The homemade chlorate and perchlorate project


The video from the process:
 

or https://www.bitchute.com/video/JsRryZQmK3Rv/ or https://odysee.com/@mx5kevin:a/Make-potassium-perchlorate-KCLO4-from-sodium-perclorate-Naclo4-with-electrolysis:8

KClO3 Vs KClO4 tests: https://www.bitchute.com/video/rkfx0mcotRcb/ or https://odysee.com/@mx5kevin:a/KCLO3-VS-KCLO4-important-differences-and-tests:c or

My website with more Hungarian description and documents: https://mx5-kevin.blogspot.com or https://sufnipiro.wordpress.com My BitChute chanel with more videos and tests: https://www.bitchute.com/channel/X6adxEKbK8Ky/

Tether USDT and BNB BEP20 or (Matic Polygon) small amount donation to support projects: 0x16829457123552A574441bf38Eeaf93B46105A1d

BTC Bitcoin donation: 16aiyTMQDagpcD1za5yoVLCMssym52QLnf

More documents: https://odysee.com/@mx5kevin:a or https://drive.google.com/drive/folders/0BwXIGQD4ku3hfjc0NXZYV2ZydnlvTXR1RkxoV09nVGgydFloWUdReVNCeXV5aThoSHlrRTQ

The setup:
Sprinkler connection module
Soft PVC Pipe Tube 6m
plastic jar lid
500ml glas jar
6V 4A car battery charger
Cathode 8mm carbon welding rood
Cathode 2: Titanium the best
Calculation: For the double displacement reaction calculated using a periodic table from relative mass the ratios (KCl+NaClO4). In a electric balance calculated 1kg water to 1000ml 1l.


Protecting the tools: The beaker: Use a Wire Gauze Heat Shield with Ceramic Center to protect the beaker from thermal shock or will be cracked or use a sand bath this is important. Do not heat directly intensive way in hot plate because this will crack the beaker. Hotplate: Protect it with aluminum foil from corrosion. Stainless steel saucepan: Do not heat it in wet NaCl, KCl, NaClO4, NaClO3 crystals in it this will rusted the saucepan immediately and contaminated the product. Do not boil HCl acidic solution in it. Use 18/10 stainless steel. Possible to heat in it wet KClO3 and KClO4 crystals without erosion. The electrodes: Only use few micron platinum or PbO2 in perchlorate cells and make the chlorate with MMO anode. Keep the pH 6-7 or 7-8 to protect the MMO and PbO2 anode from too alkali or acidic solutions using a digital pH meter. Digital pH meter: Need to calibrate with pH buffers, and always wash it with NaHCO3 solution after used in the chlorate perchlorate cell. Aluminum saucepan, ceramic pans, in oven, gas stove: In pure aluminum possible to heat wet KCl, NaCl, NaClO4, NaClO3 crystals and the pan not get rusted using a hotplate or gas stove. But pure aluminum not tolerate alkali or acidic solutions!

Protective gears: The cell must run and the processes must make in outdoor. Use a M3 protective mask, protective glasses from chlorine, protective plastic gloves!



The platinum anode and graphite 8mm welding carbon rod cathode for NaClO4 and KClO3



KClO3 from KCl after 1 week







Platinum anode parameters for KClO3 and NaClO4 Silver 70mm x 3mm pure platinum 0,2mm (200micron platinum) fully coated the silver. For 400-1500ml cells max 6V 4-6A.

Anode materials one step chloride to perchlorate setup: Platinum (thickly coated): For a 0,5l cell a 70mm long 3mm wide silver rod what is fully coated with 0,2mm (200micron platinum) thick pure platinum so that they are not attacked by chemicals a choice for life for chlorate and perchlorate production in one step. It must be made individually. For using 400-1500ml small cells are excellent. Using plastic champagne cork and silicon inside cell with less corrosion possible to connect it from the copper wire. This anode required only a cheap 6V 4-6 A car battery charger, maximum of 2 Amps will actually pass through the cell (if a 10mm carbon cathode are used) this power supply can handle this comfortably.

