My easy way of making K perchlorate

[THEONE]

I am starting a new topic because the (per)chlorate topic is already chaotic.

 

My way of making K perchlorate starts from K chloride. For a chlorate cell i use a MMO anode and a titanium cathode. The procedure of making chlorate from chloride with MMO is very well known already. My procedure for chlorate is as follows.

 

1)At the beginning i make a saturated solution of kcl. Just add some distill water into a big container containing kcl salt. Mix it untill no more kcl is going to get dissolved. The remaining undissolved kcl is going to sit at the bottom of the container.

 

2) Add the saturated kcl solution into the chlorate cell.

 

3) Add a buffer ( i add about 20g/5L of electrolyte). I use Cacl as a buffer. Buffer is used to maintain constantly the ph of the cell. While the chlorate cell is running, it is getting basic since some chlorine gas escapes. With Cacl as a buffer, insoluble CaOH is going to form and drop at the bottom of the cell, maintaining the ph neutral. I just add a few ml of HCL to redissolve the CaOH according to the AmpHrs of the cell.

 

4) I am taking every few days some density measurements to check the remaining kcl into the cell. KCLO3 will ppt out. If i remember correctly, i measure about 57g per 50ml of saturated kcl water while saturated kclo3 water is about 50,5.

 

5) When the density drops (about 53-54g per 50ml) I add the electrolyte into the kcl container and let it re-saturated. I collect the crude kclo3 from the bottom of the cell into a plastic shoe-box.

 

6) To purify the kclo3, 1st i rinse the crude kclo3 with distilled water to absorb as much remaining kcl as possible, keep the crude kclo3 and filter if needed the water and add it into the kclo3 cell. Then dissolve the crude kclo3 into distilled boiling water, filter it and let it cool. Kclo3 will ppt out. Collect the crystals and add the water again back to the kclo3 cell. Rinse the recrystallized kclo3 with some distilled water a couple of times. You can tell if your kclo3 is pure if the rinsed water has a density of about 50,5g per 50ml of water (kclo3 saturated solution density). With this method i have taken really pure kclo3 crystals. Filer if needed the rinsed water and put it back again into the kclo3 cell (nothing is wasted )

 

Repeat until no more kcl has left. Keep the electrolyte and the rinsed water for future runs.

 

Now for the perchlorate cell.

 

For k perch i use a Pt anode and a Ti cathode. The anode and the cathode are spaced as much closely as possible to allow the maximum current possible.

I prepare a saturated kclo3 solution as above. To this cell i have added a 5oz ketchup cup filled with holes (made with a hot wire). This container is filled with kclo3 crystals which is tied with a fishing line. The purpose of this container is to keep the electrolyte saturated with kclo3. Kclo4 will form at the anode and drop at the bottom of the cell. Kclo3 from the container will be getting consumed.

 

The advantage of this set up is that you are not going to use any Nacl salt since it is very messy and PITA to recrystallize and purify. Also your end Kclo4 is not going to have any sodium salt contamination. Another major advantage to this method is that since you are using pure kclo3 with very little to no kcl, you are not going to damage your precious Pt anode. The cell is running for about a month now without any sign of erosion.

 

The disadvantage of this setup is that the kclo4 is produced slowly since kclo3 has a low solubility.

 

I am posting below some photos from my kclo4 cell running right now since i am not running a kclo3 cell anymore because i already got about 10 kilos of kclo3.

The cell is running for about a month at about 1 Amp. Note that i have already taken a few grams of kclo4 from the cell.

Edited March 25, 2022 by THEONE

[CountZero]

Interesting, I think this is the first detailed description of kclo3 to kclo4 by electrolysis I have seen.

[WSM]

I wonder about a couple things with this setup;

1. how pure (chlorate-free) the perchlorate produced by this method is?
2. would it be more efficient if the system were running hotter?

The first question would be answered with an effective chlorate test (I'm aware of at least three methods to test for chlorate contamination of perchlorate).

