Sciencemadness Discussion Board

Tutorial for making a miniature chlorate cell

woelen - 24-9-2010 at 13:36

Quite a lot of tutorials are present on the Internet for building chlorate cells, using all kinds of anodes and all kinds of big containers for making hundreds of grams per day or even almost 1 kilo per day. That kind of cells are big, need a power supply capable of delivering tens of amperes and need big MMO anodes and equally big cathodes.

For the home chemist, who just wants 50 to 100 grams of KClO3 for nice fire-demos or small-scale syntheses the construction of those big cells may look rather intimidating.

I made a very small 100 ml cell, which allows one to make 30 grams of KClO3 per day and which can be operated from a simple fixed 5 volt power supply, which only needs to be capable of delivering 5A (the cell itself takes only 3 to 4 A, but using a 5 A power supply gives some headroom and allows for tolerances in construction of the cell). Cost of the cell only is $30, excluding the power supply.

http://woelen.homescience.net/science/chem/exps/miniature_ch...

The potassium chlorate, obtained from this cell is perfectly white, it really is white like snow. For making this cell, I used specially made anodes, made by our own sciencemadness member Swede. See the webpage for more info.

[Edited on 24-9-10 by woelen]

aonomus - 24-9-2010 at 13:56

Link to the actual project page: http://woelen.homescience.net/science/chem/exps/miniature_ch...

mr.crow - 24-9-2010 at 14:32

Great article! Its a shame about the bromate not working.

I am going to try making a chlorate cell this weekend using a normal scale eBay anode.

Contrabasso - 25-9-2010 at 02:46

The electrodes are critical and Swede has done lots of research into materials sizes and types to get good cell performance. He has shared his research so please don't waste the shared wisdom.

Some people found that glass containers were not best suited, and also found that power supply interruptions were very bad for the cell integrity. However this was found in larger cells running 50 to 100 amps into a large enough cell to run around the 75C mark.

woelen - 25-9-2010 at 09:54

Power supply interruptions for longer time indeed are very bad. A short interrupt for a few tens of seconds for topping up liquid level does no real harm, provided one uses titanium cathodes.

I did not know of the problem with glass. I myself don't have any problems with this, but I'll change the page and mention the problem with glass when larger cells are used. I'm quite sure this has to do with high pH, which leads to dissolving some of the silicate in the glass, which can settle at the electrodes. I, however, never allow my electrodes to get dry. I take them out of the glass jar and immediately transfer them to a beaker full of tap water. That probably greatly helps preventing the buildup of a silicate layer on the electrodes.

I also did another experiment. I have been running the cell, but now without any cooling. The glass container became so hot that I could not bear touching it. But the current efficiency is better. Already 18 hours after power on, there was a quick transition of just a little oxygen production at the anode to very fast oxygen production at the anode. This means that almost chloride has been used up at that point and that the cell simply decomposes water (MMO anodes don't make perchlorate, they simply make oxygen at the anode). In order to test my hypothesis I added a few grams of KCl, dissolved in a few ml of boiling water. Almost immediately after adding this KCl, the production of gas at the anode ceased, until after an hour or so the production of gas at the anode was quite fast again.
So, running the cell really hot is tempting from a point of view of current efficiency, but it also puts more strain on the anode and the overall cell construction. For next runs, I'll use some cooling again, I just did this single experiment to see how much of a difference it makes.

[Edited on 25-9-10 by woelen]

mnick12 - 25-9-2010 at 10:55

Now I know this is not directly related, but it is similair and does not deserve its own thread. Regular bleach is about 5% NaOCl and often times has detergents mixed in, and pool chlorinator is usually about 16% NaOCl with lots of impurities. And as you all know electrolysis of NaCl solutions first forms NaOCl which dissasociates into NaClO3 and more NaCl. So I am interested in modifying a chlorate cell to produce concentrated NaOCl solutions. How would I go about doing this? Would simply keeping the solution cold produce hypochlorite, or are there other factors? I have made a few pounds of sodium and potassium chlorate from a Co3O4/NiO coated Ti anode, but I am not quite sure how to produce the hypochlorite alone.

Oh and the reason why I am asking, is I plan on using the hypochlorite for various organic oxidations as it seems to be cheap and has good yields.
Thanks!

woelen - 25-9-2010 at 11:39

The web page is updated. The remark of Contrabasso on the use of a glass bottle is put in the webpage and also the results of the third run without cooling are mentioned in the webpage.

