making potassium (per) chlorate

[taiwanluthiers]

Those anodes are used in wastewater treatment, at least according to the guys that sells them. I'm sure the Chinese makes their own, no way they would just import the stuff. I'm sure the stuff we use comes from them. It's not that hard to import perchlorates, just import enough of it and whatever paperwork needed is just a small part of the cost. Big fireworks manufacturer and pyro suppliers probably do this. Only reason we pay what we pay is because Skylighter has to make some money, and also this kind of a hobby is very niche, like minority within a minority so the economy of scale isn't there. You either use a few pounds at a time or use them by the metric ton.

Edited November 21, 2016 by taiwanluthiers

[PTFE]

Hey guys.

Im new here, but i have read most of the topic.

In the summer i've found out that electrochemistry would be a nice new hobby and soon i discovered this page.

After a lot of Information and a lot of reading i finished my, 3l 125A Cell.

It is mostly built from PTFE Parts and i use MMO for Anode and Titanium for the cathode.

At ~80°C my cell runs without additives and active cooling.

The Ph is keept at 6 but i still got problems with the acid-adjustment.

with 1,5kg of starting material (NaCl) ill get something about 2,8kg KClO3 after double decomposition in 2,5 Days

The gases are vented through a solution of NaOH from which ill get my top-up brine.

In the next time, im looking forward to make a topic for it if you are interested.

 

And now to give you some help for the bleachiong Ph-strips:

Add some Urea (CH₄N₂O) to destroy the NaOCl for measuring.

Also after the run to get a better yield. After the run, when the electrolyte is processed, i work with 3 ways to get rid of the Hypochlorite fast.

First bring it all to a boil, then add just enough NaOH for PH 8-9 and then i add 2gUrea/l and something about 10-20ml H2O2 30%.(add the H2O2 SLOWLY with strong stirring to prevent a overflow!)

After boiling for 5minutes/until no more bubbles occur everything is fine, but u have to keep an eye on the PH within the recrystalisation.

but for just measuring within the run, add a spatula of Urea and shake it well.

 

edit: if you are interessted in Anodes, ask Tiaano in India.

Just bought 4 Anodes (2mm*100mm*400mm) for 40$ each. But with shipping and duty they were like 55$

You will get a nice service and custom made anodes right for your application.

Edited November 21, 2016 by PTFE

[WSM]

Hi PTFE,

 

Welcome to the discussion. Your cell sounds interesting, do you have photos?

 

By the way, how do you get 1500 grams of sodium chloride into three liters of water? I'd struggle to get much more than 1050 grams to dissolve in that much H₂O (at room temperature, anyway). Do you get much chlorine coming out at a pH of 6? Most producers try for a pH closer to 7.0 (where the ideal is a pH of 6.8 for the highest current efficiency).

 

Let us know when you get a chance. Thanks.

 

WSM

Edited November 22, 2016 by WSM

[PTFE]

Hey WSM,

Photos will come soon, maybe a complet season when its in work and while processing the electrolyte.

I will also show the other types of cells ive built at the beginning.

 

The Electrolyte is first saturated within boiling, and without any filtration poured directly into the cell with ~800g of salt..some still not disolved.

After a day i add ~ 200g salt per day, when i top up my cell with solution from the Gaswasher.

I dont worry about salt at the ground of my cell because after sometime it will get dissolved when the saturation of NaCl in the cell goes down. the bigger problem is that the NaClO3 is crystalising out after some time.

 

The Ph controlling system is by far the most primeval thing in my apparatus.

I add 15% HCL throug a glas valve in a simple gravity addicted system but adjustment for a slow drop rate is a pain.

Injection takes place just above the bottom of the cell trough an perfored PTFE hose.

Chlorine is not to much of an issue, but if the wind goes the wrong way, it is like WW1.

when i use more dilute acid, its a bit better, but i would have to add quite a bit at 120Amps and i'd have a much bigger volume of electrolyte at the end.

 

luckily its running in the moment, so i can give you some detailed pictures in time.

 

I also planning a new 200A cell with the new Anodes.

What do you think about 2circuits in 1 cell? do u think that would be any problem for the switching powersupplys?

I think about 4Anodes 4 Cathodes. All cathodes connected to each PSU

and 2 Anodes per PSU.

