387 replies to this topic

[knackers]

Firstly, if anyone is making 50kg aday of o4 with 80amps it must be a huge cell !! ' now secondly and the reason i'm in this forum. I viewed on one of wouters pages the mono and rombic crystal structure of kclo3 and kclo4, when i harvest my 'kclo4' from my ni substrate pt anode and ti cath cell it looks rombic ( visual not microscopic) but when i boil it in hcl and bump it with naoh it always seems to end up flat squareish mono crystals indicating present kclo3 according to wouters crystal definitions, although methylene blue tests indicate kclo4 is present, (yet the crystals are mono) i have done a rudimentary test of my ''kclo4'' with sucrose and con h2so4 and it burst into quite spectacular purple flames indicating kclo3 and i was wondering if anybody else gets mono crystals after purification, ( i know mine is not purified ) could it be mine has not finished the electrolysis cycle, mind you it has all ptt out of sol in the cel with a pt anode

[knackers]

Disclaimer,``Me again``, i am not a phycisist or a chemist and the following text is only a very small unscientific snippett of a complex science and is meant for the person whom has researched this topic and is still unshore of when perchlorate is present in their cell............. As the non professional pyro enthusiast i am, i find myself drawn into the intriege and excitment of producing my own k perchlorate, ` living in australia also necesitates the said activity`, on trolling through countless excellent( net ) information i arrived at the stage where i knew absolutely everything about nothing, exspecialy how to just simply make it, so i went in, `alone`, and this is what i found---> ( for the scratcher) carbon rods are not worth the trouble, they disolve too rapidly and the hassle of cleaning out your electrolyte for very little product is a pain in the butt, and i didn`t have much joy with cooking it to self oxidation and was extra work ... for the sake of about $80au, / 35 euros, i bought a pt anode and ti mesh cath,and felt better for it, in my ½ gal cell i run between 5--->6 volts and 6--->7 amps.....after a couple of days i had ptt happening and then it started to form more rapidly untill i had so much i started to scoop it out whilst topping it up with a saturated kcl sol, then i tried boiling it in dilute hcl for 30 min to purify it, cooling it and bringing the ph up to about 9, i washed it, dryed it then tested it and found i had no kclo4, only less kclo3, so i left it in the cupboard and kept on doing what i was doing untill i had about 1.5 kg / 3.3 lb of kclo3, then tried the auto ox , but still no purple ptt with methylene blue sol (`` still`` no perc ) so i put about 500g back in my cell and ran it for another week stiring it 2ce daily, then i noticed the ptt had turned from a rough salty looking chlorate crystal into a fine creamy iceing sugar looking crystal which was also very soft and smooth to touch and my methylene test instantly turned in to a beautifull lavender coloured purple... and waa laa !! Perchlorate.yeee—haawww!!!..... so the moral of my story is, don`t bother with carbon/graphite,, its a waste of time and effort, i can`t speak for mmo or lead oxide, but for a small outlay its much easier to do it all in one with no mess using pt, run time is alot longer than i thought and amp hours for a ½ gal cell ( acrylic latch type) 5--6 volts, 6 ½ amps continuous for about 2 weeks + or untill ptt turns from a abrasive crystal to a creamy smooth iceing sugar crystal..... `` but `` your product WILL be contaminated with chlorate still and should be handled / purified accordingly

[gilbert pinkston]

gilbert here
someone once wrote

"carbon rods are not worth the trouble, they disolve too rapidly don`t bother with carbon/graphite"

glad i diddnt know that before i converted 3 40# bags of NaCl to NaClO3 with (real) graphite not welding rods
in a properly run cell (as i have said many times but nobody wants to believe) one pound of graphite erroded will produce hundreds of pounds of chlorate
i used NaCl because i quicky recognized the disadvantages of starting with the potassium salt... for one the immensly more soluable NaClO3 produced allows for the graphite to settle out eliminating the need for filtering
then there is the soluability problem with KClO3 to KClO4 not to mention that for proper purification all products of the cell must be in solution and KClO4 is not very soluable meaning a huge amount of water must be used in the process compared to what is needed when working with sodium compounds

"then tried the auto ox , but still no purple (perchlorate)"
what can i say it worked for me but not the most efficient path to perchlorate

"for a small outlay its much easier to do it all in one with no mess using pt .............. continuous for about 2 weeks + or untill ptt turns from a abrasive crystal to a creamy smooth iceing sugar crystal"

if this is what you are saying all the literature says because of excessive corrosion Pt should not be used in a contiuous operation

in my unregarded opinion the best way to perchlorate is chloride to chlorate using graphite then chlorate to perchlorate using leade dioxide unless you have money to burn

Edited by gilbert pinkston, 17 August 2008 - 07:32 PM.

