Tweetybird88 Posted September 23, 2007 Posted September 23, 2007 OK in that case, I will start with just potassium chlorate. What is the best anode to use for making chlorates? I heard that titanium will corode pretty good when making chlorates and is not worth the expense. Should I use lead oxide? The cathode is best as titanium in both cases if I am not mistaken. And to make chlorate it is just potassium chloride---->pot. chlorate.
WarezWally Posted September 23, 2007 Posted September 23, 2007 Yes. Titanium is cheap, I picked up a large sheet for $10. Lead dioxide will make the best anode.
frogy Posted September 23, 2007 Posted September 23, 2007 Potassium Chloride + Electrolysis -> Potassium Chlorate w\ Potassium Chloride I believe you dry the KClO3\KCL crystals and then add that to water and boil off the KCL... I've always wanted to make a cell for this (I have some other cells from hydrogen, Iron oxide,... some other noob things)... But I never really understood what to do... Alan Yates likes to confuse the hell out of people by calling water an electrolyte (even though it is, but cmon it 's just water) and using weird chemicals
Tweetybird88 Posted September 23, 2007 Posted September 23, 2007 Yes. Titanium is cheap, I picked up a large sheet for $10. Lead dioxide will make the best anode. Best anode for chlorate or best anode for perchlorate and chlorate. I hear platinum is better for perchlorate since it doesn't corrode hardl and it is a tad more efficient.
frogy Posted September 23, 2007 Posted September 23, 2007 Platinum\Iridium is good for perchlorate.. I'm now sure how good it is for chlorate though... Graphite\Titanium supposably work for chlorate, but I believe both corrode\erode (graphite definitely does)... I can get titanium sheet\rod stock very cheap at some local hardware stores... but I don't really know where to get platinum wire... I have saw some platinum\Ir anodes on ebay though they're not there at the moment...
hashashan Posted September 23, 2007 Posted September 23, 2007 Titanium is crap. It will passivate within minutes and become useless as anode, however it will make a great cathode. Platinum is good if you keep the chloride levels high when making chlorate and chlorate levels high for perchlorate. If you'll try to go straight Cl->ClO4 you will kill your anode eventually. Lead dioxide is perfect for direct Cl->ClO4 YOU CANT MAKE PERCHLORATE FROM K-CHLORATE. It is just not soluble enough for any normal yield. You have to use a soluble chlorate like Lithium, Barium, Strontium, Sodium but never Potassium. 1
Mumbles Posted September 23, 2007 Posted September 23, 2007 It's almost painful reading this thread. Unless you're in france, I believe you will have trouble finding sodium chlorate as a herbicide. KCl is not water softener salt. It is available as a water softening salt, but is much rarer than the sodium variety. I believe it is in a purple or green bag, and runs about $7-8 a 55lb bag. It is also available as Muriate of Potash in garden centers. "Lo-salt" and other low sodium salts are often a mix of NaCl and KCl. Graphite is the standard electrode material for chloride to chlorate. It is cheap and readily available. It will start to corrode at low chloride concentrations however. I believe it is standard practice to run to 10-15% chloride, and remove the chlorate. Lead Dioxide and platinum are the standard materials for chlorate to perchlorate. Platinum will corrode very fast if you try to go direct from chloride to perchlorate. The Lead Dioxide might be able to handle it. For purity and longevity of the anode purposes, it is often advisable to purify the chlorate from chloride before attempting to convert it to perchlorate. To prepare potassium chlorate from the mother liquor of NaClO3 and NaCl you boil it, filter any insolubles, like graphite, and add a saturated soln of KCl. You then cool it to near freezing. The KClO3 will precipitate out. One to two more recrystalizations is advisable to get a pure product. That method given by Hashashan for conversion of K Chlorate to Na Chlorate is rediculous. There is no reason for a reconversion to sodium. Secondly, adding the ethanol will just precipitate a variety, and leave you with a cocktail of various compounds. To get pure enough chlorate for perchlorate, filter any insolubles, boil the mother liquor until crystals just start to appear, and cool to near freezing again. NaCl solubility changes very little over the temperature range, so very little will precipitate. A second recrystalization will yield a product pure enough for perchlorate conversion. You can make Potassium Perchlorate from Potassium Chlorate, just not by way of electrolysis very well. 2
WarezWally Posted September 23, 2007 Posted September 23, 2007 Best of luck to those trying to find suitable anodes for perchlorate production. If you have 70%+ nitric acid you can try making your own GSLD or TSLD anode which if well made should last quite a while.
