WSM Posted July 15, 2018 Share Posted July 15, 2018 (edited) My new approach to the High Temperature Sodium Chlorate Experiment Involves a 5 liter reaction vessel without a lid, purchased earlier this year. It is heavy walled borosilicate glass and has a large opening with a flat top and a groove for an O-ring. I've experimented with silicone tubing to determine what size and length is needed to form an O-ring for the top plate seal. 6mm diameter tubing worked but I feel the groove is made to accomodate 1/4" material. I won a bid on a good length of Viton tubing, 1/8" ID and 1/4" OD. When cut to the correct length, I plan to join the flush-cut ends with a short piece of 1/8" OD Viton tubing inside and bond them all together with acetone as a solvent. The next task will be to decide which polymer to use for the lid of the cell. In the original patent, they used a one inch (~25mm) thick piece of Lucite (Plexiglass or Perspex) with ports added for the electrodes, vent and a host of other purposes. That may work but I'm also considering either PVC, CPVC or Kynar plate. The Kynar, if available and affordable, may be the most compatible choice, considering all the parameters of this cell. If I go with that, I'll need to shop for a workable piece plus determine the best method of attachment. There's much more to do, but I'll give it my best and try this thing out! WSM Edited July 15, 2018 by WSM Link to comment Share on other sites More sharing options...
WSM Posted July 15, 2018 Share Posted July 15, 2018 (edited) The original patent used a pair of platinum plated titanium electrodes, 3" square. When running it, they occasionally reversed polarity to maintain the best environment for the electrodes. My plan is to use an MMO mesh anode surrounded by two solid plates of CP titanium for cathodes, all 4" square, which should work nicely. I hope the added size will more easily get to and operate at a high enough temperature to reach and maintain a running temperature of about 110oC, which should optimize the production of NaClO3 while concentrating the electrolyte by evaporating the excess water, making chlorate recovery at room temperature (rather than chilling the electrolyte to 0oC for oxidizer recovery, as done previously) a much simpler and less costly process. An added benefit will be using purified brine to recharge the "depleted" electrolyte, rather than dry purified salt. The whole system appears that it will easily lend itself to a continuous system, but baby steps first. WSM Edited July 18, 2018 by WSM Link to comment Share on other sites More sharing options...
WSM Posted August 28, 2018 Share Posted August 28, 2018 (edited) I'm ready to pick up my work on Part Eighteen of the series, Homegrown Oxidizers, published in the PGI Bulletin.In it I'm continuing the research into purifying potassium chloride solution for use in chlorate cells OR for use in producing purified potassium perchlorate from purified sodium perchlorate.My thinking is that since I'm bothering to make oxidizers (when I can buy them if I want), why not make them better than commercial grade material (+-99% Mil Spec standards)?I'll let you know when the draft is submitted to the Bulletin.WSM Edited September 2, 2018 by WSM Link to comment Share on other sites More sharing options...
pyrojig Posted September 10, 2018 Share Posted September 10, 2018 EXciting news. Looking forward to the new findings on your research Link to comment Share on other sites More sharing options...
tylerngo Posted October 15, 2018 Share Posted October 15, 2018 Did you finally get the help that you required? Update please. Brumer Link to comment Share on other sites More sharing options...
WSM Posted November 2, 2018 Share Posted November 2, 2018 Did you finally get the help that you required? Update please.Brumer I'm sorry, I don't follow what you mean. Can you elaborate? WSM Link to comment Share on other sites More sharing options...
WSM Posted November 2, 2018 Share Posted November 2, 2018 I apologize for not posting very much. My research has taken a back seat to several other projects, plus greater demands on my time by family and work. My work schedule is going to get much busier starting next month, and last into April. If possible, I'll see if I can make some headway on my electrochemical research and report my progress here. More later... WSM Link to comment Share on other sites More sharing options...
