Sciencemadness Discussion Board

Trinitrotoluene preparation

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madscientist - 21-5-2002 at 16:37

I no longer have Megalomania's instructions for preparation of TNT on my hardrive (computer crashed); the site I uploaded his instructions to has suffered a plague of mysterious file deletion, one of the victims being the TNT preparation file; and, obviously, Megalomania's site is gone. Anyone have a copy of his instructions, or equally reliable and accuration instructions?

Coen - 21-5-2002 at 16:38

I don't have any copies of that site. But I think you are over-crediting that procedure of megalomania. It isn't that great really.
Just use a lot of mixed acid, the more the better, but atleast twice the stochiochemical quantity. Then slowly add the toluene with a sep funnel. Start heating the mixture to about 70 dC and keep that temperature for 2 hours. Most of the toluene is converted to DNT. Then put the mixture in a sep funnel and seperate the acid from the molten DNT. Put some new fresh mixed acid with that and heat the whole mixture again to 70 dC. Put in sep funnel again and seperate. All the boiling and stuff is off course done in a RB flask with a long reflux condensor. Heating off course with a heating mantle or oil bath. This is just from my own experience and works fine. The risk of runnaway reaction should not be underestimated and is quite high.

madscientist - 21-5-2002 at 16:39

Could you share information on how to tell if runaway nitration is imminent, such as runaway nitration temperature, changes in appearance, etcetra? I'm assuming that it would also be possible to extract the dinitrotoluene by cooling it, dumping into several times its own
volume of water, neutralizing the solution, and filtering out the dinitrotoluene (cold of course). I've heard that dinitrotoluene is a waxy solid. Is this true? Thanks for the above information. I recently found some very good instructions for someone with lots of patience (very detailed, three step method). It was not some crapbook quality instructions, either... I will try to find a link to those instructions.

madscientist - 21-5-2002 at 16:41

Quote:
Mr. Cool: There is also a method similar to the aspirin method for TNP. I haven't tried it myself, but I've heard that it works. You sulphonate the toluene with conc. H2SO4 for several hours under reflux, and then add KNO3. You need more H2SO4 and KNO3 than for TNP, you let it react for longer at each stage, and you do it at a higher temperature. I think using 50% more acid, KNO3, time and temperature will work fine. The person who told me about it apparently used the same molar ratios as for TNP via aspirin on my site (www.flashbangboom.homeste...age.html), and similar times and temperatures.

PHILOU Zrealone - 21-5-2002 at 16:42

For those who have little time and a lot of chemicals for cheap the one batch process is the way to go except you manipulate bigger batches to get the same yields and spend a lot more concentrated acids. Risks of runaway are bigger since you try to perform the trinitration in one step; T control is harder too since the batch is bigger...so cooling will be harder!
The economical way to go is to go two or three steps nitration...this allows you even to separate isomers for other synthesis (toluidines, toluols, polynitrotoluens over 3 NO2, nitrobenzoic acids, ....)

The first step involve medium concentration HNO3 (50 to 70%) with a little H2SO4 (medium conc)--> you get after refluxing at 80-90°C almost only mononitrotoluens (ortho, meta and para)(major compounds are ortho and para).

The second nitration requires 70%HNO3 with a little conc H2SO4--> you get dinitroToluens; if you didn't separate the isomer in the previous stage, you will get
2,3-2,4-2,5-2,6 dinitrotoluen
3,4-3,5-3,6 dinitrotoluen
Separation will then be harder now!
Major products are 2,4-2,6!

The third step involves HNO3 conc + H2SO4 conc at the same T:
And will lead to 2,4,6-TNT as a major product and all the other trisome combinations in various amounts:
2,3,4-2,3,5-2,3,6 TNT
2,4,5 TNT
3,4,5-3,4,6 TNT
+Some tertranitroToluens + some trinitrobenzoic acid + some tetranitromethane + some nitroform +....

This mix of isomers explains why DNT is waxy liquid-solid since some form are cristaline but dissolve partially in other isomeric liquid forms; also the presence of impurities in a compound lowers its melting point!

So you see that from this method in 3 steps, you use as efficiently as possible the acids and don't waste valuable conc HNO3 or H2SO4!
You also don't risk runaways this way (since the reaction time is delayed on 3 sessions and the first very exothermic reaction is tempered by the amount of water present in the medium conc acids!

Quantities of acid used are stoechiometric + 10%; and you only require very conc HNO3 for the last step!

Lets compare the two processes:
Fictive example:
You take 10g of toluen for both mono or 3 step:

Single step reaction:
10g Tol + 40 ml 98% HNO3 + 120 ml 98% H2SO4
Total batch size 173 ml! --> 22,2g (TNT 90% yield)

3 step reaction:
10g Tol + 15 ml 50% HNO3 + 30 ml 50% H2SO4
Total batch size 58 ml! -->14,7g (MNT 99% yield)

14,7g MNT + 11 ml 70% HNO3 + 20 ml 98% H2SO4
Total batch size 46 ml! --> 19g (DNT 97% yield)

19g DNT + 7,5 ml 98% HNO3 + 22 ml 98% H2SO4
Tot. b. s. 44,5 ml! --> 23g (TNT 97% yield)

Total of total batch size:
HNO3: 15 ml(50%) + 11 ml(70%) + 7,5 ml(98%)
or 33,5 ml of HNO3 (?%) --> 22,7 ml of 98% HNO3 equivalent!

H2SO4: 30 ml(50%) + 20 ml(98%) + 22 ml(98%)
or 57 ml 98% H2SO4 equivalent!

By comparing now one step vs 3 steps:
HNO3 98%: 40 ml vs 22,7ml
H2SO4 98%: 120 ml vs 57 ml
Yields: 90% (22,2g) vs 92,2% (23g)

Where does this difference come?
-HNO3 conc is used only when needed
-H2SO4 conc is used when needed and increased when needed too
-Volume of concentrated mixed acid is lower and thus solubility of DNT and TNT is lower...lower loss of compound when manipulating
-Better T control
-Less degradation into oxydation products in the two first stages!

PH Z

TNT

Nils - 10-7-2002 at 08:59

TIP: Don't synthesize your TNT in home. When you are nitrating C7H8 into MNT it stinks really bad like Almond. Also, the smell stays a while on your glassware. So wear Gloves and don't breath any fumes(suspected to be a carcogenic).

btw, i guess you can make TNT in one step, by using a little C7H8 and lots of mixed acids(proboubly highly concentrated , H2SO4 98%> and HNO3 95%>)


madscientist - 27-8-2002 at 14:02

How are polynitrotoluenes synthesized?

madscientist - 27-8-2002 at 16:42

I just discovered that the temperature where the reaction between toluene and highly concentrated mixed acid makes the transition from nitration to oxidation (runaway nitration) is 75C.

PHILOU Zrealone - 8-9-2002 at 15:47

Actually you probably think you can only go to trinitration of toluen-as I did when I was younger; but it is not the case!
Here is an example:
If you isolate metanitrotoluen, you can stil make the trinitration almost without problem in ortho and para position yielding tetranitrotoluen 2,3,4,6!
CH3-C6H5 --> TNT -partial reduction-> CH3-C6H2(NO2)2-NH2 --> HNO3 conc + H2SO4 conc --> CH3-C6(NO2)4-NH2 tetranitrotoluidine.

How do you think it is possible to make hexanitrobenzene?
NH2-C6(NO2)4-CH3 -HNO3/H2SO4/H2O2(all 100%)-> C6(NO2)6 + CO2 + H2O

PH Z

trinitrotoluene - 17-10-2002 at 22:57

Luckly i save the information in a disk because I know that someone is gonna close down that site after the bombing in finland. So heres meglomania method of making Trinitrotoluene.

melting point
80.1 °C boiling point
ignites at 295 °C trinitrotoluene molecular mass
227.13 g/mol density
1.654 g/mL
class (ABC) sensitivity
very low chemical formula
C7H5N3O6 explosive velocity
7028 m/s estimated cost
$?.00/g


2,4,6-trinitrotoluene, or just TNT, is the oft used military and industrial explosive that may be the among the best recognized explosive around. Other names for TNT include: trinitrotoluol; sym-trinitrotoluene; a-trinitrotoluol; 2-methyl-1,3,5-trinitrobenzene; entsufon; 1-methyl-2,4,6-trinitrobenzene; methyltrinitrobenzene; tolite; trilit; s-trinitrotoluene; s-trinitrotoluol; trotyl; sym-trinitrotoluol; alpha-trinitrotoluol; tolite; triton; tritol; trilite; tri; tutol; trinol; füllpulver 1902; Fp02; tritolo; trillit; tolita; tol; and trotil. TNT was first synthesized in 1863 by a scientist named Wilbrand who treated toluene with sulfuric and nitric acid at near boiling temperatures. Although there are several isomers of trinitrotoluene, only the 2,4,6- isomer is of importance. Pure TNT is in the form of small columns or needles and is insoluble in water. It is quite stable, being meltable ,or able to act like a plastic at around 50 °C. TNT can even be boiled although the experiments did this under reduced pressure (50mm Hg) to lower the boiling point to around 245 °C. The normal detonation temperature is 333 °C, the calculated boiling point at normal atmospheric pressure is 345 °C, so don't do it. Some experiments have determined that the presence of foreign material like 1.9% of Fe2O3 will lower the amount of time it takes for TNT to explode once it reaches its critical temperature, or 295 °C, the temperature at which decomposition begins. Also, mixing pure sulfur with TNT will lower the initiation temperature and increase the explosive power. For example, pure TNT explodes at 333 °C, 5% sulfur explodes at 304 °C, 10% sulfur at 294 °C, 20% sulfur at 284 °C, and 30% sulfur at 275 °C. The increase in explosive power is gained through the addition of 5-10% sulfur. Because the stability of TNT is so great, it is harder to detonate it, the sensitivity increases somewhat above 80º C, but is still rather low even when molten. A powerful blasting cap, or booster charge, will be needed to detonate TNT. This lab is carried out in three separate operations, forming mononitrotoluene, then dinitrotoluene, and finally trinitrotoluene. CHEMICALS APPARATUS
ethyl alcohol 100/500/600-mL beaker
nitric acid Buchner funnel
sodium bisulfite graduated cylinder
sulfuric acid pipet/buret
toluene separatory funnel
water stirrer/stirring rod
thermometer


