Dinitronapthalene

[ALENGOSVIG1]

Today i made some dinitronapthalene and took some pics of the process. I originally had more pictures, but they mysteriously dissapeared from my hard drive.

Ok, first i made mononitro, then nitrated it to dinitro. I'll further nitrate it to TeNN if i have time.

In the first nitration of naphalene, i used 97g of napthalene, 130g of H2SO4, and 52g of 70% HNO3. I got about 90g of mononitro from 97g of napthalene.

When i nitrated the mononitro to dinitro, I used 108g of H2SO4 and 69g of KNO3. I havent weighed the product yet, as it isnt dry yet.

Oh yes, does anyhow know the VoD of Dinitronapthalene?

You must copy and paste the pics into your browser.

pic of the mononitro layer ontop of the spent acid:
<a href="http://www.angelfire.com/linux/alengg/tenn2.gif" target="_blank">http://www.angelfire.com/linux/alengg/tenn2.gif</a>

Pic of the mononitro yeild:
<a href="http://www.angelfire.com/linux/alengg/tenn3.jpg" target="_blank">http://www.angelfire.com/linux/alengg/tenn3.jpg</a>

Pic of solid Dinitro ontop of spent acid:
<a href="http://www.angelfire.com/linux/alengg/tenn4.jpg" target="_blank">http://www.angelfire.com/linux/alengg/tenn4.jpg</a>

Pic of the Dinitro yeild:
<a href="http://www.angelfire.com/linux/alengg/tenn5.jpg" target="_blank">http://www.angelfire.com/linux/alengg/tenn5.jpg</a>

<small>[ May 14, 2002, 01:08 AM: Message edited by: ALENGOSVIG1 ]</small>

[DBSP]

I've also been interested in TeNN but as usual I don't have enaugh H2SO4 to try it. I'm getting some conc, H2SO4 within the next month so if it seemes to work well I might try it. Did you use drain cleaner? Sweden is a good cuntry for pyros except for one thing, you can't buy conc acids and that is very frustrating. I can't get more than 37% H2SO4 and that isn't even leagal. :(

edit: typo Grrrr

<small>[ May 14, 2002, 04:06 AM: Message edited by: DBSP ]</small>

[the_unbound]

....you can't buy conc acids and that is very frustrating. I can't get more than 37% H2SO4 and that isn't even leagal.

That's not a big problem. H2SO4 is used as Battery acid and you can concentrate the acid by cooking.
Cook it until white fumes appear.
Thus, it's no big deal to get conc H2SO4

[ALENGOSVIG1]

Yes i always use H2SO4 drain cleaner, and have never had problems with it. Unfortionatelty, I broke my thermometer yestersay so i wont be able to nitrate the dinitro to to TeNN untill i get a new one. So it will be a couple weeks before I make anything.

[Mr Cool]

ALEN: It may be the lighting or the camera, but your MNN looks very dark, especially in the first picture. It's meant to be fairly bright orange.
DNN doesn't have a VoD as far as I know, I think it's too oxygen defficient to support a detonation wave.

[Semtexe]

why your links of picture of tenn.gif dont run

(They all worked fine for me. My guess is that you're an idiot and didn't paste the link into your browser.)

<small>[ May 14, 2002, 02:18 PM: Message edited by: Mr Cool ]</small>

[Anthony]

The tenn2.gif pic works fine for me.

The discolouration may be caused by dyes/additives in the H2SO4 drain cleaner. My drain cleaner makes yellow PETN :)

[DBSP]

Dear Mr unbound do you think I'm stupid? :mad: the 37% is battery acid thus I have to boil it. The problem is as I said it's illegal and I can't get any larger quantities of it..

[ALENGOSVIG1]

mrcool: No its not the camera. it was fist dark but after a few hours it turned yellow/light orange. It was wet when i took the picture so that probally made it look darker.

[S. Toppholzer]

@DBSP: If you don't have access to conc. acids - how would you make TeNN - is there a way around the "100% fuming nitric acid" as descibed on mega's site or are you preparing your own nitric acid?