[knackers]

thanks for sharing your findings,

what can i say,,................. i must have more money to burn than you .

Edited by phill 63, 17 August 2008 - 08:30 PM.

[knackers]

gilbert here
someone once wrote

"carbon rods are not worth the trouble, they disolve too rapidly don`t bother with carbon/graphite"

glad i diddnt know that before i converted 3 40# bags of NaCl to NaClO3 with (real) graphite not welding rods
in a properly run cell (as i have said many times but nobody wants to believe) one pound of graphite erroded will produce hundreds of pounds of chlorate
i used NaCl because i quicky recognized the disadvantages of starting with the potassium salt... for one the immensly more soluable NaClO3 produced allows for the graphite to settle out eliminating the need for filtering
then there is the soluability problem with KClO3 to KClO4 not to mention that for proper purification all products of the cell must be in solution and KClO4 is not very soluable meaning a huge amount of water must be used in the process compared to what is needed when working with sodium compounds.............

"then tried the auto ox , but still no purple (perchlorate)"
what can i say it worked for me but not the most efficient path to perchlorate

"for a small outlay its much easier to do it all in one with no mess using pt .............. continuous for about 2 weeks + or untill ptt turns from a abrasive crystal to a creamy smooth iceing sugar crystal"

if this is what you are saying all the literature says because of excessive corrosion Pt should not be used in a contiuous operation

in my unregarded opinion the best way to perchlorate is chloride to chlorate using graphite then chlorate to perchlorate using leade dioxide unless you have money to burn

we can agree on on the fact that there is more than one way to make pechlorate`

sorry i didn`t have enough time this morning to submit a proper reply and should have waited for this moment,, ``such is life``,.. ( Ned Kelly )

now then, `Quote`if this is what you are saying all the literature says because of excessive corrosion Pt should not be used in a continuous operation` end Quote,,. I disagree all of the literature says this,, , as long as the chlorate cell solution is kept saturated it avoids wear on the anode

i don`t know what literature you are quoting so i have added a few links of literature for you to read and they state that Graphite is a laborious method, i too have found this too be the case, i have some other literature that will also state it is somewhat wastefull, i don`t disagree for a moment that double disolution is probably the way to go,, but your graphite method is ( doubling up as far as i`m concerned ) i`d much rather and would recomomend to go platinum all the way,, load you cell, leave it go, top it up with saturated kcl ( no need even to remove sodium at the end of the run) and stir it untill it is perchlorate,, BTW, i have no need to produce hundreds of pounds or chlorate, as long as you don`t abuse you Pt anode it will probably produce enough perchlorate for the amature for years,( depending on your applications ) with no hassle, one cell one anode"

http://www.vk2zay.net/article.php/63..... Alan yates,



http://www.geocities...l</span></span> ,,,,


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http://www.wfvisser.dds.nl/EN/kclox_EN.html .......wouter visser



Quote`
[size="3"]as i have said many times but nobody wants to believe me, "one pound of graphite erroded will produce hundreds of pounds of ( chlorate ),, perhaps its not that nobody believes you, possibly it could be that nobody wants to go through that time consuming method, and produce enough to remove their neighbourhood of the face of the planet ,,when you can switch on a Pt cell and virtually leave it till its ready

double BTW, i wish i could have edited my original post but had no edit oppertunity, oh and i have since re done an auto ox with success

Edited by phill 63, 18 August 2008 - 09:37 AM.