Prepare a nitrating solution of 160 mL of 95% sulfuric acid and 105 mL of 75% nitric acid in a 500-mL beaker set in a salt-ice bath. Mix the acids very slowly to avoid the generation of too much heat. Allow the mixture to cool to room temperature. The acid mixture is slowly added dropwise, with a pipet or buret, to 115 mL of toluene in a 600-mL beaker while stirring rapidly. Maintain the temperature of the beaker during the addition at 30-40 °C by using either a cold water or salt-ice bath. The addition should require 60-90 minutes. After the addition, continue stirring for 30 minutes without any cooling, then let the mixture stand for 8-12 hours in a separatory funnel. The lower layer will be spent acid and the upper layer should be mononitrotoluene, drain the lower layer and keep the upper layer.

Dissolve one-half of the previously prepared mononitrotoluene and 60 mL of 95% sulfuric acid in a 500-mL beaker set in a cold water bath. Prepare a nitrating solution of 30 mL of 95% sulfuric acid and 36.5 mL of 95% nitric acid in a 100-mL beaker. Preheat the beaker of mononitrotoluene to 50 &Deg;C. Very slowly add the nitrating acid to the beaker of mononitrotoluene, with a pipet or buret, drop by drop while stirring rapidly. Regulate the rate of addition to keep the temperature of the reaction between 90-100 °C. The addition will require about 1 hour. After the addition, continue stirring and maintaining the temperature at 90-100 °C for 2 hours. If the beaker is allowed to stand, a layer of dinitrotoluene will separate, it is not necessary to separate the dinitrotoluene from the acid in this step.

While stirring the beaker of dinitrotoluene, heated to 90 °C, slowly add 80 mL of 100% fuming sulfuric acid, containing about 15% SO3, by pouring from a beaker. Prepare a nitrating solution of 40 mL of 100% sulfuric acid, with 15% SO3, and 50 mL of 99% nitric acid. Very slowly add the nitrating acid to the beaker of dinitrotoluene, with a pipet or buret, drop by drop while stirring rapidly. Regulate the rate of addition to keep the temperature of the reaction between 100-115 °C. It may become necessary to heat the beaker after three-quarters of the acid has been added in order to sustain the 100-115 °C temperature. The addition will require about 90-120 minutes. Maintain the stirring and temperature at 100-115 °C for 2 hours after the addition is complete. Allow the beaker to sit undisturbed for 8-12 hours, it should form a solid mass of trinitrotoluene crystals. Pour the contents of the beaker over a Buchner funnel without any filter paper to collect the bulk of the crystals, save the acidic filtrate as well. Break up the collected crystals and wash them with water to remove any excess acid. Add the collected acid and wash filtrates to a large volume of water, this will cause any remaining trinitrotoluene to precipitate. Decant off as much of the water as possible and combine these crystals with the previous ones on the funnel. Drown the crystals in a large volume of water, filter to collect them, and wash several times with water. Wash the crystals by adding them to a beaker of water, heat the water enough to melt the crystals while stirring rapidly. Repeat the melting and stirring with a fresh batch of water three or four times to wash thoroughly. After the last washing, the trinitrotoluene is granulated by allowing it to cool slowly under hot water while the stirring is continued. Filter to collect the crystals and allow to dry. The TNT can be further purified by recrystallizing from ethyl alcohol, dissolve the crystals in 60 °C and allow the solution to cool slowly. A second method of purification is to digest the TNT in 5 times its weight of 5% sodium bisulfite solution heated to 90 °C while stirring rapidly for 30 minutes. Wash the crystals with hot water until the washings are colorless, then allow the crystals to granulate as before. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.

trinitrotoluene - 17-10-2002 at 23:02

I also have another method from one of those links thats connected to meglomainia's site.Its a more easyior method and can be made form more readly avaliable chemicals.

Despite What Some Preceding Documents May have stated, Crude 2,4,6 TrinitroToluene Can be prepared from less concentrated, more commonly available, easily produced acids. The Process is a Modified Three Step Nitration, Whereby Toluene is converted into MonoNitroToluene, Dinitro, And Finally Trinitro by the addition of fresh portions of Mixed Nitric/Sulfuric Acid. An External Source of heat is neccesary

Purification is accomplished through the usage of a boiling water liquidation, Whereby impurities float to the surface, which are easily decanted.. It can be scaled up or down depending upon materiel availability.

Materiels

Sulfuric Acid 99~%

This can be Found in Home Depot, In White Plastic Containers, Marked "Instant Power Drain Opener" Marketed By Scotch Corporation Of Dallas, Texas - 64Oz Containers of Concentrated Sulfuric Acid Found in the plumbing section. It is of 93% Purity - It must be concentrated via heating at 100C+ For 10 minutes. Water will boil off yielding Theoretically pure H2SO4 - This should be done OUTSIDE, As all Experiments should be.

Nitric Acid 70~99 % Concentration

The ~70% Materiel is available commercially, 99~ materiel is available via 88~C Distillation of Potassium Or Sodium Nitrate With Sulfuric Acid. The 70 % materiel will work, although yields will be less.

Toluene

This is found in the Solvent section of Home Depot in Gallon cans

It is used as a specialty solvent. ACE May carry it if it is unavailable in Home Depot

3 Glass, Heat Resistant Container(Pyrex, Kimax Beaker or Flask Preferably)

Acid Resistant Volume Measurement device( Graduated Cylinder Or Etched Beaker)

Glass Stirring Rod

Plastic Spaluta

Plastic Baster

Heat Source

Thermometer(Optional)

This Item would greatly increase reproducibility - But TNT Will still form without careful temperature control and based on subjective sensory perception. Celsius Has been included for those who do have the luxury of a thermometer. TNT is not a sensitive HE and thus there is no danger of temperature based runaway reactions leading to detonation.

Procedure

Measure Out 300 Milliliters Of ~99% Sulfuric Acid into the heat resistant glass container. It should be able to hold at 1000 ML. Add To This 100 Ml Of Nitric Acid 70%. If One is using 99~ Distillation Acid then 75 ML Of That should be used. Or .75

This is the standard ratio 3/1 Or .75 If 99~ Acid is used. Heat will be generated upon the Nitric acid mixing with the Sulfuric acid and a cloud of barely visible white N0x should be seen wafting over the vessel. Now One adds 100 Milliliters of Toluene. Upon The Toluene contacting the mixed acid, it will convert to a yellowish/Red oil which will float on the surface of the acids - Large Amounts of heat will be generated - This is Good. Just let the vessel sit alone untouched reacting for 2 hours. A very noticeable odor shall appear - This is due to MNT. Do NOT confuse this with the odor of Reddish/Brown N02 which may begin to bubble off the beaker when the reaction temperature reaches a climax. Some reckon it smells like "shoe polish", While others relate to it smelling "Almondish". Personally, it has a completely distinct smell that i do not feel is adequately characterized by any particular description. Let it react for 2 hours

The MNT will be a Aromatic oil on the surface of the acids. It should now have turned cold - Temperature must now be maintained externally. With a bunsen burner, alcohol lamp, or other heating device, heat the beaker to 80C~. If you lack a thermometer, It should be heated to the temperature of the beaker during the vigorous reaction. By this i do not imply one wait around while it is reacting, as Volumes of Nitrogen Dioxide, a reddish Brown gas, is produced, which is quite toxic and will produce pulmonary edema which may go unnoticed for a week, at which point one may die. This does not mean you will die if you take a little whiff, No, But common sense dictates that one should distance themselves from the vessel while it is reacting and avoid inhaling any fumes. It is heated externally for 30 minutes. Now using the Plastic Baster, suck up as much of the now dilute acid from the container and transfer to another suitable container for recycling(See Below) Or should be disposed of properly. Try not to get any of the MNT in with the acid, this will take practice. Now In another container mix another batch of 3/1 acid and add this to the MNT. Repeat above steps involving 2 hour wait and 30 minute external heating. Remove spent acid and add to portion of spent acid recovered form MNT nitration. The DNT will be a Yellow oily liquid, or a waxy yellow solid. Now Comes the final nitration. To The DNT is added a fresh portion of 3/1 acid.

The vessel will get hot and when it cools after 2 hours yellow needles may be visible in addition to some DNT. After allowing the vessel to react for 2 hours, external heating should be applied for 1 hour. When heating is removed the insoluble oil floating on the surface will solidify as it cools, forming a yellow crystalline cake, with many yellow needles embedded into it - This is TNT. Earlier methods involved filtration, but due to economic reasons good filter paper is not used, instead coffee filters - Since corrosion of the cellulose based filters has been shown, a spatula is used to "Fish out" The cake from the surface of the acid and into a separate plastic container like a cream cheese container. This can be done by tilting the container gently and sliding the cake along the side of the vessel and into the empty plastic container.