 

I recall Swede making potassium perchlorate directly from potassium chlorate, but residual chlorate in the perchlorate being an issue. He solved it by treating the perchlorate (under water or electrolyte, I don't recall which) with potassium metabisulfite solution*, which produced sulfur dioxide that destroyed the chlorate contamination, leaving the perchlorate chlorate-free.

 

The second question could be answered by using a borosilicate beaker on a lab hot plate for the cell container. At higher temperatures, more potassium chlorate would dissolve in the electrolyte and be available for conversion to potassium perchlorate. I suspect that if THEONE's system assumptions are correct, the current level will raise due to more reactants being available to be converted to perchlorate. Also, if I'm right, more perchlorate would form in less time.

 

Any plans to test my theory would depend on carefully controlled conditions. I'm not able to try it at this time, but suggest THEONE might attempt it if he's got the resources to do so available to him. It would be interesting to see how it works (and if I'm right ).

 

WSM

 

* Treating perchlorate with a metabisulfite solution (SO₂) requires the use of a system of slowly administering the solution, deep under the liquid covering the perchlorate, so the sulfur dioxide doesn't "flash off" on the surface but stays in the solution where the chlorate will break down into soluble potassium salts (K₂SO₄, etc.) which are easily separated from the perchlorate crystals.

 

Speaking of perchlorate crystals, potassium perchlorate is highly insoluble at STP (standard temperature and pressure) and it is wise to remember that the faster the crystals are formed, the smaller they'll be (nearly powdered if instantly formed). Conversely, the slower the crystals form, the larger they'll be; requiring the added step of grinding them down to a useful particle size.

Edited March 26, 2022 by WSM

[THEONE]

I am pretty sure kclo4 can be purified the same way i purify the kclo3. Dissolving the kclo4 in hot distilled water and then let it ppt, then rinse it with more distilled water will most likely give you pure kclo4

 

Something i want to mention is that as long as you keep the electrodes close apart, the anode will be getting cleaned by the hydrogen the cathode produces

 

Edit. In order to increase current, due to low solubility of kclo3, i may make some Naclo3 from pure kclo3 with Sodium tartate. Isoluble K tartate will ppt out leaving Naclo3 into the solution. Add that solution into kclo4 cell for more current.

In my opinion, running the cell hotter will increase efficiency since more kclo3 will be dissolved but i will not bother with it, i dont mind to wait a bit more for the cell to complete.

 

Edit2. I tested some of that kclo4 with hcl that i have rinsed it with water and there was not any bubbling. Also i made some flash with it and it was damn powerful.

Edited March 26, 2022 by THEONE

[Arthur]

The reason why he commercial process uses the sodium salt is that the potassium salts are much less soluble meaning that a huge amount of solution would be needed to dissolve enough ingredients to make a useful yield. Using a dilute solution (solubility limited) is where erosion of the electrodes happens whch for a platinum electrode gets expensive.

[WSM]

I am pretty sure kclo4 can be purified the same way i purify the kclo3. Dissolving the kclo4 in hot distilled water and then let it ppt, then rinse it with more distilled water will most likely give you pure kclo4

 

Something i want to mention is that as long as you keep the electrodes close apart, the anode will be getting cleaned by the hydrogen the cathode produces

 

Edit. In order to increase current, due to low solubility of kclo3, i may make some Naclo3 from pure kclo3 with Sodium tartate. Isoluble K tartate will ppt out leaving Naclo3 into the solution. Add that solution into kclo4 cell for more current.

In my opinion, running the cell hotter will increase efficiency since more kclo3 will be dissolved but i will not bother with it, i dont mind to wait a bit more for the cell to complete.

 

Edit2. I tested some of that kclo4 with hcl that i have rinsed it with water and there was not any bubbling. Also i made some flash with it and it was damn powerful.

 

 

I thought you wanted to avoid sodium contamination in your system, otherwise why not just go the sodium route and avoid all the trouble and expense of boiling off excess water from your potassium perchlorate?