@mnick12: I do not think that making hypochlorite is possible by simply keeping the cell cold. As I wrote in my webpage, when the hypochlorite cannot be converted to chlorate in the liquid (either by low temperature, or by too high pH), then hypochlorite ions are oxidized to ClO radicals and these recombine and react with water to give chlorate, chloride and oxygen. So, when you keep the cell cold you also get chlorate, albeit at a lower current efficiency.

If you really want to make hypochlorite of decent purity, then I think that a much better way is to bubble Cl2 through a solution of NaOH until no more Cl2 is absorbed. For stability you then can add a little amount of NaOH again in order to bring up the pH, such that all hypochlorite is present as ClO(-) and not as HOCl.


12AX7 - 26-9-2010 at 21:23

I discovered the same problem with bromate. I once attempted to use a platinized titanium anode, which promptly resulted in a large mess of white goo.

Tim

metalresearcher - 27-9-2010 at 07:30

Ten years ago I made some KClO3 with success from diet salt (2 parts KCl + 1part Nal), it is rather pure.
See on www.metallab.net/KClO3 .
But thiis method without carbon anodes will be better.

Contrabasso - 27-9-2010 at 11:04

The industrial process for Perc is in two parts, First the chloride is electrolysed to chlorate, this is then purified. In a separate cell chlorate is electrolysed to perchlorate using precious metal electrodes. Think big batches and very big currents!

woelen - 18-10-2010 at 01:48

Last weekend I used my miniature cell for making CsClO3. The key to success with CsClO3 is not to use too concentrated solutions.

CsClO3 can be made from CsCl just like KClO3 can be made from KCl. With KCl you have to make a more or less saturated solution, with CsCl that will lead to coverage by crystals and blocking of the electrodes.

A good concentration is to take 40 grams of CsCl and dissolve that in water, such that 100 ml of solution is obtained. This solution can be electrolysed until the current drops to just a fraction of the initial current. At that point more than 90% of all CsCl is converted to CsClO3.

There are more differences with KCl. You cannot simply add some K2Cr2O7 to the solution of CsCl. It gives a nasty sticky precipitate of Cs2Cr2O7, which does not dissolve. Instead, you must dissolve just a tiny amount (e.g. 20 mg) of K2Cr2O7 in a few ml of water and add this solution to a hot solution of CsCl and stir. The resulting liquid then is yellow.

The following procedure can be used to make CsClO3. I have done it a few times and it works like a charm:

- Take 40 grams of CsCl and add 60 ml of very hot water. Dissolve all of it and if necessary, filter the solution.
- Dissolve a tiny amount of K2Cr2O7 in a few ml of water. Bring this to a boil.
- Add the boiling hot solution of K2Cr2O7 to the hot solution of CsCl and stir.
- Top up to 100 ml and stir to make the solution homogeneous.
- Start electrolysis and measure the starting current.
- Assure that the cell remains rather hot. If the electrolysis process does not provide enough heat, then use external heating. However, usually the process provides enough heat from itself.
- Keep on electrolysing until the current has dropped to just a fraction of the starting current. This may take a long time, depending on the initial current. At a current of 1 A this may take two full days. During the process it might be necessary to top up the cell with hot water. Only do this when the volume drops below 80 ml. Then top up to 90 ml.
- If no external heat is applied and the cell runs sufficiently hot from itself, then you can also notice the end of the process by cooling down of the cell.
- At the end of the process there will be a lot of crystal mass at the bottom.
- Disconnect the electrodes and allow the cell to cool down slowly to room temperature.
- After cooling down, put in the fridge to allow further cool down to 0 C or even colder (but it should not freeze).
- Decant the yellow liquid from the crystal mass as good as possible.
- Take a heap of paper tissue and put a coffee filter on it. Put the crystal mass on the filter and allow liquid to sock in the filter and paper tissue. Repeat this step one or two times.
- Recrystallize from 50 ml or so of boiling water. Assure that ALL crystals dissolve. Add portions of 10 ml of water until all crystals have dissolved.
- Allow to cool down, decant liquid, make dry on filter paper and tissue, and then rinse with ice cold water and dry another time on a fresh filter and paper tissue.
- Give a final dry at a warm place for one day (e.g. on a heating radiator for one day).

Yield of this procedure: 80%, based on CsCl, approximately 40 grams of CsClO3.