Anode materials two step chloride to chlorate and chlorate to perchlorate setup: MMO anodes RuO2, IrO2, TiO2 mesh in a titan base for chloride to chlorate production. And chlorate to perchlorate production strong beta PbO2 in titanium base, or few micron platinum in titanium base. 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. 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. 5 micron platinum coating on a titanium anode all platinized titanium anodes are poor quality. Such electrodes are destroyed quickly. Everyone who bought such electrodes this anodes are quickly damaged. These are the electrodes that multiple costumer are say that people shouldn't buy. Avoid all platinum electrode where the platinum layer are thinner than 100 micron, 200 micron platinum layer are ideal and costumer specific dimensions. Overcoat the full electrode with platinum to protect it from chemical attack. There should be no exposed silver at either end of the electrode.


Used tools: Beaker 2000ml, Stainless steel pan, Digital pH meter (need to calibrate with pH buffers pH4.01 and pH 7.01 regularly).

Used chemicals: HCl 30%, Potassium metabisulfite K2S2O5, Sodium persulphate Na2S2O8,

The cell: The cell are running outdoor with a plastic paint bucket and plastic seed bed foil it is covered. With Soft PVC Pipe Tube 6m the resulting gases are led away.

Making potassium chlorate: Every 1gramm KCl dissolved 2,9 gram H2O (saturated solution at room temperature) the pH keeped 6-7 2g/l sodium persulphate are used to reduce chlorine gas and help the process. Used cell 0,5l with 400ml solution and 138g KCl pH 6-7 used HCl cc 4ml to the 400ml solution/day and 0,5-1g sodium persulphate additive. Every day added the HCl until the process are end. 6V 4A car battery charger are used as power supply maximum 6A cell temperature 20-45°C runtime 1 week. Maximum of 2 Amps will actually pass through the cell (if a 10mm carbon cathode are used) this power supply with this small anode can handle this comfortably without overheating the cell, or overloading the power supply. The pH controll/day. Used a 1,5l plastic bootle into which the solution is poured added the HCl and shaked. All chlorine gas in the solution must be absorbed in pH 6-7. The pH are tested with digital pH meter what calibrated with pH 7.01 and 4.01 buffers. 1 week later all KClO3 are crystallized in the solutoin washed with ice cold water. Dissolved in hot water filtered with all purpose cloth and recrystallized in double water than crystals when cooled down at room temperature. When the solution are boiled and the crystals started forming this point i stopped the heat and slowly cooled down the solution. Washed again the crystals and recrystallized again, washed again the crystals and dried out the crystals using a hotplate and a saucepan. The result minimum 99,5% pure KClO3. Using MMO RuO2, IrO2, TiO2 or Platinum (thickly coated 0,2mm) are ideal this process. With daily pH control experimentally possible to make the process with graphite anode or welding carbon rood and with NaClO3 too.

Making potassium perchlorate from sodium chlorate: Every 1gramm NaCl dissolved 2,8 gram H2O (saturated solution at room temperature) the pH keeped 6-7 2g/l sodium persulfate are used to reduce chlorine gas and help the process. Used cell 0,5l with 400ml solution and 142g NaCl pH 6-7 used HCl cc 4ml to the 400ml solution/day and 0,5-1g sodium persulfate adative. Every day added the HCl until the process are end. 6V 4A are used maximum 6A cell temperature 20-45°C total runtime 3 week.