[gilbert pinkston]

"load you cell, leave it go, top it up with saturated kcl ( no need even to remove sodium at the end of the run) and stir it untill it is perchlorate"

hummmm?

i guess im not getting it

since perchlorate is formed when chloride is less than 10% but this condition is not good for Pt annodes so clorides must be added to keep the concentration above 10% when does the pechlorate form?

of course it could be done in two steps by removing less soluable KClO3 from KCl solution and KClO4 from KClO3 solution

[knackers]

i`m not saying during the process i get no errosion of my anode, ( obviously i am ) but my depleation is minute, compared to graphite is mimiscule, so far with my Pt anode i have produced 4 kg of k perc ( 8.8 Lb ), (purified) with some noticeable discolouring of my anode, i believe that my anode is good for about the same amount more, so thats about 18 odd Lb, which will last me yonks.....$ 80 Au for anode = $ 4.40 AU per Lb...... i don`t know what k perc is worth ( we can`t get it here ) but i assume that anybody would be happy with that price, and no mess and mucking around with graphite,, and the added buzz of producing it oneself,

therefore mucking around with graphite may suit you, but i wouldn`t bother with it ( again ), yes i believe it`s a good experiment and wouldn`t discourage anyone from trying it, but i would stop short of recomending it,

[digger]

I love all this home made chlorate/perc discussion. Luckily we don't need to do this in the uk.

However I would like to try it as a lab scale experiment from a pure interest point of view. What would you guys recommend as a setup to make say 200 grams of perc (easiest possible setup)?

[knackers]

I love all this home made chlorate/perc discussion. Luckily we don't need to do this in the uk.

However I would like to try it as a lab scale experiment from a pure interest point of view. What would you guys recommend as a setup to make say 200 grams of perc (easiest possible setup)?

, , for a 200g experiment i would use a mmo anode ( i know its cold most times over there so hopefully there are pool shops ) they would probably have redundant chlorinators ( exchange ) ( for salt water pools ) and would probably give you a mmo anode for free, as mixed metal oxide anodes are used in salt pool chlorinators, a strip of titanium sheet or light gage mesh cathode, ( i would use this because there is no need for other additives in the cell, ie:- dichromate ) and do the auto oxidation method.

in a acrylic type hinged snap lock lid , easy accessable, or a screw top, 1 lt container, something like a long spaghettie storage container, but not so long and skinny, ( lab exp" size ) (i use 2.2 lt) drill through the lid and glue seal in place with marine xpoxy your electrodes and install a vent pipe, " you`ll only need to vent chlorine for a short while" as the liquer has to turn in to a chlorine solution before crystals will form, then the ph will rise enough to stop production of chlorine

electrolyte...( saturated) for 1 lt.. 40g of Nacl + 360g Kcl dump in a pot of suitable capacity with 1 lt water ( i`m sure you can scale it to fit whatever size cell you use, ) boil it then let it cool, if some should recrystalise , add a little more water, ( or filter it ) and your remaining saturated sol can be used to top up your cell,

run your cell on about 3-->4 volts, 4-->5 amps, i run mine a little higher but have bigger volume to disipate heat, if heat becomes a prob, place it in a cooling bath, or lower v/a accordingly

within a couple of days you should have a ppt forming, let it run ( may need to top up ) till you have your required kclo3 , you will need more than 2oog because auto oxidation will make K perchlorate and also reduce to K chloride, ( your Nacl will stay in sol )

you can do this with graphite, although you will need to filter it and as the graphite wears and suface area decreases your resistance in your cell will rise; so you will need to increase current and therefore increase heat of cell and wear on you graphite annode,

personally i would use a larger cell as a 1lt would be restrictive and prone to heat up... keeping in mind that this is only scaled for about 200grams in a lab experiment,, "if it was an ongoing venture i would do it differently "

BTW, on previous experience conversing with you, i`m sure you know all of this , and probably more !
you did say easiest,,, not cheapest

mind you, i havn`t done it this way, but it should work and be the easiest way i can think,

Edited by phill 63, 19 August 2008 - 11:09 AM.

[digger]

, , for a 200g experiment i would use a mmo anode ( i know its cold most times over there so hopefully there are pool shops ) they would probably have redundant chlorinators ( exchange ) ( for salt water pools ) and would probably give you a mmo anode for free, as mixed metal oxide anodes are used in salt pool chlorinators, a strip of titanium sheet or light gage mesh cathode, ( i would use this because there is no need for other additives in the cell, ie:- dichromate ) and do the auto oxidation method.

