PyrofireM100 Posted December 9, 2017 Posted December 9, 2017 I think create a Cell is very difficoult , but make kclo4 with Bleach is more easy , I see on YouTube that I must boil the bleach to make naclo3, after I mix it with kcl and with this process I make kclo3. after I put kclo3 in a ceramic jar and heat up it to convert kclo3 in kclo4. I have bleach 14 %. Does it is a good procedure?
Mumbles Posted December 10, 2017 Posted December 10, 2017 Melting chlorate never goes to full conversion to perchlorate. I'm not sure about perchlorates, but chloride contamination sensitizes chlorates. Given that you'll never get rid of all the chlorate without a lot of difficulty, I'd consider anything made via this method more sensitive than pure materials.
Scorpion812 Posted December 10, 2017 Posted December 10, 2017 I don't recommend you try this method at all, its extremely expensive and inefficient. Also, in my opinion, electrolysis is really not that complicated, get this : http://store.theamateurchemist.com/lead-dioxide-anode-2-by-3-with-4-stem/ and this: http://store.theamateurchemist.com/mmo-titanium-anode-2-by-3-with-4-stem/ and build a cell from a 1 gallon pickle jar and replace the cap with a pvc end cap. Secure the electrodes with silicon and attach a tube for the gas and youre set. Be sure to read the perchlorate thread and maybe first try potassium chlorate with the mmo. also, this is a great cheap power supply that fits most need with those electrodes: https://www.ebay.com/itm/New-250W-FLEX-ATX-Power-Supply-for-HP-Enhance-ENP-2320-/130640364671 1
PyrofireM100 Posted December 10, 2017 Author Posted December 10, 2017 Thanks, but do I must prepare a solution with kcl and electrolize it for 2 weeks to make kclo4 using 5 volt and 20 Amp? Because I see on internet that convert kcl to kclo4 need al lot of time
Arthur Posted December 10, 2017 Posted December 10, 2017 Electrolytic production of chlorate and perc IS the commercial method at this time. Yes it takes amps for weeks to make much product. Remember that only platinum or Lead Dioxide anodes will add the fourth oxygen atom. Lots of cheaper materials from carbon rods upwards will make chlorate but NOT perc.
PyrofireM100 Posted December 10, 2017 Author Posted December 10, 2017 If I create a good cell how much time do I need to make a good quantity /percentage of kclo4? How do I can understand if the quantity of kclo4 is good? And how I can do to destroy the kclo3 residue?
Mumbles Posted December 11, 2017 Posted December 11, 2017 https://www.amateurpyro.com/forums/topic/1629-making-potassium-per-chlorate/
patsroom Posted December 11, 2017 Posted December 11, 2017 Looks like someone has a lot of reading to do. But if you do read it all you will have a good understanding how it is done and that it is far better that trying to use bleach. There are few shortcuts in wanting and getting kclo4, going with bleach is not one of them IMHO. And once you can make you own kclo4 you will have few limitations in making your own fireworks.............Pat
Scorpion812 Posted December 11, 2017 Posted December 11, 2017 You can NOT make KClO4 from KCl directly
MrB Posted December 11, 2017 Posted December 11, 2017 You can NOT make KClO4 from KCl directly Debatable. Lead dioxide anodes convert KCl to KClO3, and then KClO3 to KClO4, without user interaction. The problem seems to be getting quality anodes. I'm STILL looking for a tube, mesh, LD anode, preferably with a round rod, or a pair of round rods, rather then strips to connect it.
PyrofireM100 Posted December 11, 2017 Author Posted December 11, 2017 Can I do a cell with NaCl and a convert it on naclo3 and after on naclo4? After to destroy clorate can I use sodium metabisulfite? After this procedure do I must mix naclo4 with kcl to make kclo4?
Arthur Posted December 11, 2017 Posted December 11, 2017 That is, in my opinion, the way that it should be done. There are two major points to consider. 1/ getting enough sodium chlorate in a warm cell that it precipitates out cleanly when chilled, (If you can recover precipitated sodium chlorate there is little to no chloride present) 2/ getting a reliable and affordable perc cell anode If you take perc cell electrolyte and add saturated KCl solution (in water) to the it KClO4 precipitates out first, if you add excess KCl then a second crop can be recovered but it is Potassium Chlorate. Doing the calculations to quantify all of the above and allow for limited efficiency and still get the quantity of KCl required for getting clean perc is where the mathematical chemistry comes in. Remember that an electrochemical cell will heat due to resistive current, so not all electricity into the cell will make the desired product.
