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making potassium (per) chlorate


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#4841 WSM

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Posted 25 February 2018 - 07:29 PM

In the UK the stepless step drill would be called a cone drill or a taper drill. In the USA who knows (Ace Hardware doesn't) 

 

Harbor Freight Tools does has them. I don't recall exactly what they call them, though. A search through their online catalog in the "drill bit" section may reveal the name used.

 

WSM B)


Edited by WSM, 04 March 2018 - 10:42 AM.


#4842 Pyrophury

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Posted 04 March 2018 - 02:56 PM

Didn't get much done this weekend, it's been so cold... I just cut the rough shape of my RC lid from sheets of 5 and 10mm thick PVC. 

 

gallery_10990_90_70237.jpg



#4843 WSM

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Posted 21 March 2018 - 02:09 PM

Didn't get much done this weekend, it's been so cold... I just cut the rough shape of my RC lid from sheets of 5 and 10mm thick PVC. 
gallery_10990_90_70237.jpg


Hi Pyrophury,

That's a nice looking lid.

If you make another one, You may want to try making it overhang the OD of the tank so it's easier to remove when you want or need to.

My 2 cents.

WSM B)

Edited by WSM, 21 March 2018 - 02:26 PM.


#4844 eb666

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Posted 15 April 2018 - 06:42 PM

On 12 august 2017 I posted about a platinum anode.

I cannot post details here as the board will not allow me to post zip files!!!

 

See sciencemadness.org 'thoughts on anodes' in the 'Technochemistry' section if interested.

 

The anode works great and will give kg and kg of perc of used correctly. 

I subjected the Pt    to abusive conditions and it held up well. About 60 dollars will get you a one gram bar. It will make around 140 grams perc from chlorate per day at 3 amps

 

 

 

EB



#4845 Arthur

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Posted 16 April 2018 - 12:36 AM

Platinum is one of the long established electrode metals, it simply works. However  to get a decent surface area usually costs a lot. I've just found 10mm x 50mm x 1mm for about £350, then you need the connector wire and it's still only 10 cm2 which will not take much current for the money. The issue with platinum is that it erodes significantly if abused by over current.

 

Someone used a platinum wire as an electrode most currents were too much because of the small surface area. The platinum eroded next to the holder til it dropped off and fell to the bottom.

 

One reported commercial method used platinum sheet as electrodes which worked well but there was the massive investment to pay for and the cost of erosion losses measured in grammes per ton of product.

 

Does anyone want to evaluate the cost of running a platinum electrode vs the cost of using a lead dioxide electrode or any other. 



#4846 WSM

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Posted 22 April 2018 - 10:08 AM

Platinum does work and work well. Cost is the main issue. Fortunately, the working portion of the electrode is the surface. This means that platinum plated electrodes work as well as solid platinum, so long as the plating lasts.

 

Proper treatment of the platinum electrode will insure longer life and higher productivity from it. My best guess to date has been to (successfully) run my platinum plated titanium electrodes "lightly", meaning at less than maximum current carrying capacity, and only for the required amount of time. Also, I use platinized titanium (or LD) electrodes exclusively for converting sodium chlorate to sodium perchlorate, preparatory to forming potassium perchlorate (or other perchlorates). I use MMO for producing chlorates and save the more specialized and expensive electrodes for better things.

 

I've considered using platinum bullion for electrodes, but I feel the better form would be to roll the "coin" into foil and carefully spot weld it to a CP titanium frame for support. The greater surface area would allow for more workable surface of the electrode.

 

Those are some of my thoughts on the subject. I haven't pursued it due to the expense of platinum and my success to date with the lower cost lead dioxide electrodes I've managed to acquire. I've also gotten hold of several platinized titanium mesh electrodes, and their cost is well below that of solid platinum materials.

 

These are my opinions; your mileage may vary...

 

WSM B)


Edited by WSM, 22 April 2018 - 10:12 AM.


#4847 Pyrophury

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Posted 29 April 2018 - 12:58 PM

gallery_10990_90_578616.jpg

It's getting there, slowly... I made a Viton rubber o-ring and groove for it to sit in, and tapped the holes for the 3/8" NPT compression fittings.

Edited by Pyrophury, 29 April 2018 - 12:59 PM.


#4848 WSM

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Posted 30 April 2018 - 07:32 AM

It's getting there, slowly... I made a Viton rubber o-ring and groove for it to sit in, and tapped the holes for the 3/8" NPT compression fittings.

 

Good work. It looks like it's coming along nicely.

 

WSM B)



#4849 WSM

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Posted 01 July 2018 - 10:33 AM

As I've put my high temperature sodium chlorate cell experiment on hold due to my failure to get a liquid tight seal on my fabricated cell, I've considered miniaturizing an experimental setup for a "proof of concept", before continuing on the larger cell. This was briefly mentioned in the original patent, but no results were mentioned.

 

For this effort, I've managed to acquire a round bottomed, borosilicate 5 liter reaction flask without a lid, for a reasonable cost. The large diameter, top flange of the heavy walled container has a groove to accommodate an O-ring (which I plan to fabricate from Viton tubing) and I'll use a thick polymer plate for the cell lid (which can be modified to hold the electrodes and various fittings for vents and sensors) and seal it to prevent salt-creep.