Alen - your website 404?

<small>[ May 15, 2002, 02:39 PM: Message edited by: S. Toppholzer ]</small>

[DBSP]

I said that I was getting some 96% H2SO4 within a month that way I will be able to make myself some HNO3 if I buy a still wich I have got plans on doing as soon as I can get hold of some proper ammount of H2SO4. And I did not say that I would try it because I hadn't got enaugh H2SO4. I have though been interested in TeNN. Now get this back on topic.

[ALENGOSVIG1]

Does anyone know if dinitronapthalene has a VoD? Also, Is Dinitronapthalene good for sensitizing AN mixes like mononitronapthalene?

<small>[ May 19, 2002, 01:41 AM: Message edited by: ALENGOSVIG1 ]</small>

[DBSP]

There is some info in the swedish infomania files.

- Schnéiderite

Ammoniumnitrat 87,5%
Dinitronaftalen 12,5%

VOD 3815 to 5840 m/s @ 1,3 g/cc
I have no idea of the sensitivity but @ about 1 g/cc I might emagine that it would be reasonably sensitive, maby a small booster is needed but it shuldn't have to be very large.0

It was used in grenades by the french in WW1 and was then detonated by a charge of pure TNT.

EDIT: Alen I just remembered that you attemted to detonate a CnSoy charge some time ago, how did it go? I would like to know since I just prepared 1,4 kg of Cn and 5% raps oil. I'm sorry to go off topic.

<small>[ May 18, 2002, 03:54 PM: Message edited by: DBSP ]</small>

[Mr Cool]

Neither mononitronapthalene nor dinitronapthalene are detonatable on their own.
Both these substances can be used in AN or KClO3 based explosives.
I think 3-4g of HMTD or equivalent would detonate "Schneiderite" at c. 1g/cm3, depending on how well it was made. The AN/NC explosive I mentioned in the cap-sensitive AN-based explosives thread would make a good booster.

[ALENGOSVIG1]

DBSP: I never detonated the the CN charge i descibed. I was planning on detonating it but the bag it was in broke and all the prills fell into a puddle of water :mad:
I have had sucess detonating other AN based explosives with CN in place of the AN.

Oh, and I havent converted the DNN into TeNN becuase i broke my thermometer 3/4 throught the the nitration of the MNN to DNN.

I put some of my DNN to use today. I made 120 grams of AN/DNN/Charcoal. Im going to attempt detonating it tommorow morning.

13% DNN
4% Charcoal
83% Activated ammonium nitrate prills (.5g/cc prill density)

The DNN was melted and added to the AN (also being heated). I stirred it around for a minute then added the charcoal and continued stirring for a minute or two.

Pic of 120g AN/DNN/Charcoal in plastic bag:
<a href="http://www.angelfire.com/linux/alengg/ANDNN2.jpg" target="_blank">http://www.angelfire.com/linux/alengg/ANDNN2.jpg</a>

Prills on piece of paper.
<a href="http://www.angelfire.com/linux/alengg/ANDNN.jpg" target="_blank">http://www.angelfire.com/linux/alengg/ANDNN.jpg</a>

<small>[ May 19, 2002, 07:30 PM: Message edited by: ALENGOSVIG1 ]</small>

[ALENGOSVIG1]

I just detonated 10 grams of AN/DNN/Charcoal. first I pressed 1.5g of AP in a 5" long .5" diameter piece of pvc pipe. Then I placed a piece off tissue paper ontop of the AP and poured in the AN/DNN/Charcoal. The charge was taped to a large block of wood and the fuse was lit. There was a nice bang and most of the explosive detonated, but not all. There was a 1.5" long piece of pipe still taped to the block of wood with undetonated explosive in it.

[Microtek]

How much did you have to heat the DNN to get it to melt ? In COPAE there are given three isomers of DNN melting at 145, 170 and 216 C respectively. Did the DNN melt into a homogenous liquid or were there unmelted lumps?