Purification

The empty cup with the fragments of cake, acid, is covered in about 150 ML Of boiling water - This will melt the TNT into a puddle under the water and cause insoluble droplets of DNT impurity to float onto the surface as an oil. Any Acid Will dissolve in the water. Let this cool, drain off the water and remove the "Wet Cast" TNT from the container, preferably plastic "I Can't Believe Its Not Butter" container, which bends easily allowing the TNT to loosen and fallout without cracking it. Place it on Layers of Paper towel to dry, as TNT will exude a yellow oil. Puddles of such exudate can be found in munitions dumps across the country. You will notice the Paper towels colored yellow. Allow the TNT to lay undisturbed on the towels, and if neccesary fresh portions of towel should be used to dry it. Later Castings should be done dry using a bath of boiling water surrounding a dry container with the TNT in it.

One should not worry too much about possible safety dangers, as TNT is fairly difficult to initiate accidentally. Although it is better to be cautious around explosives paraphernalia.

Acid Recycling

For higher efficiency, Or for 99~ Nitric acid production, a distillation apparatus should be obtained or set up. A decent one can be made with two Flasks and appropriate rubber stoppers and glass tubing, With a bunsen burner or other heating instrument providing the means for distillation and ice water the means for condensation. The efficiency of the above mentioned reaction can be greatly improved if one uses the large amount of still usable acid present in the spent acid. Spent acid can be recycled by adding to it additional sulfuric acid , 2 parts spent acid to 1 part fresh sulfuric acid. Distillation is

effected at 80~C To obtain 99~% nitric acid, which can be reused in above reaction, or for PETN, RDX, NitroCellulose, etc... After Half An Hour of 80C careful distillation, All the Nitric Acid has been driven off, the condensation apparatus is removed and the spent acid vessel is heated to a higher temperature to drive off ALL water from the sulfuric acid. Quite Ingenious

Suggestions

If PETN is available, a Pentolite Booster can be made easily from the powdered, sieved PETN, mixed into the molten TNT, 50/50. If Cost is an issue, an AMATOL should be made. DRY Ammonium Nitrate should be mixed into the molten TNT, 50/50. There is a stichiometric fuel/oxygen balance that makes this explosive more powerful than Either components seperatly. I suggest Gentle heating in an oven on the TOP RACK to drive off any moisture. Also a Tritonal Is an interesting Explosive, If Only for its impressive Night-Time Flash. 20 Parts powdered Aluminum, available form various Mail-Order Pyrotechnics Companies, is sieved into a beaker full of molten TNT, 80 Parts.

-325 Or Better Should be used, German Black Flake 3 micron is Optimal. Care must be taken to avoid Moisture when using this in a sealed casing, as H2 gas will be generated by Aluminum Oxidation, and it may crack a casing before it is given a chance to be employed.

:)

abbreviation of explosives/chemistry

DeusExMachina - 16-11-2002 at 07:32

I never knew what all these terms meant when I was first introduced to pyrotechnics and it took me a while to learn them so here they are to make them easier for you (I got most of these from agent boris from TOTSE) :

\LE\ - Low Explosive
\PE\ - Primary
\HE\ - High Explosive
\CH\ - Chemicals
\AP\ - Acetone Peroxide
\ICPM\ - A minute post-blast taggant manufactured by Synthesia, Czech Republic. The taggant is comprised of Urea
Formaldehyde Resin, Silicon Oxide, Rhodamin B, Iron, and oxides of metal.
\HMTD\ - hexamethylene triperoxide diamine
\RDX\ - Explosive crystals used in plastic expolsives (Cyclonate)
\PETN\ - Pentaerythritol tetranitrate
\TATP\ - Triacetone Triperoxide – A highly sensitive primary explosive manufactured from common chemicals such as
acetone, peroxide, and acid
\TNT\ - Trinitrotoluene
\LOW EXPLOSIVES\Explosives which are characterized by deflagration (a rapid combustion that moves through an
explosive material at a velocity less than the speed of sound).
\DMNB\ - Dinitrobutane
\ANFO\ - An explosive material consisting of ammonium nitrate and fuel oil.
\Detonating Cord\ - A flexible cord containing a center core of high explosive and used to initiate other explosives
\Oxydizer\ - A substance, such as a nitrate, that readily yields oxygen or other oxidizing substances to stimulate
the combustion of organic matter or other fuel.
\MEKP\ - Methyl ethyl ketone peroxide is a primary in liquid form

If I can find any more things like this or write my own, I will post them up

more abbreviations

The_K5 - 17-11-2002 at 10:53

/UHE/ - Ultra High Explosive - explosives with vod > 10k/s
:cool:

Praetorian - 17-11-2002 at 14:44

Have anybody knowledge of synthesis of TNT by low concetrated acids and by catalysis of the activated copper?

trinitrotoluene - 18-11-2002 at 20:37

No i dont think low concentration acids will work. I've heard that its very dificult to get the Mono form with low concentration acids.

Praetorian - 23-11-2002 at 11:08

OK, I'm sorry for the inaccurate post. I have kept on mind this: There are fragmentary informations in the books of special preparative chemistry. They say, the synthesis of TNT should be realize without oleum (in the common process is used 20%oleum=free SO3 dissolved in H2SO4) by reaction dinitrotoluene(toluene?), nitration mixture and ACTIVATED COPPER as nitration catalyst. In according this, activated copper is going to bond the toluene temporarily(as metalic intetmediate) and allows the nitrogroup entry easily accessible. It is lesser-known method, but it works. I let react toluene, 68% HNO3, 98% H2SO4 and large-grained precipitated copper(I had supposed it could be that activated copper), but the final product brought the melting point 54°C (precipitated from acetone) and smell typically. Damned, only dinitrotoluene.. melting point of chemical clear TNT is 81,8°C. Damned, only dinitrotoluene. Ring is free, it's up for discussion. Should anybody response?

My list

DeusExMachina - 23-11-2002 at 14:25

Glossary/ Abbreviation of Explosives/Chemistry

LE - Low Explosive

PE - Primary Explosive

HE - High Explosive

CH - Chemicals

AP- Acetone peroxide

HMTD - hexamethylene triperoxide diamine

RDX - Explosive crystals used in plastic expolsives (Cyclonate or Hexogen)

PETN - Pentaerythritol tetranitrate

TATP - Triacetone Triperoxide

TNT - Trinitrotoluene

DMNB - Dinitrobutane

ANFO - An explosive that has ammonium nitrate and fuel oil in it

Detonating Cord - A cord containing a high explosive. It is used to detonate other explosives.

Oxydizing Agent- Something that causes another substance to either gain oxygen, lose hydrogen or lose electrons.

Ion - An atom that has an electrical charge. If an atom loses or gains an electron, it becomes an ion.

HEDM- High Energy Denisty Material

IM- Insensitive Munition

PBX- Plastic Bound Explosive

MgO- Magnesium Oxide

KNO3- Pottasium Nitrate (saltpetre)

H202- Hydrogen Peroxide

NH4NO3- Ammonium Nitrate

HNO3- Nitric Acid

NH3- Ammonia

ADN- An underwater explosive, ammonium DinitrAmide

DPPP- Diphoronepentaperoxide

Ketone- "any of a class of organic compounds having a carbonyl group linked to a carbon atom in each of two hydrocarbon radicals." This information was taken from www.dictionary.com

Perchlorate- A salt of perchloric acid

HClO4- Percloric acid, perchloric acid is a liquid with no colour. It is an oxydizing agent that is used as a catalyst.

Catalyst- Something that increases the rate of the process of a chemical reaction.



I made that list up myself. If there are any mistakes or inaccurate information, I would appreciate it if someone would inform me of it.

madscientist - 23-11-2002 at 14:54

What do these acronyms have to do with preparing trinitrotoluene? :o

DeusExMachina - 23-11-2002 at 22:13

shit... maybe I've been posting in the wrong topic all this time but I was pretty sure this was appropiate to be posted in another topic somewhere. Sorry about that

trinitrotoluene - 28-12-2002 at 00:20

Today I had prepeared some mononitrotoluene.I used 12 grams of KNO3 20ml of 93% H2SO4 and 10ml of toluene. My yeald was 8.5ml of mononitrotoluene. I then tried to nitrate 3 ml of toluene using the leftover acid, but that failed. After that I decided to make another batch useing the same thing and this timeI used a cool water bath and my yeald was only about 5.5ml from the 10 ml of toluene. So from my experenments I quess using a water bath or cooling the mixture will reduce your yeald. But dont get the temperature too high then NO2 gas will be liberated.I say above 45* but below 70*.

A little runaway occurs

trinitrotoluene - 31-12-2002 at 14:08

A few hours ago I had decided to make more mononitrotoluene.And this time I've decided to make a much larger batch of it. So this time I had used 30ml of toluene 45 grams or NaNO3 and 60ml of H2SO4 thats 93% in concentration.I started adding the NaNO3 to the H2SO4 after I was done the temperature shot up to 48*C then i added 20 ml of toluene and started stirring the temperature went up. When it shot up to 75*C my MNT turned from light yellow to orange and NO2 gas was being liberated.Then I stoped stirring and after 10 seconds no more NO2 was given off. Then i put it in a water bath the temperature stayed the same and added the rest of the toluene which was 10ml after that the temperture shot up to 85*C but there was no runaway. It stayed the way for 15 minutes and its slowly dropping since then.Right now my MNT is still outside. I will extract it an hour from now.