If all the rinsing water and the yellow liquid are kept, then the Cs in that also can be recovered partially. In total, I had 140 grams of CsCl available for this experiment. I made 145 grams of CsClO3 from that and from all the rinse water and so on, I also recovered approximately 20 grams of CsClO4 (by treating that with a solution of NaClO4). So, in total I lost approximately 10% of all Cs, most of that being lost in the coffee filters and the liquid, absorbed by the paper tissue. It is fun to let the coffee filters dry and then light them with a cigarette lighter. The burning of the coffee filters is quite spectacular :)

[Edited on 17-4-12 by woelen]

12AX7 - 18-10-2010 at 08:02

How's the flame color, do we get a video?

woelen - 8-11-2010 at 05:29

I tried making a video of the burning of a mix of CsClO3 and sulphur and also one of burning a mix of KClO3 and sulphur. The resulting video is disappointing and does not render the nice colors which I can see. The flame simply is over-exposed and white. I'll have to wait for a bright day and make a video on that day. My problem is that the camera takes average brightness and while the background still looks OK, the flame is way too light. Unfortunately, over here the days are very short now (I go to work in darkness and come home in darkness), so the bright day must be a weekend day.

The flame color of a CsClO3/S mix is blue/purple. It is not purely blue. The flame color of a KClO3/S mix is more pinkish, but it also depends on the amount of sulphur in the mix. When excess sulphur is used, then the color is more blue.

My idea is to make a mix of CsClO3 and S and a mix of KClO3 and S. Then CsClO3/S mix is put in the form of a line (5 cm length, 5 mm width) and adjacent to this the KClO3/S mix is put in the form of a similar line. Then I light the total line on one side. Then you first see the color of the burning of the CsClO3/S mix and then you see that color change to the color of a burning KClO3/S mix. I also might add a line of Ba(ClO3)2/S mix to this (my next project is making Ba(ClO3)2 from BaCl2, I am in the process of acquiring appr. 1 kilo of BaCl2).

[Edited on 8-11-10 by woelen]

12AX7 - 8-11-2010 at 10:37

It might help to burn the compositions in front of a white screen, to reflect the light and brighten the scene.

Tim

Arthur Dent - 14-8-2011 at 07:41

Sorry to revive this antique thread but I have a question for Woelen about the material used for this cool cell project.

Being a cheapskate, I was wondering about the Titanium / MMO electrodes. I have secured a good-sized sheet of metallic titanium (top cover of an old G4 powerbook). So my titanium cathode is good to go.

Now about the MMO anode, could I use instead Platinum wire? I happen to have two spools of "Platinum alloy" wire and was thinking of wrapping a lenght of it on a glass canule...

I imagine that the reason Titanium isn't used as the anode material is that it's attacked by the electrolysis and generates Titanium Chloride?

And if I recall, carbon anodes are very good and inert but have this unfortunate tendency of slowly disintegrating and mixing carbon residue and bonding agents with the resulting chlorate...

Anyway, just a few vague questions on the anode material. I was thinking of trying out this experiment and since I have a fair amount of Ti and a good power supply, my last hurdle was to find an alternative to the purchase of a ready to use mixed-metal-oxide anode.

I have about 400 g of Potassium Chloride to use in my future cell so I have many of the main ingredients to get this project going.

Robert

cyanureeves - 14-8-2011 at 14:00

arthur i know you summoned woelen in specific but i think titanium as an anode just stops conducting altogether after a while.nurdrage does that mmo with the stuff made from battery crud. i have gotten as far as making the battery crud manganesee sulfate stuff but stopped because i still needed cobalt nitrate for the first coat.you got two spools of platinum wire? wow i wouldve tried it out with a two inch piece for sure and i'm sure that even though its platinum alloy its still expensive. i also think i will invest on some mmo electrodes or plated ones. well i will wait on woelens response to you as well.

[Edited on 14-8-2011 by cyanureeves]

m1tanker78 - 14-8-2011 at 14:34

I've never had a problem filtering out the carbon crud from gouging rods. Each lasts many dozens of hours, or hundreds. Maybe I'm missing something but graphite rods are the perfect solution for a HC who wants to make chlorate on the cheap, seems to me.

Tank

cyanureeves - 14-8-2011 at 17:00

hey tank.i am using carbon rods from a 6 volt battery but i saw some graphite rods on ebay and thought about buying one . are graphite rods way better than the carbon rods? i googled how to make chlorate and a fella there called 6volt battery rods, graphite. this is not correct is it?

m1tanker78 - 14-8-2011 at 18:42

Reeves, I've never tried with battery carbons. I use 'graphite' gouging rods although I think that's also a misnomer. By my eyeball, they seem to be a mixture of graphite, carbon, probably clay and who knows what else. I can make 'pencil' marks on a rough surface with some difficulty. They even hold up pretty well in my sodium cells (consumable item).