[DBSP]

Nice Alen, the inconmplete detonation must have been caused by the small diameter of the pipe, if it would increase it would probaly detonate completely. Why don't yiu try to detonate some of it in a plastic baggie to see how the initiability is whith only low confinement.

[vulture]

Does trinitro or tetranitronapthalene exist? I mean like 2 dinitrobenzene molecules stuck together, maybe even hexanitronapthalene?

<small>[ May 20, 2002, 09:59 AM: Message edited by: vulture ]</small>

[Zambosan]

This is slightly off-topic, but I didn't feel it was worthy of a new topic. For nitrations of compounds like naphthalene and toluene, why is it necessary to perform the nitration as many times as the number of nitro groups added, while for a compound like trinitrophenol, the entire nitration takes only one step? Is the amount of acid intentionally scaled down to only provide enough nitro groups to on average add one nitro group to each molecule so as to minimize the heat of each reaction for safety? Or will the additional nitration physically not take place without this approach?

[ALENGOSVIG1]

I just got back from detonating 110 grams of AN/DNN/Charcoal. I dont have any pics becuase I light the fuse and threw it off a cliff. It exploded im mid air :D

The detonation was very loud and impressive. The explosive was initiated with 3.5 grams of AP. The casing was a 4.5 inch long piece of plastic pipe (dont know what kind, not abs or pvc) with an I.D. of about 1.75".

I think i will make some more of this explosive soon.

[Madog555]

there is tatranitronapthalene. its known as TeNN and the procedure is on megas and mr cool's site.

it would be possible to nitrate napthelene with up to 8 nitro groups, it will be extremely unstable though.

[Dave Angel]

Zambosan: I dunno how good your chemistry is but I'll try to explain. The OH group in phenol activates the benzene ring by resonance. That is to say there is a lone pair of electrons on the oxygen which can interact with the benzene ring. The ring acts as a conductor for those electrons forming areas of high electron density which the electrophilic nitronium ion can attack readily.

The nitro group itself is one of the strongest deactivators around, so the more nitro groups you put on the harder it is to nitrate. Fortunately the strength of the OH activation on phenol outweighs this so it possible to get three nitros on without needing fresh acids.

In the case of toluene, the methyl group (which activates by induction) is about 40 times less activating that the OH group on phenol. As you add more nitro groups, their deactivating effect outweighs the activating effect of the methyl group and the ring becomes harder to nitrate, requiring fresh and more concentrated nitrating mixtures.

Napthalene doesnt have the activating methyl group however it is activated towards substitution because of its highly delocalised nature. Still this can't outweigh the deactivation of the nitro groups that keep getting added, thus it requires very concentrated nitrating mixtures to get to the tetranitro- form.

If this makes no sense a good university level chemistry text book can probably explain it better.

[Hystrix]

Pure dinitronaphthalene is a weak explosive but it can detonate. Its VoD is 1150 m/s @ 1 g/ccm and it gives 100 ml in Trautzl's test.
BTW: DNN is a component of so-called "russian mixture" which was used for bombs' and grenades' filling in World War I. This mixture consists of DNN (48.5%) and picric acid (51.5%), it melts at 82-87 deg. C.

[Dr_Pind]

I see that several forum members have tried detonating AN/DNN/C mixes. What was the density? Was it loose, tamped or pressed? Also wondering about how sensitive they would be if pressed.
Is the sensitivity much higher than mixes with MNN?

[Jimmybooyah]

why is KNO3 used in the second step of nitration for TeNN. Could you not just use nitric acid as in the other two steps. I just got a new still and finally have the ability to make nitric, but lack a good balance.

[Dave Angel]

Jimmy, I'm actually hoping that KNO3 (and H2SO4) can be used to produce TeNN in 2 steps, as KNO3 is usually easier to get then HNO3. I'm designing a synthesis based on the nitration diagram shown in another thread on nitronapthalenes, and sooner or later someone will get round to carrying out a small scale synthesis to see if it's possible.