WSM Posted November 4, 2018 Share Posted November 4, 2018 I apologize for not posting very much. My research has taken a back seat to several other projects, plus greater demands on my time by family and work. My work schedule is going to get much busier starting next month, and last into April.If possible, I'll see if I can make some headway on my electrochemical research and report my progress here.More later...WSM A couple of the projects occupying my time include changing the power in my workshop from a line connected in from the house power, to an off-grid solar system, including a battery backup, sufficient to supply all the electricity I can use, plus... The other project is a discrete (meaning, stand-alone) purified water system. Both systems will add to emergency home preparedness, as well as supply my hobby projects. When those efforts reach a greater degree of completion, I plan to resume my electrochemical research and set up several experiments to demonstrate an ability to be more self sufficient in chlor-alkali oxidizer production (a fun challenge, for sure!). All of this depends on fitting things in, between work, family needs and any other demand on my time. Wish me luck! WSM Link to comment Share on other sites More sharing options...
PTFE Posted November 25, 2018 Share Posted November 25, 2018 Hey all.Sorry but at the moment i have no time for chemistry and hobbies but i just found a german Ebay seller who has great reaction vessles made out of glass for sale. Link to comment Share on other sites More sharing options...
WSM Posted November 27, 2018 Share Posted November 27, 2018 Hey all.Sorry but at the moment i have no time for chemistry and hobbies but i just found a german Ebay seller who has great reaction vessles made out of glass for sale.Sounds intriguing. Any photos?! WSM Link to comment Share on other sites More sharing options...
memo Posted November 28, 2018 Share Posted November 28, 2018 well i have another question, been running my 2.5 gallon cell for 120 hours.when I test with meth. blue the color goes from deep blue to lighter almost turquoise not violet. it does precip. out a very fine particulars. do you think I have sodium perchlorate ? or give it 24 hours more. Link to comment Share on other sites More sharing options...
PTFE Posted November 30, 2018 Share Posted November 30, 2018 Sounds intriguing. Any photos?! WSM i'm sorry, i forgott to add the link to it.https://www.ebay.de/itm/Reaktionsgefas-aus-Glas/264063268130?hash=item3d7b65b522:g:dQYAAOSwnNBXZS-q:rk:12:pf:0 Link to comment Share on other sites More sharing options...
WSM Posted December 6, 2018 Share Posted December 6, 2018 i'm sorry, i forgott to add the link to it.https://www.ebay.de/itm/Reaktionsgefas-aus-Glas/264063268130?hash=item3d7b65b522:g:dQYAAOSwnNBXZS-q:rk:12:pf:0 Nice! A bit pricey, though. I got one similar, but larger (5 liter) on eBay, for about half as much (maybe I'm just lucky). If you set it up, please share a photo. Thanks. WSM Link to comment Share on other sites More sharing options...
WSM Posted December 6, 2018 Share Posted December 6, 2018 well i have another question, been running my 2.5 gallon cell for 120 hours.when I test with meth. blue the color goes from deep blue to lighter almost turquoise not violet. it does precip. out a very fine particulars. do you think I have sodium perchlorate ? or give it 24 hours more. That's odd. It almost sounds like you used sodium nitrate instead of sodium chloride. Another thought, maybe it's all sodium chlorate and no perchlorate has formed (methylene blue tests for perchlorate only and chlorate won't turn it purple)? One time I ordered methylene blue from someone in Eastern Europe, but what I got was hardly water soluble (not at all what my American sourced methylene blue was like), and totally useless for the purpose. Caveat Emptor !!! Let us know if you solve the question. WSM Link to comment Share on other sites More sharing options...
memo Posted December 6, 2018 Share Posted December 6, 2018 used 10 iiters of water ( ro ) 3500 grams of salt (swimming pool pure ) the methylene blue was from the fish store. ran it for 144 hours still does not test for perchlorate. boiled 2 liters for 30 40 minutes the poured sat. potassium chloride pool grade. I it precipitated a very fine crystals right a way tested again for perchlorate only very light blue. I am stumped. memo Link to comment Share on other sites More sharing options...
Arthur Posted December 6, 2018 Share Posted December 6, 2018 What current are you running for those hours? How hot does the cell run? Link to comment Share on other sites More sharing options...
memo Posted December 6, 2018 Share Posted December 6, 2018 5 volts 20 amps Link to comment Share on other sites More sharing options...