Check your local welding supply stores to see what sizes and pricing they offer. Virtually all have copper cladding that's easy to remove in a dummy chlorate cell. Again, the little bit of stuff that does shear off is very easy to filter with frit or similar.

Real graphite is very soft and easily marks almost any surface. I can't say from experience if these graphite rods provide any real advantages over gouging carbons. If the price is right, go for it.

Tank

dann2 - 15-8-2011 at 05:32

Quote: Originally posted by cyanureeves  
.........battery crud. i have gotten as far as making the battery crud manganesee sulfate stuff but stopped because i still needed cobalt nitrate for the first coat........
[Edited on 14-8-2011 by cyanureeves]


You don't need Cobalt Oxide (from Cobalt Nitrate) as a first coat. Mn Oxide on it's own is fine. The Cobalt Oxide may even be a disadvantage. Cobalt Oxide lasts only a short time in a Chlorate cell, even less time in a Perk. cell. Use any spare money, time or energy that you may have putting on extra MnO2 coats.

Dann2

cyanureeves - 15-8-2011 at 14:25

thanks tank, thanks dann2.

Arthur Dent - 16-8-2011 at 03:22

I do have some graphite rods (I picked-up a box when I was a projectionist at a movie theatre) so I might try to use the combination of a Titanium cathode and a Graphite anode.

As for the container, I was thinking of using Silicone caulking to seal the electrode contacts and the glass vent tube on the top cover for a really airtight container and drive the resulting gases through a vinyl tube. Has anyone tried Silicone caulking, the bathroom tile joints kind? Does it resist the temperatures generated by the cell?

The cool part about graphite rods instead of carbon battery rods is that these graphite rods are extra long and when one starts to shorten because of degradation, you just push it a little further down in the solution. (the principle of the carbon arc light in these antique movie projectors, except it was a notorised insertion system that slowly pushed the rod for optimal arc).

Of course the platinum wire would be best but i've been scratching my head as how to use it effectively in a cell by wrapping it around something inert and heat-resistant.

Just thinking aloud. it would be great if I could use the materials I have at my disposal, it's just a bit of mechanical engineering I have to come up with...

Robert


[Edited on 16-8-2011 by Arthur Dent]

sternman318 - 16-8-2011 at 09:12

Quote: Originally posted by Arthur Dent  

Of course the platinum wire would be best but i've been scratching my head as how to use it effectively in a cell by wrapping it around something inert and heat-resistant.



Scroll down to the section on electrodes
http://woelen.homescience.net/science/chem/exps/KBrO3_synth/...

m1tanker78 - 16-8-2011 at 19:00

Robert, I've had good results with rubber grommets. If you want to mechanically fix the electrodes to the cell, liquid nails is the best I've used so far. JB weld (actually, most 2-part epoxy) won't stick worth a damn to plastic unless it's pre-conditioned.

If you keep the temp, pH, chloride, etc. in check, your gouging rod(s) will complete several batches without having to readjust the depth. I rigged up a crude electrolyte drip delivery system and it worked great at keeping the cell running at optimized levels.

The crude liquor looks like crap but once run through a fine frit filter, you have crystal clear, yellow-tinted Chlorate liquor ready to convert to potassium chlorate (if desired).

Must be nice having platinum wire at your disposal. :D

Tank

cyanureeves - 29-8-2011 at 17:43

dann2 is manganese dioxode really enough and no need for cobalt nitrate? i would rather bake the manganese on than electroplate the anode because nurdrage's flaked off.

plante1999 - 29-8-2011 at 17:47

Cobalt oxide form an inaderant coating for other oxide so It is normal that The MnO2 flake of.

cyanureeves - 29-8-2011 at 18:12

then i will be aroastin some titanium soon.

cyanureeves - 5-9-2011 at 18:07

thank you for the u2u dann2. what i read is exactly what happened today, that is i made a power source from an old apple g3 and forgot to mark the positive lead. the titanium anode stopped working so my titanium manganese dioxide electrode which was mistakenly the cathode, just sat there and peeled on its own and turned the solution pink. my homemade manganese nitrate baked just fine. i used a s.steel pan with a propane torch underneath. the titanium turns grey while its being baked then turns black before releasing the nitric fumes.good thing the manganese carbonate i made a couple of months ago has more manganese than the one i made two weeks ago.damn battery paste just sat in my filter and didnt release enough pink liquid last time i made the manganese sulfate. i suspect the ebay source of oxalic acid to be udultered.

