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gregkdc
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Hello everybody I am a complete noob to making chlorates/perchlorates and I have been studying it for a few weeks now. I am very active in armature
rocketry so obviously the end product that I would like to make it AP. I have been reading about the lead dioxide anodes as well as platinum for
perchlorate production, and I would really like to avoid using lead all together and we know the price of platinum is a problem. So that leaves me
with very few options, one is thermal decomp of chlorate to perchlorate or to try to use graphite in a diaphragm type cell. I was wondering if
anybody has ever tried using silicon for an anode? For chlorate production I am going to try making a magnetite anode in a microwave. I found an
interesting webpage for melting metals in the micro wave and the material that is used to heat the kiln is magnetite. The author states that he has
gotten it hot enough to melt the ceramic refractory he was using so it should be able to melt the magnetite. I also have some powdered silicon that I
bought for pyro purposes and was thinking of making a silicon/magnetite alloy for the anode if I can get it to melt in the microwave. Any thoughts
would be appreciated.
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gregkdc
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In my previous post disregard my idea of mixing silicon with magnetite (sounds like a potential thermite reaction) and if it is not that violent of a
reaction I am sure they would react at hi temps. Maybe another metal oxide would work with magnetite for perchlorate production. Anyways I will
attempt to move forward with a microwave magnetite anode for chlorate production and try converting this to perchlorate via thermal decomposition.
On a side note I read somewhere that magnetite can be used with lead dioxide for a perchlorate anode. I am not planning on electroplating an anode,
but was wondering if you could simply place a magnetite anode in the bottom of the cell so it is lying horizontally on its side, and add a thick layer
of free lead dioxide powder on top of the magnetite anode. The lead dioxide is conductive (more than the magnetite) so it should allow some of the
current to pass through it and make perchlorate with some obvious loss in efficiency. Has anybody tried something like this?
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Xenoid
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Quote: Originally posted by gregkdc  | | Hello everybody I am a complete noob to making chlorates/perchlorates and I have been studying it for a few weeks now. I am very active in armature
rocketry .... |
Yeah, yeah we've heard it all before!
"armature" rocketry, eh..! Is that some sort of new electromagnetic propulsion system 
I suggest you have a look at this video;
http://www.youtube.com/watch?v=HJVOUgCm5Jk
and read this item;
http://en.wikipedia.org/wiki/PEPCON_disaster
You want to make ammonium perchlorate and you're worried about a little lead 
I've been making chlorates and perchlorates for several years and I'm still reluctant to make ammonium perchlorate. You'll need good chemical skills
and more than "a few weeks study" before embarking on this task. I suggest you stick to nitrate based propellents, they're a little more forgiving!
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gregkdc
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Thanks for the welcome, but I fear you are already too late for me not getting involved with AP (at least purchased AP). The irony is that in some
ways I would rather stay with nitrates but nitrate based propellants, even though they are less energetic and reactive, are considered explosive while
APCP is not. That means I would have to get a LEUP and all of the federal intrusion to move into larger nitrate motors or make AP motors. Also it is
not that I really fear lead I could make a go of it, but from what I have been reading the reward is fleeting and as a whole it does not seem to be
worth the potential risks. Just my opinion from a guy that has zero experience that is why I am here to get some advice from the experts.
PS the pepcon disaster is quite an impressive blast!
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Xenoid
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| Quote: Originally posted by gregkdc | | ... but I fear you are already too late for me not getting involved with AP (at least purchased AP). ... |
Oh well, I tried.
Stick to buying professionally manufactured ammonium perchlorate, it will be safer, probably cheaper and a whole lot less of a hassle in the long run!
It's the possibility of ammonium chlorate (highly unstable) contamination in the home made product that worries me, not the AP per se.
There are lots of anode threads in Sciencemadness, and many ideas have been tried, you'll need to do a lot of searching and reading. Unless you are
specifically interested in investigating the chemistry involved in the various electrolytic and coating processes, it would be best to stick with
purchased MMO anodes for chlorates and platinum/Ti for perchlorates.
A cheap thermal coating of beta-MnO2 on an MMO anode will also allow you to make perchlorate, albeit with a little permanganate contamination to clean
up.
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hissingnoise
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| Quote: Originally posted by Xenoid | | I've been making chlorates and perchlorates for several years and I'm still reluctant to make ammonium perchlorate. |
The easy way to AP is metathesis with NaClO4 and a NH4 salt . . .
AP immediately precipitates when the solutions are mixed!
I used NH4NO3 as NaNO3 is useful.
For high purity AP, NaClO4 can be reacted with HCl, filtered and heated to drive off HCl . . .
The HCLO4 produced this way can be practically free of Na!
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gregkdc
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OK Xenoid I will take your advice and buy AP for now, this was pretty much what my plan was anyways, but you know this type of thing will drive me
crazy until someone makes a good anode.
I have been reading through most of the anode threads and I can see that the majority of the topics relate to electroplating various oxides, and then
such anodes fail due to the oxide layer breaking off or being eroded down to the substrate.
