Jump to content


Photo
* * * * * 3 votes

making potassium (per) chlorate


  • Please log in to reply
4567 replies to this topic

#4561 WSM

WSM

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 2,519 posts
  • Gender:Male

Posted 09 January 2017 - 01:53 PM

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 B)


Edited by WSM, 09 January 2017 - 02:51 PM.


#4562 PTFE

PTFE

    Playing with fire

  • Full Member
  • PipPip
  • 13 posts
  • Gender:Male
  • Interests:Elektrochemistry, high voltage stuff

Posted 09 January 2017 - 03:00 PM

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 :D ^_^ )

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 by PTFE, 09 January 2017 - 03:07 PM.


#4563 WSM

WSM

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 2,519 posts
  • Gender:Male

Posted 09 January 2017 - 06:25 PM

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 :D ^_^ )

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 B)


Edited by WSM, 10 January 2017 - 07:10 AM.


#4564 WSM

WSM

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 2,519 posts
  • Gender:Male

Posted 11 January 2017 - 11:18 PM

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 B)


Edited by WSM, 11 January 2017 - 11:21 PM.


#4565 WSM

WSM

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 2,519 posts
  • Gender:Male

Posted 14 January 2017 - 06:24 PM

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  :D !!!

 

I'll report more later...

 

WSM B)


Edited by WSM, 14 January 2017 - 06:26 PM.


#4566 taiwanluthiers

taiwanluthiers

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 1,358 posts
  • Gender:Male

Posted 14 January 2017 - 11:12 PM

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?



#4567 PTFE

PTFE

    Playing with fire

  • Full Member
  • PipPip
  • 13 posts
  • Gender:Male
  • Interests:Elektrochemistry, high voltage stuff

Posted Yesterday, 07:11 AM

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 by PTFE, Yesterday, 07:26 AM.


#4568 taiwanluthiers

taiwanluthiers

    Firebreather

  • Full Member
  • PipPipPipPipPip
  • 1,358 posts
  • Gender:Male

Posted Yesterday, 10:42 AM

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






0 user(s) are reading this topic

0 members, 0 guests, 0 anonymous users