[Edited on 6-9-2011 by cyanureeves]

dann2 - 6-9-2011 at 08:17

Quote: Originally posted by cyanureeves  

........ i used a s.steel pan with a propane torch underneath. the titanium turns grey while its being baked then .....
[Edited on 6-9-2011 by cyanureeves]


Fried you mean!!!!!!!!!!!!

Good that it worked. The MnO2 Anode is definitely a great Anode.

There is a guy back selling cheap MMO below:

http://www.ebay.com/itm/EXPANDED-TITANIUM-MESH-STRETCHED-SCR...

Dann2

cyanureeves - 18-9-2011 at 12:53

hey dann2 i got ahold of that guy on ebay. his product is like nothing i have seen before. it has been going for a week now. i havent produced much chlorate because i still need to learn more on how to make it. the liquid grows needle crystals when i let it sit overnight and they burn a purplish color. now i read that a switch mode power supply works too. there are some 5v. 3amp switch modes on ebay for $9.50. would they work?

plante1999 - 18-9-2011 at 13:42

I strongly recomend 3.3 to 3.7V and , a funny thing , I think I juste buy 6 day ago the same anode as you on ebay , I am in canada so the shiping should be somewath long.

cyanureeves - 18-9-2011 at 16:45

3.3 plante? i just happen to have exactly 3.3 volts coming out my old powermac g3. i will try 3.3 then. that guy on ebay sells mostly mmo screens by look of his selling history. i got plenty of screen. 6 by 10 in. and my mayo jars could only take a 2 by 4 in. pc. something chewed the inside of the jar because its pitted pretty bad. i put the guy on ebay on a favorite list and got no notice,good thing i came back here and used dann2's link.

plante1999 - 18-9-2011 at 16:56

You should check the composition of your mayo jar because I think your mayo jar is made in Pet (polyethylene tetraphtalate).

You should use glass polypropylene PVC or Clear PTFE.

Personaly I prefer Polypropylene because it is unbrakable and common but I use glass because I dont find suitable Polypropylene . The best is Clear PTFE but PTFE is very uncomon.


I buy this:

http://www.ebay.ca/itm/EXPANDED-TITANIUM-MESH-STRETCHED-SCRE...

[Edited on 19-9-2011 by plante1999]

cyanureeves - 18-9-2011 at 17:17

i bought from the same guy. that screen was hard as hell to cut even with tin snips. good thing you are here plante because i want to ask why you recommend 3.3 volts when most everywhere use 5volts. is it because it preserves the anode longer or does it produce more chlorate or is it because it will run cooler?

plante1999 - 19-9-2011 at 04:57

3.3V is optimal because it preserves the anode longuer run cooler and you use less energy. Industry use 3.3V.

dann2 - 19-9-2011 at 06:32


Don't be obsessing over the 'proper' Voltage needed to run a Chlorate cell. Most guys (including myself) build shitty Chlorate cells and if you place a 3.3 Volts power supply (capable of supplying 50 thousand Amps) accross them, you will get a damn small current flowing.
Think in terms of current density on the Anode and let the Voltage go to F*&%.
Most guys 'use' 5 Volts because they are using a computer power supply and they are forced to present the '5 volts' to the cell.
When using a computer power supply you can have any Voltage you like so long is it's 5 Volts (a similar suituation arose regarding the colour of the Ford model T car).

Stop obsessing over the 'best', 'proper', 'essential' etc, etc, Voltage accross cells.
There is a certain minimum Voltage that you will need in order to get a descent or proper current flowing through your shitty (like mine) Chlorate cell.

Dann2

[Edited on 19-9-2011 by dann2]

cyanureeves - 19-9-2011 at 15:52

thank you again dann2 and plante. i have let the voltage go to f*&%ing h@ll for now at 3.3 volts. i was thinking more in bubbles than current density really.

plante1999 - 19-9-2011 at 16:27

Curent density is very important for an anode. It will degrade very readily if you dont check it.

plante1999 - 21-9-2011 at 14:12

I have found my anode in my boxmail!!!




