nbk2000
June 13th, 2005, 12:02 PM
I downloaded this patent from an thread at SM.org and, having the materials on hand, gave it a try.
I can attest to it being factually correct, my kitchen still reeking of chlorine. :)
According to the patent, a mole of TCCA (Pool shock) and 3 moles of Sodium Chloride (table salt) are mixed together and a small amount of water added, the whole mixture being subjected to either vacuum or heating to release the chlorine.
The mixture, upon exhaustion of the chlorine, is composed of water and sodium cyanurate, which is what I was primarily interested in obtaining.
Sodium Cyanurate, Na3(NCO)3, seems like an excellent candidate for carbon reduction to Sodium Cyanide:
Na3(NCO)3 + 3C = 3NaCN + 3CO
I measured out the approximate ratio, at 1/100th mole quantites, thus 2.3gm of TCCA and 1.7gm of NaCl, and just enough water to moisten, in a covered glass jar placed in a hot water bath.
After a couple of minutes, the mixture turned a pale Grape Kool-Aid purple (because of the CuSO4 in the TCCA) and, upon sniffing a waft of the steamy vapor emitting from the jar, the smell of chlorine was overpowering and left me gasping and my eyes watering.
There was still particles of undissolved TCCA circulating, so the reaction wasn't over, but I dumped the mix down the universal disposal receptacle (the shitter ;)) ASAP, the experiment having been proven successful.
Since the reaction can also be run in a dry state, that would be the most desirable one to use, as then the gas would be dry and not requiring drying prior to use.
Cl3(NCO)3 + 3NaCl = 3Cl2 + Na3(NCO)3
The weight of chlorine being produced being almost equal to the weight of the TCCA in the reaction.
Though I wonder what the effect of 1% of copper sulfate has on the reaction. Probably not much.
Having a ready source of anhydrous chlorine gas for use in reactions, and getting a useable by-product, all from very cheap OTC components, seems desirable to me.
Oh, and by substituting Sodium Bromide (spa chemical) for the NaCl, you can get elemental Bromine instead of Chlorine, bromine being very useful for making powerful lachrymators such as bromacetone and brombenzyl cyanide which is even more powerful than CN, on par with CS, and can be made entirely from OTC chemicals. :)
Industrially, Brombenzyl cyanide is prepared in three steps, as follows:
(1) chlorination of toluene to form benzyl chloride (TCCA + Salt+Paint Stripper)
(2) the conversion of benzyl chloride to benzyl cyanide by the action of sodium cyanide in alcoholic solution (Cyanide made from by-product of reaction 1 + Everclear alcohol)
(3) the bromination of the benzyl cyanide with bromine vapor in the presence of sunlight. (More TCCA + Sodium Bromide spa clarifier)
According to Sartori (page 197 War Gases), it's advisable that you skip the use of benzyl chloride and use benzyl bromide instead, converting that to benzyl cyanide, then use more bromine to form the desired brombenzyl cyanide.
I can attest to it being factually correct, my kitchen still reeking of chlorine. :)
According to the patent, a mole of TCCA (Pool shock) and 3 moles of Sodium Chloride (table salt) are mixed together and a small amount of water added, the whole mixture being subjected to either vacuum or heating to release the chlorine.
The mixture, upon exhaustion of the chlorine, is composed of water and sodium cyanurate, which is what I was primarily interested in obtaining.
Sodium Cyanurate, Na3(NCO)3, seems like an excellent candidate for carbon reduction to Sodium Cyanide:
Na3(NCO)3 + 3C = 3NaCN + 3CO
I measured out the approximate ratio, at 1/100th mole quantites, thus 2.3gm of TCCA and 1.7gm of NaCl, and just enough water to moisten, in a covered glass jar placed in a hot water bath.
After a couple of minutes, the mixture turned a pale Grape Kool-Aid purple (because of the CuSO4 in the TCCA) and, upon sniffing a waft of the steamy vapor emitting from the jar, the smell of chlorine was overpowering and left me gasping and my eyes watering.
There was still particles of undissolved TCCA circulating, so the reaction wasn't over, but I dumped the mix down the universal disposal receptacle (the shitter ;)) ASAP, the experiment having been proven successful.
Since the reaction can also be run in a dry state, that would be the most desirable one to use, as then the gas would be dry and not requiring drying prior to use.
Cl3(NCO)3 + 3NaCl = 3Cl2 + Na3(NCO)3
The weight of chlorine being produced being almost equal to the weight of the TCCA in the reaction.
Though I wonder what the effect of 1% of copper sulfate has on the reaction. Probably not much.
Having a ready source of anhydrous chlorine gas for use in reactions, and getting a useable by-product, all from very cheap OTC components, seems desirable to me.
Oh, and by substituting Sodium Bromide (spa chemical) for the NaCl, you can get elemental Bromine instead of Chlorine, bromine being very useful for making powerful lachrymators such as bromacetone and brombenzyl cyanide which is even more powerful than CN, on par with CS, and can be made entirely from OTC chemicals. :)
Industrially, Brombenzyl cyanide is prepared in three steps, as follows:
(1) chlorination of toluene to form benzyl chloride (TCCA + Salt+Paint Stripper)
(2) the conversion of benzyl chloride to benzyl cyanide by the action of sodium cyanide in alcoholic solution (Cyanide made from by-product of reaction 1 + Everclear alcohol)
(3) the bromination of the benzyl cyanide with bromine vapor in the presence of sunlight. (More TCCA + Sodium Bromide spa clarifier)
According to Sartori (page 197 War Gases), it's advisable that you skip the use of benzyl chloride and use benzyl bromide instead, converting that to benzyl cyanide, then use more bromine to form the desired brombenzyl cyanide.