Arthur Posted December 7, 2018 Share Posted December 7, 2018 Work out what charge must pass (in coulombs or amphours ) to convert your total mass of chloride to chlorate, I personally suspect that it's a big number for a big cell. Only when the electrolysis is largely complete to ClO3 will production of ClO4 become established. Do tests in a smaller vessel! maybe 500ml to 1000ml Link to comment Share on other sites More sharing options...
PirocaESP Posted December 7, 2018 Share Posted December 7, 2018 i really need help with this, ive been looking all over the internet and found a heap of cell designs and precipitation methods but most of them end up failing or don't last more than 2 days i just need professional help (that works) thnx you can do it by thermal reaction you need to heat up potassium chlorate to 350 Celsius and after begin melted you just have to w8 from 40 to 45 minutes and will form like a white paste at the bottom then you let crystalized and cool down after you crush in to powder and recrystallize in water you put the powder in boil water dissolved in the boiling water for 30 minutes let it cool down and w8 for the crystal is not gonna be 100% pure but will be around 95% Link to comment Share on other sites More sharing options...
WSM Posted December 9, 2018 Share Posted December 9, 2018 used 10 iiters of water ( ro ) 3500 grams of salt (swimming pool pure ) the methylene blue was from the fish store. ran it for 144 hours still does not test for perchlorate. boiled 2 liters for 30 40 minutes the poured sat. potassium chloride pool grade. I it precipitated a very fine crystals right a way tested again for perchlorate only very light blue. I am stumped.memoIs this with MMO or some other type of anode? WSM Link to comment Share on other sites More sharing options...
memo Posted December 9, 2018 Share Posted December 9, 2018 mmo and titanium cathode Link to comment Share on other sites More sharing options...
WSM Posted December 9, 2018 Share Posted December 9, 2018 (edited) mmo and titanium cathode It's my understanding that MMO doesn't have the ability to make perchlorate (the oxygen overpotential isn't high enough), but just chlorate. In a sodium chloride system, I expect you'll only get sodium chlorate. Now NaClO3 is MUCH more soluble in water than the chloride; the same with sodium perchlorate being MUCH more soluble than sodium chlorate. To get sodium chlorate to drop out of solution requires highly concentrating the dissolved chlorate salt. This is usually achieved by boiling some of the water away, or continually adding more dissolved chloride feedstock as the cell runs, till the concentration of chlorate is high enough to drive some out of solution. Chilling the chlorate laden electrolyte to about 0oC also drives out NaClO3 crystals (some of it, but not all). When I ran a 20-25 liter NaClO3 cell, I had to run it ~6 weeks to complete the run (about 40-50 Amps and ~40oC). If you try chilling, don't go much lower than 0oC, or some chloride will also precipitate. If any of this is unclear or you have more questions, just ask. I'll try to answer. WSM Edited December 9, 2018 by WSM Link to comment Share on other sites More sharing options...
WSM Posted December 9, 2018 Share Posted December 9, 2018 used 10 iiters of water ( ro ) 3500 grams of salt (swimming pool pure ) the methylene blue was from the fish store. ran it for 144 hours still does not test for perchlorate. boiled 2 liters for 30 40 minutes the poured sat. potassium chloride pool grade. I it precipitated a very fine crystals right a way tested again for perchlorate only very light blue. I am stumped.memo I suspect you got only potassium chlorate, no perchlorate. Methylene blue tests for perchlorate and is unaffected by chlorate or nitrate. There are a few tests for chlorate and one of those will probably tell you for sure what you have. WSM Link to comment Share on other sites More sharing options...
WSM Posted December 9, 2018 Share Posted December 9, 2018 (edited) I'm sorry for slow responses to inquiries here. This month, I'm working 12 hour days, six days a week; and need to focus my energies there, so I rarely get to read through these posts. WSM Edited December 9, 2018 by WSM Link to comment Share on other sites More sharing options...
memo Posted December 9, 2018 Share Posted December 9, 2018 what step am i missing to get sodium perchlorate ? Link to comment Share on other sites More sharing options...
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