Edited November 22, 2016 by PTFE

[WSM]

Hey WSM,

Photos will come soon, maybe a complet season when its in work and while processing the electrolyte.

I will also show the other types of cells ive built at the beginning.

The Electrolyte is first saturated within boiling, and without any filtration poured directly into the cell with ~800g of salt..some still not disolved.

After a day i add ~ 200g salt per day, when i top up my cell with solution from the Gaswasher.

I dont worry about salt at the ground of my cell because after sometime it will get dissolved when the saturation of NaCl in the cell goes down. the bigger problem is that the NaClO3 is crystalising out after some time.

The Ph controlling system is by far the most primeval thing in my apparatus.

I add 15% HCL throug a glas valve in a simple gravity addicted system but adjustment for a slow drop rate is a pain.

Injection takes place just above the bottom of the cell trough an perfored PTFE hose.

Chlorine is not to much of an issue, but if the wind goes the wrong way, it is like WW1.

when i use more dilute acid, its a bit better, but i would have to add quite a bit at 120Amps and i'd have a much bigger volume of electrolyte at the end.

luckily its running in the moment, so i can give you some detailed pictures in time.

I also planning a new 200A cell with the new Anodes.

What do you think about 2circuits in 1 cell? do u think that would be any problem for the switching powersupplys?

I think about 4Anodes 4 Cathodes. All cathodes connected to each PSU

and 2 Anodes per PSU.

 

Hi PTFE,

 

It sounds excellent; I'm looking forward to the photos. It's fortunate you have access to the PTFE material, which is very expensive. If I had more, I'd use it much more than I do now.

 

I think you should try the more dilute acid since you're adding replenishment water anyway. My thoughts on the system I'm planning have been running toward 8% HCl solution (one quarter strength) so using 4 times the volume of the 31.45% original concentration (10M acid available for pool chlorinating systems).

 

I've considered running a multiple electrode cell, but I'm unsure whether the cells could all be in one container or if they should be in separate vessels from each other (plumbed in parallel). Wiring them should be in series either way. If running 3 Vdc per cell, a 12 Vdc voltage source should be used (for a four anode system) and the current will be the same throughout (no need for separate power supplies, as long as the voltage output is high enough). That's the beauty of DC series circuits, the voltage is divided by the loads but the current is the same throughout the entire circuit.

 

Your system sounds exciting, I can't wait to see what it looks like. What type and size (input and output) of power supply are you using? It sounds more robust than the modified computer power supply, used by so many beginners (and many experienced folks, too). Let us know when you get the chance. Thanks.

 

WSM

Edited November 22, 2016 by WSM

[PTFE]

My thoughts about an 200A cell started because ive got 2 switching supplys. Not equal ones, but each with 5V/100A.

At the moment i use an old Pioneer magnetics. The Voltage is adjustable between 4-7Volts, so its really comfortable to work with.

at 4V the temperature stays somewhere at 50°C and current doesnt rise above 50-60A but if u turn it up to 7V the current is rising fast, reaching 125Amps at 80°C but i have to take a watch because sometimes it will climb up to 105°C.

but normally it stays at 86°C when the current is not allowed to get over 115-120A.

Current from the mains (230V`) is about 6A and the cosPHI is with 0.7 really not the best. but i got it for about 50€ from ebay, and new it was like 2000$ so i dont worrie about it..

Also it is specificated for the use at 208V but i dont like to use a variac everytime.

The second power supply i have is a Nortel Passport PwrSply from a comunication device. Since it doesnt perform voltage regulation, i didnt test it anyway, but its good to have another for replacement.

 

My idea was first runing a cell with chambers too. wounded in series inside. but this idea will be effortful since u have to take care about proper electrical insulation between the cells.

I thought about a Design, using 2 Supplys.

Minus is combined and for every Pwrsply 2Anodes are attached within the same electrolyte.

 

This time i run my cell something is much diffrent.

After 2 days a sample of the electrolyte was taken and decomposed with Kcl.

2 test tubes, filled to half with prepared solutions where dumped together and the precipitate filled more than 3/4 of the tube.

Last time i runned the cell i had the same amount after 4 days!

 

My expection is, that i have used much smaller Cathodes this time has caused the better yield.