 

I determined years ago that if I make clean and reasonably pure sodium chlorate crystals, I can make an excellent electrolyte for my perchlorate experiments. Once I had sodium perchlorate solution in high enough concentration, I carefully treated it with sodium metabisulfite solution to destroy residual sodium chlorate in the perchlorate.

 

Next I added potassium chloride solution to the chlorate-free sodium perchlorate solution which instantly formed fine powdered/crystalline potassium perchlorate, leaving all the soluble sodium salts in solution. After removing the potassium perchlorate by vacuum filtration, the next step is careful and thorough removal of sodium contamination with rinsing of the potassium salt.

 

Industry uses these methods due to the relative solubilities and concentrations of the reactants, plus the economy of the process (yes, they're in it for the money!).

 

If you have access to commercially produced sodium chlorate (especially reagent grade), making sodium perchlorate with either platinum or lead dioxide anodes is a straight forward and simple process. In fact, it is pleasant compared to making chlorate. If done properly, there is no unpleasant chlorine odor produced. There is some ozone produced, but if done in a controlled fashion*, it isn't unpleasant at all in my experience, AND I would consider doing so indoors, rather than outdoors as I do with my chlorate cells (Yes, I live in a temperate area with moderate weather - no snow and very few outrageously hot days).

 

*I used a power supply with constant current (CC) mode capability and ran my perchlorate experiments using lower voltage than commercial systems (about 4-4.5 Vdc if I remember correctly). Everything worked well with no detectable degradation of the platinum anode. There was some minor breakdown of the LD anode, but it was what I feel to be "acceptable losses" and the anode is still fully usable with plenty of life left in it.

 

WSM

Edited April 2, 2022 by WSM

[WSM]

The reason why he commercial process uses the sodium salt is that the potassium salts are much less soluble meaning that a huge amount of solution would be needed to dissolve enough ingredients to make a useful yield. Using a dilute solution (solubility limited) is where erosion of the electrodes happens whch for a platinum electrode gets expensive.

 

 

I agree.

 

Where sodium and potassium chlorides are nearly identical in solubility, sodium perchlorate is about 100 times more soluble than potassium perchlorate is. That is KClO₄ is 0.01 times as soluble as NaClO₄, which is why potassium perchlorate drops out of solution instantly when KCl solution is added to NaClO₄ solution. The speed of the reaction also keeps the crystal size of potassium perchlorate small enough to negate the need for much processing after purification and drying.

 

WSM

Edited April 2, 2022 by WSM

[WSM]

I am pretty sure kclo4 can be purified the same way i purify the kclo3. Dissolving the kclo4 in hot distilled water and then let it ppt, then rinse it with more distilled water will most likely give you pure kclo4

Something i want to mention is that as long as you keep the electrodes close apart, the anode will be getting cleaned by the hydrogen the cathode produces

Edit. In order to increase current, due to low solubility of kclo3, i may make some Naclo3 from pure kclo3 with Sodium tartate. Isoluble K tartate will ppt out leaving Naclo3 into the solution. Add that solution into kclo4 cell for more current.

In my opinion, running the cell hotter will increase efficiency since more kclo3 will be dissolved but i will not bother with it, i dont mind to wait a bit more for the cell to complete.

Edit2. I tested some of that kclo4 with hcl that i have rinsed it with water and there was not any bubbling. Also i made some flash with it and it was damn powerful.

 

 

I recall when Swede ran an experiment to make potassium perchlorate directly from potassium chlorate solution, he ran into trouble because the potassium perchlorate crystals packed into the anode mesh and reduced the current draw of the system.

 

I believe he proved for me, the inefficiency of a potassium chlorate to potassium perchlorate system. His motive was the same as you stated, to avoid sodium contamination in the KClO₄ he produced, which would be problematic for any color star formula.

 

My concern about using sodium contaminated perchlorate for flash is the hygroscopic nature of most sodium salts and possible safety problems with the finished goods in storage.

