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making potassium (per) chlorate


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#1 gods knight

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Posted 06 July 2007 - 01:58 PM

i really need help with this, ive been looking all over the internet and found a heap of cell designs and precipitation methods but most of them end up failing or don't last more than 2 days -_-

i just need professional help (that works) ;)






thnx :)
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#2 asilentbob

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Posted 06 July 2007 - 10:11 PM

There is an edit button. :D

The only people that actually make it have extensive chemistry knowledge and have invested countless hours/days/weeks/months/+ to learning/planning/making/repairing their cells...

Buy it.

And yes there is a thread about electrolytic cells for hypochlorite, chlorate, perchlorate production.
Take one pound of pure sulfur, two pounds of grapevine or willow charcoal, and six pounds of saltpeter... Marcus Graecus - Liber ignium ad comburendos hostes
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#3 gods knight

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Posted 07 July 2007 - 06:17 AM

lets just say i have already had too many failures with my other cells ;)
buy it, like the ones on ebay, that would b going against what im trying to say, i want someone with extensive chemistry knowledge that will help me if i go into a problem,not plans i buy and have no help with. oh and by the way i said ANY way possible
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#4 asilentbob

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Posted 07 July 2007 - 08:51 AM

Then your not going to be successful. (I was never talking about buying anything off ebay, i was talking about buying KClO4.) Electrolytic cells are like salt water fish tanks... They require a hell of alot of precise adjustments and being off can kill the fish (rate of formation/forming anything at all).

Hypochlorite decomposition through heat and subsequent metal ion juggling result in a sodium infested product and its alot of work for very little payoff.

Cl2 absorption into hot caustic (-OH) solutions is extremely slow and dangerous with the Cl2 gas.

If you have a nice platinum anode laying around or are going to actually invest enough time to decide which kind of anode fits your situation best... And find one or make one, then you should be able to set up a cell with minimal effort. However, its going to fail at some point and thats really your responsibility to deal with.

The info is out there. Learn more.
We don't want to have to spoon feed you at every step.

(I'm not replying to this thread again.)
Take one pound of pure sulfur, two pounds of grapevine or willow charcoal, and six pounds of saltpeter... Marcus Graecus - Liber ignium ad comburendos hostes
(add to) The Pyrotechnic Workshop Reference - 2007 Federal Explosives Laws and Regs (PDF 100pgs)
EmergencyResponceGuidebook2008pdf - ALL MSDS PERIOD - NPG-NIOSH Pocket Guide to Chemical Hazards
Join the PGI - Join the Pyrotechnic Artists of Texas (PAT) - They need your support!
Join the American Chemical Society - Dues (really cheap for undergrads!) - 2011 Member get a member program

#5 crazyboy25

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Posted 07 July 2007 - 11:24 AM

he's a smart guy you should probably listen to him.

good luck.
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#6 gods knight

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Posted 07 July 2007 - 03:14 PM

i have searched 4 another site and i think i have found one that works.
this is what they said:

CELL PLANS


electrode materials:

potassium chloride(home depot) 40lb bags 10$

Graphite: graphite is cheap and easy to obtain. It does however corrode at a comparatively fast rate.

Platinum: The obvious disadvantage of platinum is its high price. However, platinum anodes corrode only at a very slow rate and are suitable for perchlorate.


DSA: DSA stands for Dimensionally Stable Anode. This is the common term used to refer to anodes consisting of a layer of noble metal oxides (usually RuO2 and TiO2) coated onto a substrate, usually titanium. This type of anode is finding increased use in industrial cells because of its comparatively low cost when compared to platinum and its resistance to corrosion


Magnetite: This has found use in industry in the past, but is rarely used nowadays. It corrodes, but not very quickly and it can be used for perchlorate manufacture.



CATHODE:

stainless steel rod(home depot)


pH and temperature control

Although not essential for chlorate manufacture, controlling the temperature and pH will increase cell efficiency and therefore the capacity of a cell. Temperature control can be anything from a sophisticated thermostat and heating element (or a cooling element) to simple insulation around the cell or a cold water bath.

electrolyte :

Prepare a saturated solution of sodium chloride. Take about 40 grams for every 100 ml of solution and bring the solution to a boil. Then allow to cool to room temperature again. Some sodium chloride will crystalise as the solution cools. The solution is then filtered to obtain a clear saturated solution.

2. Optionally, 2 to 4 g/l of potassium dichromate, potassium chromate, sodium chromate or sodium dichromate may be added to improve efficiency.




Destruction of hypochlorite

Next, the electrolyte is boiled to decompose remaining hypochlorite. 15 minutes of vigorous boiling is sufficient. After that, the pH of the solution is checked and it is made slightly alcaline by adding sodium hydroxide solution. Bring the pH to between 8 and 9.




i think i will try this method and ill post how it turns out.
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#7 Pretty green flame

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Posted 08 July 2007 - 12:04 AM

Just like to mention something, if you are serious about making your own Perch you might want to look into GSLD anodes (Graphite substrate lead dioxide anodes), they stand up very well to abuse when operating in a perchlorate cell. Anyway, GSLD can be made at home, the procedure is on wouter's site.