SHIT I Made Trinitrotoluene

trinitrotoluene - 25-1-2003 at 16:48

Yesterday I mixed 30ml of 98% H2SO4 with 25ml of yellow HNO3 I think its 90%+ in concentration then I added 22 grams of Dinitrotoluene that I had previously prepeared a month ago. When adding the DNT some acid splattered up and hit my hand ouch it burn. But after adding the DNT no reaction So I heated it. As soon as the reached 80*C a self substained reaction occured. The temperature went up tp 110*C and lots of red NO2 gas is given off. After the reaction died down I applyed heat. Keeping the temperature between 100-115*C. But at one point the temperature went to to 130*C. Well if the temperature goes above 110*C red fumes are given off. But I maitained the heating for 1 hour and 45 minutes. I was plannig to do it for 2 hours but its night time and too dark to work. After that I left it overnight and the next morning I went to check. I see a oily layer floating on the top of the acids. I said to myself my DNT had turned back into MNT with disapointment I extracted the oily substance and placed it in a 150ml beaker filled with water. After that I left then ate lunch. After lunch I went to check on my experiment and I see a tiny crystal floating on top of the stuff. And the oily substance had solldifild it looks like a crystalline solid. I jumped up and down and shouted with excitement. Then to make sure I heated the water and when it reached above 80*C it melted. After that I washed it a few times in a hot wter bath. The water turned yellow and the TNT turned form a yellow crystalline solid to a peach color. After purification I weighted my yealds I got 6.5 grams of TNT.And I started off with 22 grams of DNT. I am still very happy with my results because I had acomplashed my main goal in energetic materials. As for now I have no plans in detonateing it. I really think synthesizeing energetic materials is fun but there do fun with detonateing it. As for now I will continue on making MNT and DNT. I may give it a try on making TNT in the future with different methods.

Darkfire - 26-1-2003 at 21:02

"As for now I have no plans in detonateing it"

Thats the mindset of a chemist, i think the same way as you, I think the fun is in its creation, although I like a good boom here and there, I think the main thing that keeps me in it is the making of something that no one else dare make, or the great pleasure in suceding in chemistry of explosives.

Mad props my friend, good job...

CTR

Darkfire - 26-1-2003 at 21:04

WTF? no edit, how odd...

I thought that "PETN" is poly ethlyene trinitrate?

CTR

madscientist - 26-1-2003 at 22:33

No, PETN stands for pentaerythritol tetranitrate.

PHILOU Zrealone - 19-3-2003 at 02:30

Trinitrotoluene,
TNT is soluble in conc H2SO4 and HNO3; the yield of the reaction is very high from DNT to TNT you should at least get 25g of TNT (and max 27)!
Of course you have to put all the batch in iced water to allow the big % of TNT dissolved in the acid mix and then neutralise the solution with Na2CO3! You will have much more than 6g then!
If you have trowed away your acid mix, you have wasted at least 19g TNT!!!
:(:(:(

Madog - 19-3-2003 at 20:12

ive tryed far too many times to make TNT and ended up unsucessful, i have tried HNO3/H2SO4 with heating, KNO3/H2SO4 with heating too, and before that a few that were cold and stuff, very annoying! it just doesnt seem to want to strp up, i hsould try again. what i should do is make oleum and use that for the H2SO4 and try to make the HNO3 real good

NERV - 20-3-2003 at 13:06

I think I am going to attempt to make TNT. I was thinking that I could pass H2SO4 over anhydrous MgSO4 to produce SO3, which could then be dissolved in another batch of H2SO4 to produce oleum. The setup would be something like this:

Oleum rig.jpg - 52kB

Microtek - 22-3-2003 at 06:04

Oleum is unneccessary; you can use fuming nitric acid instead ( not as a substitute of course, but along with ordinary H2SO4 ). The reason oleum is used is that the product from the dinitration along with the waste acids and water from MNT + HNO3 --> DNT + H2O , is used without separation.
So if you just leave the solution of DNT in H2SO4 and HNO3 in the cold overnight most of the DNT precipitates, the acid is decanted ( easy as the DNT crystals are rather large ) and used for mononitration. The crystals can now be purified and dried, after which they can be dissolved in H2SO4 and fuming nitric is added slowly.
I suggest using 3.5 mol HNO3 per mol DNT, as the waste acid can then be decanted in the same way as from the DNT and used for MNT --> DNT.

Theoretic - 4-11-2004 at 05:56

Not exactly TNT preparation, but I didn't find a better place to post this...
TNDB - trinitrobenzodiazonium nitrate. A diazo group instead of the methyl, and a positive charge as a consequence. The negative ion is a nitrate ion.
To prepare this, oxidize TNT to TNBA (trinitrobenzoic acid), neutralize with ammonia, then heat to from an amide. The amide is then Hoffman-degraded, the resulting trinitroaniline is diazotized and that is then made into a nitrate salt. This has a better OB than TNT and should be more powerful.

tokat - 6-11-2004 at 22:35

mix tublene with nitric acid, if the nitric acid is not 99% then mix it with sulfric acid, what are you lot talking about, that the tub mixes with three nitro ions, then say it, stop wasting space with crap.

neutrino - 7-11-2004 at 06:08

If I understand that post you think that simply mixing nitric acid and toluene will give you TNT. You are mistaking this with RDX synthesis: nitration requires the nitronium ion (NO<sub>2</sub><sup>+</sup>;), which doesn’t exist in straight nitric acid but does in a nitric-sulfuric mix.

markgollum - 7-11-2004 at 16:20

You are partially correct neutrino,
The nitronium ion is present in nitric acid, even without sulfuric acid. Just at a much lesser concentration. The nitronium ion is present even to a lesser extent, in mixtures of nitric acid and acetic acid which are used in the laboratory to nitrate highly activated aromatics to the mono-nitro stage.( IIRC you can nitrate aniline to mononitro aniline with a mix of glacial acetic acid and nitric acid.)
Also, I am fairly sure that you could make TNT just from nitric acid and toluene, provided that the acid was close to anhydrous (95%+) and that you used a massive excess of it ( probably 10x at least).
It is understood that the reaction would have to be heated and left to react for a much longer amount of time.

[Edited on 8-11-2004 by markgollum]

JohnWW - 7-11-2004 at 19:35

The nitronium NO2+ ion would exist in appreciable amounts only in solution in HNO3 which contains additional N2O5 (which is nitronium nitrate), or in mixtures of HNO3 with concentrated acids which are stronger than HNO3, e.g. H2SO4, HClO4, HPF6.

mark - 7-11-2004 at 22:28

http://img36.photobucket.com/albums/v109/markthegreat/TNT.jp...

This is taking from the school chem book. Industrail process of Tnt. Perhaps some one is rich enough to make a scaled down version. Now wouldn't that be cool!

Theoretic - 8-11-2004 at 08:43

I will also post some other preparations of TNT derivatives. I will put all but this one in one file and attach it to a post I will make later. But I will post this one now.
Triperchloroaminobenzotridiazonium triazide. Souns scary, eh? :D Well, basically it's a benzene ring with three perchloratoamino (a perchlorate group attached to a nitrogen atom with a hydrogen attached to it also, the nitrogen is attached to the benzene ring) groups and three diazonium ion groups attached. The negative charge is compensated by three azide ions.
The preparation is as follows. TNT is oxidized to trinitrobenzoic acid, this is decarboxylated by boiling with alkali, the resulting trinitrobenzene is reduced in neutral solution (i.e., with zinc and ammonium chloride) to trihydroxylaminobenzene. That is reacted with perchloric acid to give triperchloroaminobenzene. That is reacted with chloramine to give triaminotriperchloroaminobenzene. This is diazotized with nitrous acid, sulfuric acid as well to give you triperchloroaminobenzotridiazonium sulfate. That is reacted with calcium azide, which precipitates CaSO4 and leaves you with triperchloroaminobenzotridiazonium triazide (TPABDA). This explosive has perfect oxygen balance, I expect it to be a crystalline solid, be quite sensitive and probably more powerful than HMX.

lefty - 24-11-2004 at 03:34

Something that's been in the back of my mind ever since College organic chem was the conversion of Picric acid to Trinitrotoluene. The molecules are about the same, with the exception of a hydroxy group in the 1 position in picric acid and a methyl group in the same place on TNT.

If one could only find a way to crack off the OH (thereby forming trinitrobenzene) and replace it with CH3. Massive oversimplification in terms, of course. I had asked my profs about converting phenol to toluene back when I was in organic chem, and they said that there was too strong of an affinity for the OH group, ergo...no dice.

It seems like there should be a more efficient way to synthesize the Trinitro though with out multiple nitrations.


Just wishful thinking

[Edited on 24-11-2004 by lefty]

Marvin - 24-11-2004 at 04:25

You arn't after a more efficient way, you are after an easier one. 3 stage nitration is very efficient.

PCl5 (I think its this and not PCl3) will turn picric acid into picryl chloride. Reacting this with a methyl magnesium should then get you TNT unless the nitro groups interfere. But even if the method works, and even ignoring the waste of fairly exotic reagents, does it really make sense to make a fairly safe explosive via a less safe one?

lefty - 24-11-2004 at 05:48

No... I agree, it's not exactly wise to use a less safe precursor if you don't have to.

enter

redneck - 24-11-2004 at 07:02

Megalomanias recipe:

--------------------------------------

EDIT BY VULTURE:

Thank you for supplying us with something we can lookup ourselves easily and which almost everyone knows.

If you haven't got anything relevant to contribute, please STFU.

Thank you.

-------------------------------------------------

[Edited on 24-11-2004 by vulture]

tokat - 1-12-2004 at 01:02

H2SO4+HNO3.H2O(less than 99% + NO) == NH4+ 02+ NO3
HNO3 = NO + NO2+ H

Any updates.

Marvin - 1-12-2004 at 02:21

tokat, what are you going on about?