The pH controll/day. Used a 1,5l plastic bootle into which the solution is poured added the HCl and shaked. All chlorine gas in the solution must be absorbed in pH 6-7. The pH are tested with digital pH meter what calibrated with pH 7.01 and 4.01 buffers. At the end the last 1 week when HCl added and no gases are formed this point the pH are keeped 7-8 and no more HCl are added. This point from pH 6 posible to go to pH -1 after a day running only in perchlorate cell. Only with Platinum (thickly coated 0,2mm) from NaCl to NaClO4 this process can make directly. With few micron platinum anode or PbO2 the chlorate must make first with MMO anode than the perchlorate with PbO2 or platinum. After 1,5 week need to test with sugar and methyline blue to calculate when the NaClO3 are complete and perchlorate start forming. At this point must change the MMO anode to perchlorate specific anode or the MMO anode will damaged. As cathode titan and graphite ar all excelent for chlorate and perchlorate production too. We will smell a strong ozone during perchlorate production. When PbO2 are used at the end of the process must keept the pH 7-8 and great care must be taken to wear the anode. Erosion is particularly high at the very end of the process. Lead dioxide is the most sensitive to this. Chlorate test here must be used in a test tube where with HCl and sodium or potassium metabisulfite are destroyed the chlorate. Do not make sensitive chlorate tests directly in the cell solution because some chlorate always left behind! This test is optional. When the perchlorate ready after that only ozone production happened. We cannot harm the process by electrolysis. When graphite cathode and platinum are used and the graphite cathode it starts to wear slightly the NaClO4 are ready. When the solution is absolute NaClO4 the erosion in the anode and cathode are extremely high. When 0,2mm platinum used in a silver rood base in KClO3 and NaClO4 setup no precise pH control is required unnecessary in such a case buy a costly pH meter. Just add the solution every 1000ml solution to 10ml 30% HCl/day this electrode does not hurt if the solution is much more acidic.

That it contains in large quantities NaClO3 it can be said with simple tests without costly sensitive tests. Dry from NaClO4 in the solution make it a fine powder and in a aluminum foil wrapped spoon start it to heat in a gas stove. You will can not melt NaClO4 just NaClO3 so not possible to melt together the crystals. Possible to use this test in a hotplate using a stainless steel saucepan is a small aluminum foil. Another test get the cell solution few mililiters heat it and mix it with hot KCl solution (the same concentration or slightly dilute solution than the double displacement reaction used). KClO3 can dissolved the hot solution, KClO4 are not. When the solution are cooled down and lot of colored large crystals forming that are KClO3. If almost nothing crystallize out when the solution cooled down thats KClO4 and thats OK. If in the hot sulution when mixed are not formed white crystals as as that point the solutions meet that not KClO4. If The KClO4 boiled with HCl and K metabisulfide and the solution will turn strongly yellow thats mean the solution strongly contaminated with chlorate. When boiled and you will not see yellowish color change and smell lot of SO2 gas, and when be concentrated, it will be dark brown not yellow thats OK. They are sensitive professional chlorate tests like N-Phenylanthranilic Acid, Aniline Reagent, Aniline Sulphate, Indigo Carmine, they cost a lot. If we keep the cell the same parameters and same runtime we does not need tests like this. We can reproduce the same quality purity from cell regularly.

