Making chlorate and perchlorate
     
This file has two parts... the first is predominantly about
KClO4, and the second about KClO3.   Both were taken from the
net, original sources unknown.



 MAKING POTASSIUM PERCHLORATE


     This proceedure is a "tried and true" method.  Unlike
     some rec.pyro postings, which are informational, or just
     plain speculative, this proceedure WORKS.  I have used it
     myself to make my own supply of perchlorate -  until I 
     decided to quit because I was making it far too fast to use.

     This proceedure works well to make chlorates as well.  The
     proceedure can be modified easily to make only chlorates.
     When using this proceedure to make perchlorate, it produces
     significant amounts of chlorate as a by-product.  This is
     because carbon rods are not highly efficient in converting
     chlorate to perchlorate. Other anodes work better, but this
     proceedure was designed using easily available common
     materials and supplies.

                              --- Author



Carbon Rods

     Get some carbon rods from the welding shop.  They are made by
     "arcair", and are 3/8" diameter by 12" long, and cost between
     40 to 60 cents(US) each.  They are copper plated, and they are used
     for a welding proceedure known as "gouging".

     Cut off the top of a plastic 1 gallon milk jug.  This is a
     good cheap source of containers for using in this proceedure.

     Dissolve 1/2 cup of salt in 2 liters of warm water.  Put this
     in a small plastic container.  Cut out a piece of coffee can,
     roughly 4" by 4" with a tab extending up to connect a wire to.
     The dimensions are not critical.  With a 6 volt battery charger,
     connect the minus (-) connector to the piece of coffee can.
     Wrap some aluminum foil on the end of the carbon rod, to improve
     the electrical connection, and connect the plus (+) connector
     of the charger to it.

     Turn on the charger, and let it run for about 20 minutes.  The
     copper will be removed from the rod.  If some still remains,
     run it for a little longer till it is free of copper.

     Discard the salt water used to remove the copper.

     <p>You can probably use a 12V charger, but the current may get too
     high, so you may need to reduce how much of the rod is being
     etched at one time.



Electrolyte solution

       Make a mixture of salt and potassium chloride solutions.
       Dissolve roughly 2 ounces (60 grams) of salt, and 8 ounces
       (240 grams) of potassium chloride in 2 liters (just a bit
       more than 2 quarts) of hot water.  There is much room for
       inaccuracy here, because the exact mixture is not absolutely 
       critical.

       At this point, it is good to add between 2 to 10 grams of
       either potassium chromate or dichromate.  While this is not
       absolutely necessary, it helps improve how much perchlorate
       is finally produced.  The process will work without it, but
       not quite as well.

       NOTE: Potassium chloride can be obtained as several commonly
          available products, such as: dietary salt substitute,
          ice melter (look at label for actual contents), and
          "muriate of potash" from farm and garden supply shops.
          Hagenow Laboratories carries potassium dichromate.

       The reason a mixture of salt and KCl is used, is two fold.
       First, salt is more easily electrolyzed than KCl, but after
       it converts to chlorate (and perchlorate), it will tend form
       the potassium salt instead of the sodium salt.  The electrolysis
       tends to work on the sodium salt, while the final potassium
       perchlorate forms, and due to it's poor solubility, tends to
       crystalize out of solution.  Secondly, the concentration of
       KCl is chosen to help prevent chlorate from crystalizing out,
       while being too high for the perchlorate to remain in solution,
       which causes it to crystalize out as it is created.  These
       concentrations may be varied, to compensate for different
       operating temperatures.  It was designed to operate at 40C, and
       will work fine above that temp, but below it, you might get
       some chlorate crysatlizing out, in which case you might need to
       reduce the amount of KCl just a little.

       I have been using a little salt in my mixture, but someone could 
       exclusively electrolyze KCl, without the addition of salt.  The
       purpose of the salt is to provide a sodium salt which is more
       easily electrolyzed than the potassium salt.  It is NOT necessary,
       and will probably work well with only KCl.