I suspect you are a gifted scrabble player and that this is over shadowing your chemistry ability.

tokat - 1-12-2004 at 03:58

Think some, then if you still say that is strange, i will have to agreee with you.

Any way i had a reaction that showed the fom, but everone execpt one say i'am wrong, so i guess i am wrong, sorry for wasting the board space.

AAAA, psh, know your you person before hand, CAN ANY ONE ANSWER THE QUESTION??

[Edited on 1-12-2004 by tokat]

CD-ROM-LAUFWERK - 25-4-2005 at 09:58

the bigest problem i see is the seperation from TNT and DNT
the most preperations of TNT i know doesnt work (like that ones whit HNO3 conc. under 90%)
i also used H2SO4 whit free SO3 and 100% HNO3 but ther wasnt any real TNT formed after some hours of heating
(more than only 2h or something)
the mp. is around 50°C and the stuff can detonat whit a large initiation
can someone make a good instruktion whitin temperaturs, heating times, and so on??
a good speration from DNT and TNT is also needed

Marvin - 25-4-2005 at 11:09

Consult Chemistry and technology of explosives volume 1 (Urbanski) on the FTP, or edonkey and in several languages.

It covers the nitration, destruction of unstable isomers and purification by recrystalisation from a melt.

I'm not a fan of TNT, I dont see the point in making something toxic and difficult to use just because of good press in cartoons.

ChemPhile - 26-4-2005 at 05:33

Quote:
Originally posted by Praetorian
Have anybody knowledge of synthesis of TNT by low concetrated acids and by catalysis of the activated copper?

I know sth about the mononitration of methoxybenzene by Fe(III) nitrate in the acetic acid. heating is prefered! actually, almost all metal nitrate occur the same reaction

[Edited on 26-4-2005 by ChemPhile]

magnum - 2-5-2005 at 09:33

there is a patent (us2435314) wich shows an other method for tnt preparation. in this process no sulfuric acidis needed and the nitric acid has not to be concentrated. does anyone know this procedure or has anyone tryed it?

CD-ROM-LAUFWERK - 3-5-2005 at 05:29

i seperate the TNT now from the DNT by melting the stuff and coolig slowly down, the TNT crystalize out and and u can remove the liquid DNT (the wory is that the TNT is a bit souble in DNT)
but after 1 week of sometime heat a mixtur of fluming H2SO4/100% HNO3 ther are only around 10% nitrated DNT....
how to get a high-yield (and a fast one) nitration??

Taaie-Neuskoek - 3-5-2005 at 07:01

Quote:

there is a patent (us2435314) wich shows an other method for tnt preparation. in this process no sulfuric acidis needed and the nitric acid has not to be concentrated. does anyone know this procedure or has anyone tryed it?


With a google search I can found this, posted on E&W a few years ago, by 'MACE':

Quote:

there is an other method of TNT preperation described in the patent US2435314. if this really works this would be very interesting because there is no need of concentrated nitric and also sulfuric isn't needed at all. the process is something like this: you have to put the nitric (concentration dosn't matter, just calculate the right ammount for the aviable concentration) , the toluene and a solvent (light gasoline, n-hexane?) in a reflux aparature equipped with a watertrap and boil it until the calculated ammount of water has collected in the watertrap. the temperature will maintain it self at ~70°C because of the boilingpoint of the solvent. this will also prevent a runaway because if the temperature rises more solvent evapoates and this cools the reaction. i don't have tryed out this method until now but i'm on to obtain the equipment needed.did anyone tryed out this method befor?


This looks like the 'one pot TNT synthesis' NBK resenty posted, which uses a solvent which should boil with toluene at around 70°C, a Dean-stark trap can be used to trap the water. I haven't tried anything of this myself, but it seems rather promising...

EDIT: Thanks, Joeychemist!

[Edited on 4-5-2005 by Taaie-Neuskoek]

magnum - 3-5-2005 at 09:31

jea this was me in the e&w who has written this post but it seems that no one was interested in this procedure. i thought of talking about this patent again because i now have the equipment and chemicals to give this a try. it's cooking otside while i write this. i use hexane as solvent and a nitric acid with 53% concentration.now there realy warter collects in the wartertrap and the liquide in the flask has turned yellow.
i don't know the 'one pot TNT synthesis' from NBK do you have a link to this?

magnum - 3-5-2005 at 11:30

finally the reaction is over. the results are really bad. the liquide seperated in the warter trap was the mainly the nitric acid from the begining wich evaporated during the process. the main product seems to be a mixture of MNT and DNT. not even a half tea spoon full of TNT was swiming on top of the liquid. i used 40ml toluene, 180ml 53% nitric acid and 200ml hexane. the setup has been run for approx 8h. may be hexane is not a suitable solvent for this reaction. the patent recommends lite gasoline but i'm not sure whats meant with lite gasoline.

Taaie-Neuskoek - 4-5-2005 at 01:21

Did you measure the temperature? Don't take it above 80°C... what did you use as watertrap, something like MgSO4?

I cannot find the topic of NBK now, it is probably not cached by google...

magnum - 5-5-2005 at 03:21

the temperature was at 70°C the whole process because the hexane limits the reaaction temperature to it's boiling point. the wartertrap is not a chemical just a part of the still. the condensate (should be warter and hexane) from the reflux cooler drips in the wartertrap and divides in two phases because of it's different density and it's inmiscibility.

Taaie-Neuskoek - 5-5-2005 at 04:04

That temperature is about right, I was worried that it could be too high, since you have a mixture of 2 organic solvents, the temp could do strange things...

Anyway, I don't know or you've got more time on your hands, but maybe you have give it a shot by refreshing you nitric, and do the nitration agian on the mixture you're left with.
Don't you have any NA at a higher conc than 52%, maybe that might improve.
Please remember that TNT is normally made by reacting DNT with 100% HNO3 in the present of a lot of sulphuric, the concentration of the nitronium ion must be rather strong to get the last NO2 attached.

Keep the good work going!

[Edited on 5-5-2005 by Taaie-Neuskoek]

magnum - 5-5-2005 at 10:58

i have 68% nitric too but i want to use the 53% because it's easyer to get. if the patent is rigt the concentration should not play an important role because the warter should be removed during the process until the concentration is high enough for the nitration. i think the problem is that not only the warter collects in the trap but also the nitric do.
i still have some cyclohexane may be i give it a second try with this. has anyone an idea for an other suiteble solvent wich boils in the range of 70-80°c, forms an azetrop with warter an is innert to nitric acis at this temperatures?

markgollum - 13-5-2005 at 13:25

I have been thinking about and working towards a method of removing water from a nitration using my dean-stark trap.
I am looking for a water azeotrope that meets the following criteria:

(1) Based on the experiences of someone from the E&W Forum who used cyclohexane (bp 80 degC) to form the azeotrope and experienced the formation of excessive NO2.

The solvent must have a boiling point less than about 76 C.

(2) The solvent must be inert toward NO2, HNO3, sulfuric acid, and air under reflux.
This means that you cant use alkenes, alcohols, esters (are in equlibrium with the alcohol) , or ethers (form peroxides with air).

My first thought was to use n-hexane because it has a bp of 68.7 C and forms an azeotrope with water bp 61 C.
Then I read an MSDS that stated that n-hexane explodes when mixed with NO2 at 36 deg C!! IIRC. I understand that almost anything combustible will explode if mixed with NO2 and exposed to the shock of a detonator, or perhaps to a flame, but at room temperature?.
The idea that NO2 from decomposing nitric could mix with the hexane and explode makes me worry.

Now, carbon tetrachloride (bp 76.4 C) is most likley inert and forms an azeotrope with water bp 66.8 C that contains 4.1% water. However, 75 C is probably to hot, and will probably decompose to much nitric. Also, CCl4 is heavier than water and will require a different and hard to find type of water trap.

Chloroform (bp 61 C) also forms an azeotrope with water bp 56.1 C but it only contains 2.8% water, is denser than water, and might not be inert.

THF is hard to get ahold of, and forms peroxides in air.
My hope is that the MSDS was wrong about the hexane and NO2.
(If I got a dollar from every inaccuracy I have found in an MSDS I would probably have a lot more lab equipment. )

Rosco Bodine - 13-5-2005 at 15:07

Maybe trichloroethylene , bp 86.9 C would be a good candidate solvent . It is or was a commonly available nonflammable degreaser and cleaning solvent . I can't recall if it is one of those solvents which has fallen out of common use because of environmental regulations or not , but I think it is still available OTC , and may even be the solvent which they use in those recirculating bath " parts washers "
at automotive shops .

You can govern the reflux temperature lower if needed by pulling a little bit of regulated vacuum on the apparatus .

[Edited on 13-5-2005 by Rosco Bodine]

Polverone - 13-5-2005 at 16:44

I have my doubts that trichloroethylene is suitable, though it is still OTC (or was a couple of years ago, when I last bought some). I bought it to attempt hydrolysis via H2SO4, which was an older industrial process to monochloroacetic acid. I had some partial success but haven't tried anything more in a long time due to shuffled priorities and pure forgetfulness. It is not entirely inert to acids, that is sure. I suppose it depends somewhat on temperature and concentration, but I'd be wary.

Rosco Bodine - 13-5-2005 at 21:51

Chloroform looks like it should work the best among the other choices of chlorinated solvents . And it is stable in contact with concentrated acids .

Nitric acid is four times as soluble in the chloroform as in carbon tet . And you likely won't find or make carbon tet . It is pretty much gone the way of carbon disulfide , disappeared for the most part from commercial use and availability .

quicksilver - 13-6-2006 at 06:47

Quote:
Originally posted by trinitrotoluene
No i dont think low concentration acids will work. I've heard that its very dificult to get the Mono form with low concentration acids.