When i add the series of pictures, you will get also a look at the test tubes.

 

to come back to the Ph i have to say, i cant really work with to much diluted acid, because i have to add ~300ml 15% per day and i really dont like to have that much elektrolyte

The next step is a pumping system to pump the acid direktly into the cell..that will avoid the adjustment of the valve.

 

 

Now i got a question:

My 5000ml boro.beaker is broken due the cold elektrolyte when i first wantet to saturate it.

so my questions are:

how do i warm up a cold solution in a glassbeaker when it breaks until the bottom gets hot?

and the other is.. when my cell is fineshed now, can i use a stainless container to bring it to a boil or am i fucked up now?

 

By the way, i speak german, so excuse me that my english is not the very best

Greetings

PTFE

 

edit: you can purchase really good industrial NT's via ebay.. sometimes very cheap.. just search for 5V and the wantet Amperage on ebay..

http://www.ebay.de/itm/Power-Supply-Nemic-Lambda-TKS-5-150A-5V-150-A-/141821195239?hash=item210533b3e7:g:014AAOSw7hRWPHwd

for the real cells

Edited November 23, 2016 by PTFE

[PTFE]

here are some pictures for the first Inspiration.

Im just at my mobile so ill write something later when im home at my pc..

Also you will get some more pictures From the Cell when ist opened

 

[Arthur]

I have heated solutions with a submersible fish tank heater, they are slow!

[WSM]

My thoughts about an 200A cell started because ive got 2 switching supplys. Not equal ones, but each with 5V/100A.

At the moment i use an old Pioneer magnetics. The Voltage is adjustable between 4-7Volts, so its really comfortable to work with.

at 4V the temperature stays somewhere at 50°C and current doesnt rise above 50-60A but if u turn it up to 7V the current is rising fast, reaching 125Amps at 80°C but i have to take a watch because sometimes it will climb up to 105°C.

but normally it stays at 86°C when the current is not allowed to get over 115-120A.

Current from the mains (230V`) is about 6A and the cosPHI is with 0.7 really not the best. but i got it for about 50€ from ebay, and new it was like 2000$ so i dont worrie about it..

Also it is specificated for the use at 208V but i dont like to use a variac everytime.

The second power supply i have is a Nortel Passport PwrSply from a comunication device. Since it doesnt perform voltage regulation, i didnt test it anyway, but its good to have another for replacement.

 

My idea was first runing a cell with chambers too. wounded in series inside. but this idea will be effortful since u have to take care about proper electrical insulation between the cells.

I thought about a Design, using 2 Supplys.

Minus is combined and for every Pwrsply 2Anodes are attached within the same electrolyte.

 

This time i run my cell something is much diffrent.

After 2 days a sample of the electrolyte was taken and decomposed with Kcl.

2 test tubes, filled to half with prepared solutions where dumped together and the precipitate filled more than 3/4 of the tube.

Last time i runned the cell i had the same amount after 4 days!

 

My expection is, that i have used much smaller Cathodes this time has caused the better yield.

When i add the series of pictures, you will get also a look at the test tubes.

 

to come back to the Ph i have to say, i cant really work with to much diluted acid, because i have to add ~300ml 15% per day and i really dont like to have that much elektrolyte

The next step is a pumping system to pump the acid direktly into the cell..that will avoid the adjustment of the valve.

 

 

Now i got a question:

My 5000ml boro.beaker is broken due the cold elektrolyte when i first wantet to saturate it.

so my questions are:

how do i warm up a cold solution in a glassbeaker when it breaks until the bottom gets hot?

and the other is.. when my cell is fineshed now, can i use a stainless container to bring it to a boil or am i fucked up now?

 

By the way, i speak german, so excuse me that my english is not the very best

Greetings

PTFE

 

edit: you can purchase really good industrial NT's via ebay.. sometimes very cheap.. just search for 5V and the wantet Amperage on ebay..

http://www.ebay.de/itm/Power-Supply-Nemic-Lambda-TKS-5-150A-5V-150-A-/141821195239?hash=item210533b3e7:g:014AAOSw7hRWPHwd

for the real cells

If using two power supplies together, unless they're perfectly matched you may run into trouble. Typically one will hog the load and possibly burn out.