The double displacement reaction: In the cell from every 100g NaCl calculated to get 210g NaClO4. The NaClO4, KCl it is never dried out. Stainless steel saucepan not tolerate to heat in in these wet crystals and get rusted and damaged when heated these wet crystals in it. This solution are boiled close to 1g NaClO4+0,5g H2O (saturated solution at room temperature) When NaClO4 intensive way start to crystalizing out. We need a saturated NaClO4 solution calculated at room temperature. Every 1g KCl dissolved 2,9g H2O (saturated solution at room temperature). And every 1g NaClO4 calculated 0,6g KCl and the KCl+NaClO4 solutions are mixed with hot minimum 80°C. From the 142g NaCl 298g NaClO4 calculated. The 298g NaClO4 dissolved 149g H2O (saturated solution at room temperature). From the 298g NaClO4 179g KCl calculated and the 179g KCl dissolved in 519g H2O (saturated solution at room temperature) and the KCl+NaClO4 solution are mixed with minimum 80°C. After this cooled down at room temperature and the crystals are washed in ice cold water mixed thoroughly with a spoon than  filtered in a all purpose cloth. First must make destroy the chlorate in the KClO4 solution calculate the total NaClO4 5-10% sodium or potassium metabisulfide and with HCl make the solution under pH 3. The HCl should be added proportionately tho the K2S2O5 (metabisulfite). For this process must be used a 2000ml beaker, do not use stainless steel! Use a Wire Gauze Heat Shield with Ceramic Center to protect the beaker from thermal shock or will be cracked or use a sand bath this is important. Directtly heating in a hot plate the beaker are easy way cracked if we heated strongly and uneven heat distribution in the hot plate. And boil it important to generate SO2 gas. When boiling add more HCl to form SO2 gas from the metabisulfite. Make first a 130g/l KClO4 solution add to it the 5% K2S2O5 and some HCl, when the salt are hot and dissolved add more KClO4 to get a concentrated solution HCl and metabisulfite. Add this as solution slowly with a pipette, or using a plastic straw and syringe under the solution. Boil it 1 hour and when the crystals start forming make tests with concentrated HCl, when they are stay white that product are ok. When the solution are clean and not yellowish color change and forms lot of SO2 gas that KClO4 are ok. After this cooled down at room temperature the acidic solution must be double than the crystals and filtered.  The crystals are washed in ice cold water mixed thoroughly with a spoon washed with potassium or sodium bicarbonate to neutralize the acidic pH washed in ice cold water again than  filtered in a all purpose cloth.The next step completely dissolve the crystals in hot water, to form the crystals under double water when the solution cooled down,  and recrystallized again 2 time (wash it gently with ice cold water between the two crystallization). The 2X recrystallization are important to get pure KClO4. If you have 200ml crystals, the solution above not be less than 600ml when all the crystals precipitate out of solution when cooled down slowly to room temperature. In a gas stove using a hotplate and a saucepan the crystals are dried out. The fine powdered KClO4 are tested with 30% HCl. First the HCl added to the powder. If stays white no reaction the KClO4 are ok. Yellowish color change are chlorate contamination. Grayish need to re crystal again! The end pure result what measured in a electric balance was 294g KClO4 from this cell. Purity around 99,7%, purer quality than the basic factory technical grade. The NaCl are recovered in a chlorate cell.

Ammonium perchlorate: Every 1g NaClO4 calculated 0,5g H2O (saturated solution at room temperature). And every 1g NH4Cl calculated 2,7g H2O (saturated solution at room temperature). Every 1g NaClO4 calculated 0,5g NH4Cl. Here need to dry the NH4ClO4 in a glass or ceramic baking dish at under 100°C because under 200°C starting the NH4ClO4 decomposition.

Potassium perchlorate alternative ways: Using sodium or potassium chlorate thermal decomposition. With NaClO3 and KClO3 all of them the minimum are 400°C where possible to start the decomposition process. Using a ceramic crucible and a bunsen burner or propane burner possible to make, High Pressure Propane Stove Outdoor Cooker are the bast way where ceramic crucible can be heated on a large surface. Need a ceramic tool what inert with the melted chlorate and tolerate the high temperature. In a gas stove not possible to get this temperature using a ceramic crucible! See patent US 2733982. Mini grill with a precise thermometer suitable for the process. Recommended to keep the temperature under 450°C. Pans are useless for this process, the chlorates are attack them and they not tolerate this high temperature. Example possible to get 400°C using a ceramic pan in a gas stove, but the pan are not tolerating this extreme heat and after few use will be cracked. When i tested using sodium chlorate are much more ideal to this process than using KClO3. The reaction proceeds faster and the NaClO4 melting point are 468°C so when the reaction complete the melted chlorate turned solid perchlorate. Recommended to using to the process KClO3 and NaClO3 too. The process depends on the temperature minimum one hour. The method is costly and difficult. The NaClO4 from NaCl need to separate with crystallization. The NaCl will precipitates which is less soluble. And the NaClO4 solution must react with KClO4/KCl product to convert all KCl to KClO4.

