making potassium (per) chlorate

[WSM]

Okay, I took the plunge and ordered some of the low cost LD anodes to try. We'll see if and how they work out. I plan to monitor various aspects of the setup and running conditions in an attempt to track what works and what harms these electrodes.

I hope we can find a happy solution to the observed problems. Even if we need to run them with a gentle current, if they hold up and run slowly, that's okay (slow perchlorate for a long time is preferable to a destroyed anode) and it'll work for me.

I'll report here what I observe and my results.

WSM

 

The electrodes arrived yesterday, wrapped very well. I unwrapped one and it looks good . By careful observation, it's clear the titanium substructures are welded together, probably by either a MIG or TIG process. The strap is on the smallish side and I suspect it can't carry much current. I'm more and more convinced the best approach is to spot weld a filled tubular titanium lead to the electrode and use it that way.

 

When Swede returned a while ago, I sent him samples of various CP titanium tubes I has collected; 6mm OD (thin wall), 6mm and 8mm (thick wall) and some small diameter Viton tubing. He was excited about the thin walled 6mm tubing so I sent most of what I had to him (I wasn't as excited about it as the thicker walled material). The point is, Swede did some tests with the tubing where he measured the temperature of the different tubes at different current levels, and what he was discovering is that they get fairly hot very quickly at not very high current loads. I think he filled the tubes with tin or something. If not, then there's another set of tests to be done.

 

His results had me thinking of searching out a source of larger diameter titanium tubing to use as electrical leads for the electrodes. I succeeded in sourcing 0.375" (9.525mm) and 0.500" (12.7mm) OD tubing to use as leads. I haven't tested their heating characteristics yet to see how much current they can safely carry, and probably should before commiting more valuable (and expensive) resources to the effort. I also have some 0.750" (19.05mm) tubing for particularly high current applications. All these tubes are CP titanium, of course.

 

To answer why I don't progress faster, I have too much going on and not enough free time to apply to the effort. So I progress at a snail's pace (actually the snails seem to be flying past me, at times). I haven't lost my passion for the research or pursuit of knowledge and understanding, so I keep at it.

 

I'll post what I learn as it comes...

 

WSM

Edited May 16, 2014 by WSM

[WSM]

I should mention, the reason I chose those sizes of CP titanium tubing is that they most closely fit the available PVDF compression fittings I use in cells to prevent the salt creep that likes to eat my electrical connections (and looks unsightly, as well). Only slight modification to the fittings is required to make them useful for the purpose.

 

WSM

[taiwanluthiers]

I'm having trouble finding anything made of CP titanium except for sheets... in fact I don't even think CP titanium bolts exist because almost all of them are 6Al4V. Problem with that alloy is the cell liquor dissolves them completely.

[WSM]

I'm having trouble finding anything made of CP titanium except for sheets... in fact I don't even think CP titanium bolts exist because almost all of them are 6Al4V. Problem with that alloy is the cell liquor dissolves them completely.

 

That's true plus adds vanadium and aluminum ions to the cell. CP titanium hardware and various shapes are hard to find unless you get lucky or live near a community where high tech materials are used and sometimes appear on the surplus market.

 

It has taken me years to source and accumulate a usable stock of CP materials (I'm not wealthy, either; just prudent). Patience and persistence wins out in the end.

 

WSM

[Arthur]

I saw a cell design once. It was an upright racetrack of big tube (prob PVC) and in one upright there was the electrode assembly. A Ti plate with electrode fins welded on the the plates placed on opposite sides of the upright pipe with the combs of electrodes interlinked. Viton gaskets and several thousand amps were supplied. the Hydrogen lift was enough to rotate the liquor and keep it hot as well as react. Brine was constantly fed in and strong solution constantly taken out.

[WSM]

I saw a cell design once. It was an upright racetrack of big tube (prob PVC) and in one upright there was the electrode assembly. A Ti plate with electrode fins welded on the the plates placed on opposite sides of the upright pipe with the combs of electrodes interlinked. Viton gaskets and several thousand amps were supplied. the Hydrogen lift was enough to rotate the liquor and keep it hot as well as react. Brine was constantly fed in and strong solution constantly taken out.

Any photos?

 

WSM

Edited May 16, 2014 by WSM

[frank]

There is always ceramic nuts and bolts of you cannot get Grade 1, 2, 3 .........Ti.

The price seems to be insane though!

http://www.amazon.com/s?rh=n%3A16403521%2Cp_n_feature_seven_browse-bin%3A3071292011

 

Can anyone think of where ceramic nuts/bolts are used in everyday products.

