making potassium (per) chlorate

[WSM]

I mentioned the PTFE (Teflon) sheet to cover the steel base of the new experimental cell. Years ago, a kind friend gave me several feet of thin, white Teflon sheet in a small roll, for use to cut stars on and easy cleanup afterward. This material is roughly one foot wide and several feet long by about 0.030" thick.

A couple days ago, I cut a piece of it just long enough to cover the top of the steel base plate (to protect it from the corrosive effects of the electrolyte). The plan is to disassemble the complete cell assembly, cut matching holes in the Teflon sheet, place it over the black steel plate and reassemble the whole arrangement.

I also plan to cover the exposed stainless threaded rod under the cell and above the base plate, to protect the tubing and hardware from the sharp threads of the all-thread rods.

I still need to drill and tap holes in the PVDF top plate of the cell for compatible fittings and ports required for the proper operation of this cell arrangement.

The weather isn't cooperating at the moment, but hopefully the weekend will afford me the opportunity to make more progress on this project.

WSM

 

I took some time after work today, disassembled the cell and added the Teflon sheet to the base plate to protect the steel from corrosive fluids.

 

I also took two photos as I was reassembling the cell, showing the covered steel base plate and the electrode assembly and also the cell body dropping over the electrodes as it was going back together.

 

 

 

I still need to drill and tap ports on the lid of the cell for fittings, et cetera; but it'll no longer require me to completely disassemble the cell (only the top portion of it).

 

I expect the Kynar fittings I ordered to arrive within a week and I can populate the cell with some of those fittings and ready the cell for operation. I still need to test the cell for leaks. Hopefully there are none.

 

This is getting exciting...

 

WSM

Edited January 7, 2017 by WSM

[pyrojig]

Holy cats!!!!! That is beautiful!!!!!! I can't believe how far the thread moves in just a few days . You guys are amazing!! Please keep upvthe good work .

[WSM]

Holy cats!!!!! That is beautiful!!!!!! I can't believe how far the thread moves in just a few days . You guys are amazing!! Please keep upvthe good work .

 

The cooler weather seems to encourage progress !!!

 

WSM

[PTFE]

Yes, this looks pretty nice WSM

I just got my PbO2 Sample from qixinti today and want to show it too you.

 

The coating is really thick.. something about 1,5-3mm and i tryed some different types to break of a little of the coating but i failed.. there is no way to crumble down.

When i holded it in my hands the first time, i was amazed, how heavy it is. Nothing, than PbO2 will be that heavy.

i payed 16$ for shippment via DHL Xpress ant the anode was 30$.

hope you will get interessted in that company.

 

Greetings, PTFE

 

[Mumbles]

That looks like a great electrode. Please keep us updated on how it works PTFE! Are you planning to do any washing or pre-treatment before use? I know some electrodes come with sort of a dull brown residue on them which can be removed with a dilute HCl soak.

[WSM]

Yes, this looks pretty nice WSM

I just got my PbO2 Sample from qixinti today and want to show it too you.

15940493_1831385620465035_6255690037075857060_n.jpg

The coating is really thick.. something about 1,5-3mm and i tryed some different types to break of a little of the coating but i failed.. there is no way to crumble down.

When i holded it in my hands the first time, i was amazed, how heavy it is. Nothing, than PbO2 will be that heavy.

i payed 16$ for shippment via DHL Xpress ant the anode was 30$.

hope you will get interessted in that company.

Greetings, PTFE

 

That's a nice looking LD anode. I emailed them weeks ago and have heard nothing from them yet.

 

I look forward to the results of you using that anode. It should work nicely.

 

WSM

[WSM]

That looks like a great electrode. Please keep us updated on how it works PTFE! Are you planning to do any washing or pre-treatment before use? I know some electrodes come with sort of a dull brown residue on them which can be removed with a dilute HCl soak.

