making potassium (per) chlorate

[dagabu]

Kaizoku,

 

We know what magnalium is and uses. It is not particularly dangerous when handled correctly. We all know that metal fires are problematic when it comes to magnesium but aluminum is almost impossible to light in a solid non-powdered form.

 

Also, magnalium does in no way create color in fireworks, it is the metal in metallic fuels, strontium, carbonates and the like create the color, not the Mg/Al and makes the flame envelope brighter but can wash out the colors.

 

Also, we like the use of proper grammar, punctuation, capitalization and no l33t or sms lingo.

 

Lastly, I have NO patience when you say someone deserves to get burned, you have no freaking idea what you are saying.

[kaizoku]

Kaizoku,

 

We know what magnalium is and uses. It is not particularly dangerous when handled correctly. We all know that metal fires are problematic when it comes to magnesium but aluminum is almost impossible to light in a solid non-powdered form.

 

Also, magnalium does in no way create color in fireworks, it is the metal in metallic fuels, strontium, carbonates and the like create the color, not the Mg/Al and makes the flame envelope brighter but can wash out the colors.

 

Also, we like the use of proper grammar, punctuation, capitalization and no l33t or sms lingo.

 

Lastly, I have NO patience when you say someone deserves to get burned, you have no freaking idea what you are saying.

 

i do know what i mean when i watched one of those youtube movies it almost happend to me i was just lucky that i had enough time to stop the oxygen supply with as outcome: a burned cooking pan and some molten plastics that's why i wrote that because i was such an idiot to follow those video's and i actually deserved that because everyone else told me not to do so. And is helping an fellow forum member bad then?? I just said so in case that he maybe did not know so, which was the same in my case so i read an book about dangerous chemicals and other chemical compositions and what do with them in case that...

And thanks for correcting me regarding the magnalium, I really do appreciate that.

Edited November 16, 2010 by kaizoku

[dagabu]

I do know what I mean when I watched one of those youtube movies it almost happend to me. I was just lucky that I had enough time to stop the oxygen supply with as outcome: a burned cooking pan and some molten plastic. That's why I wrote that because I was such an idiot to follow those video's and I actually deserved that because everyone else told me not to do so.

 

Is helping an fellow forum member bad then??

 

I just said so in case that he maybe did not know so, which was the same in my case so I read an book about dangerous chemicals and other chemical compositions and what do with them in case that...

 

 

Translation: "I followed a you-tube video and did something stupid, I got burned but I put the fire out.

 

Shouldn't I tell you not to be stupid like me?

 

I didn't know what the hell I was doing and it sounded like this guy didn't have any idea what he was doing either so I told my story to you all. I also have been doing some reading about the dangers of chemicals and such and what to do if something goes wrong"

 

There, that's better.

Edited November 16, 2010 by dagabu

[kaizoku]

that's true expect for that burned part but i was just super lucky at that time.I have to give you that. Edited November 16, 2010 by kaizoku

[dagabu]

that's true expect for that burned part but i was just super lucky at that time.I have to give you that.

 

*Sigh* "That's true except for that burned part but I was just super lucky at that time. I have to give you that."

[kaizoku]

You are right I just have to stay silent for the while being, because I am an idiot and you are not, because you know more than i do.

[dagabu]

Kai,

 

No, I am a n00b but I make darn sure that I have the correct information before I post it. Lets take ophorite, Death-Nuke used the word ophorate, simple mistake right? Five seconds on Google and I found the correct spelling.

 

This does not mean that I am smart, nor does it mean that I know more then you do, you may have a doctorate in chemistry for all I know but when you used a run-on sentence that made no sense, claimed that Mg/Al was dangerous to handle right on the heels of Necronuke's immensely dangerous post, I kind of blew my cork!

 

Use correct grammar, stop txting us, check your facts and ask questions. We like to ask and answer but we are also careful to not lead people down the wrong path, our lives may very well depend on it.

 

I apologize for jumping on you.

Edited November 16, 2010 by dagabu

[kaizoku]

It was not sarcastic it is just true compared to you I am an idiot.

[WSM]

If you hurry there is an eBay offer closing in less than three hours for MMO/titanium mesh! See item number 260691596856. It's large enough to handle up to 260 Amps! I have bought from this person in the past and he sells decent materials and ships fast. I am not connected with this individual in any way and do not receive anything for the endorsment (I'm just a satisfied customer ).

