 4-4-2012 at 21:15

I wouldn't rush to publish this. Simple inorganic salts are made all the time on the basis of suitabilities. However, I hope you have fun doing it. Watch out for complexes.

Vikascoder - 4-4-2012 at 21:50

Is it possible to make any complex using these materials. If possible please tell thereis a very long thread on complexes in this section only but if you will tell which complex can be made using these materials than its great

AndersHoveland - 7-4-2012 at 15:44

Quote: Originally posted by Vikascoder  
Is it possible to make any complex using these materials. If possible please tell there is a very long thread on complexes in this section only but if you will tell which complex can be made using these materials than its great


Yes, I already made a post in the "Complex Salts" thread:
Quote: Originally posted by AndersHoveland  
Tetramine Zinc Permanganate - [Zn (NH3) 4] (MnO4) 2 – is an ammonia complex salt, which is a relatively weak but also sensitive initiating explosive. It has an oxygen balance of -4.3 - 8 6% (since the reaction products contain a mixture of both MnO and Mn2O3), and the volume of detonation gases about 483 l / kg.


Tetramine Zinc Permanganate is unstable in storage, gradually decomposing with the loss of ammonia, resulting in a characteristic odor, accompanied by self oxidation-reduction. The latter reaction is accompanied by the release of nitrogen, water and ammonia and, because this reaction is autocatalytic, if not properly stored it can lead to an explosion, both because of the ignition, and just because of the increase of pressure in a sealed vessel. Keep substance preferably at low temperature in a dry atmosphere, as in the presence of moisture it is less stable than ammonium permanganate.

The solubility of Tetramine Zinc Permanganate in water is very small - the reaction of its formation is used in analytical chemistry (microcrystalline microscopy) for the detection of zinc (with a detection limit of 1:7000 ). As a consequence, from a solution of salt precipitated in the form of fine black powder, shiny needle crystals are formed only with careful crystallization from relatively dilute solutions. In general, due to low solubility, synthesis of Tetramine Zinc Permanganate is simple.

Required equipment: chemical glasses (or better disposable plastic) , refridgerator (or freezer), and desirable but optional, an electric mixer and filter.

Materials needed: potassium permanganate, zinc oxide and zinc chloride (or nitrate), ammonium chloride (or nitrate), 10 - 30% aqueous ammonia (ammonia), distilled water.


Stages of Preparation:

1) In 100 ml of distilled water dissolve 4g KMnO4; to accelerate the dissolution it is recommended to use an electric mixer;

2) to 8 ml 20% aqueous ammonia is added 1.1 g ZnO, and 1.4 g NH4Cl (or NH4NO3); zinc oxide should dissolve completely, instead of zinc oxide and ammonium salts can take an equimolar amount of the corresponding zinc salts;

3) The prepared solutions were mixed and rapidly cooled before freezing;

Note: The precipitation of Tetramine Zinc Permanganate takes place during mixing of solutions, cooling slows the recovery of permanganate ion and free ammonia yields a relatively pure product.

4) The bulk of the cold solution is poured, and the residue washed precipitate on the filter, the solution to further remove the filter with the precipitate on the stack of filter paper sheets, after which the product is loosened as soon as possible and dried at low temperature (optionally under reduced pressure).

The result is a 4 – 4.5 g of fine black powder (yield of permanganate 85 - 95%), the presence in it a brown powder of manganese oxides indicates that the product is partially decomposed by high temperature or duration of precipitation and drying.

In principle, the use of dilute (and not contaminated colloidal particles), the starting solution can be precipitated more pure Tetramine Zinc Permanganate in the form of small brilliant needles, but in this case the output drops sharply.