 

PTFE is showing a photo of a new lead dioxide anode from China, and it should require no pre-treatment before use.The treatment with HCl is usually done with surplus MMO stock, as supplied by eBay sellers such as laserred, not with new anode material (whether MMO or another type).

 

If PTFE has a supply of sodium chlorate, he could immediately start to produce sodium perchlorate with a solution of it using that anode and convert the perchlorate solution to potassium perchlorate with KCl solution (after destroying residual chlorates in the electrolyte).

 

I hope I hear from that company. If so, I might buy a few of the LD anodes to test.

 

WSM

Edited January 9, 2017 by WSM

[taiwanluthiers]

I would like to buy a few as well...

[memo]

me too

[PTFE]

Hey guys, nice to got so much response.

I purchased them via Alibaba.com and they will give you a fast reply usually..

https://bjqixinti.en.alibaba.com/

I dont know if you are familiar with alibaba, but it is not that difficult.

Just sign in and start a chat with the trader and ask for a customized anode or a sample if you are pleased with 100x100mm.

They also provide titanium sheets and i think also screws, washers and nuts made from titanium, so everything you need can you get from one trader.

 

I need to get my little MMO cell started to make some high concentrated NaClO3 solution to preper an other cell with the PbO2 but i think i will need some weeks, since i have some work to do atm.

Sadly i only got several grams of KclO3 but no NaClO3 because i always did a entire conversion.

maybe you dont get a response from the suplyer, because Mr. Feng has left the company and another is doing his job.. maybe its another email now.. but try it via alibaba it will be the best way i think...

 

Hopefully you will all get provided in the future,

PTFE

 

EDIT: When you like to purchase a customized anode, give them your quantity and a drawing with your request and you will get a price immediately, maybe ask for a door to door service too.

Edited January 9, 2017 by PTFE

[WSM]

Hey guys, nice to got so much response.

I purchased them via Alibaba.com and they will give you a fast reply usually..

https://bjqixinti.en.alibaba.com/

I dont know if you are familiar with alibaba, but it is not that difficult.

Just sign in and start a chat with the trader and ask for a customized anode or a sample if you are pleased with 100x100mm.

They also provide titanium sheets and i think also screws, washers and nuts made from titanium, so everything you need can you get from one trader.

I need to get my little MMO cell started to make some high concentrated NaClO3 solution to preper an other cell with the PbO2 but i think i will need some weeks, since i have some work to do atm.

Sadly i only got several grams of KclO3 but no NaClO3 because i always did a entire conversion.

maybe you dont get a response from the suplyer, because Mr. Feng has left the company and another is doing his job.. maybe its another email now.. but try it via alibaba it will be the best way i think...

Hopefully you will all get provided in the future,

PTFE

Thanks, PTFE.

 

I'll try again through alibaba.

 

WSM

Edited January 9, 2017 by WSM

[PTFE]

I will do a light washing with very dilute HCL and hot water but i think it doesnt matter..

I rellay think , that to much care is not advisable.

If you work with larger qty's of electrolyte, work with PE/PP buckets and for filtration i use some white weeds fleece and do a lot and a lot of filtrations...

One Before the run, after replenishment with NaCl, after the run maybe twice ore more times and mostley with dual layer of the fleece to get rid of the elecrode material and other stuff like hairs.

The KCL solution is also filtered and after both solutions are put together i do another filtration if there has not a bunch of crystals formed yet.

With many filtrations you'll get a quite clean product and large Crystals..

The last run gave me 6cm large, crystal clear flakes of Clorate.

My problem is the wear of the Cathodes.. after a run i can break them with a bit of bending.. i think its not grade one or two Titanium but i really dont care about some erosion products..

I think to much care about contamination will make you crazy.. specially if you have got a dog with many hairs^^

 

My filtration setup is very easy.. just the fleece on the bucket assured with a rubber band.

It has to be damped first, or you get no flow!

But when its working, its not a big deal, to filter more than 10liters in a short period of time.