Making perchlorates without platinum or lead dioxide using non reductive acids: 1 way without ozone generator: using 40% Nitric Acid HNO3 (NO2 free), boil it in NaClO3 and you will get NaNO3+NaClO3 at 3:1 ratio with 30% yield. Chlorine will produced in the reaction without explosive ClO2 gas. Nitric acid HNO3 can be prepared from Ca(NO3)2, Mg(NO3)2. H2SO4 can be prepared using oxalic acid C2H2O4 with MgSO4. 2 way more effective way with high yield using ozone generator: Use in this process 60% nitric acid boil it in 15% KClO3 and use a ozone generator minimum 2g/hour (minimum 50% concentrated HNO3 required to this second process!). Remove the KNO3 contamination using recrystallization in 316g/l water the KClO4 crystals and cool it down to room temperature. And make a secondary recystallization in pure water. See more on DTIC AD0016814 research and US 2858188 A patent. By heating a glass wrapped in aluminum foil in sand, we can make a cheap device in which we can heat and distill. By putting ice on top of a container and  nitric acid will dropping into a glass inside the glass container, you can make a cheap and simple distillation device. Using the method, perchlorates can also be prepared by those who have simple graphite electrodes and it is a problem for them to reach a high temperature. From barium carbonate with pH control easy to make BaCl2 and Ba(ClO3)2 using even a simple graphite anode, than converting it to Ba(ClO4)2 using HNO3 and ozone. Adding H2SO4 to the Ba(ClO4)2, Ba(NO3)2, HNO3 mixture will convert Ba(ClO4)2, Ba(NO3)2, to HNO3 and HClO4 with insoluble BaSO4. Using filtration, distillation you will get perchloric and nitric acid. Or you can boil in the HNO3+HClO4 mixture KClO3 in presence of ozone more effective way. Heating BaSO4 with charcoal above 600°C we can convert it to BaS, than reacting with HCl we get back the BaCl2, H2S are formed. With sedimentation, filtration, crystallization and washing the BaCl2 with ethanol we can clean it the BaCl2 crystals.

Know issues with eletrodes/synthesis: All electrodes all tolerate maximum 6V 400-5000ml setup! In a 400-1500ml setup 4-6A are used. The cell maximal temperature are 45°C. The cell must keep under 40°C in a perchlorate cell or the anode erosion will be high. In the cell with NaClO4 without pH controlling the process will be too slow, and the yield are low too. Hot cells are not important in chlorate production and heating the cell with too much amps are crash perchlorate anodes! Platinum anodes tolerate alkali and acidic solutions too. MMO anodes not tolerate highly acidic sulutions. In long term by users feedback better to protect the MMO from too much acidic cell. PbO2 anodes not tolerate highly alkali solutions slightly acidic solutions more ideal to PbO2. In perchlorate cell only working strong BETA PbO2 coating alfa coatings will crash fast in this setup. Stainless steel limited of them what working in a chlorate and perchlorate cell as cathode, i not recommend it to use. The minimum platinum size for a platinum electrode are 3x70mm pure silver core cylindrical anode with 200micron pure platinum layer. Electrodes below this parameter are unsuitable for chlorate, perchlorate production. Overcoat the full electrode with platinum to protect it from chemical attack. There should be no exposed silver at either end of the electrode. Avoid all platinum electrode where the platinum layer are thinner than 100 micron, 200 micron platinum layer are ideal! However, I do not recommend non-adjustable power supplies because they can easily be overloaded.The best choice are a 10A Laboratory DC Power Supply Variable This avoids overloading the power supply or overheating the cell.



Amp calculation for another electrodes a colder 30-45°C clorate/perchlorate setup 0,5-5l cells: As a rule of thumb no more than 2 amperes per 100 ml of electrolyte must be passed through a chlorate cell. I calculated for using 1 amperes per 100 ml for a colder setup. What good for 0,5l to 2l setups 0,5-2l 6V- 4-6A are used, for 1,5l-2l setups 5-6V. 15A are used only if the electrodes are tolerating max 15A like a minimum 50x200mm, 60x150mm and larger PbO2 anode without problems for minimum 5l cells to avoid overheating the cell!

70mm x 3mm x0,2mm pure platinum clad anode in a silver base: Maximum 6V 6A 0,5-2l cell

Platinized Titanium Mesh Anode 1" x 4" or 2" x 3"(only in perchlorate setup): 6V 6A (maximum 6A) are not problem for this anode. This should be held between two titanium plates cathode of the same size for the maximum eletrical effectivity important! Too much amps will ruin this anode! I do not recommend to use 2,5 micron platinized titanium anodes they are not durable. Platinum clad anodes 50-100 micron in a thin niobium outer layer and copper core base, or much better 200 micron in a silver base a durable solution for long term. And there is not too high difference in price in the case of size the above-mentioned electrode. For the few micron platinized titanium anodes have too many complaints users that they are not durable at long term.