Also, for detailed information, written by people who have actually made perch, read through the thread about making potassium perchlorate on UK rocketry, Click me

Cheers
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#8 gods knight

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Posted 08 July 2007 - 01:14 PM

can anyone tell me what voltage i should use for the cell?

i have a 3.7 volt charger can that be used?
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#9 Pretty green flame

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Posted 08 July 2007 - 10:29 PM

can anyone tell me what voltage i should use for the cell?

i have a 3.7 volt charger can that be used?

3.7V should be good for a chlorate cell, perch cells run at a little higer voltage, 5-6V. Although i i think it would work with 3.7V also, it's the current that counts.
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#10 gods knight

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Posted 09 July 2007 - 10:54 PM

i have finally made my cell and when i ran it it slowly emitted chlorine gas,so i thought it was working, i ran it for about 24 hours boiled it 4 15 min to destroy hypochlorate, then got a powder at the bottom , i tested it with sugar but it did not light, can someone tell me what i did wrong?
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#11 Pretty green flame

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Posted 09 July 2007 - 11:21 PM

i have finally made my cell and when i ran it it slowly emitted chlorine gas,so i thought it was working, i ran it for about 24 hours boiled it 4 15 min to destroy hypochlorate, then got a powder at the bottom , i tested it with sugar but it did not light, can someone tell me what i did wrong?

24hours ain't gonna get you much if any perchlorate, this stuff needs to be run for a week at around 6 Amps to get you some perchlorate. Also if your starting material is KCl you won't get much, if any perchlorate as the intermediate stage forms KClO3 which has a pretty low solubility so it will crystalize out of solution and solid KClO3 can't be transformed into Perch. You need NaCl as the starting material so you can make NaClO4 which you then transform into KClO4 by mixing solutions of NaClO4 and KCl, the KClO4 will precitipate out of solution in the form of fine white crystals.

Also, you need some sort of indicator so you know when the production of perch stars (for this you need a 1g/l solution of Methylene blue), you also need an indicator to show you how much chlorate remains in solution (obviously this isn't an accurate system but it will show you when the levels are high or low by the intensity of the precitipate, as these tests are pretty sensitive you will be able to detec very small ammounts of chlorate)
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#12 gods knight

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Posted 10 July 2007 - 07:20 AM

wow, a week, im going to have to make some changes to my cell,
and do you know where i can get proper Graphite substrate lead dioxide anodes?

and by the way, is the potassium chloride in those 40lb bags pure enough, the ones at lows, home depot, walmart thats what i bought?



oh and thx 4 ur help
Genius ain't anything more than elegant common sense.

Josh Billings

#13 Pretty green flame

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Posted 10 July 2007 - 07:36 AM

wow, a week, im going to have to make some changes to my cell,
and do you know where i can get proper Graphite substrate lead dioxide anodes?

and by the way, is the potassium chloride in those 40lb bags pure enough, the ones at lows, home depot, walmart thats what i bought?



oh and thx 4 ur help

GLSD cannot be bought, the only way is to make them, Wouter Visser has some instruction on how to make them.

Sorry, don't know the purity of the KCl but generally speaking the stuff grom hardware stores should be good enough.
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#14 hashashan

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Posted 10 July 2007 - 03:26 PM

I have a lot of experience with making perch at home. i have actually made some :)

well GSLD wont bring you anywhere. these are bad anodes. Very hard to make a lasting one. i couldn't even make a good looking one(not talking about lasting) you should try to look at substrate less anodes.

anyway graphite by itself also wont fit(good for chlorate bad for perch). If you have particular questions please ask. but i cant write the whole theory about making anodes here.

#15 gods knight

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Posted 10 July 2007 - 08:14 PM

Wow thanks, can you tel me what can i use for a cell body?, or the proper anodes for the cell? and how to make a proper electrolyte solution? and how much current,voltage,amps i should use?,

srry for the questions :)
Genius ain't anything more than elegant common sense.

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#16 h0lx

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Posted 11 July 2007 - 03:26 PM

arrgghh... my eyes are bleeding... please don't use 4 for the word "for" etc. This makes this forum look like totse.

#17 gods knight

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Posted 11 July 2007 - 04:05 PM

oh sorry ^_^
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#18 hashashan

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Posted 12 July 2007 - 02:13 AM

Ok so here are a few details:

Body : more or less anything non-metalic will do. take any plastic box(i use a box that once was used to buy chemicals, just a plastic box with a screw-on lid)

anodes : PbO2, this is the simplest thing that you can use,(or buy platinum but its more difficult to use it)
here you can read alomost anything you need to know about the production of those anodes http://www.geocities...e/chlorate.html

The solution is very simple : put as much NaCl ot NaClO3 as it dissolves and not falling out at room temperature

Current : 150-400 mA/cm^2

Voltage : not important the best would be about 7 volts

well thats pretty much it. ask anything else if you need to know

#19 superspike23

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Posted 12 July 2007 - 06:51 PM

I made kclo3 with kcl and chlorate sodium. I mixed 1 liter of water saturated with kcl and 1 liter of water sqtured whith sodium chlorate.
A reaction occurred by forming a white precipitate.
I then filtered the mixture to recover pure kclo3.

#20 gods knight

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Posted 16 July 2007 - 12:53 PM

has anyone tried using aluminum as anodes?, Ive tried it and it did start bubbling and steaming quickly there was no smell of chlorine
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