In answer to your question, I can't see why using the acid rather than the salt wouldn't work if you use the correct proportions. Naturally take extra care when altering any synthetic procedure involving energetic materials, common sense, but it's worth mentioning.

[Sarevok]

No temperature rise? Something went very wrong. Dave, did you crush the moth balls really hard before using
them? Did you stirr the mixture during the addition? :confused:

[Dave Angel]

Crushing was good (sublimation would be preferable though) and stirring was magnetic. Quite unexpected results. One explanation I can think of is that the moth balls may have been mostly inert with a only a small percentage of napthalene in order to make them functional. But I'm pretty damn sure the boxes (long gone) said 100% w/w...

Perhaps the napthalene decomposed in the initial stage when the nitric and sulphuric acids are mixed with a small portion of the napthalene. The procedure states to allow the mixture to cool to room temperature but not how high is tolerable during the initial mixing (although lower is better, naturally). If something untoward did happen, the 64g initial napthalene may have used up all the nitric acid leaving none for the subsequent 150g, though one would have expected to see some sort of bubbling/boiling or NOx being given off, but not so.

Whatever the case, it has been put down to experience and hopefully the next attempt will be more 'normal'.

Bitola, is it really too much to ask that you post in the correct thread about the DPPP? When you post about the AN/fuel patent it might be a good idea to post that in an ANFO thread rather than this one.

-------------
All mention of DPPP in this thread has been deleted, along with Bitola1.

Rhadon
-------------

Maybe if someone here speaks your native language, whatever it is, they could explain to you what you are doing wrong because you don't seem to be getting it!

[Edit] Re: the DNN, I like the look of Mr. Cool's method, which, incidentally says not to allow the temperature to rise above 30C during the intial addition.

[Rosco Bodine]

There has been reported a method of nitration of naphthalene
using sodium nitrate and sulfuric acid , which results in dinitronaphthalene
directly . Then further nitration to a mixture of higher nitrated
naphthalenes can be achieved by a second step using the same
sort of nitration mixture . The description of the process is not
extensive , but is briefly described in a patent which mentions the
usefulness of the mixed higher nitrated naphthalenes as an additive
to some sodium picrate / lead picrate double salts also described
by the patent .

Experiments with the sodium nitrate / sulfuric acid method could be
done to work out the details of how best to proceed with such a nitration .

US421753

Also of interest for a different nitration strategy for producing the
highest nitration of naphthalene is

GB501034

The nitrated naphthalenes may be used alone as explosive fuels in
ammonium nitrate blasting compositions . But it is particularly interesting
that the nitronaphthalenes are reported to act in combination with very
small percentages of specific organic substances like glycine , benzoic acid ,
salicylic acid , lactic acid , ethyl acetate , dichlorethylene , ect . ,
as *detonation catalysts* for mixtures which contain ammonium nitrate
with other nitrated aromatic compounds , producing sensitive mixtures which
exhibit great brisance and power .

GB497145

Since the above patent discloses that the detonation catalyst effect
applies to any nitroaromatic compound in ammonium nitrate compositions ,
this would be of particular interest with regards to nitrocresol and the
nitrocresol mixture with small percentages of lower nitrated cresols ,
which results from the oxynitration of toluene , using ordinary 68 per cent
nitric acid and a mercuric nitrate catalyst . Nitrocresol may be produced
by the "catalytic nitration" of toluene , analogous to the production of
picric acid from benzene , which produces the highest nitrated aromatic
obtainable by a simple and high yield nitration under mild conditions .
The "catalytic process" for picric acid is described by Davis in COPAE ,
and by the patents referenced below . There is no need to isolate the
trinitrated product from the mixed nitrates produced from such nitrations ,
when the nitrated products are to be used as an explosive fuel sensitizer
for ammonium nitrate explosives . The mixed nitration product is separated
from the spent nitration mixture and used directly .

