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making potassium (per) chlorate


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Posted (edited)

Can you order one more on my behalf?

 

At least it would save a little bit on shipping.

Edited by taiwanluthiers
Posted

Can you order one more on my behalf?

At least it would save a little bit on shipping.

 

If I do the deal with them, I'll have extras to make available.

 

WSM B)

Posted (edited)

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.

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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 B)

 

The stainless steel belleville washers arrived from McMaster-Carr a couple days ago and I installed them on the cell.

 

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These four spring washers will absorb minor expansion due to the heating of the cell without damaging the seals. We'll see how it works in practice, when I get the cell operational.

 

WSM B)

Edited by WSM
Posted

 

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 B)

 

WSM

keep me in mind for a couple

 

memo

Posted

WSM keep me in mind for a couple

memo

If this works out, I'll be happy to. I don't know what difficulties may be involved but we'll cross that bridge later.

 

WSM B)

Posted

 

LD anodes will be much easier to ship within the US. I don't know what the challenges would be to ship them internationally.

 

This requires further investigation.

 

WSM B)

Posted

There should be no challenge apart from paying higher shipping fees and filling out one extra form.

 

As long as you pack them properly they should not be damaged.

Posted

i have a USA drop ship address so that is not problem

 

memo

Posted

There should be no challenge apart from paying higher shipping fees and filling out one extra form.

As long as you pack them properly they should not be damaged.

 

The shipping fees could be very high depending on the destination.

 

I plan to pack them similarly to the way Swede shipped MMO stock to me years ago, with careful wrapping and sandwiched between two thin plywood sheets. They should arrive in good shape.

 

WSM B)

Posted

i have a USA drop ship address so that is not problem

memo

 

Well that certainly simplifies things. Whenever (or if ever) I get my hands on a batch of LD anodes, I'll be in touch. Thanks, memo.

 

WSM B)

Posted (edited)

I've got the experimental high temperature sodium chlorate cell fundamentally completed. The last preparatory step before running it is to test it for water-tightness. I would have done this already, except the weather isn't cooperating (lots of rain this weekend).

 

Once it's proven to be water tight, I need to populate the top and bottom plates with the plumbing and connections for proper cell operation, including pH control for the second run and thereafter.

 

The plan is to use depleted liquor from last Summer's cell run, recharged with purified brine. This is all new territory for me so we'll see how it goes and what, if any, modification is required to get it operating correctly.

 

As always, there's more to come...

 

WSM B)

Edited by WSM
Posted

I've got the experimental high temperature sodium chlorate cell fundamentally completed. The last preparatory step before running it is to test it for water-tightness. I would have done this already, except the weather isn't cooperating (lots of rain this weekend).

Once it's proven to be water tight, I need to populate the top and bottom plates with the plumbing and connections for proper cell operation, including pH control for the second run and thereafter.

The plan is to use depleted liquor from last Summer's cell run, recharged with purified brine. This is all new territory for me so we'll see how it goes and what, if any, modification is required to get it operating correctly.

As always, there's more to come...

WSM B)

 

The rain is over for now and none forecast for the next week so I'll see if I can make more progress this weekend, if not sooner. There's still a lot of standing water out where I run my cell so I may have to wait for the ground to be more firm before resuming my work (otherwise it's likely to be a glorious mess).

 

I'll post more of my progress as I'm able to get to it.

 

WSM B)

Posted

Why is rain such an issue? Do you run your cell outside?

 

Why not run it in the garage or build a simple shed so that rain isn't an issue?

Posted (edited)

Why is rain such an issue? Do you run your cell outside?

Why not run it in the garage or build a simple shed so that rain isn't an issue?

Yes, I do run my cell outside. I find it more convenient for safely venting hydrogen as well as avoiding smelly or toxic fumes accumulating.

 

That's the same reason I don't run it in the garage, plus I hate to see my expensive machine tools turn brown. As for the simple shed, I'm all for it; but my wife isn't. Our understanding is that I can have things, but she doesn't want to see them. If it's visible, it's an issue.

 

I don't need any issues with her; life's simpler that way. ;)

 

WSM B)

Edited by WSM
Posted

Our understanding is that I can have things, but she doesn't want to see them. If it's visible, it's an issue.

