Thunder75007 Posted August 15, 2014 Posted August 15, 2014 PyroChile, I bought them on EBay. http://www.ebay.com/sch/i.html?_odkw=platinumized+anode&_osacat=0&_from=R40&_from=R40&_trksid=p2045573.m570.l1311.R1.TR3.TRC1.A0.H1.Xplatinized+anode&_nkw=platinized+anode&_sacat=0 If the link does not work, just search on platinized anode. Cheers
pyrojig Posted August 16, 2014 Posted August 16, 2014 Expanded mesh gives you more surface area. So the stretched material is the best approach . As for a anode. I too though that the mesh was less surface area when I started , but with research found I was very wrong. If your after just kclo3 then use the cheap MMO and, for perch I believe that Na salt is the best approach for less wear and tear. Just required one extra step to double decomposition the salts to get the desired Kclo4
pyroChile Posted August 18, 2014 Posted August 18, 2014 (edited) PyroChile, I bought them on EBay. http://www.ebay.com/sch/i.html?_odkw=platinumized+anode&_osacat=0&_from=R40&_from=R40&_trksid=p2045573.m570.l1311.R1.TR3.TRC1.A0.H1.Xplatinized+anode&_nkw=platinized+anode&_sacat=0 If the link does not work, just search on platinized anode. Cheers Thanks! these anodes have 2,5 microns, therefore can resist this amperage... What is the distance between the electrodes (anode and cathode)? Best, =) Edited August 18, 2014 by pyroChile
taiwanluthiers Posted August 18, 2014 Posted August 18, 2014 I think I'm just going to terminate any and all experiments on making perchlorate... I'm going to the states and I can't take any of that with me. Besides it's easy to buy them cheaply in the states. 1
WSM Posted August 18, 2014 Posted August 18, 2014 I think I'm just going to terminate any and all experiments on making perchlorate... I'm going to the states and I can't take any of that with me. Besides it's easy to buy them cheaply in the states. Where in the States are you going? WSM
abbykarim Posted August 18, 2014 Posted August 18, 2014 this is a long thread. i dont know if anyone has tried or seen this method, but my pyro career is going to be hinged on this....no way can i get perchlorate in my country and other methods of production seem toooo expensive.. can any one view and comment on this guys video http://youtu.be/w-a4FsjAlUU
WSM Posted August 18, 2014 Posted August 18, 2014 Expanded mesh gives you more surface area. So the stretched material is the best approach . As for a anode. I too though that the mesh was less surface area when I started , but with research found I was very wrong. If your after just kclo3 then use the cheap MMO and, for perch I believe that Na salt is the best approach for less wear and tear. Just required one extra step to double decomposition the salts to get the desired Kclo4 I'm back from the PGI Convention (and I'm still recovering)! The MMO mesh used for making chlorates has such great surface area (due to it's cracked mud appearance, on a microscopic scale) that it's area is roughly equal to solid plate (which is convenient for surface area calculations). That's a material savings to the manufacturers and doesn't harm our process at all. For making perchlorates, platinized titanium does not seem share this benefit (if it has a smooth metal surface), but PbO2 anodes do, somewhat, due to the microscopic crystalline surface structure of the beta form LD. WSM
MrB Posted August 18, 2014 Posted August 18, 2014 I'm just checking of so i got at least some grip on whats going on. Please point out any errors. If one were to go from KCI to KClO4, Lead dioxide anode is the order of the day. Mesh, is as good, or better then plate. Stainless steel, preferable something very stainless, such as acid proof variants, or better yet titanium for the cathode. If possible, double up on cathodes, or, in case of multiple anodes, use one on each side of the anode. You want to figure out what square area you got, and run roughly 200mA / cm2. More, and your going to cause wear on the anode, less and your going to have longer batch production-times. I suspect it will also affect the heat, which might turn out to be a good thing, since you want to keep it hot, but below 55c.Using an AMP-meeter, would let you check the distance between your anode & cathode, and leaving it in as you run the system would give you a means to see how your progressing.Cave-eat. At this point i'm not sure what would be a reasonable cut of point. Other unanswered questions:When said cut of point is meet, can you simply filter the still hot solution to extract the perchlorate, stick it back on a heater, add water and KCI, and put it back in to your system, to minimize waste, or would that be the wrong way of doing things? It should be, as i understand it, since evaporation on larger open systems is held in check by adding a pre-heated KCI solution.Would using a magnetic stirrer for the purpose of maintaining a even temperature, and providing the highest concentration solution to the anode be beneficial? I'm thinking it would be, but...Where the hell do you obtain a LD anode in the first place? And which kind... Since i got a call earlier today letting me know my 50 kilos of KCIO4 is being delivered tomorrow, i shouldn't be in any kind of hurry to get this to work, but i am darn sure i want to get this figured out while there is still people willing to talk about it.B!