 

WSM

Edited April 2, 2022 by WSM

[Arthur]

ALL the commercial purification steps rely on solubility to precipitate out either the wanted product or the unwanted component. The interesting bits include the fact that sodium chloride has a solubility that changes little with temperature but the sodium chlorate solubility changes wildly with temperature.

 

The final purification in the conventional process is to have a highly soluble NaPerc in solution then add KCl soln to the cell content and ppt out the only pure KPerc by fractional crystalisation. In industry no-one wants to destroy chems that you have made simply on a cost basis -you've paid for the electricity, and no-one wants to add oddities to the solution that you will want to recycle.

 

A cell working the conventional way -NaCl to NaClO₃ to NaPerc then ppting out the Perc with KCl_(aq) makes little waste and uses only KCl . By being careful with the amount of KCl used only the perc is produced as product and all the rest is completely recyclable.

Edited March 28, 2022 by Arthur

[WSM]

ALL the commercial purification steps rely on solubility to precipitate out either the wanted product or the unwanted component. The interesting bits include the fact that sodium chloride has a solubility that changes little with temperature but the sodium chlorate solubility changes wildly with temperature.

The final purification in the conventional process is to have a highly soluble NaPerc in solution then add KCl soln to the cell content and ppt out the only pure KPerc by fractional crystalisation. In industry no-one wants to destroy chems that you have made simply on a cost basis -you've paid for the electricity, and no-one wants to add oddities to the solution that you will want to recycle.

A cell working the conventional way -NaCl to NaClO₃ to NaPerc then ppting out the Perc with KCl_(aq) makes little waste and uses only KCl . By being careful with the amount of KCl used only the perc is produced as product and all the rest is completely recyclable.

 

 

In making sodium perchlorate I have found in my own experience that the simplest method is to electrolyze sodium chlorate to sodium perchlorate using an appropriate anode and cathode combination. Lacking the availability of commercial sodium chlorate, I've opted to research home production of my own NaClO₃ to use for continuing research of amateur scale perchlorate production.

 

The method you allude to starts with sodium chloride and finishes with sodium perchlorate. As an amateur, I think this type of system needs careful control and monitoring to prevent damage to expensive and hard to obtain electrodes (platinum or lead dioxide, commonly). Most of the perchlorate-worthy anodes I've encountered are either platinum or lead dioxide coated titanium.

 

The only anode material I've seen used to go directly from chloride to perchlorate (and survive long term) is graphite substrate lead dioxide (GSLD), and that requires a sodium fluoride catalyst to function efficiently. If I ever get my hands on one, I plan to try that type of system out; but for now I do my perchlorate experiments in two steps.

 

I like the quality control of doing this in steps (NaCl to NaClO₃ , allowing for later doing NaClO₃ to NaClO₄ and then NaClO₄ to KClO₄) where I can control the product with purification and quality control (QC) steps.

 

I see the benefit of the system you describe, and I may try an experiment with it on a small scale later; but for now I'm still pursuing the steps I started years ago that produced my first successful potassium perchlorate. I'd like to see if it's safe, possible and practical to make hobbyist quantities of high quality KClO₄ for amateur use.

 

I've also considered investigating NH₄ClO₄ and Ba(ClO₃)₂.H₂O production on a hobbyist scale, sometime in the future.

 

In a world of questionable future availability of pyrotechnic materials, knowledge of how to safely make them is priceless.

 

WSM

Edited April 2, 2022 by WSM

[Arthur]

The final liquor after filtering out KPerc will be totally recyclable into the sodium cell whether that's a chlorate cell using MMO or a perc cell using lead dioxide. The big problem will be letting the volume of solution in process grow. The volume loss due to the chlorine being oxidised by oxygen from the water needs to be made up by the water used to make the saturated KCl used in the metathesis.

[THEONE]

The biggest issue with Nacl system is to purify the Naclo3. When you start your perc cell, even the smallest amount of Nacl will destroy your anode. With kcl system you can easily purify kclo3.