US2455322
US1380186
US1396001
US1417368

Ammonium nitrate explosives fueled with nitroaromatic mixtures derived
from methods as above , should exceed in performance and sensitivity
the mixtures of ammonium nitrate with nitromethane . And depending
upon the melting point of the nitroaromatic mixtures obtained , some of
the mixtures may even be castable , and should have performance and
sensitivity exceeding amatol . It is also possible that nitrocellulose or
some other material soluble in the melted nitroaromatic mixture could
act as a gelling agent for the nitroaromatics and result in a plastic
mixture with ammonium nitrate , a sort of "gelatine dynamite" based
upon an aromatic base instead of nitroglycerine , which would be more
stable in storage .

[Myrol]

Hmm, today I've made some Mononitronaphthalene with pure Naphthalene (Merck).

I Nitrated 50g of C10H8 with 80,5g of the following Nitration mix: 40,5g 65% HNO3 and 40g 96% H2SO4. The Acids combine to a mix wich the Germans used in WW1 (33% HNO3, 47,5% H2SO4 and 19,5% H2O). I've used 7% HNO3 excess. Ordinary 1% is enough :eek:

So far so good. I added the stinky Naphthalene in a rate to get 55°C in the vessel and the Nitration runned then at this temperature forward. It was my first Attempt, so I was really surprized as I saw how much NO2 this reaction forms.

Even if I nitrate Toluene like a Butcher there isn't so much NO2, just some faint orange clouds instead of barely visible reddish gasses like this time.

My Product was first deep orange and later Desert-Orange. Its a little NaOH-basic now, because I dont want Oxidation products (Phtalic Acid) or tarry stuff in my MNN.

Later I will Nitrate it to TNN wich seems like the perfect sensitizer for AN mixes.

TNN is explosive for itselfs, you can detonate it but the performance is quite poor.

In mix with AN, it should work very good. Even if it's not castable. You can heat the stuff until it softens a little and then press it into your desired container.

In France, TNN was made with a 40/55/5er mixed Acid (HNO3,H2SO4,H2O). I think we can recunstruct this mix also with AN/ H2SO4.

I think/hope H2SO4 reacts with AN mainly to HNO3 and Ammonium Sulphate. If this is true, a mix of 96ml H2SO4 96% and 100g dry AN should work for the Tri-Nitration.

My statement was the following reaction: 2 NH4NO3 + H2SO4--> (NH4)2SO4 + 2 HNO3. I added then the necessary amount of H2SO4 to get the preferred mix, calculated the watercontent back bla bla...and thats all!

100g MNN and 120g AN+ 115ml H2SO4 mix at 60°C should form within 60-120min. around 140g Trinitronaphthalene.

[Rosco Bodine]

The AN + SA reaction should read

NH4NO3 + H2SO4 -----> NH4HSO4 + HNO3

[K9]

Well I just made some MNN with 30 ml H2SO4, 15 grams NH4NO3 and about 37 grams naphthalene. It's still drying so I'm waiting to weigh the yield.

Here are pictures -
http://img.photobucket.com/albums/v78/wolfhound/mnn1.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn2.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn3.jpg

Here's a pic of the final yield - http://img.photobucket.com/albums/v78/wolfhound/mnn4.jpg

The yield is about 40 grams which seems to be not too bad.

So does this look normal colourwise?

And for making it into DNN, would I just renitrate what I have here with the same type of nitrating mix - and how do I tell if it has worked?

Thank you.

[K9]

Well I just made some MNN with 30 ml H2SO4, 15 grams NH4NO3 and about 37 grams naphthalene. It's still drying so I'm waiting to weigh the yield.

Here are pictures -
http://img.photobucket.com/albums/v78/wolfhound/mnn1.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn2.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn3.jpg

Here's a pic of the final yield - http://img.photobucket.com/albums/v78/wolfhound/mnn4.jpg

The yield is about 40 grams which seems to be not too bad.

So does this look normal colourwise?

And for making it into DNN, would I just renitrate what I have here with the same type of nitrating mix - and how do I tell if it has worked?