Thunder75007 Posted August 19, 2014 Posted August 19, 2014 Thanks! these anodes have 2,5 microns, therefore can resist this amperage... What is the distance between the electrodes (anode and cathode)? Best, =)I placed the electrodes 30mm apart. Please be aware that I am not stating that this is the best way to do things. I built these cells before I found this site. Cheers!
Thunder75007 Posted August 19, 2014 Posted August 19, 2014 this is a long thread. i dont know if anyone has tried or seen this method, but my pyro career is going to be hinged on this....no way can i get perchlorate in my country and other methods of production seem toooo expensive.. can any one view and comment on this guys video http://youtu.be/w-a4FsjAlUUThese crystals that he made look like KCLO3 to me, not KCLO4. I use the exact KCL to start with as he did and even running the cell seven days, I have KCLO3.
taiwanluthiers Posted August 19, 2014 Posted August 19, 2014 I have not decided where I will ultimately settle but for the time being I will be going to Fremont, CA.
MrB Posted August 19, 2014 Posted August 19, 2014 These crystals that he made look like KCLO3 to me, not KCLO4. I use the exact KCL to start with as he did and even running the cell seven days, I have KCLO3.Temperature? I'm far from an authority on the subject, but it's my understanding that if the temperature drops, the chlorate falls out of solution, if you can keep the temp up the perchlorate will be what falls out of solution first. Also, you could simply "wash" it with cold water to separate them after production. If the water is evaporated, and the chlorate is recovered it will still have some perchlorate contamination but it shouldn't be bad.One way of testing it, i suppose, is simply using hot water. @ 40c you should be able to dissolve 13gr of chlorate in to a DL of hot water, but only 4.7gr of perchlorate.B!
abbykarim Posted August 19, 2014 Posted August 19, 2014 Temperature? I'm far from an authority on the subject, but it's my understanding that if the temperature drops, the chlorate falls out of solution, if you can keep the temp up the perchlorate will be what falls out of solution first. Also, you could simply "wash" it with cold water to separate them after production. If the water is evaporated, and the chlorate is recovered it will still have some perchlorate contamination but it shouldn't be bad.One way of testing it, i suppose, is simply using hot water. @ 40c you should be able to dissolve 13gr of chlorate in to a DL of hot water, but only 4.7gr of perchlorate.B! yes mr.B. know that in room temperature water the chlorate is soulbe while the perchlorate is not. and thus with the washing shown here i would assume that the chlorate should dissolve out. i really do believe that the heat of the solution and the concentration of the chloride may have something to do with it. i am going to try this method. one question. the kcl he uses i cant get that. but i can get agricultural white potash which is usually pure kcl as well...i wander if it would make a difference
schroedinger Posted August 19, 2014 Posted August 19, 2014 If the potash isn't the carbonate , the chloride then it is the right stuff 1
taiwanluthiers Posted August 19, 2014 Posted August 19, 2014 I have several Kg of chlorate that I'm not using and I don't feel good about tossing it in the trash.... How do I dispose of it? I am actually thinking I got lots of stray plants around the property that needs to die (weeds, grass, etc. growing out of concrete). Maybe I should use it on that...
Thunder75007 Posted August 20, 2014 Posted August 20, 2014 Temperature? I'm far from an authority on the subject, but it's my understanding that if the temperature drops, the chlorate falls out of solution, if you can keep the temp up the perchlorate will be what falls out of solution first. Also, you could simply "wash" it with cold water to separate them after production. If the water is evaporated, and the chlorate is recovered it will still have some perchlorate contamination but it shouldn't be bad.One way of testing it, i suppose, is simply using hot water. @ 40c you should be able to dissolve 13gr of chlorate in to a DL of hot water, but only 4.7gr of perchlorate.B!MrB, I am in no way an authority on any of this. I run my cells at 55 to 65c continually. Everything that I produce has been KCLO3 until 2 weeks ago when I accidently ran from KCL to KCLO4 for the first time. It took my cells 9 to 10 days to produce 95% KCLO4 with the rest being KCLO3. I only run the cells at 5vdc @ 13a though. There was some fiber/string like substance that dropped out of solution first, you can see the story on page 149, and I still do not know what they are.
