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Synthisis Of Potassium Perchlorate


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#241 leosedf

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Posted 10 October 2006 - 11:17 AM

Well... I found something HERE (look at the platinised Ti anodes) but the cost is high.

#242 newtoolsmith

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Posted 10 October 2006 - 02:24 PM

Theese solutions seem to be very expensive.

Im not very happy with my GSLD anodes, they work bur the lead oxide is to brittle to give a perfect protection.

Now I try to make epoxy resin substrate anodes. Results will come soon.

MfG
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#243 leosedf

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Posted 10 October 2006 - 03:43 PM

You mean take apart lead batteries with resin to create rods? i'm very interested if you find anything.
I think those have a high resistance, so you will waste a lot of power.

What if you use a coil of platinum wire?? There is a lot of it on ebay and it seems cheaper than rods.
There is also a new shop i found HERE .

Edited by leosedf, 10 October 2006 - 04:10 PM.


#244 pkhow

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Posted 10 October 2006 - 10:43 PM

Replacement electrodes are widely available in Australia for Domestic Swimming Pool chlorination equipment so I imagine you can find them in Europe. A 200mm x 60mm anode should retail for under $50(US$35) and a Ti cathode of the same size should be half the price. If you can not find them I know that manufacturers here export to Europe so I would be able to find a supplier of replacement Electrodes. I think if you approach the Electrode manufacturers direct the cost is very high unless you purchase large quantities but manufacturers of Chlorination equipment supply their replacement electrodes at a reasonable price. I know in some countries use of Domestic Chlorinators for Swimming Pools are not as common as here but they are available and for Chlorates the material is excellent and will last indefinitely.

#245 newtoolsmith

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Posted 11 October 2006 - 04:51 PM

@leosedf:

Batteries? No.

I took some epoxy resin and glass fibres and made a sheet 300x100mm and 2mm thick.

It is made of several layers and the outer layer on both surfaces are covered with pulverized lead dioxide. It sticks on the epoxy surface.

This sheet will now be covered with lead dioxide by electrolysis as I did it with the graphite rods - without spinning of course.

MfG
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#246 leosedf

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Posted 11 October 2006 - 05:03 PM

I mean that lead batteries are a source of powdered lead dioxide.
Anyway we will wait for details...
I found some *cheap* platinized titanium anodes, i'll buy them if i have the cash.

#247 newtoolsmith

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Posted 19 October 2006 - 08:34 AM

Hi friends,

here some results:

The epoxy/glass fibre anode production totally failed.

While electrolysis some PbO2 appeared on the anodes surface but it didnt adhere at all. Even worse, the PbO2 I applied to the anodes surface dissolved partially in the plating solution. I think this will have been the non electrically connected locations as the resistance of the applied PbO2 powder was very high, some aereas even didnt show any conductivity.

Another test was made . Some glass fibre cloth was coated with a PbO2/water slurry and the slurry was kneded deep into the cloth. The electroplating was started and didnt give any result.

Parts of the PbO2 fell off the cloth when they got wet and the conductivity was drastically decreased. Once again the unconnected parts were disolved and I was left with a shining white glass fibre cloth without anyPbO2.


Next I tested plating a piece of stainless steel mesh. Lead dioxide forms but not quick enough to protect the stainless steel from corrosion. Only parts of the mesh piece survived this test.


Has anyone tested plating Pb sheet metal? It wopuld be easy available, cheap and could be plated in sulfuric acid as if you would be going to produce a lead-accu.


...further resuilts will follow.

MfG
newtoolsmith

#248 Aeed

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Posted 23 November 2006 - 05:08 AM

What if I run 500 Amperes on my cell?
I saw a lot of adapter in market the seller told me he have adapter DC 500 Ampere = 100 K.D (330 US Dollar) Should I buy it to make Potassium Perchlorate in short time??

Excess me for bad english

#249 newtoolsmith

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Posted 26 November 2006 - 06:35 PM

@Aeed:

Before passing 500A through a cell, you should try to solve the basic problems.

