WSM Posted June 2, 2015 Posted June 2, 2015 Hello WSM. I am interested in your publications. Where i can buy it?Best Regards,=)Thanks pyroChile, The first four parts to the series are formatted and posted here in the Blogs section. As time allows I'll put the rest of them here, too. The other option is to join the PGI (Pyrotechnics Guild International) and buy back issues of the PGI Bulletin. WSM
WSM Posted June 2, 2015 Posted June 2, 2015 What about this ?http://www.oocities.org/capecanaveral/campus/5361/chlorate/remove.htmlAnswer: Tailor made for our purposes. It would be nice if it were as simple and straightforward as turning potassium chloride into potassium chlorate, but that's just not the way it is. Since everything in the sodium chlorate cell is liquid, we need to proceed with faith until we can test the final product. If industry can do it, so can we (if we're willing to take the necessary steps to accomplish it). I hope to step up to the challenge after I finish making pure potassium perchlorate. As always, I plan to share my experiences here so all of us can benefit. WSM
taiwanluthiers Posted June 3, 2015 Posted June 3, 2015 It's pointless at this point anyways when I can just about buy them at around 4 bucks a pound... I just hope the US doesn't do that EU crap anytime soon.
pyrojig Posted June 3, 2015 Posted June 3, 2015 @ taiwanluthiers: I find that cleaning the sodium Chlorate ( from talks with WSM) are mostly killing the chlorides, but leaving the chlorate in solution for the next process. As there is no need to remove sodium chlorate out of solution , then go to perch .. It is better to keep the chlorate in sol. and go to the next step (perch) .It may be cheaper to purchase industry made perch, but a home - brewed sys . is a accomplishment , and a achievement. One can produce the needed oxidizers if that material becomes hard to procure .
Arthur Posted June 3, 2015 Posted June 3, 2015 In the UK perc is available to registered individuals only, In the EU perc is only available to businesses. If/when this sort of restriction hits other places than making it may be the only option.
taiwanluthiers Posted June 3, 2015 Posted June 3, 2015 Which is why it is important to make sure nobody takes away the second amendment, because that also allows a lot of the pyro chemicals to be legal/unregulated. Once second amendment is gone, pyro stuff will soon follow.
Arthur Posted June 3, 2015 Posted June 3, 2015 The new regs in the UK removed Explosives Precursors and Poisons from the retail market, hence we refer to them as the EPP regs. In the UK there is a means of getting a permit for home use.
THEONE Posted June 3, 2015 Posted June 3, 2015 At the page that i post before it tells that by having a solution of nacl and naclo3, when you cool it to 0°C and below, naclo3 will ppt out and not nacl. Also by adding nacl to the solution, this will drop the solubility of naclo3 and more naclo3 will ppt out. That looks interesting
frank Posted June 4, 2015 Posted June 4, 2015 For the NaClO3 to come out of solution there needs to be a very high concentration of NaClO3 in the solution. Only a small amount will come out of solution with the vast majority of it staying in solution.The best way to make solid sodium chlorate (if you want solid sodium chlorate) is to keep adding (THATS KEEP ADDING) salt solution to a working Na Chlorate cell at a similar rate to the rate that the salt is being converted to chlorate. After some time solid sodium chlorate will start to appear on the bottom of the cell . It has been said a hundred and one times (getting sour now!!!).The page above shows what happens in industry. Industry use a crystalliser system which does NOT consist of a dude or number of dudes slobbering around with some buckets/beakers/containers and some hot/cold water etc etc. It's a crystallizer system. You don't have one. I don't have one. No amateur has one. They are a great big piece of plant.Use the 'keep adding salt solution to cell' method and you will see (the very very elusive ) solid sodium chlorate.
pyrojig Posted June 4, 2015 Posted June 4, 2015 I believe that the goal for most of us making Naclo3 is to be feed-stock for a Perch sys. . I see no benefit to bringing Naclo3 out of solution otherwise . It may come to us hobbyist self - producing our own chems, if a over protective government takes control. Sadly it seems that the Gov. operates independently of us, and what we say has little influence . I think they have a god complex. ( off my soap box now) . I hope more folks take the plunge and enjoy the ability of being "self reliant " , not out of need but education , in case it becomes a need.
schroedinger Posted June 5, 2015 Posted June 5, 2015 There is a good reason to bring NaClO3 out of solution. Thats getting rid of Cl-. If you have a low chlrode concentration (less then 100g/L for Pt) electrodes will massivly corode. If you have a Cl- free cell, the don't.