 

WSM

[WSM]

Now that my continuous experiment (the one with the concentric electrodes) tanks are complete, I've been working on populating them with plumbing and wiring to attend to the monitoring and fluid flow control of the system. I still need to fabricate some specialized parts needed for the system; first, an accurate timer like Swede described in his blogs to control acid injection for pH control (and higher cell efficiency) and second, a special pump to send the depleated liquor back to the reaction chamber from the crystallization chamber (maintaining a constant fluid level in the RC and EC, while the CC fluid level will vary between high and low level float switches; controlling a makeup water/salt solution injection system into the RC).

 

Following the guidelines Swede showed for the timer, I plan to build a similar setup for my system. For the pump, I plan to build a compatible diaphragm pump using PVDF plate and fittings, Viton rubber sheet and PTFE bolts to hold it all together. The idea is to bury the pump under the fluid in the CC in a heated PVC chamber to prevent crystal fouling of the pump. The diaphragm pump is pneumatic and is powered by an aquarium air pump. A simple timer circuit controls the pulse width and duration and outputs control of an air diverter solenoid through a relay mounted on the timer circuit board. In essence, the diaphragm pump "breathes" fluid in and out with each cycle and moves the liquor from the CC and to the RC in pulses. The beauty of the pump is it runs on about three watts of energy! At twelve cents per KW/h, it'll cost me about a quarter dollar per month to run it!!!

 

I'm monitoring the power used by the whole system so I can know the real cost of the oxidizer salts I produce.

 

More later...

 

 

WSM

[WSM]

I've attached an early prototype of the diaphragm pump.

 

This design used PVC and silicone rubber and is bolted together with stainless steel hardware. It works fine outside the cell but the pump I described in the last post is made to be compatible with the nasty environment inside the chlorate cells. The old design utilized home made check valves made from PVC unions with silicone internals. Silicone is not the ideal material to use with hypochlorite and hydrochloric acid but it holds up for a while. The design allows for easy replacement of those parts prone to wear out.

 

I'll show a photo of the improved version when I get it built. I have components ordered and on the way.

 

More later...

 

 

WSM

[WSM]

The last time I wrote I mentioned working on a design for a submersible diaphragm pump, I've attached two files that show the basic design and a working prototype. The design drawing shows a pump made by milling out solid Kynar (PVDF) blocks.

 

 

I wanted to place the pump on the bottom of the CC so the diaphragm port is plumbed in from the side rather than the bottom as in older designs. The design utilizes a pair of commercial check valves and compression fittings, also of PVDF and Viton.

 

The prototype is bolted together from two plates and a short section of pipe (all PVDF). To put them together I turned the check valve in a lathe to remove the hose barb from one side of each one. I used Teflon tape on the threads of the fittings and cut the thin Viton rubber to create the diaphragm and seal.

 

 

The Kynar, or PVDF (polyvinylidine difluoride) is an excellent material to use in cells ("poor man's Teflon" I call it ) and Viton B is a synthetic rubber material that can withstand a lot of abuse also. I think these materials will hold up to whatever the cells or acid tanks can throw at them. I'm on the lookout for an affordable source of 1/8" ID Viton B tubing also. Till then I'm using Norprene tubing from Saint-Gobain, which should hold up for a while.

 

To supply power to the pump I'm planning to use an aquarium pump with the air supply controlled by a valve and timer that adjusts the pulse width and duration of the air in to push the diaphragm (similar to how we breathe air), making the pump move fluid in pulses and all at very low power consumption .

 

With the experimental system, I've plumbed the RC and EC and now have to plumb the CC with float switches and a return pump/heat well area so I can put the whole continuous experiment together and get it running. I designed a simple control circuit which will maintain the fluid levels in the system without overflowing the crystallizer. It involves float switches and relays so when the low level switch is activated the input water flows into the RC till the high level switch activates and deenergizes the water pump. For safety, I'm adding a third float switch as a failsafe to the high level switch (can't be too careful here!). Another float switch for an interlock will be added to the RC lid to cut off acid injection when the lid is open (I don't want acid pumping in when I've got the thing open !!!).

 

That's it so far but I'll add more later...