If you reed this and other topics carefully, you will notice that the required amperage is the least problem.


I dont have any time for experiments theese days but even if I had the time, I wont have solved the anode Problem yet.


Start small.


MfG
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#250 selwyndog

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Posted 20 February 2007 - 02:40 PM

Hi friends,

I did it!

Some month ago I prepared leadnitrate and coppernitrate from lead, copper and nitric acid. That was the easyer part.

The next step was made this week, as I prepared my first GSLD (Graphite Substrate Lead Dioxide) Anodes.

A spinning setup was build, similar to the ideas of wfvisser's homepage.

The first try failed because a thermofuse inside the motors windings actuated and the motor stopped spinning. I didnt realize because I sat down to eat something. The anode colected little bubbles and got holes in its coating. It was not so easy to disassemble the winding and solder the fuse out. I then decided to mount a cooling fan to the motors shaft. That works now.

The second try failed because I allowed the stup to run too long. The plating got too heavy and flew away short before I decided to stop the proces. F...!

The third try was really good. I let it run at 6 ampere for 30 minutes and the layer became approx 0,8mm thick and has no holes or cracks.

The fourth try did exacly the same.

The anodes are placed parallel with 25mm distance from center to center. A 4mmx24mm bar of stainless stell is placed between them. The top sides are sealed with two compoments silikone. The working length is 20cm so the anodes area is around 110cm?. The cathode area is almost exactly the same.

The bath has 1,8 litres and containes 600g NaCl.

I use a PC power supply, it runs 21A @ 4,85V through the cell.

The only thing I am wondered about is the very strong chlorine smell!!!!!!!!

I even thurts when breathed in unfortunately!

Much hydrogen is formed at the stainless cathode, it builds up a lot of foam.

The chlorine bubbles are much less then the hydrogen but I really want to drcrease further!!

Any ideas?
(photos will follow)
MfG
newtoolsmith


Edited by selwyndog, 20 February 2007 - 02:44 PM.


#251 Caramanos2000

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Posted 20 February 2007 - 08:38 PM

Use Tungsten welding anodes. I tried it, they dont corrode and they are $3 US.

#252 hashashan

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Posted 22 April 2007 - 09:43 AM

Hey guys, Well ive tried a million ways to make PbO2 electrodes and found that the best way is cloth reinforced anodes.
you just rub in some PbO2 into a thick cloth (i used a sock) and after that you electrolize it with graphite connections(PbO2 would be superior). You electrolize at very low currents my anode was about 15sq cm and i electrolized for 3 days at 0.4 amps. after that you apply some silver paint to it(nothing else will give you a good contact... every other metal will oxideize and stop functioning) and on the silver you just clamp a contact.
got 100 grams of P.Perch after about 10 hours from chlorate.

cheers

#253 gilbert pinkston

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Posted 22 April 2007 - 03:02 PM

100 grams of P.Perch after about 10 hours from chlorate

quite a bit it sounds good did you destroy all the chlorate?

#254 hashashan

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Posted 22 April 2007 - 04:48 PM

After the destruction of the chlorate and recristalization got 60 grams about 50% product, however i know that a lot was lost in KClO3->NaClO3 and recrystallizations(there were 3)
so i do think that it is good yield, soon ill launch the process from NaCl to test the anode.
and the 10 hours was an overkill, i electrolyzed at about 8 amps.

#255 gilbert pinkston

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Posted 22 April 2007 - 05:44 PM

here's what i do
make NaClO3 from NaCl with graphite
remove dichromate from NaClO3 and reuse it
keep adding saturated NaClO3 solution to perchlorate cell untill NaClO4 crystalizes out
when enough O4 comes out drain off the liquid and there is almost no waste when removing O3 from the crystals
NaClO4 is much easier to purify than KClO4
making chlorate from chloride may be problamatic using PbO2
do you have indego carmine to make sure you have removed all the chlorate?
how are you getting the chlorate out?




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