387 replies to this topic

[ridesideways]

yeah i probably agree with not buying from a random web site advertising KClO4 with not much data backing it up.

another thing that seems to make sense for people desperate to make KClO4 is to start with NaClO3, which should be easily purchased anywhere in the world at a gardening center (weed killer). by starting with Sodium Chlorate, you're at a big advantage over starting with NaCl. because now you don't have to worry about the low-percentage chlorides attacking your Pt anode (there will be none if you start with NaClO3). of course you'll need a dash of of potassium dichromate (easily made if not bought) to prevent decomposition of the chlorates to chlorides as the perchlorate is being made.

maybe that above is moot anyways because if you're willing to go to the trouble of adding the protective potassium dichromate (and then removing it afterward), then you might as well go straight from NaCl to NaClO4 anyways using a Pt anode-- you shouldn't have much anode wear with the dichromate additive.

but if i were making perchlorate for the first time, i would probably start with NaClO3 just to get a head start.

Edited by ridesideways, 05 September 2008 - 08:51 PM.

[knackers]

yeah i probably agree with not buying from a random web site advertising KClO4 with not much data backing it up.

another thing that seems to make sense for people desperate to make KClO4 is to start with NaClO3, which should be easily purchased anywhere in the world at a gardening center (weed killer). by starting with Sodium Chlorate, you're at a big advantage over starting with NaCl. because now you don't have to worry about the low-percentage chlorides attacking your Pt anode (there will be none if you start with NaClO3). of course you'll need a dash of of potassium dichromate (easily made if not bought) to prevent decomposition of the chlorates to chlorides as the perchlorate is being made.

maybe that above is moot anyways because if you're willing to go to the trouble of adding the protective potassium dichromate (and then removing it afterward), then you might as well go straight from NaCl to NaClO4 anyways using a Pt anode-- you shouldn't have much anode wear with the dichromate additive.

but if i were making perchlorate for the first time, i would probably start with NaClO3 just to get a head start.

if only it was so easy, unfortunately Naclo3 / kclo3 is not purchased easily all over the world, i have searched high and low in gardening centres and major/minor one stop hardware centres, for all sorts of chems, and mostly if not all the weed killer and stump removers are Glyphosate based,

if i could purchase Naclo3 /kclo3, i would deffinately go that way,,,

but if i was going ahead to do a lab experiment ( or making it for the first time ) i would start at the begining and observe the complete reaction, "chloride - chlorite -hyperchlorite -chlorate -perchlorate" .....otherwise i would feel i have cheated myself......... and then go the chlorate way if i could

Edited by phill 63, 06 September 2008 - 06:26 AM.

[Arthur Brown]

I can get huge drums of chlorate herbicide locally ( B&Q garden department in the UK) BUT it has a deliberate and unspecified fire depressant additive and is about 50% chlorate. There is no point in electrolysing this chlorate to perc and putting so much else in the cell as well which would certainly clog, maybe poison the reaction.

[digger]

I believe the fire depressant is either sodium metaborate or ammonium phosphates, if that is any help.

[knackers]

it has been quite a while since my last scout around the garden shops, i think an excursion is on the cards,, no doubt i`ve missed a few... ( there are so many chems to keep an eye out for )...... anything worth utelising has almost surely been substituted for an inferior product by our nanny govt in this land of the southern cross,


the unspecified fire deppressant must be the ammonium phosphate, as the sodium metaborate is a pesticide and not a good mixture with a strong oxidiser............ the ammonium wouldn`t pose much trouble to disipate in a boiling solution but the remaining phosphate acid may prove to be more difficult, but like they say,,, where there`s a dill there`s a way , if i find some, it`ll go on my experiments to do list,

[Arthur Brown]

Somewhere the approved formula for the inhibited chlorate must have leaked onto the web. There must be an approved fire inhibitor and a means of testing for it.

[MDH]

Wouldn't they be concerned about the formation of ammonium chlorate?

[seymour]

Perhaps like Ammonium chloride, Ammonium phosphate does not easily form Ammonium chlorate, doe to Sodium phosphate being less soluble than Ammonium chlorate...

May I emphasize "perhaps", please don't go out to your shed and start mixing your chlorates with Ammonium phosphate!

While we are on the Ammonium topic, has anyone out there tried manufacturing their own Ammonium perchlorate from homemade Sodium perchlorate? And if so, what method did you use to destroy decisively any chlorate contamination?

[knackers]

no worrys guys,,,
i wasn`t about to go out to my lab and mix chems willy nilly,, not without some thorough research and cross referencing information

( once i disipate the ammonia off, there will be no ammonia, only acid of phosphate and kclo3 ) but i havn`t got far enough yet to even have sourced any ) i still have enough KP to last me for a while,,
i also don`t realy have the need to do so,, it just sounded an interesting challenge
thanks for the fore warning

oh yea,,,,,, i havn`t manufactured any AP

[digger]

the unspecified fire deppressant must be the ammonium phosphate, as the sodium metaborate is a pesticide and not a good mixture with a strong oxidiser............

However Sodium borate is a cheap mineral and can be used as a fire retardant.

[gilbert pinkston]

"While we are on the Ammonium topic, has anyone out there tried manufacturing their own Ammonium perchlorate from homemade Sodium perchlorate? And if so, what method did you use to destroy decisively any chlorate contamination? "

yes from sodium perchlorate and ammonium nitrate
the ammonium perchlorate will drop out
the chlorate should all be removed BEFORE adding the ammonium salt indigo carmine is the indicator used to make sure all chlorate is removed (although im convinced there are other less exotic dyes that would work and be just as sensitive)
i run a cell until the perchlorate crystalizes out this is vacuum filtered so it contains little chlorate then disolved in a little boiling water acidified and i add "iron out" (sodium-sulphite,hydrosulphite,metabisulphite) which is used to get the iron out of wash water a few drops of indicator is added from time to time to make sure the solution will hold a blue color
this method is much better than HCl alone purification (my old method) for obvious reasons
of course this solution must be brought to pH7 after all chlorate is destroyed
any (which is significant) perchlorate left in solution can be dropped out by adding KCL
the ammonia MUST be removed from this and nessler reagent is really nice to have as an indicator

[Mumbles]

but if i was going ahead to do a lab experiment ( or making it for the first time ) i would start at the begining and observe the complete reaction, "chloride - chlorite -hyperchlorite -chlorate -perchlorate" .....otherwise i would feel i have cheated myself......... and then go the chlorate way if i could

I think that should be chloride - hypochlorite - chlorite - chlorate - perchlorate.

[knackers]

oops, !
i should have written, chloride- chlorine-, hypochlorite- chlorite- chlorate- perchlorate