 

As to heating in stainless steel, I prefer borosilicate glass which will not react or add unwanted ions to the solution. Heating the glass is best done evenly and slowly with an electric hotplate (for better control).

 

WSM

[WSM]

here are some pictures for the first Inspiration.

Im just at my mobile so ill write something later when im home at my pc..

Also you will get some more pictures From the Cell when ist opened

DSC_1118.JPG

DSC_1122.JPGDSC_1124.JPGDSC_1123.JPGDSC_1125.JPGDSC_1134.JPG

DSC_1133.JPGDSC_1120.JPGDSC_1138.JPG

Very nice setup. Thanks for posting the photos for us to see what you're describing.

 

WSM

Edited November 25, 2016 by WSM

[WSM]

I have heated solutions with a submersible fish tank heater, they are slow!

Yes they are, plus they have limiting circuitry to keep the temperature from running away and killing the fish.

 

An immersion heater would work better.

 

WSM

Edited November 24, 2016 by WSM

[Arthur]

My fish tank heater is in a glass tube and sealed, so no need to bother about corrosion resistance, It gives liquids a help in the warming direction!.

[WSM]

My fish tank heater is in a glass tube and sealed, so no need to bother about corrosion resistance, It gives liquids a help in the warming direction!.

I have a friend who suggested placing an immersion heater in a test tube to use as a tank heater. To prevent shock to the borosilicate glass test tube, I surrounded the heating element with silica sand.

 

Used in concert with a heating controller, they can do an admirable job.

 

WSM

[OldMarine]

I do work for a small cosmetics manufacturer and she has silicone oil filled glass immersion heaters she uses in her oil/butter type products to keep them liquefied. This is the same lady who told me about using dry ice mixed with stearin to grind it so she's a smart cookie. I'll try to get some info from her.

[WSM]

I do work for a small cosmetics manufacturer and she has silicone oil filled glass immersion heaters she uses in her oil/butter type products to keep them liquefied. This is the same lady who told me about using dry ice mixed with stearin to grind it so she's a smart cookie. I'll try to get some info from her.

I have a couple different grades of silicone oil but avoided using them, fearing a mess if the glass envelope should break during use. My concerns may well be unfounded, but the test tube with a heating element in silica sand works.

 

I like the idea of milling soft things with ice or dry ice. That makes powdered wax and other things possible which otherwise wouldn't be.

 

WSM

Edited November 25, 2016 by WSM

[greenlight]

Hey just a quick update on the perc cell.

I am awaiting arrival of the ammeter and shunt from the ebay numbers you posted a couple pages ago WSM.

When these come i can accurately calculate the runtime til completion.

Only thing is I ordered a 20 amp shunt as it matches my power supply current.

Will that still be okay do you think?

[PTFE]

Hey greenlight.

If i unterstand it the richtig way, you got a 20a shunt for a 20a pwrsply.

That is not much of an Problem if your Powersupply cant give more amps.

My nt is rated for 100a but it can deliver up to 125a without Problems..

If your shunt is built for 20a the current must not be higher.

If you Do so,it will get quite hot and the current measuring will become also inaccurately.

 

Edit: some Ampere more will not harm the shunt although

Edited November 26, 2016 by PTFE

[WSM]

Hey just a quick update on the perc cell.

I am awaiting arrival of the ammeter and shunt from the ebay numbers you posted a couple pages ago WSM.

When these come i can accurately calculate the runtime til completion.

Only thing is I ordered a 20 amp shunt as it matches my power supply current.

Will that still be okay do you think?

The plan you describe sounds good.

 

When I order panel meters that require a shunt (where the shunt is ordered separately) I get a shunt that matches the range of the meter, just to be on the safe side.

 

I also usually order a meter-shunt combination with a range a bit higher than the output of my power supply (if my supply outputs 30A, I'll order a 50A or higher ammeter). This way, I won't worry (about the meter) if the current output of the supply goes higher than I planned.

 

I hope it all works out for you. Please let us know. Thanks.

 

WSM

[greenlight]

Thanks guys, the shunt matches the maximum current of my power supply.

It was only a few dollars anyway so I can get another if it isn't right.