hashashan Posted September 23, 2007 Posted September 23, 2007 Mumbles you are entering my specialty here However if you do insist to go into a debate I'll translate a part of the book where i read it and DID IT. here we go : Dissolve 100 grams of KClO3 and 60 grams of Na2SO4 in 600 ml of water. While hot add 375ml of EtOH(K-sulfate will immediately precipitate), leave the vessel to stand for 2 days. decant the fluid and save it. Wash the K-sulfate with 30% EtOH and save the liquid. Pour the two liquids in one vessel and distill off the EtOH(if you need it). Boil the liquid until crystals start to form, cool and filter. For a more pure product recrystallize from water. Sorry for my bad translation I really don't have the nerves to rephrase it \ And about making KClO4 from KClO3 being impossible i meant electrolysis. Of course there are other working method.
invisibleworld Posted October 7, 2007 Posted October 7, 2007 has anyone ever bought guide from ebay ? i want to know if its reliable enough or is it just a ripoff heirs a link to it: http://search.ebay.com/search/search.dll?f...rate&category0= Ya, I read the adds on E-bay and purchased the plans. Went out and got a good power supply, you need to set amps at between 3 to 4.5 and voltage at 3 to 5 volts and run for a day or two and cool and strain and add to the rest to the next batch because it becomes more efficient and concentrated the more you add etc. The problem was, that the anodes would desintegrate and contaminate the batch using carbon anodes with stainless steel for the cathode. I never got to the point of using platinum anodes (way to expensive) for the small batches I would need. all and all I gave up the Idea. The amount of potassium chlorate and perchlorate I use never justified the hassle, the mess and the expense of making my own. The stuff is easy to obtain and not that expensive. Now if someone was using the stuff on a large scale, then I suggest spending a lot of money on a large scale cell and power supply or using the nitric acid way to make it. Basicly it wasn't worth the hassle for small scale production. That's my opinion anyway, for what it's worth.
LGM Posted October 28, 2007 Posted October 28, 2007 Hate to kick this up again, but earlier in the thread there was a method mentioned that involved the use of straight lead as an anode. This would be much easier for me to manage and if anyone has had experience with it it would be great if you could give me some info on it.
invisibleworld Posted October 30, 2007 Posted October 30, 2007 straight lead will not work. Lead Dioxide is the only lead anode that will, as in car batterys. That is according to the guide that I have read. Many tried, but with no success.
tentacles Posted October 31, 2007 Posted October 31, 2007 There have been successes with lead dioxide anodes, but so far there is no step by step guide to making a good, long lasting one. It's not cheap to make lead nitrate, for one - nitric acid is usually expensive, or it's a considerable effort if you make you own. I've been working on making lead nitrate as a precursor step to making LD anodes. Mumbles has a method of making the lead nitrate without using nitric acid, but I haven't been able to get it to work yet. Making it with nitric is a bit dangerous and messy - I've found it necessary to heat the solution and stir for 3-4 hours per batch. Anyways, I will write up what I learn once it's less sloppy.
hashashan Posted October 31, 2007 Posted October 31, 2007 Damn people .. why would you say anything like that without checking? There has been success with LD. I have made the anode and the perchlorate. here is a step by step guide : Lead dioxide anodes and you dont have to heat up anyhting. Itll take about a week for the lead to dissolve(and you have to uise diluted acid about 20%-30% for it to be fast enough)
tentacles Posted November 1, 2007 Posted November 1, 2007 hashashan: my lead has 3% tin in it, it seems to inhibit the dissolution quite a lot, giving me a lot of metastannic acid precipitate which further interferes. Plus, I'm impatient. I'm curious, what method did you use for your anodes? did you do a LDSLDA type, or is it GSLDA? Or something exotic?
