Sciencemadness Discussion Board

Formaldehyde from Hexamine

Hawkguy - 21-8-2015 at 08:15

Hello. I'm getting into a project now to make Pentaerythritol from the most easily available chemicals possible. I've already made very pure Calcium Oxide from eggshells, and I've gotten most of the way making Acetaldehyde from OTC solvents(Ethanol/ Acetone). All I need is Formaldehyde. I've tried oxidizing Methanol with a hot copper catalyst, but it was slow, inefficient, and dangerous. I was running Methanol vapour over red hot copper, and into water. At one point it exploded violently. Not a woosh, but an explosion. So that was that. I then found a method of making formaldehyde on Erowid, and also in a related Sciencemadness thread. Apparently Hydrochloric Acid will make Ammonium Chloride and Formaldehyde from Hexamine and water, in a reaction I'm assuming to be: (CH2)6N4 + 4HCl + 6H2O -> 4NH4Cl + 6CH2O. I'm asking if anyone has done this, and what they can say about it. Or if it even works.

PHILOU Zrealone - 21-8-2015 at 08:45

You haven't read the entire sheet...
Methylamine Synthesis FAQ

You also get mostly methylamine, dimethylamine and eventually trimethylamine hydrochlorides...aside with formic acid (methanoic acid) because the CH2=O oxydo-redox to discrete methanol and formic acid.

chemrox - 21-8-2015 at 14:15

hexamine plus acid should release formaldehyde and ammonia

Camroc37 - 17-11-2015 at 19:13

Quote: Originally posted by Hawkguy  
Hello. I'm getting into a project now to make Pentaerythritol from the most easily available chemicals possible. I've already made very pure Calcium Oxide from eggshells, and I've gotten most of the way making Acetaldehyde from OTC solvents(Ethanol/ Acetone). All I need is Formaldehyde. I've tried oxidizing Methanol with a hot copper catalyst, but it was slow, inefficient, and dangerous. I was running Methanol vapour over red hot copper, and into water. At one point it exploded violently. Not a woosh, but an explosion. So that was that. I then found a method of making formaldehyde on Erowid, and also in a related Sciencemadness thread. Apparently Hydrochloric Acid will make Ammonium Chloride and Formaldehyde from Hexamine and water, in a reaction I'm assuming to be: (CH2)6N4 + 4HCl + 6H2O -> 4NH4Cl + 6CH2O. I'm asking if anyone has done this, and what they can say about it. Or if it even works.

How did you go about getting the CaO from eggshells?

Hawkguy - 17-11-2015 at 21:30

Quote: Originally posted by Camroc37  
Quote: Originally posted by Hawkguy  
Hello. I'm getting into a project now to make Pentaerythritol from the most easily available chemicals possible. I've already made very pure Calcium Oxide from eggshells, and I've gotten most of the way making Acetaldehyde from OTC solvents(Ethanol/ Acetone). All I need is Formaldehyde. I've tried oxidizing Methanol with a hot copper catalyst, but it was slow, inefficient, and dangerous. I was running Methanol vapour over red hot copper, and into water. At one point it exploded violently. Not a woosh, but an explosion. So that was that. I then found a method of making formaldehyde on Erowid, and also in a related Sciencemadness thread. Apparently Hydrochloric Acid will make Ammonium Chloride and Formaldehyde from Hexamine and water, in a reaction I'm assuming to be: (CH2)6N4 + 4HCl + 6H2O -> 4NH4Cl + 6CH2O. I'm asking if anyone has done this, and what they can say about it. Or if it even works.

How did you go about getting the CaO from eggshells? [/requite] I dissolved them in Hydrochloric Acid and filtered it, collecting a solution of Calcium Chloride. I mixed the solution with another solution of sodium Hydroxide, to precipitate pure Calcium Hydroxide. I filtered and rinsed it, and dried it (this took too much effort, the Ca(OH)2 snot was like toothpaste). I dried it in a microwave, and heated the samples in little crucibles to about 6 or 7 hundred degrees C. It decomposes to Calcium Oxide, and would heat the hell up when I added water to a sample of the CaO on my palm.

Hawkguy - 17-11-2015 at 21:32

I did the experiment, and found that very little Formalin was produced by the Acid/ Hexamine. Most was oxidized to Formic Acid. I also made Acetaldehyde by chlorinating Ethanol, so far the best method by far. Pentaerythritol... Still far off though

macckone - 17-11-2015 at 22:33

You can buy formaldehyde and paraformaldehyde.
Commercially formaldehyde is made by basically the same process you
described. You have to have really close regulation of the oxygen or air.
Sounds like you had too much air. It is slow and tedious if you don't
have good regulation. You also wind up with a lot of formic acid and
other by products.

ps. The main difference in the commercial production is the catalyst
and careful control of conditions.

[Edited on 18-11-2015 by macckone]

ave369 - 17-11-2015 at 23:27

Quote: Originally posted by Hawkguy  
I did the experiment, and found that very little Formalin was produced by the Acid/ Hexamine. Most was oxidized to Formic Acid. I also made Acetaldehyde by chlorinating Ethanol, so far the best method by far. Pentaerythritol... Still far off though


Maybe, synthesize formic acid by this method (or any other, such as from glycerol and oxalic acid), neutralize it with chalk and calcine the resulting calcium formate, which results in more formaldehyde?

[Edited on 18-11-2015 by ave369]