I know this is a VERY old thread but I wanted to add that both TNT and PETN may be produced by lower concentrations of acid than what one would normally expect (distilled HNO3, etc). I guess I have seen time and again that 70% HNO3 could not be used or that mixed solid nitrates could not be used for both benzene ring nitrations and nitric estors, that I wanted to post an example or two.

**************
for TNT synth:
**************
Trinitrotoluene - single batch method.
Yield is approx. 85% of theory, crude product.
Patent supports the only singe batch method in current usage.

NOTE: alkaline (sodium hydroxide) will sensitize TNT, Sodium Sulfite is used to bring the crude product to a technical chemical level. The product below is some rather crude stuff but MAY be brought up to higher purity level. However the end result will work.

Procedure: Place 191 grams of 70% nitric acid into a beaker, and then gradually
add over a period of 2 hours, 420 grams of 98% sulfuric acid. (Total; 611gr of
mixed acid) Then place the beaker into a cold-water bath and cool to 10 to 15
Celsius. When the acid mixture reaches a temperature of about 10 to 15 Celsius,
pour 96 milliliters of this acid mixture into a clean separate beaker, and then
cool to 10 to 15 Celsius by means of a cold water bath. When the temperature of
this 96-milliliter portion of acid mixture reaches 10 to 15 Celsius, slowly add
46 grams of toluene over a period of 4 hours while rapidly stirring the acid
mixture and maintaining its temperature at 10 to 15 Celsius. After the addition
of the toluene, continue stirring the reaction mixture for an additional 2 hours
while keeping the reaction temperature at 10 to 15 Celsius. After which, add the
remaining acid mixture obtained at the start of the procedure, to the reaction
mixture and then after the addition, raise the temperature of the reaction
mixture to 70 Celsius, and hold this temperature while rapidly stirring the
reaction mixture for 2 hours. After 2 hours, raise the temperature to 80
Celsius, and heat at 80 Celsius for 2 hours while rapidly stirring the reaction
mixture. After heating the reaction mixture to 80 Celsius for 2 hours, remove
the heat source, and allow the reaction mixture to cool to room temperature.
Then add the entire reaction mixture to 1000 milliliters of cold water, and then
filter-off the precipitated TNT product. After which, wash the TNT precipitate
with 1000 milliliters of water, and then vacuum dry or air-dry the TNT
precipitate. Then, place 400 grams of 70% sulfuric acid into a beaker, and then
add the dry TNT product. Afterwards, stir the mixture to form a slurry. Continue
to stir the slurry for 2 hours at room temperature, and then filter-off the TNT
product, wash with 1000 milliliters of cold water, and then vacuum dry or air
-dry the TNT product

Extrapolated from Legard's book and one of the FEW patents that could actually be varified :P IIRC it was a guy working for ISCC who developed it.


***********
for PETN synth
***********
Verified efficient method of preparing PETN from diluted HNO3

use
32,7 ml of 70% HNO3 (75% excess)
18,9 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,0 ml of 65% HNO3 (66% excess)
24,8 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------

or
34,8 ml of 58% HNO3 (48% excess)
36,3 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------


Nitration:
1. Cool nitration mixture during mixing of acids, thus minimalize even minimal decomposition of HNO3. Nitration mixture must be cooled before nitration process to temperature of 10°C.
2. While stiring, add pentaerythritee in small portions (1-2g) to nitration mixture, always after previous batch is dissolved. Nitration mixture gradually thicken as PETN forming in solution.
3. Constantly monitor reaction temperature and maintain it in 10-15°C range. Interval of adding pentaerytritol conform to reaction temperature, must not rise over 15°C, leave beaker in cold water.
4. Stir with mixture for next 5 minutes after all pentaerythrite is added and dissolved. Mixture is now thick, but stirring is going well. During nitration process must not be developed any brown fumes of NOx!
5. Now put beaker with mixture into water bath and maintain temperature at 50°C, continuously stir with mixture. During 20 minutes at this temperature, all of possible sulfoesters come into PETN for maximal yield of nitration.
6. While maintaining mixture at higher temperature, mixture must be monitored for developing of NOx fumes. Only light brown colour can be in shrouded beaker. Raised development of NOx pointing to higher temperatures used (even during previous nitration) or insufficient chmemicals purity and further heating may end up in uncontrolled reaction and oxidation of formed PETN. In this case it is better to do not heat at all and end just after nitration (if brown fumes apperas during nitration), the yield will be lower. In case of accidentally runaway reaction during heating, immedialtely pour mixture into cold water, don't try stop reaction by cooling beaker, it will not help.
7. When heating after 20 minutes pass off, pour reaction mixture into cold water and follow standart procedure of filtration, neutralization and purifying of PETN.

Yield was 22,1g of PETN from 10g of pentaerythrite, ~95% of theoretical yield (with 65% HNO3 used).

This procedure is result of research of most effective method preparing PETN from diluted HNO3. Acid ratios are precisely calculated on data from PETN nitration graph published by T. Urbanski in his book vol. IV. Look at the graph from the FTP and it makes a great deal of sense. Generaly said, PETN is forming to maximum 30% of water portion in nitration mixture. But, when also H2SO4 is contained in nitration mixture, minimum amount of water must be keep, or oxidation with small yields occur. With this acid ratios 20% of H2O is minimum. So, this nitration mixture has 20% of water on nitration start and 30% at the end, area for most effective nitration, but again only with this ratios. For other acid ratios must be all recalculated. Excess of HNO3 is used to controll amount of reaction water. Only amount of nitration mixture can be extended for lower mixture thickness, but it lower utilization of acids and overall efficiency. But it isn't necessary.


-=-=-=-=-=-
The TNT synth is somewhat scaleable - the PETN is not due to the above stated issues. (both of these have been floating around for a few years, I believe)





[Edited on 14-6-2006 by quicksilver]

Rosco Bodine - 2-7-2006 at 17:42

@quicksilver

Quote:

"Extrapolated from Legard's book and one of the FEW patents that could actually be varified IIRC it was a guy working for ISCC who developed it."


What is the patent number ?

jimwig - 3-7-2006 at 11:50

The stepwise nitration of toluene

Journal of chemical education


article online


http://www.jce.divched.org/cgi-bin/JCE/jce-idx.pl?type=goto&...

Rosco Bodine - 3-7-2006 at 12:08

Do not sneeze during the process or the entire sample
will be gone with the wind :P


Here is a good reaction vessel for microtek ;)


http://cgi.ebay.com/Large-reactor_W0QQitemZ110003787509QQihZ...

Sickman - 3-7-2006 at 13:09

Rosco,

I have the second edition of Jared Ledgard's book,
"The Preparatory Manual of Explosives" in front of me,
which I assume is the book Quicksilver extrapolated the synthesis from, which is located in chapter 11 of that book and NO PATENT NUMBER IS GIVEN. At least not in the edition I have.

As for the nitration to tnt in a "single pot" reaction starting from toluene without the further addition of concentrated acids it just doesn't seem the reaction kenetics are very favorable or economical which is why it seems in the literature it's done in a three step process.

However the conditions for a "one pot" synthesis of TNT directly from toluene may be more easily accomplished if a different nitration agent than nitric acid is used. For example Tetranitromethane in the presence of boric acid or nitrogen pentoxide added directly to toluene. They may be more costly than mixed acids, but may also prove to be greater nitraters when starting from toluene in a single step process or in first sulfonating the toluene, then substituting the nitro groups for the sulfonic groups in a two step process.

Note: see Urbanski Volume I, page 390

[Edited on 3-7-2006 by Sickman]

Rosco Bodine - 3-7-2006 at 15:47

Here is an old patent which relates to nitration catalysts
which may have some usefulness regarding TNT as well as other nitroaromatics . I have not done any experiments regarding the patent , but the procedure for tetranitronaphthalene is on my " experiments to do list " . Vanadium phosphate is one of the catalysts which I would look at . The TNN would likely make a good stable base charge for caps and is a bit more powerful and sensitive than TNT , about like picric acid but non-corrosive , has a good crystalline form and doesn't have the purification / separation problems of TNT . The patents mention of even higher penta and hexa nitro forms of naphthalene is also interesting , as well as the obscure primary initiating composition which may be formed from the hexanitronaphthalene in combination with an oxidizer . This is an intriguing old patent which may or may not withstand scrutiny . In fact it was the first patent which I communicated here in this forum as being " interesting " :D in its implications . You see if the nitration catalysts do
work as advertised , then higher nitrations of aromatics can be performed under less rigorous conditions for acid concentration and temperature which would be very helpful
for our purposes .

Attachment: GB501034 nitration catalysts.pdf (212kB)
This file has been downloaded 1213 times


Rosco Bodine - 22-7-2006 at 16:44

@quicksilver

I knew that TNT synthesis looked familiar

It was posted here nearly three years ago
by a one time poster . Strange huh ?

https://sciencemadness.org/talk/viewthread.php?tid=943#pid85...

You mentioned the ISCC ......what is that ?

BTW , WTF is the USASDDS , anybody have a clue ?


[Edited on 23-7-2006 by Rosco Bodine]

quicksilver - 24-7-2006 at 06:34

Quote:
Originally posted by Rosco Bodine
@quicksilver

I knew that TNT synthesis looked familiar


You mentioned the ISCC ......what is that ?

BTW , WTF is the USASDDS , anybody have a clue ?