I will make my Sodium chloride to chlorate cell in few minutes , I will post a picture when it will be finish.

cyanureeves - 21-9-2011 at 14:30

wow! do you mean table salt? are you going to boil it first? i even liked the smell of the mmo when i first got it. by the way i lowered the voltage to 3.3 on my cell and was only getting teenie bubbles because i was using a single thin copper wire for connections. my power source started getting really hot and i ran it like that for a whole day, the following day i added another strand of wire and i got bubbles galore and my power source cooled down a bit.i still havent dropped much salt but i know the solution has a lot of chlorate because coffee filter saturated in the solution will burn like a firecracker fuse when dried.

plante1999 - 21-9-2011 at 16:06

I made my first cell with mmo anode , I run with 28% NaCl sol. , but with an exess of it on the bottom of my cell. This will make the solution satured from the start to the and of the run , I also ad 60g of Na2CO3 to get rid of the starting hypochlorite smell and by this way reduce the effiency of the cell.

You can see my big high quality 1963 , plain aluminium , varriable power supply . It cost my 30$ CAN but I imagine the price when it was made....It was new when I buy it and in original box.




[Edited on 22-9-2011 by plante1999]

[Edited on 22-9-2011 by plante1999]

plante1999 - 23-9-2011 at 04:07

I dont know how but at 3.5V approx I passivated my first anode , so I made a second cell....Hop it will not degrade.







metalresearcher - 23-9-2011 at 09:03

Nice! But where do you use the Na2CO3 for ?
Last January I prepared 200g KClO3 from diet salt 2 parts KCl and 1 part NaCl.

Here my results

www.metallab.net/KClO3.php

plante1999 - 23-9-2011 at 14:59

After 22h of run the anode seem okay but the Stainless cathode make rust where it is not immersed and the rust flake of in the solution.

cyanureeves - 23-9-2011 at 17:34

dear chlorators,i have a cell that has been running for three days on 3.3 volts and today i took out some salt that dropped to the bottom which i will burn tomorrow to see if it is chlorated. how long should i let it run before i let it cool so it will drop more salt? should i chill the solution or evaporate it? if i let it cool and extract the precipitate will i get more afterwards if i evaporate the solution some or would it be best to electrolyze it more and repeat the procedure?is it possible to over do it on the zapping time? last year i dropped more salt with carbon rods and a cell phone charger. the only thing i did different this year was to use tap water instead of distilled water to first boil then collect the precipitated salt which i am using. i am getting much cleaner salt though and the cell does have distilled water.

plante1999 - 23-9-2011 at 17:51

Does your cell heat more than 40 degree celcius if yes , simply ad 28% salt solution to replace the evaporated water , if no boil the solution to 3/4 of its volume and ad 28% sol. of salt to replace the 1/4 that you have boiled of and continu the electrolisis. It should greatly help. Could you post some picture of your cell?

I will update a page about making NaClO3 on my website , I made a rough draft.

http://hclo3chem.weebly.com/naclo3-sodium-chlorate-making-el...

[Edited on 24-9-2011 by plante1999]

plante1999 - 24-9-2011 at 13:07

If it is so hot you only need to re ad time to time satured salt sol. and chlorate will precipitate.

sternman318 - 25-9-2011 at 19:17

I saw the same listing for the mmo anode and long story made short, I had to buy it before I could get an update on how they were holding up. So i guess I might as well ask now, how have they been working so far?

here is the ad: http://www.ebay.com/itm/EXPANDED-TITANIUM-MESH-STRETCHED-SCR...

cyanureeves - 26-9-2011 at 15:50

sternman318 the mmo i got from that fellow has been making a million bubbles for 2wks. now. i havent made much chlorate because i'm still learning voltage and overheating and stuff but the mmo is going strong. the guy is hiking the price since last time i bought and some pcs. are getting smaller.

dann2 - 26-9-2011 at 18:21

Quote: Originally posted by cyanureeves  
...............now. i havent made much chlorate because i'm still learning voltage .................






On the MMO. The seller did not realize it had MMO on the Ti at all. Someone told him it had MMO on it as he was just selling it as 'Ti mesh' (and for stone noting too!!)

Dann2

hope I'm not banned for the yellow thing?

cyanureeves - 26-9-2011 at 18:53

i understand now why titanium is used for anode. as the mmo wears away,the titanium is exposed and titanium passivates when used as anode so it does not conduct and therefore wont erode leaving only the mmo coating as conductior. this came to me as i was thinking of using the platinum coated discs from my apple g3. any scratch on the disc will just give way to almost instant erosion, if it is even platinum.(damn freakin space bar on my apple keypad sticks like crazy)

[Edited on 27-9-2011 by cyanureeves]

plante1999 - 27-9-2011 at 08:14

My cell is going good but i think I will attemp Calcium chlorate cell soon , Dan2 does your anode made from tin/antimony solder make residu in the solution ?

