Ralph Posted August 18, 2009 Posted August 18, 2009 I don't see it the smaller one is lead nitrate and the larger one is difficult to tell as the chemical formulla is kinda sideways does it say kno3?
Bonny Posted August 20, 2009 Posted August 20, 2009 I will be making a cell in the near future, just waiting on my electrode set for chlorate production. As for the conversion to perc, I don't think anyone has made a functioning LD anode (yet). If I'm going to use platinum, can platinum/iridium wire be used or must it be pure platinum??
Swede Posted August 20, 2009 Posted August 20, 2009 I will be making a cell in the near future, just waiting on my electrode set for chlorate production. As for the conversion to perc, I don't think anyone has made a functioning LD anode (yet). If I'm going to use platinum, can platinum/iridium wire be used or must it be pure platinum?? I suspect Platinum/Iridium alloy would work. It might not be as efficient as Pt, but it'll probably make perchlorate nicely, depending upon the percentages. Possibly like you, I've always looked at my chlorate as feed stock (ultimately) for a perchlorate cell. I am not afraid of chlorate, but I'd rather have perc. I have used the jewelry-trade Pt plated anodes successfully. They're still pretty expensive, but I think they are a better deal than those Pt anodes sold to pyro hobbyists. In all cases, the Pt erosion is real and inevitable, and the big factories have Pt recovery procedures in place. Otherwise, the cost would go way up. My LD anode still awaits tests! It looks good, and I am very hopeful.
Swede Posted August 20, 2009 Posted August 20, 2009 Sorry for the double posting, but I have to know how to remove the hypochlorite from the KClO3 wield. Boiling for 20 minutes really doesn't help much. Does your dried chlorate crystals smell of hypochlorites? I've heard of this, but personally I have never had a hypo smell from the Xtals once dried. I think if I were into serious chlorate production (as opposed to creating feedstock for perchlorate), I'd definitely execute at least one recrystallization. If it can be done on a very large scale, it won't be so much of a hassle, and again, any waste is not lost but simply recycled. That is why I always advocate a pretty vigorous washing during the initial harvest, and also during recrystallization. The recrystallization especially should be very effective at cleaning the chlorate, because you are totally dissolving those fat xtals, and any volatile contamination should gas off, while the more soluble contaminants will be removed in the waste/wash water. I do my recrystallizations in a big 16 liter Pyrex beaker I got off eBay for $25. It's like a beaker on steroids, although it could also be done with a turkey fryer or similar.
Ventsi Posted August 20, 2009 Posted August 20, 2009 What the heck do you guys use to boil stuff? I dont meant tortallini either. Everything I've tried cracks during cool down, I've tried Pyrex bowls, jars, coffee machine glass ...? My first time boiling hypochlorite was in a "stainless" sauce pan, lesson learned it wasn't so stinless after that I'm lucky it didn't go through the bottom. Maybe a nice heating element is on order , or a hot dish? I believe that thats what they are called.
50AE Posted August 20, 2009 Posted August 20, 2009 I use a regular kitchen saucepan, but it is painted inside with a somewhat resistant paint. Swede, when dried my crystals don't smell the hypochlorite anymore. But a friend chemist told me that hypochlorite decomposes from the CO2 in the air to chlorate and chloride. That's why I worry if it could increase much the chloride concentration, but I doubt, because I've already tested a dried sample. Of course, I'm performing a recrystallization.
Bonny Posted August 20, 2009 Posted August 20, 2009 What the heck do you guys use to boil stuff? I dont meant tortallini either. Everything I've tried cracks during cool down, I've tried Pyrex bowls, jars, coffee machine glass ...? My first time boiling hypochlorite was in a "stainless" sauce pan, lesson learned it wasn't so stinless after that I'm lucky it didn't go through the bottom. Maybe a nice heating element is on order , or a hot dish? I believe that thats what they are called. I've never boiled chlorates per say, but have used glass cooking pots (Visions Corningware?) many times boiling homemade nitrates with no problems. I use a small hot plate as a heat source.
50AE Posted August 20, 2009 Posted August 20, 2009 I really want to synthesize barium chlorate by electrolysis, but by looking at the solubilities of BaCl2 and Ba(ClO3)2, I get a headache. Their solubilities are very similar and I don't know if I should try start this work. But barium chlorates gives awesome greens. http://en.wikipedia.org/wiki/Solubility_table
Ralph Posted August 20, 2009 Posted August 20, 2009 (edited) Dont use your mmo if you do make it because barium is a poison to mmo and you will ruin your lovely electrodes Edited August 21, 2009 by Ralph
50AE Posted August 21, 2009 Posted August 21, 2009 (edited) You mean it will make my electrodes erode ? Edited August 21, 2009 by 50AE
Ralph Posted August 21, 2009 Posted August 21, 2009 well it will damage the MMO so in the long run yes
50AE Posted August 21, 2009 Posted August 21, 2009 Alright, I won't be doing barium chlorate, sadly. Swede, by the way after 1 week and a half of run, I start to get small flakes of MMO in my KClO3. They aren't much, there are 4 or 5 flakes per 100 grams of KClO3. But I worry, is this normal ? Should I make a pH control and increase the MMO's life ?
