387 replies to this topic

[gilbert pinkston]

i think you might find Pb(NO3)2 is much more expensive and harder to get than HNO3 [but buying it may give you a purer chemical] Cu(NO3)2 may be a similar story to a lesser degree ive never bought HNO3 been makin it since i was 12

[pyromania]

I take it you have a distilation set up then? Do you distill it under vacum? Do you have any ideas as of how much copper and lead nitrate id need to make for a modest sized cell of around 8 litres? or is that just find out through experimentation lol.

[gilbert pinkston]

yea ive always had something i could use for nitric some set ups better than others dosent take much just have all your ducks in a row before you start .....good work area and plenty of water incase of a spill (HNO3 has no surface tension) a plan to take care of foaming and take your time with small batchs heat slowly.....ive never used a vacuum or urea for that matter
a modest cell? 8 liters? your joking right?
ive made at least 100# of NaClO4 with PbO2 and the biggest nitrate bath i had was a gallon pickle jar and that was too big i went to a one liter graduated cylinder......but i still have a lot to learn....do what you like
an 8 liter cell is a lot of soluable Pb accidents do happen you just dont need that much first time out get a feel for things first if you have problems you may want to blame it on your electrolyte (because there is nothing left to blame and your pulling your hair out wondering why your coating is falling off the substrate)and what happens when you want to replace or get rid of all that to make more?..... easy does it......may i suggest about 250 ml electrolyte and get your tecnique right before you make all that chemical and be braced for failure (after failure after failure)etc
as far as how much of anything you might need you will just have to do the math....
although anything you try to do has its hazards IMO almost anything is safer than being forced to work with chlorates for color and such

[paul]

I don?t want to interrupt your discussion here, but I found an Article that describes in DETAIL how the Perchlorates are made with electrolysis.

Unfortunately it is an german article. www.kkpaul.rpgames.de/perchlorat.pdf

BUT, if somebody could translate it into english, I think you all could profit from it. My english unfortunately isn?t good enough to translate such an article without going over important facts or something.

With best regards,

paul

[completebeginner]

ok so i am going to try amd make some kclo3 from ice melt salt although it is not pure kcl so i was wondering if there was a way to purify it before use to make kclo3. it contains kcl nacl and nh2conh2 I understand that nacl can be used aswell to aid the speed that the product is produced any help is appreciated

edit oh yeah it also contains calcium magnesium carbonate

edit # 2 ok so i put a little water in it as i read that kcl is very soluble in water so then i drained it and was wondering if this is a good way to obtain a high purity of kcl

Edited by completebeginner, 15 November 2005 - 02:53 AM.

[Mumbles]

I would dissolve it in boiling water, filter the coating(CaMg(CO3)2) off. Then cool the soln to 0C, and filter the precipitate. To decompose the urea heating it outside will work just fine. It will form H2O, Ammonia, CO2 amongst other intermediates. They shouldn't react with KCl. That should leave you with relativly pure KCl.

[completebeginner]

ok thanks and if i were to use the same method that alany uses in his tutourial posted earlier, if i were to use a battery that was 1.5 amps and 8 volts would i still end up with the same product but over a longer amount of time?

[alany]

Might be easier to just use NaCl for the cell and then use this impure mixture to precipitate out KClO3 after the cell is finished. The sodium content makes doing this about as bad as electrolysing the mixture directly, you are still going to have to fractionally crystalise and wash it several times.

If you melt the mixture in an open crucible the urea will decompose and burn off, and the dolomite can be physically removed as slag once it calcines. However beware that urea decomposition products include ammonia, be sure to get it *really* hot and liquid so no ammonia is left. Even then be cautious about using the result in a cell, ammonia ions will react and become nitrogen trichloride, which is *far* worse than ammonium chlorate or nitroglycerine. Calcium and Magnesium are also something you don't want in your resulting Chlorate.

Don't use a battery, that will just drive you insane, they don't have the energy density, you will be forever recharging it. Invest in a power supply of some kind, in fact just use the battery charger if it has suitable ratings. Think of it this way, all the energy you are going to get out of the Chlorate in a composition has to be put into the cell as electricity, plus the losses.

[completebeginner]

i dont quit understand how after i make naclo3 how i make it into kclo3 and i took some of the ice melter and wet it down with water and left it to recrystalize , if i were to boil this over a camping stove for a ffew hours until it recrystalized and then melted would that work to make it pure? because there are 3 different crystals left in the left over in the ice melter after i filtered the water out.

Edited by completebeginner, 15 November 2005 - 04:03 PM.

[alany]

If you add potassium ions to a fairly saturated solution of sodium chlorate the metathesis reaction will form potassium chlorate, which has rather low solubility and will precipitate out. This also works with sodium perchlorate and a potassium salt only better because potassium perchlorate is even less soluble than potassium chlorate in water.

A reasonable percentage of sodium ions won't hurt, so you can use a mixture of KCl and NaCl, like those "Lo Salt" salt replacements. Obviously it is easier to just start with pure KCl if you can get it. It wasn't very hard, I purchased a 25 kg bag after a few calls. Starting with KCl all you need to do is filter and recrystalise which is quite nice, but it limits you to Potassium Chlorate.

[completebeginner]

another question about purifying kcl, when i recrystalize it, i use a camp stove on the lowest it will go, but after it starts to recrystalize, it turns blue, then white and before it entirely turns whit it turns brown, so is there a way to get rid of the blue die without heating it? And is it really neccessary to get rid of the blue die before making the kclo3? Could I get rid of it afterwards?

Edited by completebeginner, 17 November 2005 - 06:12 AM.

[alany]

How are you recrystalising it?

You can get almost 600 g/litre of KCl into boiling water, but at 4 degrees (in the fridge) it will hold less than 300 g/litre. You simply boil, adding water until everything that will dissolve has, then filter and allow to cool, seperate out crystals, generally by filtering and washing. Repeat until sufficiently pure.

The big problem is the similar solubility and ion size of K and Na. It is quite difficult to seperate them, so your main aim should be to get rid of everything else that isn't an alkali Chloride, then let the low solubility of Potassium (Per)Chlorate make is easier to seperate the final product.

The dye should be fairly easy to seperate, but you can always try to destroy it with some hypochlorite bleach.

[completebeginner]

the problem with the method of recrystalizing that you mentioned is that i cannot get a pure solution of kcl as i only have it mixed with the other chemicals and i know that nacl is soluble in water. To get the die out of the kcl would it be safe if i used 5% sodium hypochlorite bleach? would there be any other steps I would have to do before electrolosis?

Edited by completebeginner, 18 November 2005 - 12:39 AM.

[Mumbles]

Yes, NaCl is soluble in water. However it has a property that is very helful for us. The change in solubility over temperature is very small. This means very little precipitates out. Let me give you an example to show you how it works. Lets assume that there is a 50/50 ratio of NaCl to KCl.

Say in 1 L of boiling water you can dissolve one kilo of this stuff(fairly close to actual). When you cool this to zero. 250g of KCl precipitates out, about 10g of NaCl will crystalise out. So 2% of the NaCl will precipitate with 4% NaCl contamination. If you don't have a fully saturated solution, even less will precipitate. If you recrystalise again you have just excluded 99.96% of the NaCl and you will only have .16% NaCl contamination.

[completebeginner]

I got my chlorate cell running about 6 hours ago and it is working a lot faster than I expected! After 6 hours I have about a one inch layer of chlorate on the bottom of the container (coolwhip container) I am very excited for when I get my strontium and barium carbonate.