WSM Posted June 12, 2015 Posted June 12, 2015 There is a good reason to bring NaClO3 out of solution. Thats getting rid of Cl-. If you have a low chlrode concentration (less then 100g/L for Pt) electrodes will massivly corode. If you have a Cl- free cell, the don't. I believe removing the chlorides from chlorates is reason enough to precipitate crystalline sodium chlorate. Whether chloride removal is necessary from an LD system is something that isn't clear yet. Certainly, it'll help in a Pt based perchlorate cell. Sorry I've been mostly absent in the past two weeks. My computer froze and the only remedy has been formatting the hard drive (a royal pain, to be sure), and I'm still hunting for my collection of disks to reinstall my most used drivers. Fortunately, a good friend was able to help me download the bulk of my files before I had to format the hard drive, so I lost very little of the current research (it's good to have friends like that!). Until I can find my drivers and get them loaded, my computer won't feel like "mine", but at least I can do something. WSM
Rocketier Posted June 13, 2015 Posted June 13, 2015 Here is a pdf related to this subject W Visser put online a while ago. Chlorate and Perchlorate Manufacturing.pdf
WSM Posted June 13, 2015 Posted June 13, 2015 (edited) Here is a pdf related to this subject W Visser put online a while ago. Thanks, Rocketier. I have a copy in my files but it's good to post it for others who may not have seen it. Knowledge is King. WSM Edited June 13, 2015 by WSM
WSM Posted June 15, 2015 Posted June 15, 2015 (edited) This past Saturday I made my first potassium perchlorate. After destroying the residual chlorate* in a 100 ml sample of the liquor from the LD cell, I neutralized the acid with sodium hydroxide solution. It was tricky to get to a pH of exactly 7.0, but by careful adjusting with HCl and NaOH, I got there. *I used sodium metabisulfite solution to destroy the residual chlorate. Now I added concentrated KCl solution and immediately it looked like milk; lots of very fine potassium perchlorate crystals, as seen in the attached photo. The rest of the liquor is full of sodium, sulfate and chloride ions. I'll remove the potassium perchlorate with vacuum filtration and rinse the crystals with chilled distilled water to remove the residual liquor with its contaminants. The liquid filtrate will be treated with calcium chloride solution to drop out the sulfate ions (as calcium sulfate [gypsum]) and leave just sodium chloride in solution, and maybe a few potassium ions. The purified sodium chloride solution will be saturated with more sodium chloride and used for a sodium chlorate cell later. There's much more work to do, plus testing; but I'm glad to be documenting my work and publishing it in the PGI Bulletin (and later, here in the blog section). WSM Edited June 15, 2015 by WSM
WSM Posted June 16, 2015 Posted June 16, 2015 This evening I set up a vacuum filtration arrangement and separated the potassium perchlorate from the liquid. I then added chilled distilled water to wash away any soluble salts that might be clinging to the white crystals. Next I dumped the moist crystals into a porcelain drying dish and placed it over boiling water to dry them out. When the crystals dry out I'll weigh them carefully to get an estimate of the CE of the run in the LD cell. I'll report more later... WSM
MrB Posted June 16, 2015 Posted June 16, 2015 You still rock. Been a while since i said (wrote) it, so i thought it was time for a new run at it.Cheers.B!