 

Get her hooked on Facebook games, and you can have anything you want, anywhere you want it? Her eyes will be glued to the screen 24/7, and you are set for life. Sort of lonely, for life as well, i suppose, but...

 

Anyway, she sounds like a keeper.

B!

Posted (edited)

Get her hooked on Facebook games, and you can have anything you want, anywhere you want it? Her eyes will be glued to the screen 24/7, and you are set for life. Sort of lonely, for life as well, i suppose, but...

Anyway, she sounds like a keeper.

B!

Thanks, MrB. She's definitely a keeper.

 

The question sometimes is will she keep me? Hence, the reason I try not to push it too far. ;)

 

WSM B)

Edited by WSM
  • Like 1
Posted

just made a batch of potassium chlorate. I mixed it with a little sugar 50/50 and put a couple of drops of 97% sulfuric acid on it. no fire only pops like it was crackle mix. I have not seen that before. your thoughts ?

Posted (edited)

just made a batch of potassium chlorate. I mixed it with a little sugar 50/50 and put a couple of drops of 97% sulfuric acid on it. no fire only pops like it was crackle mix. I have not seen that before. your thoughts ?

 

If you mixed the sugar/chlorate 50:50 by volume (or even by weight) it would be highly fuel-rich and less inclined to fully ignite. I suggest mixing the small, powdered sample 70:30 (oxidizer to fuel) by weight, mix thoroughly and try the acid test again.

 

I think you'll see better results, if the KClO3 is pure.

 

For safety, be sure to perform this test outdoors using very small amounts.

 

WSM B)

Edited by WSM
Posted

just made a batch of potassium chlorate. I mixed it with a little sugar 50/50 and put a couple of drops of 97% sulfuric acid on it. no fire only pops like it was crackle mix. I have not seen that before. your thoughts ?

 

Another thought, there are several factors to making pyrotechnic mixtures perform reliably:

  • the coarseness of the particles (how fine are they?)
  • the intimacy of mixing (how well are they mixed?)
  • the degree of contact (are they packed tight or a loose mixture with lots of space between the particles?)
  • the size of the ignition surface (how much area is exposed to the propagation impetus?)

There is much more at play here and these are just a sample of the considerations.

 

Have you tried it again? Let us know.

 

WSM B)

Posted

potassium chlorate is pretty potent, and I have made a very imprecise mix before and they would always ignite reliably. So I think there's other factors at play.

Posted

potassium chlorate is pretty potent, and I have made a very imprecise mix before and they would always ignite reliably. So I think there's other factors at play.

That may well be. Without more information, we can't know for sure.

 

WSM B)

Posted

after I pulled the crystals out of the hot solution I let it cool and what I tested is what was in the bottom of the bucket of cold electrolyte.... I guess that is my problem. the other tested great.

 

memo

Posted

after I pulled the crystals out of the hot solution I let it cool and what I tested is what was in the bottom of the bucket of cold electrolyte.... I guess that is my problem. the other tested great.

memo

 

It sounds like it's impure; mixed chlorate and chloride maybe? I think you solved the mystery.

 

WSM B)

Posted (edited)

Between a heavy work schedule (>60 hours a week) starting this Saturday and lasting for months (till April), and preparing to go to the Western Winterblast (in about two weeks); I plan to put off the start of the high temperature NaClO3 experiment till after my return from Winterblast.

 

I'll see if I can get the cell ready to start in the meantime, but not start it till I get home from Arizona.

 

WSM B)

Edited by WSM
Posted (edited)

Hey guys :)

I've boiled down my stock electrolyte from 40l to 8l.

I was able to get out 806g KClO3 wchich remained in solution.

It was really pure due to lots of filtrations between the evaporation steps.

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Now im boiling the last 8l down to 1-2l and i start harvesting again over the year.

This morning i came down to my workplace and take a first look into the bucket with cooled electrolyte.

Now mostly of the Chlorate is pecipitated and the Chlorides start to fall out of solution.

Since i dont work with proper calculations, ive got lots of chloride left but im not be able to tell which one ive got here.

 

assuming that the Kcl is much more soluble i first thought that it must be NaCl.

I washed a crystal fairly and gave it a taste and it tasted much like Kcl.

What do you think, and what can i do to find out which chloride i have left here.

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Edited by PTFE
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