 ****** (Chlorate note) ******

      BTW, chlorates are produced here as an intermediate chemical
      product.  Chlorates tend to be the predominant component around
      1 1/2 to 2 days of operation.  Chlorate could be caused to
      crystalize out during electrolysis if the concentration of KCl
      in the starting electrolyte solution is increased to nearly 
      saturation (about 21 ounces KCl/ with 2 ounces of salt). Although 
      I have not concentrated on chlorate production, I would expect that 
      you could actually run it for more than 2 days - possibly up to
      4 or 5 days, and keep building up a layer of largely chlorate 
      crystals on the bottom.  In that case, I would _GUESS_ that you could
      get around 2 pounds of chlorate after 5 days of operation.  



Electrolysis

      Using a coffee can for a source of steel, cut it out to form
      an inverted U shaped trough.  Insert it in the mixture of salt
      and KCl dissolved in water.  The (-) connector is connected to
      the steel.  The steel U trough (similar to a rain gutter, except
      upside down) is setting at an angle to increase the amount of
      surface area in contact with the liquid.  The carbon rod has
      some aluminum foil wrapped around the end of the rod, and the (+)
      connector is connected to it.  The rod is positioned within the
      U shaped trough - under it, without touching.  The charger is
      turned on, and he position & depth of the rod is adjusted to
      get 8 to 12 amps of current.

     NOTE: A setup with the electrodes running electricity through
           an electrolyte is called a "Cell".  This setup is commonly
           refered to as a cell throughout this description.

      Let the liquid electrolyze for about 5 days continuously.
      Add water to make up for water lost during the process, and
      try to keep it roughly constant.

      A couple times a day, you will need to check the current level,
      and adjust the rod position to keep the current in the 8-12amp
      range.  Mine has been running between 40 - 50C, but commercial
      proceedures keep the temp just below 40C to reduce carbon rod
      errosion.  The rods will gradually errode away, but if you use
      a 6V charger, one rod will probably last for the full 5 days.

     You can also use higher voltage chargers, but you will probably
     need to connect several electrolytic cells together to keep
     the voltage accross ONE cell to be about 6 volts.  If you use
     a 12 V charger, you will need 2 cells ( 12V/(6V per cell) = 2cells).
     If you connect more than 1 cell in series, you may need to use
     a voltmeter to check the actual voltage accross each cell - because
     it will change depending upon the resistance differences between
     the cells, which can be adjusted by re-positioning the rods.

     The purpose for the U shaped trough cathode (-) electrode, is to
     cause the gas bubbles formed to generate a convection flow up
     through the trough.  This causes the chemical products produced
     at each electrode to mix and react efficiently.  Other electrode
     geometries will work, some better, and others worse.  The key
     is to cause the two electrodes to be very close to each other,
     and cause the chemical products to mix well to help form chlorate
     and perchlorates.  The WORST case situation is where the electrodes
     are on opposite sides of the cell, causing the chlorine gas
     produced at the anode (+) to tend to bubble and escape
     out of solution into the air.



Crystalization

     The potassium perchlorate crystalizes out
     as it electrolyzes.  When you're done, you have a mixture of
     black carbon, perchlorate, and some chlorate after you drain
     off the liquid.  I generally get a layer of perchlorate
     crystals about 1 inch (2.5cm) thick on the bottom, which tends
     to be about 1 pound.

      Cool the liquid in a freezer to help increase the amount of
      perchlorate that is crystalized out, before draining the electrolyte
      liquid.  When draining the electrolyte, save it if you want to
      re-electrolyze it to make even more perchlorate again.

      Load the crystals into a filter, and use boiling water to 
      dissolve the perchlorate out.  As it filters, the perchlorate forms 
      nice flat rhombic shaped (almost square) flakes that float out of
      solution.  You watch it as it cools, and watch for chlorate crystals, 
      which tend to look like clusters of cactus needles.  When they
      start to form (well after the perchlorate has largely
      crystalized out), you drain the liquid, and add some room
      temp water which is to be about 2 - 3 times the volume of the
      crystals you have in the container.  Shake them, and let it
      stand overnight to dissolve any chlorate crystals.  Then
      drain, wash (with ice cold water), and dry the crystals.