Thank you.

[K9]

Well I just made some MNN with 30 ml H2SO4, 15 grams NH4NO3 and about 37 grams naphthalene. It's still drying so I'm waiting to weigh the yield.

Here are pictures -
http://img.photobucket.com/albums/v78/wolfhound/mnn1.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn2.jpg
http://img.photobucket.com/albums/v78/wolfhound/mnn3.jpg

Here's a pic of the final yield - http://img.photobucket.com/albums/v78/wolfhound/mnn4.jpg

The yield is about 40 grams which seems to be not too bad.

So does this look normal colourwise?

And for making it into DNN, would I just renitrate what I have here with the same type of nitrating mix - and how do I tell if it has worked?

Thank you.

[Myrol]

Wow, look like a nicely pure MNN wich you've made!

Mine one is more orange, so NOx could be occluded in the crystals....Unfortunately my MNN stinks like Naphthalene, so I'm sure theres unnitrated Naphthalene in it.

Well, pure MNN should look like sandy crystals. And your MNN is sandy-brown.

The Di-step is very easily made with KNO3/ H2SO4 or NH4NO3 but because the mix is very anhydrous you get a lot of TNN in your product. I think this is good.

Just Nitrate the MNN at 60°C with your mix. Then you will be fine and get mostly DNN and TNN.

[Myrol]

Wow, look like a nicely pure MNN wich you've made!

Mine one is more orange, so NOx could be occluded in the crystals....Unfortunately my MNN stinks like Naphthalene, so I'm sure theres unnitrated Naphthalene in it.

Well, pure MNN should look like sandy crystals. And your MNN is sandy-brown.

The Di-step is very easily made with KNO3/ H2SO4 or NH4NO3 but because the mix is very anhydrous you get a lot of TNN in your product. I think this is good.

Just Nitrate the MNN at 60°C with your mix. Then you will be fine and get mostly DNN and TNN.

[Myrol]

Wow, look like a nicely pure MNN wich you've made!

Mine one is more orange, so NOx could be occluded in the crystals....Unfortunately my MNN stinks like Naphthalene, so I'm sure theres unnitrated Naphthalene in it.

Well, pure MNN should look like sandy crystals. And your MNN is sandy-brown.

The Di-step is very easily made with KNO3/ H2SO4 or NH4NO3 but because the mix is very anhydrous you get a lot of TNN in your product. I think this is good.

Just Nitrate the MNN at 60°C with your mix. Then you will be fine and get mostly DNN and TNN.

[K9]

Mine still smells a little bit like naphthalene and I think I saw some white crystals here and there still in there, but it definitely doesn't smell as bad as regular naphthalene so I guess most converted. Is it possible that some went to DNN in this one step, or would that not happen?

And for the DNN/TNN step, I just re-prepare a nitrating mix and let it go for about an hour at 60 C? I figured it would be something like that. I'm just wondering how that compares to Megalomania's synthesis -

"Prepare a second nitrating mixture by putting 300 mL of 53% sulfuric acid in a 1000-mL beaker. Cool the acid to 25 °C by placing in a salt-ice bath. Add 152 g of potassium nitrate to the acid while stirring rapidly. Remove the mononitronaphthalene from the previous reaction and crush it up, add it in small bits while stirring to the mixture, maintain the temperature between 38 °C and 45 °C. The addition should require about 1 hour, do not allow the temperature to go over 45 °C at any time during the addition. After the addition, continue stirring and heat the beaker to 55 °C until the formation of dinitronaphthalene crystals begin. Filter the contents of the beaker on an acid filter to collect the crystals of dinitronaphthalene that should have formed. Wash the crystals with six portions of cold water and allow them to dry. Dissolve the dry crystals in boiling acetone. Filter this solution while hot to remove any undissolved impurities, collect the filtrate and allow it to cool by placing in a salt-ice bath. Filter to collect the pure crystals of dinitronaphthalene. Collect the acetone filtrate from this filtering, boil it to reduce the volume by half, and cool in a salt-ice bath. Again filter to collect a second crop of dinitronaphthalene, add these crystals to the previous and allow them to dry."