[WSM]

The biggest issue with Nacl system is to purify the Naclo3. When you start your perc cell, even the smallest amount of Nacl will destroy your anode. With kcl system you can easily purify kclo3.

I was able to solve the problem with purifying sodium chlorate by crystallizing a portion of it from the electrolyte and filtering those crystals out before recharging the electrolyte with more chloride and then running it again.

 

The dry sodium chlorate crystals are used later to make up the electrolyte for the perchlorate cell.

 

WSM

Edited March 29, 2022 by WSM

[kingkama]

I was able to solve the problem with purifying sodium chlorate by crystallizing a portion of it from the electrolyte and filtering those crystals out before recharging the electrolyte with more chloride and then running it again.

 

The dry sodium chlorate crystals are used later to make up the electrolyte for the perchlorate cell.

 

WSM

The best solution Is plating lead dioxide on Platinum, Easy and durable, and if lead come off you can plating again.

[WSM]

The best solution Is plating lead dioxide on Platinum, Easy and durable, and if lead come off you can plating again.

 

 

This sounds good but the process is not trivial (or inexpensive). Platinum alone works as a perchlorate anode, why plate it with LD?

 

Swede made his own lead dioxide anode by plating LD on an MMO/titanium substrate. This eliminated the difficult task of carefully preparing the CP titanium substrate for lead dioxide plating.

 

None of these steps are simple or easy.

 

WSM

[Arthur]

One of the reasons why Perc was made by the sodium route is that, then, the big need for perc was Ammonium Perchlorate for such things as rocket motors for NASA and the military It's possible to metathesise NaPerc to AP but not KPerc to AP.

In the days when platinum was the only anode material that worked preventing anode erosion was essential -they held the platinum loss down to grammes per ton of perc by using the sodium route with it's high solubilities. Now that lead dioxide is available and (cheaper to erode!) the potassium salt may be a viable route to KPerc but not AP.

[WSM]

Depending on how you get there, once you have chlorate-free sodium perchlorate, making potassium perchlorate is simple. Even making ammonium perchlorate is possible, depending on your methods or technique.

 

WSM

Edited March 31, 2022 by WSM

[mx5kevin]

Deviate from the factory setup not effective at all. The unique solution which is not in professional patents it's all wrong. The using of factory methods works at home. Those methodes are not worth to try which are not prove by professional patents. A lot of nonsense is done by many people at home which are described in professional documents say that they should not to do.

 

I used this KCl to KClO3 and KClO3 to KClO4 process. It's easy for who can't calculate in a NaClO4 setup how to do it.

 

In a electric balance every 1 gram KCl dissolved 2,9gramm H2O (saturated solution at room temperature). Keeped the pH 6-7 using HCl every day (cc 500ml to 5ml 30% HCl/Day without pH meters shaken in a 2l plastic bottle to dissolve the chlorine gas) and 1 week later all KCl converted to KClO3. Maximum 6V and 4-6A used to a 0,5l cell the power source are a car battery charger. If someone is a professional using 2-4g/l sodium persulphate. All the KClO3 completely dissolved in water and with sedementation/filtration cleaned up few days the insoluble contamination. With two recrystallizations in water and washing the cristalls from the solution resoult pure KClO3. Sedementation/filtration enough when used to convert KClO4.

 

For KClO4 every 1 gram KClO3 dissolved 13,7 gram H2O (saturated solution at room temperature) pH 6-7 used small amount of HCl which is a few drops. It is important that it does not crystallize out of solution the KClO3 and must keep the solution not lower than 25°C and not higher than 40°C! In a 0,5 l cell are 36g KClO3 can dissolved the solution which is very small. And several days until it the KClO4 crystallizes out than add the same solution another KClO3. The solution should be reused here because too much KClO3 and KClO4 is dissolved in the solution. When ready with potassium metabisulfite K2S2O5 and HCl proportionately added and completely dissolved the KClO4 boiled to generate SO2 gas must destroy the KClO3 in the crystalls. I used 5-10% K2S2O5 calculated the total KClO4. 100g KClO4+5g K2S2O5. Heare need a beaker in a stainless steel not possible to boil this acidic solution. Than must wash the crystals with ice cold water, and recrystal 2X the KClO4 minimum double water then crystal must see in the solution when cooled down at room temperature.