Its also very easy to filter when you do a recrystalisation because its fast and nothing will get blocked.

After every filtration step, you can wash the fleece with water or if you have got enough, take one for every step and wash them all together for the next time you need them.

 

Its also a good idea to take an PP or an Acrylic tube with fleece->filter cotton manteled with fleece-> activated charcoal-> Fleece to get a very very clean electrolyte.

With a big diameter youll get a good flow in the filtration system and the media has not to be changed too often.

 

I do it this way before i put everything(washing water, recrystalisation water, desaturated electrolyte and so on) together in a big tub for evaporation, when nothing is in progress .

Then you've got a very clean electrolyte and as it evaporates large crystals will form.

I've harvested more than 30l in the last Year and now there is a 3-4cm layer of Chlorate at the bottom..

You have to take it out several months because at some point NaCl will start to fall out and will contaminate your "post-product" which is normaly the most cleanest which don't have to be recrystalised in my opinion.

 

For heating i have built a immersion heater from two 230V/1,5kw Heat spirals connected in series for a lower wattage, since it gets hot enough to destroy the PTFE easily.

Ive put them in a PTFE tube (10x1) with a little bit of transformer oil.

The problem with this idea is the fluid in your tube... if you dont use it, the PTFE will get to hot at some places and will get destroyed i think. But with oil you have the problem of boiling oil in a tube.

This causes bubbles to build up and the oil gauge will rise continously if you dont provide a form wich allowes every bubble that forms to get to the top of the liquid. This is impossible if you make a simple spiral, so i use only that much oil, that it can boil the entire way in my heating spiral without a rising of the oil gauge.

(i hope you can understand what im trying to say )

This is a great way to boil 2-10liters of electrolyte or anything other corrosive stuff you might want to boil. ( my first attempt with this techique was some years ago with a boro. glass tube for a solution of CuSo4)

 

I had also the case, that boiling oil leaked out of the top of the PTFE immersion heater direktly into the electrolyte but with several filtrations with the fleece i got rid of it ..also i had some contamination wit Loctite (for the screws in the bottom of the tank which i had to remove last time) which was no deal for the fleece.

for oily contaminations a cotton T-shirt might also work great.

 

If you are now in a new mania of making high purity ClO3/4 please take a look, that your fleece is made from PP/PVC/PE or any material which will withstand the corrosive environment of the Chlorate industry.

 

PTFE

Edited January 9, 2017 by PTFE

[WSM]

I will do a light washing with very dilute HCL and hot water but i think it doesnt matter..

I rellay think , that to much care is not advisable.

If you work with larger qty's of electrolyte, work with PE/PP buckets and for filtration i use some white weeds fleece and do a lot and a lot of filtrations...

One Before the run, after replenishment with NaCl, after the run maybe twice ore more times and mostley with dual layer of the fleece to get rid of the elecrode material and other stuff like hairs.

The KCL solution is also filtered and after both solutions are put together i do another filtration if there has not a bunch of crystals formed yet.

With many filtrations you'll get a quite clean product and large Crystals..

The last run gave me 6cm large, crystal clear flakes of Clorate.

My problem is the wear of the Cathodes.. after a run i can break them with a bit of bending.. i think its not grade one or two Titanium but i really dont care about some erosion products..

I think to much care about contamination will make you crazy.. specially if you have got a dog with many hairs^^

My filtration setup is very easy.. just the fleece on the bucket assured with a rubber band.

It has to be damped first, or you get no flow!

But when its working, its not a big deal, to filter more than 10liters in a short period of time.

Its also very easy to filter when you do a recrystalisation because its fast and nothing will get blocked.

After every filtration step, you can wash the fleece with water or if you have got enough, take one for every step and wash them all together for the next time you need them.

Its also a good idea to take an PP or an Acrylic tube with fleece->filter cotton manteled with fleece-> activated charcoal-> Fleece to get a very very clean electrolyte.

With a big diameter youll get a good flow in the filtration system and the media has not to be changed too often.