hashashan Posted November 4, 2007 Posted November 4, 2007 I tried various methods. The one that worked for me is the cloth reinforced substrateless anode. It is described in the geocities site. Now I am making an anode that is grown on Ti substrate(temprary) through some thick(about 4mm) plastic fiber. Tried exotics..... didnt work the GSLD is crap ... you will never make it good(It is just to hard)The LDSLD is good but somewhat not economic. And my lead also contains a lot of impurities (maybe up to 20%) It still takes several days to dissolve in 30% Nitric acid. Of course after the process is finished you should clean up your lead nitrate. 1
rev.redneck Posted November 4, 2007 Posted November 4, 2007 I noticed some dont seem to have access to platinum, some vehicals use PT in the Catalytic converter. http://en.wikipedia.org/wiki/Catalytic_converter maybe do some research and visit a junk yard.could it be possible to use that?
hashashan Posted November 4, 2007 Posted November 4, 2007 good luck with that. ebay is full of that .. you dont really think that there is just a chunk of Pt lying around there. Some process is required to take it out. and you are not the only one who knows that ... the converters that do contain Pt will be sold adequately. Once again .. Pt is not a must in Perchlorate synthesis ...
Mumbles Posted November 6, 2007 Posted November 6, 2007 Don't be an asshole. That price is outrageous, and the shipping method you're using is illegal. 1
WarezWally Posted November 7, 2007 Posted November 7, 2007 Don't be an asshole. That price is outrageous, and the shipping method you're using is illegal. ???????????
invisibleworld Posted November 7, 2007 Posted November 7, 2007 Don't be an asshole. That price is outrageous, and the shipping method you're using is illegal.??????????? I think he was referring to a post that was removed. Post was advertizing potassium perchlorate
Mumbles Posted November 7, 2007 Posted November 7, 2007 Yes, said person was offering it for $14 a pound and using a flat rate shipping box. If you want to see it, there is another one I locked in the pyrotechnics section.
tentacles Posted November 10, 2007 Posted November 10, 2007 Been fucking around, made a test anode with my Pb(NO3)2 and a dash of Cu(NO3)2 with copper cathodes and a cloth type substrate anode - with some twistings. I used some (presumably alpha) PbO2 that FrankRizzo gave me, two small vials about 9g each of powdered PbO2. I used only one vial for this anode. The way I made the original substrate was to take a 6" piece of my .030" pure Ti wire (CP2 grade I think) and stitch it through a piece of furnace filter - the pleated kind, a cheap walmart brand one. It's much like scotch brite without abrasive, and thinner. I then sprayed the filter with NC+acetone (ping pong balls actually, that burn very fast). I sprinkled the PbO2 powder on and gently rubbed it in, sprayed more NC on it until it was slightly pasty, and basically saturated a portion of the filter material with the PbO2 paste. I let it dry 24 hours (with some heat to accelerate). I attached my little leader of the Ti wire to one of my meter probes (to measure current) and began plating on my hotplate/stirrer. Plating solution was 326g of Pb(NO3)2 dissolved in 900ml of water, with about 3ml of 98% nitric added (not really necessary, my water's PH is like 7.2) and 2g of Cu(NO3)2. The copper nitrate is probably not necessary if you use copper cathodes, since all you accomplish is to plate copper... onto copper. I plated at about 5ma/cm^2 (it drew 380ma) for about 18 hours, and got a nice hard plating that was somewhat smooth with some rough edges that probably don't matter much. (see pic 1) When I put it back in, I cranked the power up to 680ma (it was either this or 2.5A which made the connection hot) Pic 1 - first pull out, weight was about 45g (not sure what the original weight was; probably about 15g) http://www.apcforum.net/files/DCP_2492.JPG Pic 2 - 75g, I broke off the loose crumbly stuff that was forming at the edges. Before that it was 95g. What's left is pretty solid. This was about 24hrs after the first pull. http://www.apcforum.net/files/DCP_2496.JPG I got quite good conductivity from the pasted PbO2 where it was thoroughly wetted and mashed down a bit. I think this method would work very well if one was to press it into a rod or a bar shape and slowly dry it. The ping pong ball lacquer is probably a better choice than pure NC as it should be more elastic and stay together better as it dries. Some of the areas had resistance as high as 15k ohms (resistance through the Ti wire) and still plated just fine. I believe what happens is that soon after the plating starts the resistance drops sharply as the gaps are plated in. 1
hashashan Posted November 10, 2007 Posted November 10, 2007 Damn I knew I forgot to tell you somethingNEVER, UNDER NO CIRCUMSTANCES INTERRUPT THE PLATING PROCESSthe anode will be bad. Most chances that the part that was plated in the second time will be damaged and it will detach soon into the perchlorate production.
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