Ralph Posted August 21, 2009 Posted August 21, 2009 scary i taught mmo was invincible 50AE why dont you just make barium chlorate with carbon electrodes
50AE Posted August 21, 2009 Posted August 21, 2009 Or I think the flaking is occurring because bastards here are fucking with the electricity and maybe it stops at night while I'm sleeping. This way, the cell maybe acts as a battery and pumps current to the power supply, which maybe has damaged the anode. I will turn the cell off while I'm sleeping and I'll try to find a powerful diode as soon as possible.
Swede Posted August 24, 2009 Posted August 24, 2009 Black flakes - I have seen these in my own work, and I am 90% convinced they came (in my case) from a black nylon fitting which was literally disintegrating. If you have NO OTHER SOURCE that could create small black particles, then it may very well be MMO. The loss of power can't help things, but from an electrochemical POV I can't see why power-off would hurt the anode. The cathode perhaps, but not the anode. Consider the volume of the particles. If you are getting a significant amount in just a few grams of chlorate, then it's probably excessive. If it's 6 or 8 minute flecks in a kilogram, then the erosion is just part of doing business. Nothing is indestructible, there is always going to be some erosion, but it can be minimized by following a few rules. 1) Keep the chloride ion concentration up by halting the run maybe a little earlier than you would otherwise. Decant the used liquor into a poly container with a few cm of KCl crystals at the bottom. Stir thoroughly or simply let it sit a few days so an equilibrium is reached. Decant back into your cell, and the liquor will be adequately recharged with chloride, and by definition it will already be saturated with chlorate. The chlorate will begin to drop within hours rather than days when you work the used liquor in this manner. 2) Avoid current densities out of the normal range. An average MMO mesh will have a surface area 2X the measured rectangle. Off the top of my head I don't remember the numbers, but they should be available on dann2's or Visser's web pages. 3) pH control: I'm not sure of the effect of good pH control on the longevity of MMO. I do know that MMO resists strong mineral acids very well, so it may be "happier" at neutral or below. But again, I'm not sure on this. An alkaline liquor at 9 or 10 may be harmless... or it may be detrimental. Really, if it's just a couple of pinpricks of black, I wouldn't worry. The anode should still look sound, no pitting or flaking. It tends to get a whitish smut but I don't think the smut hurts anything. If it's significant erosion, then something may be wrong. I wish I could help more. Probably the best approach would be to scale up the process if you can afford the components so that you are making more chlorate, faster; I think this will minimize MMO erosion as a % of product created.
Arthur Posted August 24, 2009 Posted August 24, 2009 Electrolysis is best done with sodium chloride! This is to enable the cell resistivity to be as low as possible. If you try to use other solutions the cell resistivity goes up and the cell efficiency goes down. One guy on the UK forum had a LD electrode running at 80 amps. Then someone sold him a sack of perc so he broke the cell for bits!
Bonny Posted August 24, 2009 Posted August 24, 2009 (edited) Electrolysis is best done with sodium chloride! This is to enable the cell resistivity to be as low as possible. If you try to use other solutions the cell resistivity goes up and the cell efficiency goes down. One guy on the UK forum had a LD electrode running at 80 amps. Then someone sold him a sack of perc so he broke the cell for bits! Maybe not as efficient, I intend to make mine "A La Swede" using KCL. That way I don't have to worry about Na contamination at any point in the process. When building a cell, how long can I get away with for the vent hose? I don't want to start punching holes through walls...depending on where I locate the cell. Edited August 24, 2009 by Bonny
Arthur Posted August 24, 2009 Posted August 24, 2009 You need a flow through your vent pipe towards somewhere non corrosive! There was discussion about getting a small "PC" fan and using it to drive a venturi so that you could let the venturi suction arm suck the stink out of the cell, without drawing the fumes through a fan and motor.
50AE Posted August 25, 2009 Posted August 25, 2009 Yell, it has stopped eroding for now. I turn it on while I'm here and I turn it off when I'm going to sleep or I go out somewhere. The current stays at max 8A, which doesn't exceed the limit. Thanks for the info.