 

End result must the fine powdered KClO4 test with concentrated HCl. And if it doesn’t stay white then it’s not clean. All yellowish, grayish discoloration, other reaction like bubbles shows contamination.

 

The problems with this: Lots of material loss and low yield, lots of time and work. Compared with a pro NaClO4 setup what you can get pure KClO4 1 run from this setup. With the KClO 3 to KClO4 setup lasts for months. And in the NaClO4 setup sedimentation are easy. KCl and NaClO4 sedimentation are easy, the KClO4 are impossible at room temperature. Boiling NaClO4 are easy, boiling KClO4 a nightmare. KClO3 to KClO4 electrolysis KClO4 forms in the anode lead dioxid can not used it would be full of deposits. It also puts a much heavier erosion on the anode.

 

CaCl in a chlorate perchlorate cell. The calcium must keep the possible lowest this saying the professional documents in chlorate perchlorate cells. What i readed in professional documents I have not heard CaCl as buffer adattive. On the deposition of calcium on the cathode I read a lot. I saw this from a Youtuber but all the professional documents I have found is all against it. There are proven additives used in the industry no one will invent any better.

Edited April 2, 2022 by mx5kevin

[mx5kevin]

I started making chlorate and perchlorate 15 years ago. I dealt with the thame regularly on a daily basis. I was looked for methods withot using electroliysis with the limited perchlorate anodes. There is a reason that everybody use the NaClO4 electrolysis setup. Very few people using the KClO3, and NaClO3 thermal decomposition to make NaCO4, KClO4. Does not hearing about other solutions in the homemade setup. Everything that is not using the NaClO4 electrolisys to make KClO4 the price and work are too high. Just an example a lower melting point (248°C) NaClO3 thermal decomposition to make NaClO4 US 2733982 pantent says 400-600°C to need the process and 0,167-8 hour the time range specified by the patent using NaClO3. And other documentts says 400°C the minimum temperature with NaClO3 and KClO3 too for this perchlorate conversion. In a ceramic crucible using a normal gas stove the temperature under 350°C which is still under the KClO3 melting point. The special inert heat and melted chlorate resistant material because the household utensils mainly metals are dissolved by the melted chlorate. The only solution that is not yet complicated without special limited perchlorate anodes. For many years, I haven’t seen anyone produce in large quantities with the method KClO4 or NaClO4. At the right temperature for a small amount chlorate, most people take an hour to complete the process. Special circumstances are required in each case where the precisely controlled high temperature range and time keept for a long time in this process. See the DTIC AD0016814 and DTIC AD0017221 : Research on the Exploration of Methods to Produce Chlorates and Perchlorates by Means Other than Electrolytic documents.

Edited April 2, 2022 by mx5kevin

[WSM]

Deviate from the factory setup not effective at all. The unique solution which is not in professional patents it's all wrong. The using of factory methods works at home. Those methodes are not worth to try which are not prove by professional patents. A lot of nonsense is done by many people at home which are described in professional documents say that they should not to do.

 

I used this KCl to KClO3 and KClO3 to KClO4 process. It's easy for who can't calculate in a NaClO4 setup how to do it.