 

WSM

[WSM]

Between poor weather conditions and being extremely busy this past month, I haven't been able to do anything but think about my experimental continuous system. I also misplaced one of the two digital aquarium thermometers I'm using to meter the temperatures of the CC and RC, until last week when I found it. The thermometer has held up the populating of the CC with metering and sensing equipment so it would be finished and allow me to fill the whole system with salt solution and apply DC power so I can determine how much acid will be required to increase the cell efficiency to over 90% (based on the current [amperage] demand of the system).

 

I need to build a protective shelter for the system since I do all my electrochemical experiments outdoors to avoid any fumes turning my expensive tools brown or creating any kind of health hazard .

 

I did acquire two of the LD anodes that Patsroom is offering, and hope to try them out as soon as I can seal a little damage that occured to them during shipping. The second anode has an improved power lead which is wider, thicker and has a 1/4" hole in it for connecting power to the electrode with a stainless steel bolt. If Pat can solve the shipping problems, these anodes will be a real boon to those wishing to convert their chlorate to perchlorate, without resorting to making their own electrodes . I hope he'll keep supplying them and not just be a temporary source. I'll report back when I set up an experimental chlorate to perchlorate cell. I have a Pyrex battery jar which is 6" in diameter and about 12" tall which I may use to try the electrodes out. A permanent batch cell may be in the future if I can obtain some 6"-10" diameter CPVC pipe to make a cell using the CPVC flat sheet I got off eBay and some industrial CPVC cement I have. I plan on using CPVC unless I can run the cell at lower temperatures than the highest upper limit suggested for PVC (140^oF or 60^oC).

 

I'll write more when I have more to tell or show ...

 

 

WSM

Edited January 2, 2011 by WSM

[Suseer]

thanks for the information, this forums great!

[WSM]

thanks for the information, this forums great!

 

You're welcome, and yes it is!

 

WSM

[Crushedknee]

Has anyone tried a Diamond-Like carbon coated material as an Anode..Hard Dist Patters are coated with it Might Make an interesting Experiment specially if you can get the Electrons Quantum tunneling from the Substrate to the solution..

[Mumbles]

You may want to give your posts a once over to ensure they make sense.

 

The item he was trying to talk about are hard disk platters, as in the individual disks that make up a computer hard drive.

 

Is this suggestion based on any sort of theory or evidence or actual usage, or it just a random suggestion out of left field?

[Crushedknee]

I guess it is somewhat out of left field..I was checking out Boron doped diamond electrodes to produce sodium and or Potassium perchlorate..Stumbled onto diamond like carbon coatings And Hopping conductivity. With a conductive aluminum Core "unless its Ceramic Composite" and a thin Insulating Diamond like carbon coating it would seem likely to have Electron Hopping occurring. Bypassing the Inert coating thus reducing Oxidation and erosion. But I have know Idea what part the Cobalt platinum and whatever alloy that makes up the Magnetic layer would do. Here is some work on the Coulomb blockade at room temperature and low voltage http://arxiv.org/ftp/arxiv/papers/0804/0804.2164.pdf..I love Home tinkers doing High Science..What do you guys think ?

Edited January 5, 2011 by Crushedknee

[WSM]

I have to apologize for the slow posts. I've been inundated with other tasks and haven't been able to work on my electrochemical experiments for many weeks. I'm not sure when I'll be able to resume; but rest assured, I will get back to them.

 

When I get a chance to test the experimental continuous system and sort out the various details I need to have figured out, I plan on going "full steam ahead" with "The Monster", and crank out a stock of chlorate to feed the perchlorate cell(s) that will follow. My goals aren't to produce salts for commerce (others can do that), but to learn how it can be done on a hobbyist scale.

 

I've always liked the notion of being self sufficient and any progress toward that goal is very satisfying to me. I'm sharing the lessons learned here so others can benefit from them, and if any want to produce oxidizer salts for themselves, I welcome them and will share whatever wisdom I can (as long as their goals are honorable, ie; pyrotechnics for entertainment, education, et cetera).

 

WSM

[athlon]

My my, this is one monster of a post with so much information to digest that I have to split it into several days! Got through half of it yet, probably missed something so that I have to reread it.

 

Unfortunately though I'm not able to see any attachments that are hosted on APC, outside links works fine though.

 

Thank you all for a very informative read

 

ETA: attachments seems to work now, just had to make a post. Now back to see all the photos!

 

regards,

Newbie in the chlorate world.