     NOTE: Coffee filters generally aren't good enough to filter out
           the black carbon particles.  You can load a coffee filter
           with a good layer of diatomaceous earth, and then use it
           to filter the liquid.  Diatomaceous earth is used to filter
           swimming pool water, and a 10 pound bag can be obtained
           for less than US$10.00.  

       You can purify them again by weighing the dried crystals,
       and adding enough water to dissolve the whole mass as if it
       was pure chlorate (i.e. 7g/100ml water)*.  Use hot water, and
       then cool it down to room temp.  You might even need to cool
       get the perchlorate to begin to crystalize (it seems to
       super saturate commonly). You might be able to get it
       started by adding a small amount of perchlorate dust as
       crystal seeds - if you have some to start with.. Then wash
       your crystals (with ICE COLD water), and dry them.  That will
       help produce a higher purity product of perchlorate.  If you
       want to make a chlorate-free batch of perchlorate, repeat this
       process again. It will be essentailly free of chlorate if you
       double crystalize it, and make certain you wash the crystals
       several times with cold water.

       Example:  100 grams of crystals would require
       100grams/(7gm/100ml) = 14.3 (100 ml), or 1430 ml of water,
       or about 48 ounces.

       NOTE: When harvesting the crystals, a cotton cloth makes a 
       good filter.  I wear rubber gloves, and squeeze the excess liquid 
       from the crystals before & during washing them.  Squeezing
       helps remove additional contaminants which are dissolved
       in the liquid that wouldn't otherwise be removed by
       simple gravity filtering.  While this method loses very
       small crystaline particles, the loss tends to be very small
       in comparison to the amount of crystals harvested.

        Perchlorate is very easy to make, but it takes a little
        work.  The hardest ingredient to get is patience.

      
WARNINGS


     This proceedure generates small amounts of chlorine gas, as well
     as hydrogen gas.  It should be conducted outdoors, or in a well
     ventilated building which is NOT used for living quarters!  Hydrogen
     can accumulate in non-ventilated and sealed rooms to form potentially
     explosive mixtures with air!!  Chlorine generally is more of a 
     irritant, but can be poisonous at high concentrations.  There are
     also other (?) chlorine oxides and/or ozone produced which should
     also be avoided.

     Chlorates and perchlorates are NOT chemicals for playing!!  They
     are serious oxidizing agents which can be used to make VERY DANGEROUS
     pyrotechnic mixtures - _ESPECIALLY CHLORATES_ !!!  Be certain to
     read up on all litterature describing the use and dangers of these
     compounds!  It is VERY EASY to forget the safety hazards associated
     with these oxidizers in a time of haste - and lose a limb or your
     life as a result of your forgetfulness!  Be careful to clean up
     any oxidizer which is spilled on carpets, or solutions which have
     spilled or splashed on any form of flamable material, including
     clothes, wood, paper, etc. 

CHLORATES ARE ESPECIALLY FRICTION AND SHOCK SENSITIVE!  
PERCHLORATES CAN ALSO PRESENT THE SAME HAZARDS, BUT NOT AS 
BADLY AS CHLORATES! 
 
ALSO, AVOID THE DISASTEROUS MIXTURE OF CHLORATE WITH SULFUR.  
NEVER MIX EITHER OF THESE WITH ANY FORM OF PHOSPHORUS, AS IT 
CAN IGNITE OR EXPLODE BY THE FRICTION OF SIMPLY MIXING THEM!!!!! 

Also, chlorates must be kept from any form of acids, especially
sulfuric.  Even small traces of acids (from the presence of sulfur,
etc) can cause what "appeared" to be a stable mixture, to ignite at
some unknown time later!