 

In a electric balance every 1 gram KCl dissolved 2,9gramm H2O (saturated solution at room temperature). Keeped the pH 6-7 and 1 week later all KCl converted to KClO3. If someone is a professional using 2-4g/l sodium persulphate. All the KClO3 completely dissolved in water and with sedementation/filtration cleaned up few days the insoluble contamination. With two recrystallizations in water and washing the cristalls from the solution resoult pure KClO3

 

For KClO4 every 1 gram KClO3 dissolved 13,7 gram H2O (saturated solution at room temperature). In a 0,5 l cell are 36g KClO3 which is very small. And several days until it crystallizes out to add the same solution another KClO3. The solution should be reused here because too much KClO3 and KClO4 is dissolved in the solution. When ready with potassium metabisulfite K2S2O5 and HCl proportionately added and completely dissolved the KClO4 boiled to generate SO2 gas must destroy the KClO3 in the crystalls. I used 5-10% K2S2O5 calculated the total KClO4. 100g KClO4+5g K2S2O5. Heare need a beaker in a stainless steel not possible to boil this acidic solution. Than must wash the crystals with ice cold water, and recrystal 2X the KClO4 minimum double water then crystal must see in the solution when cooled down at room temperature.

 

End result must the fine powdered KClO4 test with concentrated HCl. And if it doesn’t stay white then it’s not clean. All yellowish, grayish discoloration, other reaction like bubbles shows contamination.

 

The problems with this: Lots of material loss and low yield, lots of time and work. Compared with a pro NaClO4 setup what you can get pure KClO4 1 run from this setup. With the KClO 3 to KClO4 setup lasts for months. And in the NaClO4 setup sedimentation are easy. KCl and NaClO4 sedimentation are easy, the KClO4 are impossible at room temperature. Boiling NaClO4 are easy, boiling KClO4 a nightmare. KClO3 to KClO4 electrolysis KClO4 forms in the anode lead dioxid can not used it would be full of deposits. It also puts a much heavier erosion on the anode.

 

CaCl in a chlorate perchlorate cell. The calcium must keep the possible lowest this saying the professional documents in chlorate perchlorate cells. What i readed in professional documents I have not heard CaCl as buffer adattive. On the deposition of calcium on the cathode I read a lot. I saw this from a Youtuber but all the professional documents I have found is all against it. There are proven additives used in the industry no one will invent any better.

 

 

Thank you for the description of the process you use.

 

I see it as justification for my decision to copy industrial methods of perchlorate production. My biggest problem was getting sodium chlorate (it's not available here), and so my focus has been to produce my own. I succeeded but I'm trying to make enough that I can do all of my perchlorate manufacturing experiments from the same stockpile. This is leading me in efforts to optimize my sodium chlorate production (plus simplify it if possible).

 

Obviously making potassium perchlorate from potassium chlorate is possible, but the economy of doing so is poor. Copying the industrial method uses a LOT less energy and effort, let alone expense, to make perchlorates.

 

WSM

Edited April 2, 2022 by WSM

[mx5kevin]

 

 

Thank you for the description of the process you use.

 

I see it as justification for my decision to copy industrial methods of perchlorate production. My biggest problem was getting sodium chlorate (it's not available here), and so my focus has been to produce my own. I succeeded but I'm trying to make enough that I can do all of my perchlorate manufacturing experiments from the same stockpile. This is leading me in efforts to optimize my sodium chlorate production (plus simplify it if possible).

 

Obviously making potassium perchlorate from potassium chlorate is possible, but the economy of doing so is poor. Copying the industrial method uses a LOT less energy and effort, let alone expense, to make perchlorates.

 

WSM

 

My research is available in Hungarian language: https://mx5-kevin.blogspot.com and https://sufnipiro.wordpress.com

 