Edited January 23, 2011 by athlon

[WSM]

My my, this is one monster of a post with so much information to digest that I have to split it into several days! Got through half of it yet, probably missed something so that I have to reread it.

 

Unfortunately though I'm not able to see any attachments that are hosted on APC, outside links works fine though.

 

Thank you all for a very informative read

 

ETA: attachments seems to work now, just had to make a post. Now back to see all the photos!

 

regards,

Newbie in the chlorate world.

 

Hi Athlon,

 

Welcome. Yes, you are right about there being a lot to read (but DO read and reread it; there's too much to take in all at once).

 

I remember the minor difficulties I had when I first found this newsgroup; but what a wonderful find it is. Have a good time pouring through the earlier posts and learn as much as you can. There are several reference volumes available also on industrial electrochemistry that will help establish a foundation of knowledge to build upon. Don't be afraid to ask honest questions about what you find there and here. Usually someone here will try to answer and then others will add in more till either the topic is covered or the discussion dies.

 

As for building a cell: I take a casual approach. I studied for literally years before I ventured to build my first functional cell. You don't have to wait that long but also don't be in too big a hurry or you may waste a lot of time and money while creating a hazard for yourself and others if you are impatient. My first functional cell, by the way, was a glass one gallon pickle jar with a PVC end cap for a lid and holes drilled in for the electrodes and a gas vent. No scientific measuring or metering, no pH control or other fancy gear and no great efficiency (it was roughly 50% efficient), BUT it did produce chlorate; several kilos over the time it ran. It sits idle now as I pursue other challenges.

 

I didn't need the oxidizer, but I learned a lot! As you read through the posts here you will see more advanced work and highly complex as well. Just take it in. Above all, just ask questions and learn all you can. It's fun and challenging, but ultimately, satisfying to make stuff yourself. I suppose most amateur pyrotechnists who build their own fireworks feel exactly the same. Again, Welcome.

 

WSM

[athlon]

Thanks for the welcome and yes, safety always comes first! I just love the idea of being able to make what I need, back to basics so to speak, whether it be a lovely home made bearnaise sauce or forge a knife from raw steel.

 

I have just ordered a mesh with MMO coating and am for the lookout for a suitable canister to use it in. Meanwhile I'll be reading this thread and see if I can source some nice books on the subject. Unfortunately I'm having a hard time finding any pure KCl to use in my cell, the only thing I've found around here is is a table salt consisting of 69% KCl and 29% NaCl.

 

Well, I'm of to go study now.

 

regards,

Athlon

[ausgoty]

What do you use as a chlorate test when preparing perchlorate?

 

I have heard calomel? is the easiest to get hold of, is that what you use?

Edited January 23, 2011 by ausgoty

[WSM]

Thanks for the welcome and yes, safety always comes first! I just love the idea of being able to make what I need, back to basics so to speak, whether it be a lovely home made bearnaise sauce or forge a knife from raw steel.

 

I have just ordered a mesh with MMO coating and am for the lookout for a suitable canister to use it in. Meanwhile I'll be reading this thread and see if I can source some nice books on the subject. Unfortunately I'm having a hard time finding any pure KCl to use in my cell, the only thing I've found around here is is a table salt consisting of 69% KCl and 29% NaCl.

 

Well, I'm of to go study now.

 

regards,

Athlon

 

Hi Athlon,

 

For KCl try Home Depot or grocery stores for the sodium-free water softener salt (40 lbs for about $20). The MMO on CP titanium mesh makes an excellent anode (positive connection) for the cell. A compatible and excellent cathode (negative connection) is commercially pure titanium (CP titanium). The nice thing is that the product comes out very clean (no graphite sludge to filter out). It's best to have a very solid electrical connection to the electrodes like stainless steel nuts and bolts, well tightened, so the maximum current is transferred to the electrodes and not wasted as heat.

 

Of the available materials to use for cell bodies, the least expensive compatible material is PVC. The main limitation of PVC is that the highest recommended temperature is 140^oF (60^oC).

 

Ask questions if you need more information.

 

WSM

[WSM]

What do you use as a chlorate test when preparing perchlorate?

I have heard calomel? is the easiest to get hold of, is that what you use?

 

Well, no, not calomel (calomel is mercurous chloride, used in fireworks in the old days as a chlorine donor). The easiest to get reagent to test for chlorate is indigo carmine, a biological stain.

 

WSM