I will probaly make KClO3 but the kclo3 source I found cost my 7$ for 312g so it is a little to high.

dann2 - 27-9-2011 at 10:20


The Tin Oxide Anode does not leave any residue but it appears to be no good at making anything even though it lasts a long time.



Dann2

ryan0713 - 27-9-2011 at 15:00

I liked the article. I might try it.

cyanureeves - 27-9-2011 at 16:07

plante i am using hi-yield brand muriate of potash. it is dirty as hell with some red clay stuff but i have made chlorate with it before. you just have to filter it and you get more than three pounds of it for your 7 dollars. something is wrong with my 5volt output wire because it gets too hot too quick and too bad because as it gets hot and starts bubbling i can see it making instant chlorate plumes.i got one mean,mean,nasty punch out of the wet anode when i had it on 5volts.

[Edited on 28-9-2011 by cyanureeves]

m1tanker78 - 27-9-2011 at 16:20

Quote: Originally posted by plante1999  
My cell is going good but i think I will attemp Calcium chlorate cell soon


How will you deal with the calcium hydroxide buildup on the cathode?

Tank

cyanureeves - 27-9-2011 at 16:31

how about using ice melting salt?some have potassium chloride,sodium chloride,calcium chloride and urea.

plante1999 - 28-9-2011 at 07:57

Quote: Originally posted by m1tanker78  
Quote: Originally posted by plante1999  
My cell is going good but i think I will attemp Calcium chlorate cell soon


How will you deal with the calcium hydroxide buildup on the cathode?

Tank


I will scrap it of in the solution time to time .

When y go see my cell it was realy acidic and a lot of crust was on the cathode....?

plante1999 - 30-9-2011 at 08:08

I just started a KCl to KClO3 cell. Dan 2 : Why it does not make anything?

Chemistry Alchemist - 1-10-2011 at 18:20

Im sorry if its a bit of a change of subject but this forum post is on chlorates so i though i could quickly ask this...

What type of Oxidizing agent should be used to oxidize Calcium Chloride to Calcium Chlorate?

cyanureeves - 2-10-2011 at 05:55

ChemistryAlchemist isnt voltage what does that or is it amperage? speaking of amperage(ha ha), is amperage what makes my chlorate cell melt the epoxy and cap? i am running of a computer power supply and have to use the 3 volt lead because the 5 volts will just get too hot after 2hrs. my electrodes are about 1/2 inch apart. 3 volts is just too slow. i would like to run at 5volts but want to know if there is a way to drop the amperage on my 5 volt leads? arent there inline amperage lowering thingamajiggers that can be added?my other cell is doing better with an old 6volt 250ma charger.somewhere i saw that a person used a car battery charger with a nichrome heating element coil to reduce voltage. if one lowers voltage with a nichrome wire,wont amperage drop too?

[Edited on 2-10-2011 by cyanureeves]

Chemistry Alchemist - 2-10-2011 at 06:43

On the wiki page it said that you can use a oxidizing agent...

"It can be formed by oxidation of calcium chloride by a strong oxidizing agent."

http://en.wikipedia.org/wiki/Calcium_chlorate

m1tanker78 - 5-10-2011 at 17:23

Quote: Originally posted by cyanureeves  
[...]arent there inline amperage lowering thingamajiggers that can be added?my other cell is doing better with an old 6volt 250ma charger.somewhere i saw that a person used a car battery charger with a nichrome heating element coil to reduce voltage. if one lowers voltage with a nichrome wire,wont amperage drop too?


Reeves, you can try adding some more space between the electrodes first. If that isn't an option, why don't you build another cell and connect it in parallel?

Nichrome wire - any resistance, really - will dissipate (waste) some energy as heat. You might as well put it to good use by adding another cell in parallel, IMO.

Tank

cyanureeves - 5-10-2011 at 18:14

ooh! thank you tank. you are certainly correct about the waste and i just happen to build another cell.parallel would be jumping from the neg in #1 cell to neg in #2 cell with a jumper wire and likewise pos to pos? i never would have thought of doing that even though i now recall reading your post on a similar matter before. series would be neg from#1 cell to pos in #2 and neg in #2 cell to pos in#1 cell ?