I am thinking of ferrite screw-ins (the bit you screw in) in electrical chokes (inductors).

You only have the screw bit though the 'nut' is usually plastic with the wires would upon it and there is no 'head'

on the screw bit (they are best described as a slug).

I have seen ceramic nuts on bolts somewhere. Can't think where though.

 

Some grade 2 bolts here:

http://www.titane-services.eu/epages/230155.sf/en_GB/?ObjectPath=/Shops/230155/Categories/visserie-titane-tige-filetee-titane/vis-titane-BHC

 

The price is a steal. (they are stealing off you)!!

 

Some more edits.

The threaded bar looks good. The price is good (22 euro for half a meter).

It is very easy to make titanium nuts yourself. Just purchase a threder (a tap) and drill a hole in a flat piece of Ti and thread the hold. Usually you will simply drill the piece of ti that you are working with, tap in the threads and the 'hole' is your 'nut' (if ya know what I mean).

Edited May 16, 2014 by frank

[MrB]

I cant help but think "rivets" for permanent assembly... The old school kind, that starts out as a short bar, and ends up being beat over the head with a hammer to lock it all in place. Just heat it until it's yellow, put it in place, and make it permanent.

B!

 

Edit

If beating it in to submission isn't right for where it's at, squeezing it works to. But that takes some squeezing...

/Edit

Edited May 16, 2014 by MrB

[WSM]

Some grade 2 bolts here:

http://www.titane-services.eu/epages/230155.sf/en_GB/?ObjectPath=/Shops/230155/Categories/visserie-titane-tige-filetee-titane/vis-titane-BHC

 

The best price I've seen on CP titanium machine screws was a year or two ago on eBay. They had a lot of about 50 or so for about $1.00 each. I passed on that and considered other options. I like the idea of CP titanium threaded rod (known here as "all thread") and making matching nuts. In fact, I have some CP titanium square rod which would work perfectly for square nuts.

 

All that is a moot point since I've invested in a spot welder and have practiced using it successfully. Welding is a lot faster and, if done correctly, permanent (plus it won't loosen with time).

 

The ceramic fasteners would probably work but seem too costly. If I were to consider an insulator material for binding parts together; PVC, PVDF or PTFE would be my first considerations. Compatible, conductive fasteners seem to be the best option I see here...

 

WSM

[WSM]

I cant help but think "rivets" for permanent assembly... The old school kind, that starts out as a short bar, and ends up being beat over the head with a hammer to lock it all in place. Just heat it until it's yellow, put it in place, and make it permanent.

B!

 

Edit

If beating it in to submission isn't right for where it's at, squeezing it works to. But that takes some squeezing...

/Edit

 

When I purchased some CP titanium tubing from a dealer, I also picked up some 1/8" diameter CP titanium round rod. I was thinking of rivets because I have a hand rivet setter for that size rivet.

 

I imagine the best way to make a rivet is to heat the end of the rod till it glows and form the round head with the setter. then cut the cooled rivet to the proper length. Heating the rivet, pushing it through the pre-drilled hole in the electrode/strap and setting it with the setter with a hammer on an anvil should complete the task.

 

I'm very glad I invested in that spot welder!

 

WSM

[frank]

It will be quite difficult to heat these very small rivets and then have time to grab a hammer or whatever and beat them while they are still red. It works OK on large rivets but these tiny rivets will cool much too quick (IMO).

No need for heat anyways as g 2 is fairly soft.

Beating rivest doesn't sound too good on a LD anode though. I would be afraid all the LD would land at your feet.

I attempted to make some Grade 2 bolts by cutting some square bar from a g2 sheet, rounding in a lathe and then threading using a die (the thing you usually use to make threads).

Grade 2 is too soft and it just twisted like plasticine as the threader (the die) attempted to cut the threads. Perhaps you could make the threads on a lathe if the lathe has a thread cutting facility.

Grade 5 would be easier to thread with a threader as it is not so soft and inclined to twist into a corkscrew instead of becoming a threaded bolt! Grad 5 is no good for our job alas.

 

Who was it above that suggested getting a piece of one gram Pt (bullion) and clamping it between two pieces of Ti and lowering the Pt + joints into a Perc cell. It should work IMO. I am going to try this myself using a piece of 'bent around like a fish hook'

piece of flat Ti (Grade 2). The Ti will be bent enough so that the Pt bullion will be placed into the hook (as it were) with the springinness of the hook acting a the clamp (it will look simply when you see a picture).