 

As the goal is to run the cell at approximately 110oC, so it will naturally concentrate the NaClO3 by evaporation of the water as the cell runs, I'll run the current as high as possible to the electrodes and monitor the temperature carefully. If the electrodes aren't enough alone to heat the cell that high, I have heating mantles that can be used to boost the temperature, if required.

 

I hope to set this experiment up by September at the latest, to test the system and verify what the patent declares. 

 

WSM B)


Edited by WSM, 02 July 2018 - 07:02 AM.


#4850 WSM

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Posted 04 July 2018 - 09:29 PM

Happy Fourth of July to all the US readers here. Be safe tonight, as you celebrate our nation's 242nd birthday.

WSM B)

#4851 WSM

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Posted 15 July 2018 - 08:02 AM

My new approach to the High Temperature Sodium Chlorate Experiment Involves a 5 liter reaction vessel without a lid, purchased earlier this year. It is heavy walled borosilicate glass and has a large opening with a flat top and a groove for an O-ring.

 

Attached File  IMGP0002.JPG   95.86KB   3 downloads

 

I've experimented with silicone tubing to determine what size and length is needed to form an O-ring for the top plate seal. 6mm diameter tubing worked but I feel the groove is made to accomodate 1/4" material. I won a bid on a good length of Viton tubing, 1/8" ID and 1/4" OD. When cut to the correct length, I plan to join the flush-cut ends with a short piece of 1/8" OD Viton tubing inside and bond them all together with acetone as a solvent.

 

The next task will be to decide which polymer to use for the lid of the cell. In the original patent, they used a one inch (~25mm) thick piece of Lucite (Plexiglass or Perspex) with ports added for the electrodes, vent and a host of other purposes. That may work but I'm also considering either PVC, CPVC or Kynar plate. The Kynar, if available and affordable, may be the most compatible choice, considering all the parameters of this cell. If I go with that, I'll need to shop for a workable piece plus determine the best method of attachment.

 

There's much more to do, but I'll give it my best and try this thing out!

 

WSM B)


Edited by WSM, 15 July 2018 - 08:03 AM.


#4852 WSM

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Posted 15 July 2018 - 08:21 AM

The original patent used a pair of platinum plated titanium electrodes, 3" square. When running it, they occasionally reversed polarity to maintain the best environment for the electrodes.
 
My plan is to use an MMO mesh anode surrounded by two solid plates of CP titanium for cathodes, all 4" square, which should work nicely. I hope the added size will more easily get to and operate at a high enough temperature to reach and maintain a running temperature of about 110oC, which should optimize the production of NaClO3 while concentrating the electrolyte by evaporating the excess water, making chlorate recovery at room temperature (rather than chilling the electrolyte to 0oC for oxidizer recovery, as done previously) a much simpler and less costly process. An added benefit will be using purified brine to recharge the "depleted" electrolyte, rather than dry purified salt.
 
The whole system appears that it will easily lend itself to a continuous system, but baby steps first.
 
WSM B)

Edited by WSM, 18 July 2018 - 02:58 PM.


#4853 WSM

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Posted 28 August 2018 - 07:20 AM

I'm ready to pick up my work on Part Eighteen of the series, Homegrown Oxidizers, published in the PGI Bulletin.

In it I'm continuing the research into purifying potassium chloride solution for use in chlorate cells OR for use in producing purified potassium perchlorate from purified sodium perchlorate.

My thinking is that since I'm bothering to make oxidizers (when I can buy them if I want), why not make them better than commercial grade material (+-99% Mil Spec standards)?

I'll let you know when the draft is submitted to the Bulletin.

WSM B)


Edited by WSM, 02 September 2018 - 11:21 AM.


#4854 pyrojig

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Posted 09 September 2018 - 10:22 PM

EXciting news. Looking forward to the new findings on your research  



#4855 tylerngo

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Posted 15 October 2018 - 02:26 PM

Did you finally get the help that you required? Update please.

 

Brumer



#4856 WSM

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Posted 02 November 2018 - 05:25 AM

Did you finally get the help that you required? Update please.

Brumer

 

I'm sorry, I don't follow what you mean. Can you elaborate?

 

WSM B)



#4857 WSM

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Posted 02 November 2018 - 05:32 AM

I apologize for not posting very much. My research has taken a back seat to several other projects, plus greater demands on my time by family and work. My work schedule is going to get much busier starting next month, and last into April.

 

If possible, I'll see if I can make some headway on my electrochemical research and report my progress here.

 

More later...

 

WSM B)



#4858 WSM

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Posted 04 November 2018 - 10:28 AM

I apologize for not posting very much. My research has taken a back seat to several other projects, plus greater demands on my time by family and work. My work schedule is going to get much busier starting next month, and last into April.

If possible, I'll see if I can make some headway on my electrochemical research and report my progress here.

More later...

WSM B)

 

A couple of the projects occupying my time include changing the power in my workshop from a line connected in from the house power, to an off-grid solar system, including a battery backup, sufficient to supply all the electricity I can use, plus...

 

The other project is a discrete (meaning, stand-alone) purified water system. Both systems will add to emergency home preparedness, as well as supply my hobby projects. 

 

When those efforts reach a greater degree of completion, I plan to resume my electrochemical research and set up several experiments to demonstrate an ability to be more self sufficient in chlor-alkali oxidizer production (a fun challenge, for sure!).

 

All of this depends on fitting things in, between work, family needs and any other demand on my time. Wish me luck!

 

WSM B)






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