Chemistry Alchemist - 14-10-2011 at 02:41

I just saw a video on youtube about making a 250ml solution of water with 90 grams of iodized salt and placing a 9 volt battery in the solution and leaving it... it produces Sodium Chlorate... is this true? i know its made by electrolysis but can this method be true? Is it a safe method of making it?

http://www.youtube.com/watch?v=AokqCrFqLWs

Steve_hi - 14-10-2011 at 03:11

I guess the best way to find out is try it it's pretty simple i'm going to do it when I get back I like your you tube on producing Naoh by electrolysis

Chemistry Alchemist - 14-10-2011 at 03:48

Yeah i guess i could check it out, no harm in trying i guess... can you over electrolysis it... if u know what i mean... yeah thanks for checking it out :)

ScienceSquirrel - 14-10-2011 at 05:15

I might be wrong as it is decades since I did any electrochemistry but;

According to this a 9V battery is good for about 300 to 600 mAh

http://data.energizer.com/PDFs/522.pdf

Let us assume that it is 600mAh ( best case scenario )

Then it will produce 2160 Coulombs

http://en.wikipedia.org/wiki/MAh

Using Faraday's 1st law

http://en.wikipedia.org/wiki/Faraday%27s_law_of_electrolysis

I make it that the best case yield is 0.79g of chlorine or 11 millimoles of molecular chlorine!

It requires 3 moles of chlorine to make 1 mole of sodium perchlorate so assuming 100% yield we would end up with around 1.17g.

nomcopter - 8-8-2023 at 21:20

Quote: Originally posted by woelen  

I made a very small 100 ml cell, which allows one to make 30 grams of KClO3 per day and which can be operated from a simple fixed 5 volt power supply, which only needs to be capable of delivering 5A (the cell itself takes only 3 to 4 A, but using a 5 A power supply gives some headroom and allows for tolerances in construction of the cell). Cost of the cell only is $30, excluding the power supply.


Love the tutorial - and have had good success making one with a platinized titanium anode and a titanium cathode I made by bending a 12 gauge titanium wire into a nice mesh. Why is it so important to remove the crystals with a plastic spoon? Are you worried about contaminating the product with metals (a fuel) and that leading to a fire risk? Aren't they already contaminated with a fuel from electrode corrosion?

Started the recryst of my first batch, used 1.6mol of potassium chloride in a 250mL schott duran bottle and did 50 hours at 8A. This should have left ~80g/L of chloride left according to https://www.chlorates.exrockets.com/table54.html assuming 54% current efficiency. But all the chunks didn't dissolve until I'd boiled it in more than a liter of water and boiling it in 1.5L still wasn't enough to make it a clear solution - it was still quite turbid and overall white. Theoretically 1.6mol of potassium chlorate should dissolve in ~370mL of water. I can't imagine I have _that_ much perchlorate production. Perhaps it is titanium dioxide contamination from corrosion of my cathode..?

woelen - 8-8-2023 at 23:11

The liquid is quite corrosive, and if you scrape the crystals out of the container with a metal spoon, then this might damage the metal spoon. It adds additional impurities to the KClO3, and it spoils the spoon. No need to worry about adding fuel in the form of metal ions, but adding additional impurities never is a good thing, hence the use of a plastic spoon.

If the liquid remains turbid, even at quite high dilution, then I'm quite sure that you have some contaminant in your solution. It might be TiO2 from one of the electrodes, it also could come from the KCl you used. Sometimes, anti-caking agent is added to KCl, which is intended to be used as salt-replacement. There also is KCl, intended to be used for melting snow on roads. This is used in places, where NaCl is too harmful for plants. Such KCl, however, is impure and may contain MgCl2 or CaCl2.
I would just let all of the solid matter settle at the bottom and decant the clear liquid from it. The clear liquid then can be worked up for the KClO3.

nomcopter - 8-8-2023 at 23:36

Aha you are totally right - it's tricalcium phosphate listed right on the bag as an anti caking agent. My electrodes looked pretty untouched I was shocked at the volume of white fluff. Well at least hot-filtering/decanting is a lot easier when it is super diluted and then I can boil off the excess. Thanks for the tip! Love your home science website - great explanations I've used it a lot for reference and to come up with fun ideas.

One change I recommend to your procedure is to make the holes in the cap by heating the tips of the electrodes with a blowtorch and then melting it through. Ends up making a hole that is a perfect fit and is less dodgy than with a knife.

[Edited on 2023-8-9 by nomcopter]