Although what I did for the MNN doesn't really match his either.
I guess I'll just try it out this way. Is there anything that will be a visual sign that this has worked, or is that just a matter of checking melting points?

Thank you again for the help.

[K9]

Mine still smells a little bit like naphthalene and I think I saw some white crystals here and there still in there, but it definitely doesn't smell as bad as regular naphthalene so I guess most converted. Is it possible that some went to DNN in this one step, or would that not happen?

And for the DNN/TNN step, I just re-prepare a nitrating mix and let it go for about an hour at 60 C? I figured it would be something like that. I'm just wondering how that compares to Megalomania's synthesis -

"Prepare a second nitrating mixture by putting 300 mL of 53% sulfuric acid in a 1000-mL beaker. Cool the acid to 25 °C by placing in a salt-ice bath. Add 152 g of potassium nitrate to the acid while stirring rapidly. Remove the mononitronaphthalene from the previous reaction and crush it up, add it in small bits while stirring to the mixture, maintain the temperature between 38 °C and 45 °C. The addition should require about 1 hour, do not allow the temperature to go over 45 °C at any time during the addition. After the addition, continue stirring and heat the beaker to 55 °C until the formation of dinitronaphthalene crystals begin. Filter the contents of the beaker on an acid filter to collect the crystals of dinitronaphthalene that should have formed. Wash the crystals with six portions of cold water and allow them to dry. Dissolve the dry crystals in boiling acetone. Filter this solution while hot to remove any undissolved impurities, collect the filtrate and allow it to cool by placing in a salt-ice bath. Filter to collect the pure crystals of dinitronaphthalene. Collect the acetone filtrate from this filtering, boil it to reduce the volume by half, and cool in a salt-ice bath. Again filter to collect a second crop of dinitronaphthalene, add these crystals to the previous and allow them to dry."

Although what I did for the MNN doesn't really match his either.
I guess I'll just try it out this way. Is there anything that will be a visual sign that this has worked, or is that just a matter of checking melting points?

Thank you again for the help.

[K9]

Mine still smells a little bit like naphthalene and I think I saw some white crystals here and there still in there, but it definitely doesn't smell as bad as regular naphthalene so I guess most converted. Is it possible that some went to DNN in this one step, or would that not happen?

And for the DNN/TNN step, I just re-prepare a nitrating mix and let it go for about an hour at 60 C? I figured it would be something like that. I'm just wondering how that compares to Megalomania's synthesis -

"Prepare a second nitrating mixture by putting 300 mL of 53% sulfuric acid in a 1000-mL beaker. Cool the acid to 25 °C by placing in a salt-ice bath. Add 152 g of potassium nitrate to the acid while stirring rapidly. Remove the mononitronaphthalene from the previous reaction and crush it up, add it in small bits while stirring to the mixture, maintain the temperature between 38 °C and 45 °C. The addition should require about 1 hour, do not allow the temperature to go over 45 °C at any time during the addition. After the addition, continue stirring and heat the beaker to 55 °C until the formation of dinitronaphthalene crystals begin. Filter the contents of the beaker on an acid filter to collect the crystals of dinitronaphthalene that should have formed. Wash the crystals with six portions of cold water and allow them to dry. Dissolve the dry crystals in boiling acetone. Filter this solution while hot to remove any undissolved impurities, collect the filtrate and allow it to cool by placing in a salt-ice bath. Filter to collect the pure crystals of dinitronaphthalene. Collect the acetone filtrate from this filtering, boil it to reduce the volume by half, and cool in a salt-ice bath. Again filter to collect a second crop of dinitronaphthalene, add these crystals to the previous and allow them to dry."

Although what I did for the MNN doesn't really match his either.
I guess I'll just try it out this way. Is there anything that will be a visual sign that this has worked, or is that just a matter of checking melting points?

Thank you again for the help.