This should last a very long time as a perchlorate anode. 1 gram pieces of Pt are around 60 dollars (I think). The one gram piece should make an approx. one amp anode at about 350mA per square com. This does not sound much but one amp for a month will make quite a lot of Perchlorate.

[taiwanluthiers]

I'm tending towards platinum coated titanium anodes... the problem with bullion is that it's going to be hard to attach them and the surface area on them is going to be extremely small... Now if there were facilities to dissolve the platinum and plate them it would work better but that's a whole other set of problems. I tried to buy a one gram platinum one time from some precious metal dealer but they had a minimum order of about 5 ounces of gold (or equivalent). I don't even have enough net worth to buy that. If you could somehow physically manipulate the platinum bullion to increase its surface area, it might work...

 

I don't really know how long a 1 micron platinum coated anode is going to last but according to that oxidizing page, it should last a long time, and one day when they wear out they can be reused as cathode. I guess so long as it is used for perchlorate only and the run condition is kept at optimum level (meaning you constantly add chlorate to the tank and use a circuit breaker to cut the power when the amperage suddenly rises)

[Arthur]

Swede found a way to make a spot welder using the (rewound) transformer from a microwave oven. I guess that you could search youtube or Swede's blog. He was able to weld up anodes with Ti and DSA/MMO perfectly satisfactorily. I'm not saying that it was a replacement for a commercial unit -it wasn't. BUT for a few welds in small parts it was a good design.

 

youtube has lots try

for a starter welder. OR let's face it you need 5 spot welds on each electrode you could get a welding shop to do the welds for pence.

[WSM]

The spot welder video Arthur shared is inspiring. I'd change a few things on it though.

 

The welding tips are too small and larger diameter copper tips, turned slightly to make just the contact points smaller, would last considerably longer and make better welds (see the commercial units for a better idea of the tip configuration). Over all a great DIY presentation.

 

WSM

[WSM]

Who was it above that suggested getting a piece of one gram Pt (bullion) and clamping it between two pieces of Ti and lowering the Pt + joints into a Perc cell. It should work IMO. I am going to try this myself using a piece of 'bent around like a fish hook'

piece of flat Ti (Grade 2). The Ti will be bent enough so that the Pt bullion will be placed into the hook (as it were) with the springinness of the hook acting a the clamp (it will look simply when you see a picture).

This should last a very long time as a perchlorate anode. 1 gram pieces of Pt are around 60 dollars (I think). The one gram piece should make an approx. one amp anode at about 350mA per square com. This does not sound much but one amp for a month will make quite a lot of Perchlorate.

 

I was thinking a one or five gram bullion bar, rolled out thin to foil and carefully spot welded to a CP titanium frame would make an excellent perchlorate anode. If one were to carefully follow the best perchlorate making parameters, I think it would do an excellent job and last a long time.

 

WSM

[frank]

http://www.ebay.co.uk/itm/10-x-Hex-Socket-M6-16mm-Grade-TA2-Titanium-Screws-Bolts-/320737213674?pt=UK_BOI_Metalworking_Milling_Welding_Metalworking_Supplies_ET&hash=item4aad6d7cea

 

10 grade 2 titanium bolts for approx. 5 dollars.

 

At WSM. Will Pt weld to Ti (there's one you don't know!!!!!!!!)

I would be hoping that you don't need to weld. Just clamp and keep the whole lot under solution surface.

[WSM]

http://www.ebay.co.uk/itm/10-x-Hex-Socket-M6-16mm-Grade-TA2-Titanium-Screws-Bolts-/320737213674?pt=UK_BOI_Metalworking_Milling_Welding_Metalworking_Supplies_ET&hash=item4aad6d7cea

 

10 grade 2 titanium bolts for approx. 5 dollars.

 

At WSM. Will Pt weld to Ti (there's one you don't know!!!!!!!!)

I would be hoping that you don't need to weld. Just clamp and keep the whole lot under solution surface.

 

Actually, it should. I know that some companies have used very small (about 0.00067" diameter) platinum wire as a bridgewire in auto airbag initiators. Platinum appears to be resistive enough to spot weld easily. The problem will be getting the power setting right so the foil will be properly bonded to the titanium and not have holes blown in it.

 

The main problem is getting my hands on the tiny bullion pieces without breaking the budget.

 

WSM

[WSM]

http://www.ebay.co.uk/itm/10-x-Hex-Socket-M6-16mm-Grade-TA2-Titanium-Screws-Bolts-/320737213674?pt=UK_BOI_Metalworking_Milling_Welding_Metalworking_Supplies_ET&hash=item4aad6d7cea

 

10 grade 2 titanium bolts for approx. 5 dollars.