Has anybody tried making massive anodes that would be chemically solid? In particular making a magnetite type anode by melting the material instead
of thermal decomposition or electro-plating. From what I have read the magnetite anode seems to have remarkable corrosion resistance and I can't help
but wonder if it is from the way it is manufactured. Sure, electro-plating may be the way to go for industry because it is cost effective for
materials but maybe it is not the way to go for the armature. I am particularly interested in seeing what would happen if you melted cobalt II,III
oxide into an anode. It decomposes when it melts but from web sources the reaction appears to be in equilibrium with ambient oxygen so the end
product can be either cobalt II or III depending on if the environment is oxygen rich or starved. So the questions is would you be able to create an
atmosphere that would have the proper amount of oxygen that would keep the original II,III oxide in equilibrium? Also if this doesn't work I wonder
if a eutectic mixture of something like bismuth oxide could be used to get it to melt at a temperature lower than the decomposition temp of cobalt
II,III?
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Xenoid
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| Quote: Originally posted by gregkdc | OK Xenoid I will take your advice and buy AP for now.....
Has anybody tried making massive anodes that would be chemically solid? In particular making a magnetite type anode by melting the material .....
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Good! I believe the professionally made AP has a specific grain size distribution that is required for rocketry. This is also hard to achieve by
amateur producers.
Yes! Yes! It's all been tried, but we would welcome any input you care to make.
There is a section at dann2's web site pertaining to his efforts at making massive magnetite anodes;
http://www.oxidizing.110mb.com/chlorate/anodes.html
Go to the magnetite anode section, and near the bottom are two links.
If you haven't checked out his site previously, it might be worthwhile you doing so!
I don't believe anyone has tried a massive Co3O4 anode, I don't think it's readily available (Co3O4, that is). I think it is even worse at making
perchlorate than magnetite 
If you do experiment with making anodes and chlorates and perchlorates, whatever you do, don't try electrolysing ammonium chloride, it will produce
extremely sensitive and highly explosive nitrogen trichloride. Skilled chemists have lost fingers and hands with that
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tnphysics
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What about using electrolysing lead chlorate (to make perc)? This should form a PbO2 layer at the anode and a Pb layer at the cathode, protecting the
substrate. Keeping lead in the solution should maintain this layer. The solution will drift acid, and will eventually cease making PbO2. The cathode
will need to be replaced at this point-Pb is terrible at making hydrogen, which is what we want in this case.
Also, what about Ti in a ph-controlled cell?
Au is probably great for perc, if Cl- is absent.
I LOVE science!
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dann2
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Hello,
Been running some Mn Dioxide Anodes in various cells to see how they performed. The star performer seems to be a
MnO2 Anode in a non pH controlled Potassium Chlorate cell. The Sodium cells give disappointing results for some
reason or other. The SS Cathodes seem to corrode more in Na cells too.
All the Anodes has 5 coats of Mn Nitrate solution except the Anode that had two coats of Co Oxide first + five coats of Mn Nitrate on top.
This is a light coating of Mn Oxide IMO. I don't know if having 10 coats is twice as good as having five (etc) but five certainly give a good working
Anode.
Forget the Mono metal spinel (Cobalt Oxide) IMO as it's a waste of time.
I regret not running the pH controlled K cell at an Anode CD of 50mA per square cm (like all the rest). I ran it at 80 to hurry things along but if
failed much sooner than expected. One liter cells are a bit too small for pH controlled cells as you have to change the liquor too often and the cell
spends a lot of time in 'start up' mode (adding lots of extra acid to get pH to go where you want it).
How would one identify the brown gunk that is suspended in the cells. I suspect it is coming from the Cathodes.
I hope to run another pH controlled K cell (50mA/cm^2 Anode CD) with Ti Cathodes to see if they run any clearer.
I weighed the brown gunk (dried) from a cell run and it was 2.33 grams. A small amount of material that is able to turn the solution completely
opaque brown.
I attach all and every gruesome detail. What do you's think of the colour scheme?
Dann2
Attachment: mno2.zip (95kB)
This file has been downloaded 657 times
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dann2
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Hello,
The Manganese Dioxide Anode finally give up the ghost after 97 days! @ 50mA per square cm. It was working in a non pH controlled Potassium
Chlorate cell. There was a total of five liquor changes, the fifth change was on day 98. The cell Voltage on day 97 was around 7 Volts. It fell just
below 7 Volts after liquor change but then started to rise. A few days later the Voltage was 10 Volts. The CE was good during the last run (day 77 to
day 97) at 47%. Average for the 97 days was about 47%. The liquor was clear for most of the last run with some brown stuff appearing towards the end.
The Anode was run at 2.52 Amps which gives a total of 2100g of K Chlorate formed. It's a fairly small Anode.
Perchlorate was inclined to appear in the cells as detected my Methylene Blue.
Dann2
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12AX7
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Found something quite interesting today,
http://www.dextermag.com/upload/TDK_Dexter_Ferrites_Electrol...