WSM Posted June 17, 2015 Posted June 17, 2015 (edited) You still rock. Been a while since i said (wrote) it, so i thought it was time for a new run at it.Cheers.B! Thanks MrB, I guess I got tired of waiting for someone else to do it, so I did it myself. Truth be told, I don't do anything alone, but with input and assistance from all of you (plus a self imposed deadline for the articles) I'm motivated to forge ahead. I enjoy the challenge, too. The many small achievements along the way are very encouraging. I finally got the perchlorate sample dried out and it looks like the LD cell is holding enough sodium perchlorate to produce about 1.6 Kg (3.5 lbs) of potassium perchlorate. I still have the Pt cell product to process, also. I better get going on the sodium chlorate cell so I can run the perchlorate cells longer and determine how long my anodes will last . WSM Edited June 18, 2015 by WSM
Arthur Posted June 18, 2015 Posted June 18, 2015 Simple question, for those who have run a chlorate cell. What temperature did you run it at, and what limited the temperature?
WSM Posted June 19, 2015 Posted June 19, 2015 (edited) Simple question, for those who have run a chlorate cell. What temperature did you run it at, and what limited the temperature? The last time I ran a potassium chlorate cell, it ran at 55oC and I'm not absolutely certain what limited the temperature besides cell volume and electrode size. WSM Edit: I believe the electrode size limits the maximum current the anode will demand, and that limits the temperature, if I'm not mistaken. Edited June 19, 2015 by WSM
WSM Posted June 19, 2015 Posted June 19, 2015 I realize the yield of my potassium perchlorate was lower than I hoped for (55g/100ml), but I checked the leftover liquid and got a weak positive for perchlorate; so there's still some in there. WSM
WSM Posted June 19, 2015 Posted June 19, 2015 (edited) I realize the yield of my potassium perchlorate was lower than I hoped for (55g/100ml), but I checked the leftover liquid and got a weak positive for perchlorate; so there's still some in there.WSM I think the small amount of perchlorate left in the filtrate won't be worth the extra effort required to wring out every last bit of it. That said, it won't be wasted since I plan to use the purified filtrate as base stock to re-saturate with sodium chloride and run a sodium chlorate cell with it. A little perchlorate in my sodium chlorate won't hurt, especially since I plan to use it to run in my sodium perchlorate cell. Like Swede indicated, nothing's wasted; just recycled. I still have a lot of sodium perchlorate solution to process into potassium perchlorate, plus I want to see the difference between the yields from the LD anode and the platinized anode. WSM Edited June 19, 2015 by WSM
Arthur Posted June 20, 2015 Posted June 20, 2015 (edited) I've just been reading an old patent that indicated that chloride was electrolysed to chlorate at greater than 100c (resulting in lots of water loss) BUT most of the chlorate would drop out of solution on cooling to 45c -which can be cleaned by a brief wash then put into a Perc cell. The process was two loops, one for chlorate and one for perc, neither was done or extracted to completion but as any chlorate being sent back to the chloride feed was never lost it didn't matter, likewise perc being sent back to the chlorate feed. Running the chlorate cell at 100+c by electrolytic heating seemed to be the key. Edited June 20, 2015 by Arthur
WSM Posted June 20, 2015 Posted June 20, 2015 I've just been reading an old patent that indicated that chloride was electrolysed to chlorate at greater than 100c (resulting in lots of water loss) BUT most of the chlorate would drop out of solution on cooling to 45c -which can be cleaned by a brief wash then put into a Perc cell.The process was two loops, one for chlorate and one for perc, neither was done or extracted to completion but as any chlorate being sent back to the chloride feed was never lost it didn't matter, likewise perc being sent back to the chlorate feed. Running the chlorate cell at 100+c by electrolytic heating seemed to be the key. Hi Arthur, I just read through the referenced patent and I'm intrigued by the experiment number two where they used a four liter glass cell. Have you been able to determine the yield from their experiment? I'm guessing about 1500-2000 grams if run to completion (which they didn't, but at least 1000 grams per time unit, as a continuing process). Is that how you read it? The power requirements of such a system are low enough to be easily achieved without undue stress.This certainly bears further review and may work on a hobbyist scale if one were willing to go to such lengths. Thanks for sharing this patent. WSM
WSM Posted June 20, 2015 Posted June 20, 2015 Running the chlorate cell at 100+c by electrolytic heating seemed to be the key. Now if it would work as well at 90oC, a cell tank made from heavy wall CPVC pipe (rated to 93oC) would work beautifully. Any thoughts?! WSM
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