[theodusta]

Hey guys,

 

after all of my electrolysis is done, I am now at the step in cleaning out my perc solution and get rid of the remaining chlorate. Adding slowly the solution of metabisulfite created a heavy reaction. As I am calculating with a theoretical maximum of 1400g perchlorate in my liquor, I dissolved 150g of sodium metabisulfite to in about 600ml of destilled water, made my liquor to pH 3 and then added slowly the metabisulfite and checked for chlorate in several steps. The indigo carmine test still reacts with clear spots which always indicate chlorate present - and that regardless of the fact, that I added the whole solution of 150g metabisulfite. It seems, that I get a false positive test. How do you guys indicate chlorate with the indigo carmine spot test? What if I add "too much" metabisulfite? Can it also destroy my perchlorate? I have no possibilty to get NPAA. What should I do now?

 

Thank you and kind regards

 

Theo

[WSM]

Hey guys,

after all of my electrolysis is done, I am now at the step in cleaning out my perc solution and get rid of the remaining chlorate. Adding slowly the solution of metabisulfite created a heavy reaction. As I am calculating with a theoretical maximum of 1400g perchlorate in my liquor, I dissolved 150g of sodium metabisulfite to in about 600ml of destilled water, made my liquor to pH 3 and then added slowly the metabisulfite and checked for chlorate in several steps. The indigo carmine test still reacts with clear spots which always indicate chlorate present - and that regardless of the fact, that I added the whole solution of 150g metabisulfite. It seems, that I get a false positive test. How do you guys indicate chlorate with the indigo carmine spot test? What if I add "too much" metabisulfite? Can it also destroy my perchlorate? I have no possibilty to get NPAA. What should I do now?

Thank you and kind regards

Theo

 

Hi theodusta,

 

The indigo carmine test doesn't work with the metabisulfite treatment because the sulfuric acid residue interferes by giving a false positive for chlorate.

 

I discovered this when I was neutralizing the chlorates in my sodium perchlorate solution before making potassium perchlorate from it.

 

My fix was to use NPAA testing instead. Another test is the aniline HCl test. If you can get aniline or aniline HCl, it makes an effective test for chlorates. See Google under "test for chlorates", for more details.

 

WSM

[theodusta]

Hi WSM,

 

thank you for your response, but I have also no possibility to get aniline. A few minutes ago I tested again a sample mith methylene blue and the violet colouration indicates perchlorate. So it is still present. Isn't there any other possibility beside aniline or NPAA? I want to clear out my sodium perchlorate solution before adding KCl. I don't know what to do now as I am not able to get the other reagents. Any suggestions?

 

Thank you

 

Theo

[WSM]

Hi WSM,

thank you for your response, but I have also no possibility to get aniline. A few minutes ago I tested again a sample mith methylene blue and the violet colouration indicates perchlorate. So it is still present. Isn't there any other possibility beside aniline or NPAA? I want to clear out my sodium perchlorate solution before adding KCl. I don't know what to do now as I am not able to get the other reagents. Any suggestions?

Thank you

Theo

Hi theodusta,

 

Those three tests are the only ones I've used to test for chlorates. I know that the two you can't get work without interference from too many other oxidizers.

 

I'm away from home, visiting family, at the moment; but I can study it further when I get back home (where my library lives).

 

WSM

[WSM]

What if I add "too much" metabisulfite? Can it also destroy my perchlorate?

 

I don't think so. I believe the chlorate will be broken down and the left over metabisulfites will just float around in the mix.

 

WSM

[WSM]

Adding slowly the solution of metabisulfite created a heavy reaction.

 

If you add the metabisulfite solution to the top of the electrolyte solution (especially when it's hot) it tends to flash off the sulfur dioxide as gas into the air, wasting it.

 

I find that if it's added slowly and deep under the surface of the electrolyte, the sulfur dioxide gas tends to stay in solution where it works to break down the residual chlorate, leaving the sodium perchlorate essentially chlorate-free (once enough metabisulfite is used, AND enough time has passed at a high enough temperature).

 

Once the residual chlorate is gone, the sodium perchlorate can easily be converted to other useful perchlorates. If, for example, you add potassium chloride solution to the purified sodium perchlorate solution, potassium perchlorate immediately drops out of solution as a fine white powder, leaving everything else dissolved in the liquid state.

 

WSM

Edited December 1, 2016 by WSM