Perhaps some samples can be tested. And what do you know, spec'd for corrosion resistance in NaCl solution, albeit dilute.
Tim
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hissingnoise
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Right, now where are those old radios?
Magnetic anode-sludge is a cut above fine graphite for starters . . .
Long time no, er, read, 12AX7!
Welcome home!
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hissingnoise
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Ahem! Post Harlot crown slipping somewhat . . . ?
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tnphysics
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Why does ClO- + 4OH- -> ClO3- + 2H2O + 4e- not occur in a non pH controlled cell?
I LOVE science!
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symboom
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tungsten anode
tungsten from an TIG electrode
coatings are
mine i have is orange thorium oxide up to 4%
tungsten alloys
Green None
Gray ~2% CeO2
Black ~1% La2O3
Gold ~1.5% La2O3
Sky-blue ~2% La2O3
Yellow ~1% ThO2
Red ~2% ThO2
Violet ~3% ThO2
Orange ~4% ThO2
Blue ~2% Y2O3
Brown ~0.3% ZrO2
White ~0.8% ZrO2
which one would be best at handling as an anode
tungsten is resistant to oxidation, acids and bases at normal temperature Ive read somewhere an experiment making chlorate replacement for platinum
but it does not say much just that it was abandoned when they heard of lead dioxide anodes
http://en.wikipedia.org/wiki/Gas_tungsten_arc_welding
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dann2
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Paper attached on Diamond Anodes.
Attachment: diamind.pdf (804kB)
This file has been downloaded 827 times
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dann2
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Hello,
Slightly off topic but since this thread is mostly about making Anodes for Chlorate and Perchlorate........
The Chlorates and Perclorates.
Naval report. Size is 20Mb
Lots of data about Chlorate and Perchlorates
http://www.dtic.mil/cgi-bin/GetTRDoc?AD=AD242192&Locatio...
Thanks to the Wizard.
Dann2
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dann2
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Another one for the Sodium Chlorate making guru's.
Thanks to Potassium Mn04 for that one.
Dann2
Attachment: TES000093.pdf (429kB)
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White Yeti
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You mentioned palladium, but palladium, from what I understand, is even more expensive than platinum.
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the mentalist
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Hello,
Alright, that was a long thread to read. So on my long quest of making APCP I have successfully made only the aluminum so my question, request for help/advice has to do with the synthesis of ammonium
perchlorate, More so about chlorate and perchlorate cells, considering that every route leading to ammonium perchlorate uses sodium chlorate and some
type of (per)chlorate cell. So I'm more than prepared to start at the bottom and do my research before I get any final product. With that said, my
first cell I want to construct will be making sodium chlorate from sodium chloride. So i guess I'm just looking for advice on the steps I should take
to construct a cell. Like what I should use for the cathode and anode, what concentration of salt should be in the water, does it have to be air
tight? Any advice it awesome!
And please don't try to scare me off, I'm in this for the long haul, thus I'm willing to do my research and am not afraid to work with lead.
[Edited on 3-8-2011 by the mentalist]
Also what are your thoughts if I was to buy a mmo anode, rod sheet or mesh?
[Edited on 3-8-2011 by the mentalist]
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Xenoid
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Hah! Clearly you are NOT! Otherwise you would not have made this post!
There are literally dozens and dozens of threads on chlorate and perchlorate making on this forum alone. As well as several books and manuscripts
available to download!.
Also, check out dann2's site, if you haven't seen it before you have clearly done no research at all!
http://www.oxidizing.110mb.com/
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jpsmith123
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Bismuth Metal Oxide Pyrochlores As Electrode Materials For Electrolytic Ozone And Perchlorate Generation
Here's an interesting patent.
Attachment: WO2010148107A2.pdf (418kB)
This file has been downloaded 713 times
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dann2
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Thats in interesting one. If Sn could be got to work instead of Ru it would be very cheap.
1200 degreese C is needed though. You would have to make a rod of the stuff and hope the salts being conducted up the sintered rod would not be too
much of a problem messing up the connection at the top.
Dann2
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jpsmith123
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I wonder if you would really need a stoichiometric Bi2Sn2O7 pyrochlore?
Or if just a solid solution of Bi2O3 with SnO2 (or with TiO2 for that matter) would work?
Maybe the take home message is that Bi2O3 is the critical oxide for perchlorate? And if you have Bi2O3 + SnO2 you have the De Nora patent, and if you
have Bi2O3 + TiO2 you have one combination that seems like it's missing from Beer's patents?
BTW here's a paper that goes into detail on making Bi2Ru2O7. What's interesting is the sol-gel method they use where they dissolve Bi2O3 in a citric
acid + ethylene glycol solution then they add RuCl3 and fire it. That method might work with SnCl2 and/or SnCl4. Who knows, maybe it wouldn't
passivate your Ti substrate.
Attachment: Bismuth Ruthenate Pyrochlore.pdf (621kB)
This file has been downloaded 849 times
[Edited on 6-8-2011 by jpsmith123]
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