PyrofireM100 Posted December 11, 2017 Author Posted December 11, 2017 But If I make a cell for naclo3, how I can do the naclo4? Electrolizing the solution for a lot of time?
scoin56 Posted January 22, 2018 Posted January 22, 2018 hi guys, so i was able to buy some kclo4 dirt cheap,but i think their might be a problem with it. I got in contact with my supplier and said it was nothing wrong with his product. but after doing some research and running some tests i came to my conclusion i was sold kcl. would love your help assuring me the product is bad. thank you guys tests done:solubility testi was able to dissolve about 20 grams of the presumed kclo4 in 100ml of water. did not pass burn test with sulfur 50:50 mix will barely burn burn test with sugar 50:50it did burn aluminum test kclo4 was balled milled 7 hours passed my 325mesh screenmixed 70:30 eckart german blackhead 5413 h superit would barely burn and when it did it was very slow final testmethlelyne blue test mixed in a test tube and didnot turn dark violet it stayed blue
MrB Posted January 22, 2018 Posted January 22, 2018 KCl and 50% sugar, pretty much just wouldn't burn, at all. The sulfur mix might burn, but leave the KCl untouched. Well, i think. 1
scoin56 Posted January 22, 2018 Posted January 22, 2018 Thank for the respond mrb, im baffled ive never had this problem. any other suggestions in testing it you might have? Im just a bit frustrated because i purchased 100# pounds of it.
pyrojig Posted January 25, 2018 Posted January 25, 2018 I would return that junk asap.... It clearly is not kcl04 . At this point does it matter what it is . ?
MrB Posted January 25, 2018 Posted January 25, 2018 I'm not convinced that this is junk, and not KClO4, or possibly KClO3. Test i'd perform again. Boil water. Make a saturated solution by adding the salt, leaving some that doesn't dissolve on the bottom.Pour of a know quantity, like 100ml, and evaporate it. Check how much salt was, by weight. (21 grams for KClO4, 53,5 for KClO3. 36 for KCl, but that isn't really a viable result, since KCl wont burn with sugar.) Mix 10 grams of sugar with 25 grams of salt. This should burn rather violently and be possible to light by fuse. For a reasonable burn test, dry your chemicals.Sulfur and KClO4 pretty much does nothing, as seen earlier, not really worth testing again. The only thing that is out of character is the methylene blue test. Worth redoing while waiting for the 100ml of saturated solution to evaporate, and leave it's dry content behind, to verify proper testing procedures? Chill the leftovers of the saturated solution, and siphon of a small volume. Using a 0.3-0.5% solution of methylene blue, add a single drop the the test sample. Ignore the color of the fluid, and look for a light violet dusting settling on the bottom of the container.(As far as i know, the fluid could remain blue, you are just going to get a violet precipitate if there is perchlorate present. Someone more familiar with this test might want to jump in here. Also, the test is VERY sensitive, and tiny amounts will give a positive result, so this is by no means an indication of purity.)
scoin56 Posted January 29, 2018 Posted January 29, 2018 Ok guys im back, i got back in to the work shop after dealing with the stomach flue. so i was able to run some test and take video. got the methylene blue test done<iframe width="560" height="315" src="https://www.youtube.com/embed/qDPRkumHQXI"frameborder="0" allow="autoplay; encrypted-media" allowfullscreen></iframe> sugar test<iframe width="560" height="315" src="https://www.youtube.com/embed/AI9xHmZVqlM"frameborder="0" allow="autoplay; encrypted-media" allowfullscreen></iframe> I was able to get a flash with a little help with a catalyst and in this ratio30/40/30 kp/s/al still drying the saturated solution
scoin56 Posted January 29, 2018 Posted January 29, 2018 (edited) Ok the 100ml of saturated solution finaly dried, 36g finall product. Edited January 29, 2018 by scoin56
MrB Posted January 29, 2018 Posted January 29, 2018 Results are all over the place. Not really sure what to make of it. Weight of dry chemical after pulling a saturated 100 ml sample indicates KCl, but KCl just wont burn with sugar.Dunno what to say. I'd have to agree with pyrojig above, and suggest returning it, if at all possible.
scoin56 Posted January 29, 2018 Posted January 29, 2018 Could it be its just low purity? I was also wondering if re-crystallization would work. I will have to contact the supplier if its returnable, but highly doubt it as it was final sell at $2 a #.He assured me it was 99% pure.
pyrojig Posted January 30, 2018 Posted January 30, 2018 I would hold his feet to the fire on this . It sounds like a scam , and at $2 lb that is drum price if you have kick ass connections . I rarely ever see this material for under $3 lb even at drum priced weights on a co-op buy. I would stop wasting time researching this and get a refund ASAP dont waste time with these scam artist on the internet . Just my 2cents worth .
scoin56 Posted January 30, 2018 Posted January 30, 2018 (edited) 😈 Edited January 30, 2018 by scoin56 1
scoin56 Posted January 30, 2018 Posted January 30, 2018 Ill have to contact my supplier but as a direct chem importer,he should have known it was a bad batch.
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