OK....I F*cked up there. That was a typo and a hurried job of typing when I was running out the door for work. What I thought was a file from a collection of ISEE stuff (International Society of Explosive Engeneers) was simply another file from Legard's book, it wasn't the correct file - The typo was ISCC. I spent sometime tracking down what the existing citations in that damn book were. Some lead simply no-where - others had some interesting origins but I also have one unholy collection of files and need some way to organize them better. I didn't notice the whole thing until it had been posted quite awhile. - appologies....:(

What I looked for at the time was some US Gov't patents issued to a "H. William Voigt, Jr". of Wharton, NJ and a Mr. Bernard R. Banker, also from NJ. The patent number (like a WHOLE LOT OF STUFF IN LADGARD'S BOOK) was supposedly application # 104,499 12-17-79. That was a dead end. But somewhere I have a patent from 1981 that was a contractor to the gov't that looked like what it could be. That's a long convoluted story; I got that one from a guy who told me he submitted stuff he worked on via a university prof who published stuff for the ISEE.... a volume on nitrobenzenes has the same labs. However; the one-pot process can work; too many people have worked with it and it does produce a scalable, crude product. If I find the EXACT PDF file I'll append this and post it.



[Edited on 24-7-2006 by quicksilver]

Rosco Bodine - 24-7-2006 at 08:58

Doesn't it seem strange that in a book which proposes
many procedures for syntheses of energetic materials , and given the potential dangers attendant to such business , that there would be such dismal performance in providing the references to sources which were the basis for the procedures being described ?

It doesn't exactly seem to be a trivial failing in my estimation , in fact it is a troubling departure from the accepted convention for technical writing . All the fancy graphics don't mean shit if a writer can't be bothered to cite accurate references to substantiate his proposed synthetic procedures . Such a writing style for describing chemical syntheses should be reassigned to storytelling and banned from technical writing all together :o:D

Is there even one single good patent number given as a reference in that Ledgard work ?
( which we should perhaps rename )
Energetica Ledgerdermainica Acta ....
written by Poofer the Magician :P

quicksilver - 25-7-2006 at 06:32

Quote:
Originally posted by Rosco Bodine
Doesn't it seem strange that in a book which proposes
many procedures for syntheses of energetic materials , and given the potential dangers attendant to such business , that there would be such dismal performance in providing the references to sources which were the basis for the procedures being described

Is there even one single good patent number given as a reference in that Ledgard work ?
( which we should perhaps rename )
Energetica Ledgerdermainica Acta ....
written by Poofer the Magician :P


To be blunt with you I could only find less than half a dozen and I went through the whole book....I was obsessed with that book as I thought I got ripped off - I agree; there is a serious lack of "science-style" to it. I actually am suprised when one of his citations is correct. I always expect to hunt and hunt and hunt! And that is NOT the way such a book should be written!

quicksilver - 19-12-2006 at 06:46

Quote:
Originally posted by hector2000
every time that i made tnt it was red.and when i add water to it, again red water.
i done these three steps from rougerscience (without oleum)and i think that information on this site is true.
when i melt my tnt and add some naco3 to it.the color will be brown red.and this step will
repeat if i add naco3 again too.
does tnt made ?


What exactly did you do? I am sure everyone would be happy to help you but there is a wee lack of clarity in youf questions that needs a bit of follow-up.....

quicksilver - 21-12-2006 at 06:46

Quote:
Originally posted by hector2000
i use this method



The diluting of your nitrating acids may be the biggest problem. It seems that the addition of water serves no purpose. You started off with nice 90% HNO3 and then put water into it.....

nitro-genes - 21-12-2006 at 07:27

The red colour is caused by impurities, most likely they consist of partly nitrated toluene groups that still carry a sulfonic acid group, these can be bright red and it would explain why they are water soluble. At these temperatures, there will also be some oxidation, especially since there is still a lot of water present during the last step. Every TNT synthesis that I have read used oleum during the final nitrating step. As a concequence, I think there may still be a fair amount of DNT present in your final product...

The final yellow colour after the washings is perfectly normal. TNT can be everything from a very pale yellow, like shaved almonds, to a very dark brown, depending upon the amount of impurities...

[Edited on 21-12-2006 by nitro-genes]

Maya - 21-12-2006 at 10:24

Yes, along with dnt and a host of other things it seems.

Why don't you do a melting point determination and find out for yourself the purity, its very easy to do

CD-ROM-LAUFWERK - 25-12-2006 at 09:09

my TNT did melt around 81°C, wich is pure
the crackling is coming from entraped water in the TNT, u should meld it in a boling water bath and remove the water floating on top of it
than slowly cool it down, let the DNT crystallise out and pour the still liquid TNT out
repeating this two or three times will purify ur TNT to a mp. >80°C (if u make it properly)
than its time for a Na2SO3-treating to remove the last impurities (4% solution at around 95°C whit strong stirring)
if the solution stays clear yellow, not red, its a very pure TNT

Sauron - 25-12-2006 at 09:32

Reliable procedures abound.

The Chemistry of Powder & Explosives available free in this site's Library

TNT - a dedicated volume on just this subject also in the Library here freely downloadable.

If memory serves the mononitration uses ordinary mixed acids at moderate temperature; the dinitration uses same at somewhat higher temp; and the final stage is the only one that employs fuming acids again at higher temps. But see the above for all the details

Vogel also has at least steps 1 and 2 in his Practical Organic Chemistry, q.v. From the Library here.

Org.Syn. (Organic Synthesis, books and website with searchable complete set) will also have at least the first two steps, it is noteworthy for the published procedures being scrupulously annotated, checked and verified because it dates from a period during the WWI years when American chemists HAD to make their own organic chemicals simply because they were cut off from the German suppliers and there was no US manufacturing-chemical industry then. Eastman (Kodak) changed that and Org.Syn. is partially an outgrowth of that. Its raison d'etre has shifted since then but its basic format remains: tested proven reliable well annotated procedures that anyone with the skills can replicate.

Nitroaromatics are rather toxic, protect yourself. Beware or NOx as you were given good advice above. A friend of mine spent time in a hospital due to a fume-off of a nitration he was carrying out at home.

CD-ROM-LAUFWERK - 30-12-2006 at 09:36

i cant open both of it...

quicksilver - 14-2-2007 at 07:01

I was very curious about something related to TNT and didn't want to start another thread so I thought I would reserect this one. I have two questions that I was wondering about :

1.) TNT appears to crystalize in needles and in platlets. What contributing factors allow TNT to crystalize in needle form?

2.) Has anyone developed a solid nitrate synth for TNT? It appears that those who have attempted same have not had success. I have put together what looks like a good experiment for a solid nitrate / nitrafication of toluene but wanted to know if there are circumstances that inhibit the synth of TNT using soolid nitrates. Superficially it appears to solve the higher nitration issue in the "German" single pot
nitration.

nitro-genes - 14-2-2007 at 07:21

IIRC, higher concentration solutions of TNT favor plattlets while lower concentrations favor needles...

YT2095 - 14-2-2007 at 07:23

I made a few milligrams of TNT many moons ago following an A level text book, my Nitric acid wasn`t all that strong though and so my crystalisation took place in the fridge to leave waxy needle like crystals growing off the walls in the test tube under the soln.
they were an off white color and washed up very nicely.

so a Not so strong nitrating mix and fridge cooling over a few days seemed to work for me.
other than quantity of the reaction mix being less that outlined that`s the only deviation I made from the text book.

quicksilver - 14-2-2007 at 07:54

From what I had seen temp and nitration concentration had direct effects on crystal structure but I would not quantify the results. I had two observations of two nitrations; both equal. One went to needles (nice ones) the other platlets... it was infuriating.
I am convinced that TNT is one of the easiest energetic materials to synth aside from NG and I love crystal structue in general so it has been a favorite of mine for many years to study. However there seems no reason not to be able to utilize a solid nitrate to this end and that would put it in the realm of hobbiest material. There was someone who attempted it awhile back and said that it appeared that the nitration went too fast! -That the high concentation of acids didn't allow for the control needed to maintain temp, etc. This seemed too much for me. Higher concentrations have always been just as easy to control if the temp was controlable. This is the same issue as tetryl. Dimethylaniline (also a benzene) nitrates much too vigorously in streight HNO3 so the use of sulfonation (via H2SO4 in a prior solution) controls that issue. But most of the original material calls for a higher concentration than 70% HN03. So why not use a mixed acid in addition to the sulfonated solution? It works with no problem so long as the original H2SO4 is accounted for in the nitration (no by products). -Extrapolating this and attempting it with toluene would seem even easier. Toluene is easy to nitrate. But the original material calls for 75% HNO3 and indeed, if the level IS higher the yield should be better and product purer. With 68-70 % it's easy to get an 80% yield. I believe that with using a solid nitrate the yield should be vastly higher and the product purer due to lack of water in the nitration. But I have not heard of it being done. This is something that if successful, would produce a workable secondary of consistent quality.
TNT may be a gateway to a heck of a lot of fun stuff.