 

Thanks frank. Closer to $6, but that's brilliant. I think the free shipping would seal the deal. A nice find, to be sure!

 

WSM

[pex]

Can somebody help my with calculate please?

How many pottasium chloride, and disstilt water do i need to convert 1 kilo naclo4. To kclo4. And what will by my yield? Maybe there is someone with better calculation skills than me.

 

Thanks allot

[WSM]

Can somebody help my with calculate please?

How many pottasium chloride, and disstilt water do i need to convert 1 kilo naclo4. To kclo4. And what will by my yield? Maybe there is someone with better calculation skills than me.

Thanks allot

 

I just calculated the amounts based on molecular weights and solubilities. To the solution of 1 Kg NaClO₄ add 609g KCl in 2 liters H₂O. The theoretical yield of KClO₄ is 1131.5g and 477g of NaCl will be left in solution. If you vacuum filter the KClO₄, rinse it with chilled distilled H₂O and dry the resulting salt.

 

If you get a chance to study chemistry and learn to balance formulas, you can do this for yourself.

 

WSM

[WSM]

I scored an awesome piece of equipment this weekend, a small home water distiller. I'm planning to take it apart and rebuild it for producing water for electrochemical experiments !!!

 

 

WSM

Edited May 21, 2014 by WSM

[pyrojig]

http://www.ebay.co.uk/itm/10-x-Hex-Socket-M6-16mm-Grade-TA2-Titanium-Screws-Bolts-/320737213674?pt=UK_BOI_Metalworking_Milling_Welding_Metalworking_Supplies_ET&hash=item4aad6d7cea

 

10 grade 2 titanium bolts for approx. 5 dollars.

 

At WSM. Will Pt weld to Ti (there's one you don't know!!!!!!!!)

I would be hoping that you don't need to weld. Just clamp and keep the whole lot under solution surface.

LOL Frank , you are totting a very skilled fellow who has been around the block a few times ( no offense or pun intended ) . You should be careful who you assume knows or doesnt know things . He never ceases to amaze me of the wealth of knowledge he graciously shares. just watch out ,,,,,he might poke back

 

@ Wsm

Nice score .. do some runs and keep us posted if it in fact is cheaper to make your own distilled water.

Edited May 21, 2014 by pyrojig

[pex]

Hello WSM,

 

Thanks for your calculation. I am not that good in chemistry. My 9 liter cell is running no for almost a month. My lead dioxide anode was damaged at the start. But is still running. I lookt at the anode yesterday. And there is no extra damage. I waiting for a few extra days to be sure that al naclo3 is converted. In naclo4. I did a test with suger and sulphuric acid. And not tong is happening. Only a lite bit of fume is produced. The indigo test stil give traises of clorate. I waiting till everything is done. Than clean with some sodium metabisulfite.

 

 

[MrB]

@ Wsm

Nice score .. do some runs and keep us posted if it in fact is cheaper to make your own distilled water.

I'm going to jump in here. It's my experience that distilled water never is worth the effort over RO-water. Depending on your water-quality needs, a 3 step, or a 4 step system is right. (Particle, activated charcoal, and Reverse Osmosise membrane for a 3 step system, a 4'th step would be a second membrane running of the product water from the first one.)

A 3 step setup provides water thats the equivalent of your home distillery, a 4 step systems leaves nothing but homeopathic memory effects... (pretty much nothing, that is)

Even crappy RO-membranes have a 95-99.99% rejection rate. Get a good one, and rejection rate should be above 97+% across the board. Run 2 after one and other and you get a 99.91% rejection rate at worst. Since RO-systems are "dirt cheap" and cost to run them is zero, all you need to worry about is replacing the prefilters regularly, and the membranes when your TDS meter starts showing that your not getting purified product.

 

Thats if we are talking cost effective. If we are talking best possible water, buy lab grade distilled water. You cant beat that with a home distiller, or a RO-system.

B!

[WSM]

@ Wsm

Nice score .. do some runs and keep us posted if it in fact is cheaper to make your own distilled water.

Thanks pyrojig, I will post the results when I have them.

 

The efficiency will depend on how much distilled water is made and how fast. Dividing the total cost by the results (kilowatt-hours consumed) will give me a cost per gallon and I'll know whether it's a bargain or not. It might just be better to buy gallons of distilled water from Walmart than to make it at home.

 

I'll let you know...

 

WSM

Edited May 21, 2014 by WSM