My specialty is potassium perchlorate. I've been making it for 15 years. For a 0,5l cell a 70mm long 3mm wide silver rod what is fully coated with 0,2mm thick pure platinum so that they are not attacked by chemicals a choice for life for chlorate and perchlorate production. It must be made individually. For using 400-1000ml small cells are excelent. If I find a better solution or something new, I will update the content regularly. There is a detailed video of how I make it from NaCl to KClO4. I don't really like to write on the forum because things can't be edited later. However, I am creating a blog in which I can describe things more accurately in English and can edit it. You can always do it better and thoughtfully the KClO4 synthesis from NaClO4 as someone does more and more. A sodium or potassium chlorate is so simple that anyone can make it with a graphite anode only the pH should be maintained 6-7 especially for graphite to significantly reduce the graphite crashing. Modern MMO anodes can buy everywhere for making lot chlorates what not crash like graphite. Making NaClO3 and KClO3 chlorates is a simple thing. Large surface PbO2 or a few microns platinum mesh anodes not to hard buy too for perchlorates in larger cells. For thin platinum on a titan base or PbO2 making the NaClO3 first with MMO, than the NaClO3->NaClO4 conversion with Pt, PbO2 are the best. Multiply by many the lifetime a few microns platinum coated anode. In the case of strong beta lead dioxide anodes, this is only allowed in the two MMO/PbO2 step.

Edited April 2, 2022 by mx5kevin

[mx5kevin]

The Chlorates and Perchlorates one of the best page on the theme for amateurs. The site writes about all the important things for amateurs. Experiments tests like the graphite anode in pH controlled KClO3, NaClO3 cell using HCl where not crash so fast the graphite. From chlorate and perchlorate specific anodes detailed descriptions.

 

http://www.chlorates.exrockets.com/chlorate.html

[Richtee]

 

My research is available in Hungarian language: https://mx5-kevin.blogspot.com and https://sufnipiro.wordpress.com

 

Hey! a Fellow Hunky!

 

A gratuitous pict of some pogácsa I made...

[WSM]

 

My research is available in Hungarian language: https://mx5-kevin.blogspot.com and https://sufnipiro.wordpress.com

Hey! a Fellow Hunky!

A gratuitous pict of some pogácsa I made...

 

 

 

Interesting! I have MANY hobbies myself, including cooking and baking (why not, it's all chemistry! ).

 

WSM

Edited April 3, 2022 by WSM

[WSM]

My research is available in Hungarian language: https://mx5-kevin.blogspot.com and https://sufnipiro.wordpress.com

My specialty is potassium perchlorate. I've been making it for 15 years. For a 0,5l cell a 70mm long 3mm wide silver rod what is fully coated with 0,2mm thick pure platinum so that they are not attacked by chemicals a choice for life for chlorate and perchlorate production. It must be made individually. For using 400-1000ml small cells are excelent. If I find a better solution or something new, I will update the content regularly. There is a detailed video of how I make it from NaCl to KClO4. I don't really like to write on the forum because things can't be edited later. However, I am creating a blog in which I can describe things more accurately in English and can edit it. You can always do it better and thoughtfully the KClO4 synthesis from NaClO4 as someone does more and more. A sodium or potassium chlorate is so simple that anyone can make it with a graphite anode only the pH should be maintained 6-7 especially for graphite to significantly reduce the graphite crashing. Modern MMO anodes can buy everywhere for making lot chlorates what not crash like graphite. Making NaClO3 and KClO3 chlorates is a simple thing. Large surface PbO2 or a few microns platinum mesh anodes not to hard buy too for perchlorates in larger cells. For thin platinum on a titan base or PbO2 making the NaClO3 first with MMO, than the NaClO3->NaClO4 conversion with Pt, PbO2 are the best. Multiply by many the lifetime a few microns platinum coated anode. In the case of strong beta lead dioxide anodes, this is only allowed in the two MMO/PbO2 step.

 

 

I agree. Nice blog, too.

 

I've written a series of articles (17 to date) on the subject of home made oxidizers, which are published in the Pyrotechnics Guild International Bulletin, under the title of, "Homegrown Oxidizers". They detail some of the research of some like-minded friends and I have done. I haven't continued the series in several years, but I'm not done yet (Part 18 is sitting on my computer desktop, waiting for me to continue my research ). Part of the series are in the Blog section here in APC.

 

I look forward to you continuing posts here on the subject.

 

WSM

Edited April 3, 2022 by WSM