Found some answers. (Friends at the local university are great)

Notes on trinitrotoluene 1/14/07
TNT has isomers in its production as a crude product. These produce differing crystal: needles palettes, rhomboids, etc. The isomers are alpha, beta, gamma, delta, epsilon, & zeta. Alpha produces needles. Beta –thin platelet’s, gamma –rhomboids & zeta possibly plates of a differing type.
The MP of the differing isomers are : alpha – 80C beta- 112, gamma 104, delta-137, epsilon- 97, & zeta-79.5
Gamma isomer crystallizes first from recrystalized material dissolved in hot (boil level) ethanol. This is a crude separation from fractional crystallization.
Alpha isomer is separated by fractional precipitation from warm etoh: Alpha being slightly more soluble than the others.
Alpha, beta, & gamma will react with aniline (or dimethylanaline but it will or course be a dimethyl isomer) and this gives distinctive products – nice crystals.
Alpha crystallizes in long glinting VIOLET needles! (the same as trinitrobenzene – mp 83C)
Beta – deep red plates, Gamma – reacts w/ hot alcoholic aniline to give orange rhomboids.
Super Sensitizing Idea;
Beta & Gamma Isomers react w/ NaOH to sensitize powerfully. But NaOH is not the only salt that will sensitize TNT thus the care in which anti acid wash should be chosen. Even carbonates of the alkali metals will sensitize (barium carbonate used in Japan?) Sodium carbonate (alcoholic solution – 1% in reaction) precipitates a dark blue substance in the solution being treated w/ acid. – Turns out this substance is dinitrocresol! However 1% sodium carbonate in alcoholic solution also produces dinitrotolyloxides. When they are formed salts of this complex are very explosive (primaries?)
Ammonium sulfide in reaction w/ TNT isomers yield interesting color variations.
Alpha – deep red. Beta –greenish yellow Gamma – blue! Epsilon –rose red (light). Zeta – orange
TNT dets from heat! There is something called “Goettig’s Mixture”. Heat from platinum wire causes explosion! Actual detonation as in primary is yet to be proven. Data from German text book (1907).
TNT - 22.22%
Barium Nitrate - 9.83%
Nitro Cellulous (smokeless powder nitrate level - 67.96%
Intimate mixture via whetting, etc.

So why does a batch have one isomer greater or another?? Well I have a collection of isomers in each batch. So the primacy of one, let's say alpha is more determined by getting rid of the rest via either recrystalization or happenstance when a batch is finished. Since hobbiest lab conditioons vary no matter what due to small batch size and lack of automation I don't think I can do much about it other than "weed-out" the unwanted isomers rather than the other way....



[Edited on 15-2-2007 by quicksilver]

quicksilver - 25-2-2007 at 10:50

Interesting crystal growth pictures utilizing differing re-crystalization methods....
Using acetone and ethanol differing crystals may be obtained. Rhomboids (acetone) are unusually dense while needles (ethanol) can be grown up to one inch in size. MP on both 80 C.


[Edited on 25-2-2007 by quicksilver]

Attachment: pics.rar (806kB)
This file has been downloaded 1137 times


Rosco Bodine - 25-2-2007 at 11:52

Hey quicksilver . Could you please edit that image size
downward to about half what it is .....so that it doesn't
mess up the text page width formatting ?

quicksilver - 26-2-2007 at 06:28

Sorry about that. I thought it was a querk of FireFox and would be compensated for in a relaod of the page.

optimum nitrating acid composition

Rosco Bodine - 21-4-2007 at 09:45

This short article provides some insight concerning the
optimum yield nitrating acid composition for nitration of
a mononitrotoluene precursor to the trinitrated TNT .

As the article states , this data is not pertinent to the
disclosure of the most economical proportions or stepwise
process , but only studies the composition and quantity
of acid in order to identify the optimum conditions in terms
of yield for the complete nitration of a mononitrotoluene
precursor , to develop good data which is relevant to
further process modeling . The most pertinent data is
the perhaps surprising result concerning the beginning and final water content of the nitration acids , where the result is that some water content actually provides a higher yield than
anhydrous nitration acid mixtures which are attained by
use of fuming sulfuric acid , as oleum .

This result has also been reported for nitration mixtures for nitroesters , where some small water content in the nitrating acids also results in a higher yield than absolutely anhydrous
nitrating acids .

Anyway , the charted nitrating acid data should be useful in projecting and calculating what may also be a useful acid composition for a more typical nitration which is applied to a dinitrotoluene precursor . For example something a bit over half the quantity and composition of acid reported optimum
for the conversion of mononitrotoluene to TNT should be
applicable for conversion of dinitrotoluene to TNT , resulting in a similar spent acid composition .

I believe this is also good news with respect to the possible usefulness of dehydrating salts which might be an included part of nitrating acid mixtures , as an alternative strategy to the use of oleum to reduce the water content of nitration acids for TNT . I have long had the idea that a respectably efficient nitration mixture for TNT could be attained by use
of dehydrating salts , and perhaps added nitration catalysts also , if indeed the dehydrating salt did not serve that function also , without the need for nitration mixtures made up from oleum .

Attachment: Nitration of Toluene to TNT.pdf (308kB)
This file has been downloaded 1680 times


tito-o-mac - 14-7-2007 at 01:51

You can find TNT preparation here with many other explosives: http://www.roguesci.org/megalomania/explo/trinitrotoluene.ht...

Zinc - 3-2-2008 at 03:06

When I make MNT I will not convert it to DNT right after I make it. I will store it for around 1 week. Can I just remove it from the spent acid or do I also have to neutralize and wash it?

quicksilver - 3-2-2008 at 05:24

In order to complete a synthesis you should do your best to clean the product from it's lab components and clean your equipment as well. Things should not be haphazard in any of your work. YES, clean the product; that way you'll know that you have that material, not many others in that container. Additionally it will keep better and be less reactive.

Just like doing homework for school, you wouldn't do a half-job there / so why do that in your lab? Be thorough and complete; reach for exacting standards.

Zinc - 3-2-2008 at 10:37

To 60 ml of conc. H2SO4 (made by boiling down the acid extracted from a old car battery) I added 45 g of NaNO3. When the NaNO3 dissolved I added 30 ml of toluene in 4 portions). The toluene first turned in a red liquid, then orange and then again to red. After around 45 min it looked like this:



Then I added it to water, then to a sodium bicarbonate solution and then in a saturated salt solution. Final yield is around 26 ml of non-clear orange MNT (it has a very nice smell) :)

Zinc - 3-2-2008 at 11:20

Does anyone know in what ratio should I add MNT to a H2SO4/NaNO3 mixture to nitrate it to DNT?


You know there is an edit button for your previous post, so you should have edited and added this to that post as opposed to making a new post. Next time it gets deleted.
-Davster

[Edited on 3-2-2008 by The_Davster]

quicksilver - 5-2-2008 at 05:57

How do you know you did something "wrong" or "right"? What mechanism are you using for verification of success?

Zinc - 5-2-2008 at 10:49

Quote:
Originally posted by quicksilver
How do you know you did something "wrong" or "right"?


If I did something right the product is what it must be. If I did something wrong the product is not what it must be.

Quote:
Originally posted by quicksilver
What mechanism are you using for verification of success?


By the color, smell, and does it float or sink in water.

Sobrero - 5-2-2008 at 11:40

I've made TNT a few times, by first nitrating toluene to DNT and then to TNT.
I like this path a lot since it contains only two steps and proceeds just as fine!
Toluene can be easily nitrated to dinitrotoluene by adding , for example, 10ml of toluene to a cooled nitrating mixture comprising 18g of ammonium nitrate (130% of theory) and 32ml sulfuric acid, and heating this for 2 hours at 60°C, with stirring. Then, after drowning, washing and neutralising, DNT is obtained in 95% yield, as a light yellow, slightly waxy solid :).

So, @ Zinc, for the preparation of DNT from MNT, a nitrating mixture containing a slight (~5-10% excess) molar excess of (in your case) sodium nitrate and sulfuric acid should be entirely adequate (with reaction conditions mentioned above).

Fashist - 7-2-2008 at 22:46

I made tnt very easy by reflux system(see below picture)
First i made Dnt and then made tnt in the reflux system(100-105c, 2hour)





Zinc - 8-2-2008 at 03:00

I have tried the method that Sobrero posted only a little upscaled and used sodium nitrate instead ammonium nitrate. I heated the mix for two hours (sometimes even hotter than 60 C). At the begging I had a runaway but I cooled it fast and then again put it on a hotplate to heat it. After two hours there is an orange oil on top of the acid. As DNT is solid I think that the reaction failed. What did I do wrong? At least I got some MNT:)

Fascist what ratios of chemicals did you use to make your DNT and how long did you heat it?

Sobrero - 8-2-2008 at 04:37

You mean liquid at elevated (60-70°C) or at room temperature (after 'drowning')? Dinitrotouene melts quite easily (around 50-60°C IIRC, for a mixture of isomers).

[Edite le 8-2-2008 par Sobrero]

Zinc - 8-2-2008 at 11:33

It was liquid at the elevated temperature.

Fashist - 8-2-2008 at 12:31

I used this book Ratio
http://rapidshare.com/files/90231545/fmx.zip.html

Zinc - 9-2-2008 at 15:08

Thank you!

Very interesting book.

Zinc - 10-2-2008 at 11:57

Today I made more MNT. Now i have 132 g:) I want to make DNT from it using a mixture of sodium or ammonium nitrate and H2SO4. So how much of NO3/AN should I use? As far as I know I need one mol of NO2 anions per one mol of MNT to make DNT. 132 g of MNT is around one mol. So for that I need one mol of NH4NO3 (or NaNO3) and that is around 80 g (or 85 g of NaNO3) as one mol of NaNO3 or NH4NO3 gives one mol of NO2 anions. So how much of H2SO4 should I add to the nitrate (I think one mol as the nitrates turn to bisulfates and how much more to absorb the water?)? And how much excess of nitrate and sulfuric acid should I use? And under what conditions should the reactants to be to react (heat how long and that things)? And are the things I wrote above correct?

Sorry for too much questions but I don't know a lot of theoretical chemistry.

Fashist - 10-2-2008 at 12:03

My Suggestion is Using Con.Nitric Acid
I Made it Using Dry Mg(NO3)2 + HNO3(57%) and then Distil.

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