PbO2 and MMO anode: For 50x200mm, 60x150mm and larger anodes 6V max 15A are not problem. For minimum 5l setups 15A are recommended, under 2l max 6A. MMO anode be held between two titanium plates cathode of the same size for the maximum electrical effectivity. PbO2 must keep far from the cathode what pH are alkali and this does not like the PbO2.

For minimum 5l setup a computer or used server power supply with 5V 15-17A with connecting together parallel thin wires ideal to cheap way set the required amps for the cell without costly adjustable precision PSU (with adjustable current Amps). Less than 5l with 15A are overheating the cell if the Amps are not precisely controlled! However, I do not recommend non-adjustable power supplies because they can easily be overloaded.The best choice are a 10A Laboratory DC Power Supply Variable This avoids overloading the power supply or overheating the cell.

Increasing unstable KClO3 stability: First need to grind the KClO3 to a fine powder. Than this powder need to heat at 150-200°C to get a moisture free powder. When cooled down need to mixed with +5% KHCO3 potassium bicarbonate. If sulfur are used mix the sulfur with 1/4 KHCO3 too important! This process reduce friction sensitivity. I do not recommend the use of potassium chlorate except smoke bombs, mach compositions, shoot plastic disc caps where it cannot be replaced. With Sulfur, Mg, Sb2S3, extremely sensitive for friction. If anyone wants to experiment with it and want make unstable mixtures like KClO3/Mg/S this process reduces minimal to ignite the composition when friction temporarily. The technique could reduce the problem but not eliminate it! In stars, flash powder, whistle mix, highly not recommended to use KClO3!

KClO3+NaClO4 setup for cyclic potassium perchlorate production (for advanced users): Platinum anode is recommended for this, because KClO4 can be deposited on lead dioxide. For every 1 cell KClO3 crystals calculated 1 same sized NaClO4 cell solution for the reaction. The KClO3 513g/l added to the not concentrated NaClO4 and both solutions are degree 90°C. The KClO3 must added slowly to the NaClO4 solution, KClO4 crystals must formed, and if this stops, it must be stopped adding the KClO3 because the solution in this case will contaminated with large amount of KClO3! This is therefore very important to monitored. After the reaction the solution with the crystals are cooled down to room temperature and filtered.  The NaClO3 converted back to NaClO4 and the KClO4 crystals are boiled in the cell solution, (do not try to dissolve in this solution) to make the crystals less chlorate contamination as possible. After this cooled down to room temperature, filtered and the crystals are putted in ice cold water stir it in the water and filter. This conversion are will be fast! The idea are using the CN102807192A patent. Its reaction formula is following: NaClO4+ KClO3=KClO4+ NaClO3  After this the chlorate are destroyed with the metabisulfite+HCl boiling method. After this cooled down at room temperature and the crystals are washed in ice cold water mixed thoroughly with a spoon washed with potassium or sodium bicarbonate washed in ice cold water again than  filtered in a all purpose cloth. And with 2X recrystallization in pure water, and washing the crystals in ice cold water the KClO4 are cleaned. The NaClO4 can be recovered unlimited time in this process. Just need to refill the cell small amount of NaClO3 some times. With this process chlorate anodes does not contact perchlorate ions, and in the perchlorate cell does not have lot of chloride ions what are highly corrosive for the anodes if the sodium are recovered. The method is especially recommended for those who can produce KClO3 quickly, but NaClO3 and NaClO4 production is slow for them. pH control are required in this setup!

Sources:
http://www.chlorates.exrockets.com/kperchlo.html
http://www.chlorates.exrockets.com/destroy.html
http://www.chlorates.exrockets.com/tests.html
https://patents.google.com/patent/US2733982A/en