in a acrylic type hinged snap lock lid , easy accessable, or a screw top, 1 lt container, something like a long spaghettie storage container, but not so long and skinny, ( lab exp" size ) (i use 2.2 lt) drill through the lid and glue seal in place with marine xpoxy your electrodes and install a vent pipe, " you`ll only need to vent chlorine for a short while" as the liquer has to turn in to a chlorine solution before crystals will form, then the ph will rise enough to stop production of chlorine

electrolyte...( saturated) for 1 lt.. 40g of Nacl + 360g Kcl dump in a pot of suitable capacity with 1 lt water ( i`m sure you can scale it to fit whatever size cell you use, ) boil it then let it cool, if some should recrystalise , add a little more water, ( or filter it ) and your remaining saturated sol can be used to top up your cell,

run your cell on about 3-->4 volts, 4-->5 amps, i run mine a little higher but have bigger volume to disipate heat, if heat becomes a prob, place it in a cooling bath, or lower v/a accordingly

within a couple of days you should have a ppt forming, let it run ( may need to top up ) till you have your required kclo3 , you will need more than 2oog because auto oxidation will make K perchlorate and also reduce to K chloride, ( your Nacl will stay in sol )

you can do this with graphite, although you will need to filter it and as the graphite wears and suface area decreases your resistance in your cell will rise; so you will need to increase current and therefore increase heat of cell and wear on you graphite annode,

personally i would use a larger cell as a 1lt would be restrictive and prone to heat up... keeping in mind that this is only scaled for about 200grams in a lab experiment,, "if it was an ongoing venture i would do it differently "

BTW, on previous experience conversing with you, i`m sure you know all of this , and probably more !
you did say easiest,,, not cheapest

mind you, i havn`t done it this way, but it should work and be the easiest way i can think,

I have read a bit about it, but I have never tried it. This is where experience comes into play as it would appear that there are a few methods "out there" for this process which would either have extremely low yields or simply not work.

So thanks for your reply it will give me a basis for a lab experiment at some point in the future when it works its way up the project list. I am not to worried about initial price within reason if it makes things easier and total cost of ownership can often be lower.

Edited by digger, 20 August 2008 - 12:05 PM.

[Arthur Brown]

The biggest difficulty in previous projects has been getting enough power at an appropriate voltage, and getting the power into the cell.

Carbon electrodes will get chloride to chlorate but then they start to disintegrate, and will nit form perc. Carbon electrodes will conduct (as in a wick) the corrosive liquor and the connections will die where you try to put the current in. Platinum wire has been fused into glass dip tubes with some success. There is always a need to get the evolved gasses vented away as they will corrode the PSU and wires

[knackers]

The biggest difficulty in previous projects has been getting enough power at an appropriate voltage, and getting the power into the cell.

Carbon electrodes will get chloride to chlorate but then they start to disintegrate, and will nit form perc. Carbon electrodes will conduct (as in a wick) the corrosive liquor and the connections will die where you try to put the current in. Platinum wire has been fused into glass dip tubes with some success. There is always a need to get the evolved gasses vented away as they will corrode the PSU and wires

carbon electrodes will succumb to ( creep ) due to their reducive nature, and will not hold a seal with whatever sealant is used, thereby shrinking loose,, however, more stable metals will not succumb to creep with an appropriate sealant and all connections will stay corrosive free, ( marine epoxy is the best i`ve come across, but will eventually fail because of the corrosive nature of the electrolyte but it will take weeks and maintenance can over come this,,,, Pt wire is a good anode as all platinum is ultimately the best
although, platinum wire wrapped around a glass cylinder in a helix is not using your anode optimally, as only the part facing the cathode is ulimately being used, therefore it is a more viable option to arrange your wire anode in verticle parrallell fashion sealed in a hole off clearence diameter (with marine grade epoxy ), venting is very important as chlorine is evaporated and will condense causing corrosion, although i have not had any trouble with this

Edited by phill 63, 22 August 2008 - 09:07 AM.

[ridesideways]

I've enjoyed reading through this thread and learning about the associated chemistry. however, since this thread started out as a problem with getting KClO4 outside the USA, couldn't you just buy it from this web site? They seem to ship anywhere. www.potassiumperchlorat.com

Would you buy from this site?

[pyromaniac303]

With it being an unknown supplier I wouldn't risk it, if I did buy from there then I would check for the presense of chlorate and other impurities, as no information is given.

[Arthur Brown]

The chance of a correctly labelled pack of perc arriving from the US -they use $ and lbs. is remote. Also the price is fair in the USA postal area but would certainly cost more to get it to the UK.