I do it this way before i put everything(washing water, recrystalisation water, desaturated electrolyte and so on) together in a big tub for evaporation, when nothing is in progress .

Then you've got a very clean electrolyte and as it evaporates large crystals will form.

I've harvested more than 30l in the last Year and now there is a 3-4cm layer of Chlorate at the bottom..

You have to take it out several months because at some point NaCl will start to fall out and will contaminate your "post-product" which is normaly the most cleanest which don't have to be recrystalised in my opinion.

For heating i have built a immersion heater from two 230V/1,5kw Heat spirals connected in series for a lower wattage, since it gets hot enough to destroy the PTFE easily.

Ive put them in a PTFE tube (10x1) with a little bit of transformer oil.

The problem with this idea is the fluid in your tube... if you dont use it, the PTFE will get to hot at some places and will get destroyed i think. But with oil you have the problem of boiling oil in a tube.

This causes bubbles to build up and the oil gauge will rise continously if you dont provide a form wich allowes every bubble that forms to get to the top of the liquid. This is impossible if you make a simple spiral, so i use only that much oil, that it can boil the entire way in my heating spiral without a rising of the oil gauge.

(i hope you can understand what im trying to say )

This is a great way to boil 2-10liters of electrolyte or anything other corrosive stuff you might want to boil. ( my first attempt with this techique was some years ago with a boro. glass tube for a solution of CuSo4)

I had also the case, that boiling oil leaked out of the top of the PTFE immersion heater direktly into the electrolyte but with several filtrations with the fleece i got rid of it ..also i had some contamination wit Loctite (for the screws in the bottom of the tank which i had to remove last time) which was no deal for the fleece.

for oily contaminations a cotton T-shirt might also work great.

If you are now in a new mania of making high purity ClO3/4 please take a look, that your fleece is made from PP/PVC/PE or any material which will withstand the corrosive environment of the Chlorate industry.

PTFE

 

Thanks for describing your processes and techniques, PTFE. I had a bit of difficulty following the details and wish there were photos to go along with the written explanation, so I could understand clearly.

 

If you get a chance, can you show some pictures of the process? That would be great. Thanks.

 

WSM

Edited January 10, 2017 by WSM

[WSM]

I got an email notification from FedEx today, that my Kynar fittings are due to arrive tomorrow. I can then soon finish the top plate of the cell and get it set up after I test the cell to ensure it's water-tight.

 

I'm also still waiting for some larger crimp-on cable lugs for the welding cable leads (I expect them by this weekend).

 

I'm anxious to get the high temperature sodium cell set up and running. I hope for great things from it.

 

WSM

Edited January 12, 2017 by WSM

[WSM]

Well, it's Saturday, I'm off work and the weather is cooperating, so I'm back to working on the high temperature sodium chlorate cell.

 

I drilled 5 holes for 1/2" NPT fittings, and I'm planning on drilling 4 more holes for 1/4" NPT fittings. All the tapped holes that aren't going to be used for the immediate project will be stopped with some PVDF plugs I just got from Ozone Solutions a few days ago.

 

The next stop will be testing the cell to confirm that it's water-tight. If not, I'll do what's required to make it so. After that, it's time to set it up and run the high temperature sodium chlorate experiment !!!

 

I'll report more later...

 

WSM

Edited January 15, 2017 by WSM

[taiwanluthiers]

Is there a way for one guy to just order from Alibaba and then sell it to us?

 

The reason I ask is because I feel intimidated to deal with Chinese suppliers, they seem to want big numbers and I don't see how an individual can do this. Perhaps a group buy?

[PTFE]

The most asian sellers are really kindly if you ask for samples or limited quantitys for private projects even if they provide large quantitys for big companies.

Especially the one i've posted earlier is really encouraged in helping you with your questions.

Maybe you have to ask through alibaba, because WSM did not get any reaction from the mail adress listed on their homepage.

