Large-Scale Methamphetamine Manufacture

5.2 Chemicals

To make a useful amount of methylamine, the following is required.

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  10-20 gallons of 35-40% Formaldehyde
  
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  10kg Sodium hydroxide (lye)
  
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  Distilled water
  
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  A 40lb block of dry ice, wrapped in newspaper and stored in a good ice chest.
  
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  About 40lb of ice cubes or block ice from the supermarket
  
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  40-50kg of ammonium chloride. Industrial grade ammonium chloride is normally mixed with a little calcium chloride to keep it from clumping up and hardening and is called "treated" ammonium chloride. The calcium chloride does not affect the reaction, so one can use the cheap industrial 50lb bags.
  

5.3 Methylamine Hydrochloride

Set up the 10-liter rigid base heating mantle inside the fume cabinet. We will be generating some formaldehyde gas which one does not want to breathe.
Charge the reaction vessel with 3kg of ammonium chloride and 6 liters of 35-40% formaldehyde. The ammonium chloride will not dissolve, so stir it with a section of wooden dowling. Attach a 30cm West condenser, a vacuum takeoff, and a 2000ml receiver RB flask. Lead a short section of plastic tubing from the vacuum takeoff to a small pail of water. Use a clamp to place the end of the tube just under the surface of the water. Some of the gas generated will be absorbed by the water; the rest will go out the vent. Place a one-hole rubber stopper with a thermometer in one of the side holes on the triple-neck so the solution temperature can be easily read. The chemist then turns on the heat, setting the controls on 70% full-scale for a short time. When the solution temperature reaches 60°C, reduce the heat controls to about 25% and slowly bring the temperature up to 100°C. The ammonium chloride will now start to dissolve, and can be aided with some quick stirring with a dowling rod. As the solution reaches 70°C, a little gas will begin bubbling in the water pail. As the temperature climbs towards 100°C, a lot of gas will be generated, causing pressure inside the vessel. The pressure builds up because of the back pressure created by the West condenser, which is too small. In fact, the condenser is the limiting factor in this reaction, otherwise one would use a 22-liter setup and double the volume. This writer has performed this reaction in a 22-liter rig and does not recommend it. Those familiar with methylamine manufacture will be wondering why a pot of oil warmed to the correct temperature is not used; the answer is that this writer discovered that the solution temperature can be held at 104-106°C using a carefully controlled heating mantle. One will need to play with the control adjustments a little, but it is not difficult. If the chemist experiences difficulties holding a stable temperature, simply go back to the oil pot method. Reduce the heat to about 15% when the solution temperature reaches 100°C. Once the solution stabilizes at 105°C and the gas no longer bubbles in the water pail, the chemist can apply an aspirator vacuum at 15-30 minute intervals over the next 5 hours. At the end of 5 hours, turn off the heat, remove the triple-neck from the heating mantle, and let it cool down overnight to room temperature. The cooling causes a lot of ammonium chloride crystals to precipitate out of solution. Filter out the crystals, saving them in a separate bucket for later reuse, and save the light yellow filtrate in another bucket. Repeat this procedure several more times until a 20-24 liter bucket is full of liquid.
Next, set up the 10 liter triple-neck in the same manner as before and add about 7 liters of the accumulated intermediate-stage liquid. Set the heating mantle to about 30% and apply an aspirator vacuum of -28"Hg using a bleeder on the vacuum system. One should be careful to thoroughly grease all fittings with Dow-Corning High Vacuum Grease or it's equivalent to prevent glassware freeze-ups. The chemist now patiently distils water and acid out of the mixture until solids begin to come out of solution and strong "bumping" begins to occur inside the reaction vessel. This can take 5-6 hours or longer. At this point, turn off the heat, disassemble the rig, and pour the contents of the reaction vessel into a bucket inside the fume cabinet. Leave overnight to cool down to room temperature, at which point there will be another large slug of ammonium chloride crystals to filter out. This time, however, a little methylamine hydrochloride will be mixed in with the ammonium chloride. Because methylamine hydrochloride is very hygroscopic, the salts may be gooey. Filter through a Buchner, keeping the recovered salts in one bucket and the yellowish liquid in another. Repeat until there is enough liquid in the second-stage bucket to proceed to the third stage. One should be getting the idea now that one can increase the throughput in the system by simply setting up another 10-liter rig and processing in parallel. By organizing the separate stages properly, one person can produce about 80 liters of 40% methylamine in 9 weeks if one is dedicated. This is enough methylamine to make 175lb of pure methamphetamine.
In the third step, we use the second-stage liquid we have collected and pull more water and acid out of the solution using a vacuum of 26-27"Hg, which is slightly lower than the vacuum used during the second stage. The vacuum setting is important because if the vacuum is too strong it will induce "bumping" inside the reaction vessel and if it is too weak, not enough water will be pulled out to give us good quality crystals that do not melt the instant they contact moist air. Pull as much water as possible out of the solution before the methylamine hydrochloride crystals precipitate out of solution and strong "bumping" begins, then pull the reaction and let the hot mixture cool overnight. Using a clean Buchner, filter out the methylamine hydrochloride crystals thoroughly, then dump them into a 5 gallon bucket that has been resting in the freezer for a few days. Methylamine hydrochloride crystals are whitish platelet-type crystals. Keeping the crystals in the freezer where it is too cold for water to remain in the air prevents the crystals from picking up water from the air and melting. Throw out the residual thick golden liquid. Repeat the procedure until one has accumulated a full 5-gal bucket of frozen crystals, which is the amount that one can turn into methylamine solution in one day.