shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 09, 2001 12:13 AM
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OLD SOVIET METHOD
A nitrator is filled with 300kg of 93-95%nitric acid is fed with 60kg pentaerythritol previously dried at 100c.By means of a cooling jacket at a temperatuer of 20c is maintained in the nitrator.The equipment is constructed of aluminium, and fitted with a stirrer operating at 120r.m.p,with a funnel for adding the pentaeryritol and with an outlet for discharging the product at the bottom.
After all the pentaerythritol has been introduced the contents of the nitrator are mixed for half an hour,after which the nitration product is allowed to flow to a vacuum filter.As pentaerythritol tetranitrate is present in the form of crystals,filtration is very easy and is complete in about 10-15 min.The concentration of the filtered acid is 78% while the residual acid content in the separated PETn does not exceed 25%
the product is trasferred to a washing tank of acid resistant steel,to be drowned in 800l of water,and stirred for 15 mins.The washer has a double bottom,the upper porous stoneware layer acting as a filter-floor.After being washed PETN is seperated on the filter where it is washed again three times 180l batches of water.the washed product contains 1% of acid.it is neutrlized in a special tank by means of an eight to tenfold amount of1%sodium carbonate solution at 85-90c,the process taling centriuged prior to crystalation.At this stage it still contains0.3-0.5 of acid
crystalation is carried out as follows;2.2kg of acetone and twice as much sodium caronate as needed to neutralize the acid contained in the substance are used for every kilo of petn.the solution is warmed to 58.c and stirred at this temp for 1 hour after which is passed under a presure of 1 atm through a filter and into a crystallizer to45-50.c.The contents of the crystalizer are cooled very slowly;first at a rate 1.c per 5 min,later at 2-2.5.cper 1 min.crystallization is finished within 2 hr.The crystalline PETN is seperated from the solvent in a vacuum filter down to a 15-205acetone content.the residual acetone is later removed by washing with a small amount of ethl alcohol.The final product is dried at 40.c.PETN crystallized from acetone should forfill the following conditions;m.p 138-140.c content of moisture and volatile components max0.1% substances unsoluble in acetone max0.1%,mineral content{as ash]max0.25PETN should be completely free from acid.


Agent Blak
Frequent Poster
Posts: 765
From: Sk. Canada
Registered: SEP 2000
posted February 09, 2001 04:46 PM
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So you don't actually require "White-Nitric Acid(HNO3)"?
has any body that lives in Canada ordered Nitric Acid in through a Pharmacy?
I have access to sulfuric acid so I would like to try the KNO3 Acid method. anybody know if this will work?
Is Pentaerythritol a substance that raises suspition?

------------------
A wise man once said:
"... As He Waits For The Time When The Last Become First And,
The First Shall Become last"
--RATM

Agent Blak-------OUT!!


shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 09, 2001 05:23 PM
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JAPANESE METHOD
At the Maizuru plant, in Japan PETN was manufactured in World War 2 in a plant comprising a nitrator lined with acid-resistant steel and provided witha stirrer{140rpm}, a tank made from acid-resistant steel,a centrifuge,a steel crystallizer and a unit for recovering acetone.
The nitrator is charged with 825kg of concentrated nitric acid[98%}and cooled to 10-15c,after which 150kg of pentaerythritol are added slowly,while the temperature is kept below 15c.The addition of pentaerythritol takes about 2and a half hours.The contents of the nitrator are then allowed to stand quietly for half an hour brfore drowning in some 2000L of water
The aqueous solution of acid is decanted from the above penthrite and run to waste sinse the acid is too dilute to be worth recovering.PETN is stirred with water which is then decanted.In order to ensure thorough washing this operation is repeated 5 times.To the last wash aqueous sodium hydroxide solution is added to form a 0.5%sloution.Mext the PETN is washed again by alternate agitation with water and decantation,four times.An aqueous suspention of the washed product is run into a centrifuge by means of an impeller pump.After being centrifuged,PETN is transported to another building to be purified.
To purify the product,60kg pf moist PETN are thrown into 150kg of acetone warmed to 50-55c and stirred until completelt dissolved.The solution is then filtered through a cotten cloth into a vessel filled with 150L of water.The prwcipitated pentaerythritol tetranirate is centrifuged and dryed in a special room for 22hr at 55c.


pete
Frequent Poster
Posts: 56
From: u.k
Registered: JAN 2001
posted February 09, 2001 05:39 PM
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I would also like to know where or how to get hold of Pentaerythritol, as the explosive PETN sounds resonable to make!!!


MacCleod
Frequent Poster
Posts: 215
From:
Registered: DEC 2000
posted February 10, 2001 07:11 AM
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Pete:you can buy it through the mail from Pyrotek,for $9.95 a lb..All the lit. I've read suggests it is(was?)used in pesticides,but I've not been able to find it anywhere.I'm gonna guess it would be a suspicious chem, as it's rather easy to convert to a very speedy high explosive.Makes me wonder about Pyrotek...Though I do order my alum. and mag. powders there,as they don't impose a qty. limit on them (Firefox does on the finer mesh grades).If anyone finds a commercial source for Penterithritol,feel free to share it!.I think some PETN would be just the thing for making imp. linear shaped charges.