Also i am going to buy a second time this year, so i could provide a group buy, but its not so good since im located in the EU and duty will be an effort.

Also you should think about your plans, since you usually can get every Titanium product you need for electrolysis very cheap from those Chlorkali-suppliers.

Edited January 15, 2017 by PTFE

[taiwanluthiers]

yea but getting pre made lead dioxide anode is another kettle of fish.

[eb666]

yea but getting pre made lead dioxide anode is another kettle of fish.

 

See ptfe's post of 17 Dec 2016

[memo]

 

See ptfe's post of 17 Dec 2016

 

g, I wish I could hav said that

[WSM]

Hey guys..

If yome of you need PbO2 Anodes ask www.qixinti.com sales@qixinti.com

They've got 100x100x2mm Samples with terminal for 30$+shippment

Hi All,

 

I didn't hear from them by direct email, but (as PTFE said) through Alibaba they are responding. I got a quote for $37 per unit plus shipping for 4 units. The final price for the delivered anodes would be about $45 each.

 

Before I commit to buying some, I've asked for information about price breaks for larger quantities of these anodes (100mm x 100mm plus a 10mm x 50mm titanium strap). If I can get a better price for a reasonable quantity of them, I may go for a larger number of them.

 

I realize they're not the only suppliers. I got another quote for 5 anodes at $25 each, not including shipping from another company, but their quality and reputation are unknown to me (I need to investigate further).

 

I'll continue to research this and report back.

 

WSM

Edited January 17, 2017 by WSM

[WSM]

I drilled 5 holes for 1/2" NPT fittings, and I'm planning on drilling 4 more holes for 1/4" NPT fittings. All the tapped holes that aren't going to be used for the immediate project will be stopped with some PVDF plugs I just got from Ozone Solutions a few days ago.

 

I managed to finish drilling the holes and tapping them, and then plugged them with PVDF plugs and Teflon tape for testing the cell integrity. Later I'll populate the lid with other fittings needed for the proper operation of the cell.

 

 

Arthur raised a question about thermal expansion of the cell when operating at higher temperatures. The answer I came up with is to add belleville washers to the top hardware assembly holding the lid on the cell, for spring tension on the lid. This would allow for expansion without compromising the integrity of the Viton seals. When I locate the spring washers and install them, I'll show a photo of the assembly.

 

WSM

Edited January 18, 2017 by WSM

[OldMarine]

McMaster-Carr is your friend! You'll spend all your money with them and they have EVERYTHING!

https://www.mcmaster.com/#belleville-spring-washers/=15ygcp9

[WSM]

McMaster-Carr is your friend! You'll spend all your money with them and they have EVERYTHING!

https://www.mcmaster.com/#belleville-spring-washers/=15ygcp9

 

Yes, my friend; you are correct! You forgot to mention that they have 95% of everything in the catalog in stock!

 

I just ordered the correct size in stainless steel and will probably have them by this weekend.

 

Thank you for mentioning McMaster-Carr (how could I have forgotten? I used them all the time when I was self-employed [a terrible time; I had a jerk for a boss ]).

 

WSM

Edited January 18, 2017 by WSM

[WSM]

Hi All,

I didn't hear from them by direct email, but (as PTFE said) through Alibaba they are responding. I got a quote for $37 per unit plus shipping for 4 units. The final price for the delivered anodes would be about $45 each.

Before I commit to buying some, I've asked for information about price breaks for larger quantities of these anodes (100mm x 100mm plus a 10mm x 50mm titanium strap). If I can get a better price for a reasonable quantity of them, I may go for a larger number of them.

I realize they're not the only suppliers. I got another quote for 5 anodes at $25 each, not including shipping from another company, but their quality and reputation are unknown to me (I need to investigate further).

I'll continue to research this and report back.

WSM

 

The communication with suppliers on Alibaba is progressing. If I can work out a deal, I plan to order some LD anodes from them. We'll see how it goes.

 

WSM