387 replies to this topic

[lord_dranack]

I have been trying to get some KClO4 for some time, but all the chemical suppliers I have tried only seem to offer AR grade, which is a little beyond my means at ?50+ per kilo!
So I have decided that the only practical option is to manufacture it myself. Has anyone here manufactured it, using either the thermal decomposition of KClO3 to KCl and KClO4, or the electrolysis of NaClO3 to form NaClO4?

[BigG]

Ah!!! Good ole chemistry. Yes!

First, forget thermal decomposition. It?s very easy procedure to execute, but you will need professional analytical tools to know that you got the decomposition going and to stop it at the right moment.

As for electrolysis ? Don?t even think about it unless you got platinum wire or large lead dioxide anode, and a titanium cathode. Once you got those, you can make perchlorates, however, I found that getting read of residual chlorate is not as easy as some suggest ? and you better have some way of testing for existence of chlorates at the end of the process.

In general ? while it?s fun chemistry project ? try to buy perchlorates. There are too many things that can effect the quality of your final product, and render it as sensitive as chlorate. Then again, where Bernie and me practice pyrotechnic, we can just order from Skylighter aren?t we lucky?!?!?

BigG

[Stuart]

What does AR mean? Is LR related to grade?

[BigG]

What does AR mean? Is LR related to grade?

AR = Analytical Grade,
LR = hmm, can’t remember…
TR = Technical Grade.

Analytical grades are very pure.

[Rhodri]

Too right BigG - the electrolytic method will produce good O4 but you'd better find a way of venting all that explosive H gas that's evolved!

I belive they manufacutre O3/O4 this way comercially to produce AR grade in France.

Not that this helps at all but I thought it might just add to the conversation.

[Stuart]

Getting rid of the H gas is easy-use a lighter.
Like I always say, petrol is very clean-if you spill any, light it and its gone

[BigG]

Getting rid of the H gas is easy-use a lighter.
Like I always say, petrol is very clean-if you spill any, light it and its gone  

Not Funny

Actually, just ventilate the room and you should be fine. The real problem is the removal of whatever chlorate is in the composition.

BigG

[Rhodri]

There's a link put up by "Head Honcho" from an earlier post. The link provides detailed information for construction of one of these 'cells'.

Personally, I think it's a bit of an ambitious project.

O4 is obviously very useful for colours but it may have to remain on the 'unobtanium' list.

That reminds me, Steve was hopefully going to procure some.

Steve, are you out there? Anything going on in that department?

[lord_dranack]

LR= laborotory reagent (normal grade for general use)
I'm planning on making lead dioxide graphite substrate anodes, based on what i read on wouter's practical pyrotechnics. Of course, buying KClO4 would be preferable...
I was looking in an old 1950s chem textbook today. It said the best way of making perchlorate in the lab is thermal decomposition from ClO3 at 370 celcius so i might try that, even if the ClO4 id contaminated with chlorate, although i remember reading somewhere that it was possible to destroy chlorate by a chemical method that won't damage perchlorate.

[BigG]

LR= laborotory reagent (normal grade for general use)
I'm planning on making lead dioxide graphite substrate anodes, based on what i read on wouter's practical pyrotechnics. Of course, buying KClO4 would be preferable...
I was looking in an old 1950s chem textbook today. It said the best way of making perchlorate in the lab is thermal decomposition from ClO3 at 370 celcius so i might try that, even if the ClO4 id contaminated with chlorate, although i remember reading somewhere that it was possible to destroy chlorate by a chemical method that won't damage perchlorate.

Good luck If you need pointers let me know. It took me about 15 tries before I managed to get an anode that lasted. Then again, I did not have much written text at the time.

Still, unless you have a analytical way of identifying that you got rid from chlorates, at as good as using chlorates.

BigG

[lord_dranack]

I believe there is a simple colourimetric test for chlorates, that is not disturbed by nitrate or perchlorate. It involves making a solution of phenylanthranilic acid in conc. sulfuric and adding a few drops to the solution to be tested.
http://huizen.dds.nl...ml#introduction has some useful and detailed information for anyone interested.

[sasman]

Hi
Thanks to Google Groups i have been looking at How to make KCLO4 ..Lots of postings and 1 or 2 good web pages.
However its always best to hear from real people who have actually made it themselves..The cost of buying it for me is way to much(?40 + kg )..I cant understand why its so expensive...Now i'm only just starting out in pyro and havent even made any BP yet!..But im just making sure i can get everything i need for good Constistant & repeatable results.


Has any1 in the uk made usable quantities?....I Just got a few books & Video tapes on pyrotechnics From the USA. and lots of formulas require this Compound so methinks that i will need to make reliable way of making it my self but would like some hints tips etc.. on what to do?..real tips/advice would be much help ..


The intial cost of getting the equipment is quite expensive..and i would hate to invest time and money only to find its not worth the effort(Im 100% sure it will work )
Cheers
sasman

Edited by sasman, 11 March 2005 - 06:22 PM.

[BigG]

Let me start by saying that this is not a beginners project. It does not matter how much you read about it, you always should practice extreme cautious and get an environment ready only for the purpose of this experiment. Any ammonium compounds should not be in the area, and you need good ventilation – because the chlorate phase smells. All ignition sources should be far far away. Ammonia is very good at taking fire.

Second – out of the two “commonly used option”, platinum is the safest and produces the best quality perchlorate. However, the only inexpensive sort (usually very thin wire), will produce perchlorate at an extremely slow rate. Think about 15%-20% efficiency. The other option (lead dioxide) is poisonous to handle, and from personal experience – get a few tries to get right. The insert I was most successful with was titanium insert – but that is not easy to make home. Ceramic insert was second best – and carbon – complete failure.

The main problem I found was that even under the best conditions, your perchlorate is contaminated with chlorate – and separating between the two is a real headache. Even small quantity of chlorate make this as sensitive as chlorate….

Anyway – feel free to ask me questions – but I have to warn you I have done this many years ago, in lab conditions – and my memory might be little rusty…

[sasman]

Hi Big G
Originally i was going to Start from chloride to chlorate to Perchlorate But i have just Bought some sodium chlorate so i'll Go from chlorate to perchlorate..My question is efficiency of the cell?..What kind of yield did you get from your cell?..
You mention titanium insert? was this coated with platinum?
I have searched the net for some Pt/Ti anodes and found a few ..price ranges from $30 to $70+....They only Have a very small suface area though..... The most promising is a Pt/Ti mesh i'm waiting for a reply on the cost..As for chlorate contamination that is solved by chemicaly destroying the chlorate then recrystalizing the perc a few times and it hopefully should be very pure..

Then run a few tests to make sure no acid or chlorate present with the Indigo Carmine test..
My main concern now is buying these Ti/Pt anodes i dont want to buy a few and find out they dont work ,There is one anode measures 6mm x 254mm (30cm surface area)thats not a bad surface area. about 10 amps worth
Cheers
sasman

Edited by sasman, 19 February 2005 - 10:55 PM.

[BigG]

Yes, Titanium insert means it is titanium coated by platinum. 30cm surface area is not bad for home cell. Efficiency really depends on the designed of your cell. Open cell with no PH control and you still have to except only 25-30% efficiency (which is fine if you just want to leave it outside and let it run). You will be able to get up to about 55-60% with a close cell design and PH control – but you will NEVER get VERY PURE product. The connection to the anode will corrode – the dust in the area with contaminates the cell etc, etc. If you get 94-95% pure product with no chlorate then consider yourself a happy men.

For cathode, I suggest you will use Titnium wire. You can get it cheaply from www.wires.co.uk. Their titanium wire is very pure and works very well in a cell.

BigG