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted February 10, 2001 07:13 AM
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PETN would be very nice if PE could be obtained easily. It's more powerful than RDX, so I've heard, it's stable, safe, sensitive to initiation and not hard to make.
However, I know of nowhere that you can get PE from. You can make it by reacting formaldehyde with acetaldehyde, but you'd probably have to make the acetaldehyde by oxidising ethanol with H2SO4 and potassium bichromate. This works, I have tried it, but it's more trouble than it's worth to make a useful amount. And I've never made PE from it.

So, does anyone know where to get PE from? I think it's used in industry to make paints, resins and varnishes... there could be a possible source for it in this area.


Agent Blak
Frequent Poster
Posts: 765
From: Sk. Canada
Registered: SEP 2000
posted February 10, 2001 05:11 PM
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Someone was saying a while back that you can get it order in through a pharmacy.
does anybody know if the KNO3/H2SO4 method works? if so in what proportions?

------------------
A wise man once said:
"... As He Waits For The Time When The Last Become First And,
The First Shall Become last"
--RATM

Agent Blak-------OUT!!


shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 11, 2001 10:20 PM
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Pentaerythritol was obtained by Tollens andWigand in 1891 from acetaldhyde and formaldehyde according to the following reaction;
CH3CHO+4CH2O+1Ca{OH}2------C{CH2OH}4=1{HCOO}2Ca
- -
2 2


wantsomfet
Frequent Poster
Posts: 233
From: EU
Registered: JAN 2001
posted February 18, 2001 05:12 PM
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I've put together a .pdf of some PETN production patents. Very interesting.
<a href="http://internettrash.com/users/altreal/petn.html" target="_blank">http://internettrash.com/users/altreal/petn.html</a>
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for best catfood visit:
catfood.tsx.org

I was wondering if it were possible to prepare PE by mixing the appropriate volumes (have'nt worked them out yet) of Trioxane and Metaldehyde in an H+ solution. Trioxane is trimerised HCOH and is sold as fuel tabs instead of Hexamine and Metaldehyde is a tetramer of acetaldehyde sold as slug/snail bait, although the strongest soln I have found so far is 20% metaldehyde :( .

I am currently conducting an experiment to make PE using paraformaldehyde/trioxane fuel tablets and metaldehyde slug killer, with Ca(OH)₂. It's the "cold, slow" method since I didn't want to boil several litres of strong formaldehyde solution <img border="0" title="" alt="[Eek!]" src="eek.gif" /> .
The slug killer I am using is "Slug Clear", a 20% w/w emulsion of metaldehyde in (water?).
Ratios are as follows:

250mL of "Slug Clear", corresponding to 57g of metaldehyde,
217g of trioxane fuel tablets (which I get at £1/100g. I love army surplus :) ),
75g of calcium hydroxide,
An extra 1L of water.

I think this is it's fifth week of sitting in the garage, I've forgotten exactly when I started the experiment. There is a load of white sediment at the bottom, which literally until I started writing this I thought was unreacted metaldehyde, but could also be excess calcium hydroxide. I never thought of that before, stupid me. So while I thought it was a failure, it could have worked...
I'll find out soon :) .

I thought 40-50% H2SO4 would de-tri/tetramerize trioxane and metaldehyde into formaldehyde and acetaldehyde :confused: .
Also K-persulfate oxidizes CH3OH to formaldehyde (I think Polverone
tried this sometime) so I suppose one could oxidize vodka to acetaldehyde too :p .

I too have tried to make pentaerythritol from 20% metaldehyde liquid slug clear. I used 35% formalin and calcium hydroxide, and have heated the mixture and left it cool, neither method yielding any PE in detectable quantities.

I believe I may have found the problem which is pretty obvious in hindsight. Metaldehyde is sometimes stabilized with hydroxide to prevent it breaking down into acetaldehyde. If one trys to react it directly with formaldehyde and hydroxide, the metaldehyde will not break up, nor will the formaldehyde attack the metaldehyde to break it up. The metaldehyde must be depolymerised to acetaldehyde first with the use of an acid catalyst, as had been mentioned previously.

I tried this, using sulphuric acid and distilling the acetaldehyde directly into warmed 35% formalin with magnesium hydroxide, (I have read that this can give up to 90% yields, and is readily available as milk of magnesia). I have not got round to isolating and identifying the product yet, but I am cetain that it was acetaldehyde distilling across, which I will probably collect and store next time rather than reacting it directly with the formalin.

As a side note, a couple of useful bits of information I found whilst researching pentaerythritol: It has a solubility of 25g/L in water (though one source states 27g/L) and its solubility increases as the concentration of dissolved formaldehyde increases.

Well I have boiled down the reaction mixture and have good and bad news. The bad news is that the milk of magnesia tablets I used also contained some sucrose making the product very hygroscopic and 'gloopy'. I think I'll stick with simple NaOH as my base next time. The good news however, is that the mass of 'gloop' left is just far to great to be the hydrated remnants of the milk of magnesia tablets. I'm hoping this means that PE was made!

The next lot of acetaldehyde will be collected and I will try the synthesis again under more controlled conditions.