MrB Posted August 20, 2014 Posted August 20, 2014 Without pictures, or better yet, testing, we'll never know what those first seeds are, but i suspect they are simply KClO4. it could of course be contaminations from your water or salt-source as well. Platinum anodes makes you able to run slightly higher temps, but suffer when you leave it running. I intend to stick to an anode that can survive going from KCl to KClO4, and as far as i know thats leaddioxide, and pretty much "only" lead dioxide. So i'll have to keep the temp slightly lower. I also intend to use 2 cathodes, at least for the "test" setup when ever that gets going. Trying to help prolonging the life of the leaddioxide anode by avoiding hotspots. 200mA / cm2 of anode area, is my target starting point, which might mean that i need to experiment with the distance they need to be apart from one and other. So far i haven't really decided on a method for measuring the amp's, but right now i'm mostly just trying to understand most of this. The main problem with going straight to KClO4 seams to be getting the KClO3 to dissolve after it has fallen out of solution. There needs to be circulation in the lower part of the cell, i'm thinking a magnetic stirrer, and a ceramic stirring rod for it. I suspect it wouldn't take a whole lot, and it could run on a timer, not needing to run all the time. For testing and smaller systems, a number of stirrers would work great. For something larger like the bucket sizes people experiment with you might need something larger, and the bonus with some of those is that that come with a heating element, so you can keep the batch @ working temp even when the volume of the cell is so large that the process cant maintain the heat. But, i'm speculating. Anyway, temp seams to be the main issue. Either to hot, or not hot enough, sometimes both at the same time.B!
WSM Posted August 20, 2014 Posted August 20, 2014 I have not decided where I will ultimately settle but for the time being I will be going to Fremont, CA. That's Northern California. If you move to Southern California after that, we'll have to talk. WSM
WSM Posted August 20, 2014 Posted August 20, 2014 yes mr.B. know that in room temperature water the chlorate is soulbe while the perchlorate is not. and thus with the washing shown here i would assume that the chlorate should dissolve out. i really do believe that the heat of the solution and the concentration of the chloride may have something to do with it. i am going to try this method.one question. the kcl he uses i cant get that. but i can get agricultural white potash which is usually pure kcl as well...i wander if it would make a difference At room temperature, some chlorate is soluble. See if you can get the solubility chart which compares the various chlorides, chlorates and perchlorates at different temperatures, to get the relative solubilities. By this you can determine which temperature to aim for for different results. If your agricultural potash is white, I wonder if it's chloride or carbonate? Where is it found (what Country)? WSM 1
WSM Posted August 20, 2014 Posted August 20, 2014 I have several Kg of chlorate that I'm not using and I don't feel good about tossing it in the trash.... How do I dispose of it?I am actually thinking I got lots of stray plants around the property that needs to die (weeds, grass, etc. growing out of concrete). Maybe I should use it on that... Sodium metabisulfite in solution is supposed to break down chlorates. I'd have to study the process further to understand what temperature and pressure is most effective in achieving this. Chlorates are indescriminate herbicides and kill weeds very well. Unfortunately, they kill every other plant as well (that is what indescriminate means. after all), so be very careful where your runoff may go. PM me when you get to the States. WSM
WSM Posted August 20, 2014 Posted August 20, 2014 Some comments were made regarding making perchlorates directly from chloride using lead dioxode anodes. Please be aware that the only pilot cell I've read about in literature was a sodium based cell and the anode was made by the researchers, and was beta form lead dioxide over graphite. They also buffered the liquor with sodium fluoride. Due to problems with fluorides in contact with titanium anodes, I'm concerned that LD over CP titanium anodes would be negatively effected by such a system and the effectiveness would be seriously compromised. I plan to do my perchlorate studies with LD over titanium anodes, titanium cathodes and using sodium chlorate. After converting the chlorate to sodium perchlorate, I'll neutralize the residual chlorate with sodium metabisulfite and then exchange the perchlorate with KCl. I'll collect and rinse the resulting potassium perchlorate in a Buchner funnel with distilled water, then dry and store it for later use. WSM
dangerousamateur Posted August 20, 2014 Posted August 20, 2014 I have another question for the experts: If I run a perchlorate cell, starting with chloride or maybe a chloride and chlorate mixture, the end product is purified by the destruction of the remaining chlorate. At this point, can I assume that all chloride is converted, or will there be some chloride contamination?
schroedinger Posted August 20, 2014 Posted August 20, 2014 (edited) No there will be chloride present, you get rid of the chloride during the exchange reaktion. Pottasium and ammonium perchlorate have both poor solubility where as the chloride has a god one and stays in solution. If not all stood in solution just recristallize. Edited August 20, 2014 by schroedinger
dangerousamateur Posted August 21, 2014 Posted August 21, 2014 I know schroedinger. But when you run a chlorate cell you can run it until all chloride has converted. The anode will suffer of course.Now if you have a perchlorate cell, it runs so much longer, but even at at the end of the chloride-chlorate process there should be little chloride left. You understand my thought? If a perchlorate cell runs to 80-90% perchlorate, how much chloride will be in the crop? Maybe i want pure sodium perchlorate.
schroedinger Posted August 21, 2014 Posted August 21, 2014 I would assume about 5% at if you run it further down the anode will fail before the all chloride is converted, this has been described quite often in the geocitties site and happened to all elctrodes tried.
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