Swede Posted August 25, 2009 Posted August 25, 2009 The venturi concept is sound. When you use 6mm or 12 mm tubing, even a 2 meter length will contribute enough back pressure to create a wicked salt creep. A vent hose should be as wide-bored and as short as you can get away with if you are using plain tubing. I think 90% of setups can get away with a short section of tubing vented to the outside through a window frame or similar. Drilling a hole in the wall is not hard at all, and a small 12mm hole will be very hard to see. The gasses need to be vented away from any pedestrians or anyone who might say "WTF is that odor" and call the authorities. If the hole is up high, normal wind and circulation takes care of it pretty well. 50AE, I don't know what your budget is, but you can make a quantum leap if you can find a surplus 5V supply (very common) that can do 50+ amps. With just a little shopping, 50 to 100 amp 5V fixed switching power supplies can be had for $10 to $30... cheaper than a PC supply if you have to buy one.
Bonny Posted August 25, 2009 Posted August 25, 2009 The venturi concept is sound. When you use 6mm or 12 mm tubing, even a 2 meter length will contribute enough back pressure to create a wicked salt creep. A vent hose should be as wide-bored and as short as you can get away with if you are using plain tubing. I think 90% of setups can get away with a short section of tubing vented to the outside through a window frame or similar. Drilling a hole in the wall is not hard at all, and a small 12mm hole will be very hard to see. The gasses need to be vented away from any pedestrians or anyone who might say "WTF is that odor" and call the authorities. If the hole is up high, normal wind and circulation takes care of it pretty well. Anyone have a diagram of how I could make up a venturi using a PC cooling fan? I think to start I will be using a 10 or 20l pail as the cell, and will try and get some 1" tubing for venting. Also would the vacuum created by such a fan create problems with the cell? I'm sure this could easily be remedied with a small intake hole though. I'm guessing I'll need to go 6-8' to hide where my vent line will exit. I know it is easy to drill a hole through the wall, just don't like putting holes into wall when I don't need to...
Swede Posted August 25, 2009 Posted August 25, 2009 Bonny, I don't think it is truly needed in your setup, especially if you are using such a large vent tube. I noticed overpressure + excess salt creep when using a 3/16" ID tube about 8 feet long, with 50 amps or so. I replaced that with a 5/16" ID tube, and that solved most of the problems. Ideally, hard PVC pipe would be best, especially if you joined your cell to the exhaust pipe with a short section of flexible tube. Orient everything so that it drains, as mist and vapor will condense on the walls of the tube or pipe. The issue with venturis is that you need fairly rapid flow through it to generate much vacuum. I'm not sure a little muffin fan could do the job with any sort of efficiency. I should have qualified my statement "The venturi concept is sound" with "when you have an adequate flow through it." All you'd need, though, is enough suction to overcome the drag and restriction of the tubing. Mazzei venturis are used in the hot tub and aquarium industry, and can be picked up with pipe threads moulded in fairly cheaply.
50AE Posted August 30, 2009 Posted August 30, 2009 Swede, I disassembled the cell today. It seemed that the flaking came Swede, I disassembled the cell today. It seemed that the flaking came from the welding points. No visible flaking from the other sides. That's good for now.
Swede Posted August 31, 2009 Posted August 31, 2009 Swede, I disassembled the cell today. It seemed that the flaking came Swede, I disassembled the cell today. It seemed that the flaking came from the welding points. No visible flaking from the other sides. That's good for now. Good! They will wear out eventually; nothing lasts forever. Likely flaking or wear points are like you noticed, the weld spots, where MMO is overheated and mechanically pressed by the weld tips, and the other location might be those areas where bare Ti can be seen, like the edges. But I've not noticed that yet. I get the feeling that MMO these days is made very well... they see tremendous use in many processes besides chlorate, and the MMO technology is mature. Almost everything these days is made from cut sheet, and the cut portions are not re-plated with MMO, so I think there will be few problems.
Swede Posted September 1, 2009 Posted September 1, 2009 For those living in the U.S. I found a reasonable deal on eBay... the price of KCl has gone up a bit, and the big nuggets in the water-softener sacks are neither easy to dissolve, nor particularly pure. The last time I looked, a 40 lb sack of these nuggets was about $20. Here's a guy on eBay selling 25 pound lots of finely-divided KCl, shipping paid, for $25. If I were to guess, it's probably of a superior purity than the nuggets. So if KCl cannot easily be found in your area, or you worry about purity, this might be an option. http://cgi.ebay.com/ws/eBayISAPI.dll?ViewI...em=250460868854 He has some other chemicals and a few other cool things.
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