Non-electrolytic barium chlorate synthesis

[50AE]

From http://www.oxidizing.110mb.com :

 

Non-Electrolytic production of Barium chlorate

A non-electrolytic method of making Ba(ClO3)2 requires some other starting materials, but works very well.

By the Tinman

 

You will need:

KClO3

Tartaric Acid (C4O6H6, a harmless, inexpensive material extracted from fruit)

Ammonia water

and either Barium Hydroxide or Barium Carbonate

I always used the hydroxide, but I don't see why the carbonate wouldn't work as well. If you make BaCO3 from either sodium carbonate or sodium bicarbonate, be sure to remove all the sodium, or your final product will be contaminated and not give you the green you want. This may require MANY washings.

 

BaCl2(aq) + Na2CO3(aq)----------------> 2NaCl(aq) + BaCO3(ppt)

 

Or

 

BaCl2(aq) + 2NaHCO3(aq)---------------> 2NaCl(aq) + BaCO3(ppt) + H2O + CO2(g)

 

A small sample of the washed BaCO3 may be put on an iron (careful that you don't heat the nail too much or it will show a yellow colour, don't use the end of the nail either) nail (don't use copper wire) and held in the flame of a propane torch to see if there is any yellow color from sodium contamination. If there is, keep washing it until there isn't.

 

Now, make a solution of tartaric acid in hot water and add enough ammonia to make ammonium bitartrate. Do not add excess ammonia.:

 

C2O6H6(aq) + NH4OH(aq)---------------> C2O6H5NH4 + H20

 

[i'll let you figure out the proper weights according to these equations.]

 

Next, make a near saturated solution of KClO3 in near-boiling water to add to the ammonium bitartrate from the previous rxn.:

 

KClO3(aq) + C2O6H5NH4(aq)-------------> C2O6H5K(ppt) + NH4ClO3(aq)

 

The potassium bitartrate (a.k.a. cream of tartar) is only sparingly soluble in cool water, and this leaves ammonium chlorate in solution after you have let the rxn mixture cool. Do NOT try to isolate the NH4ClO3, leave it in solution where it will be stable.

 

Finally, add the BaCO3 to the NH4ClO3 sol'n and boil. boil, boil until you no longer smell ammonia coming off. Add water as necessary to maintain liquid volume:

 

2NH4ClO3(aq) + BaCO3(aq/slurry) + [boiling] ------> Ba(ClO3)2(aq) +2 NH3(g) + H2O + CO2(g)

 

The boiling may take several hours. This will leave you with a solution of Ba(ClO3)2, possibly having a slight potassium contamination, which will not affect flame color.

 

Continue boiling until you see crystals of barium chlorate appear, let cool and filter. The filtrate liquor may be evaporated to dryness for further product retrieval, if desired.

 

If you decide to do an electrolysis, it is not worth making Barium Perchlorate, as it is hygroscopic.

 

IMHO, Ba(ClO3)2, when used with the right comp, makes a superior green to anything I have seen made with just Ba(NO3)2 as the colorizing agent.

 

As you correctly guessed, using potassium bicarbonate (if you can conveniently get it) instead of sodium bicarbonate will eliminate the sodium contaminating problem, and KHCO3 will react in the same manner as NaHCO3 here. But it still must be a reasonably purified finished product. I say this because some of the problems I've seen you post about poor flame colors sound very much like a contamination problem.

 

I'd like to hear your opinion about this method of synthesis. I'm impatient to try, I just have to find a hot plate. I have all the chemicals needed. What do you think about it? Would it work with barium carbonate instead of barium hydroxide?

Edited January 14, 2010 by 50AE

[Miech]

I personally wouldn't use chemicals in pyrotechnics if there only would be the slightest chance of ammonium chlorate contamination. Although this method is probably a working I'd rather go for a different synthesis.

 

Also, barium carbonate can be bought cheaper than barium chloride, so I'd rather skip the whole step making it and avoid sodium contaminations.

 

In my opinion bubbling chlorine gas through a concentrated hot solution of barium hydroxide would be a better way to make barium chlorate, given you have the resources and at least a decent fume hood. Electrolysis of barium chloride probably works as well, but I recall there were a few problems concerning the electrodes.

 

Edit: Of course, chlorine is very toxic and nothing to mess around with without the proper safety precautions. Do not attempt to make or handle it if you don't know how to handle it safely!

Edited January 14, 2010 by Miech

[50AE]

The chlorine method seems expensive to me. I will have to buy a lot of HCl to synthesize the chlorine I need.

I already have the barium carbonate in lots. I don't really need it.

I think complete boiling should destroy all of the ammonium chlorate.

[Bonny]

The chlorine method seems expensive to me. I will have to buy a lot of HCl to synthesize the chlorine I need.

I already have the barium carbonate in lots. I don't really need it.

I think complete boiling should destroy all of the ammonium chlorate.

 

As the tutorial states - boil,boil,boil... If this is anything like trying to boil the ammonia off when making strontium nitrate from ammonium nitrate, which I have done, you will be adding a LOT of water and boiling for hours and hours.

[50AE]

Youpiyee! I synthesized my first batch of Ba(ClO3) yesterday! It oxidizes fuels and it really does green, it was very little though, I made it to test the method only.

 

Now I'm doing a synthesis for a 400g batch of Ba chlorate!

[pyrogenius007]

Hi, 50AE, since you have successfully made a batch of Barium Chlorate can you please give me a simpler explanation e.g (qs) is from what I know a latin word meaning quantity sufficient (correct me if I am wrong) and if possible a step by step guide of how it is made i.e how many grams of chemicals to how much quantity of water,temp. of water when heated etc., If what I am asking for is time taking or tedious can you please suggest any site or book which can be downloaded. Thanks, P.G007

[Mumbles]

This is definitely too advanced and dangerous of a procedure to be trying if you don't understand the basic chemistry posted above.