View Full Version : making pentaerythritol
zylion
January 9th, 2003, 07:53 AM
To begin production, a clean plastic 5- gallon(18,945 liters) pail is filled with 2160 grams(2000 ml) of 37% formaldehyde solution(formalin) or 800 grams of paraformaldehyde, 210 grams (275 ml) of acetaldehyde, and 4 quarts (3,785 liters) of water. Technical grade is just fine. Stir and mix this solution, then begin adding powdered quicklime(CaO, calcium oxide)with vigorous stirring. The CaO should be added at such a rate that the temperature of the solution rises to 50 celcius(a little over 120 F)within the first half hour of adding the CaO. Then continued to be added at such a rate the temperature of the mixture does not go over 55 celcius(about 130 F). As can easily be imagined, the fumes of formaldhyde and acetaldehyde get pretty intense as the solution gets hot. They get less revolting as the reaction nears completion and the aldehydes get consumed. The total amount of CaO added is 180 grams.
When all the CaO has been added, the stirring is continued at a more leisurely pace for another three hours(10800 seconds). This long stretch of stirring is bound to tire even the most dedicated explosive manufacturer so an alternative which can be used where electricity is available is to suspend an electric drill or similar motor over the pail, and use a clean paint stirrer attachment to stir the solution. The fumes are not especially flammable, so fires are not the hazard they often are when dealing with more flammable chemicals. Even so rigging an extra long stem for the stirrer, so the motor is elevated above the pail rim, is a wise precaution.
When the stirring is done, it is time to filter the now yellowcolored solution. A large coffee filter fitted inside a plastic funnel will do a good job of this. The total volume of liquid amounts to about 3 gallons(11,355 liters). Contained in this 3 gallons(11,355 liters), is about 3/4 pound(9 ounces=31.103x9=279,927 grams) of pentaerythritol. Now the real work begins as the workaholic explosives manufacturer isolates his product from the mixture.
First, the mixture must be made slightly acid. To do this, hydrochloric acid (the 28% strength material available from hardware stores is good enough) is diluted 50-50 with water. Then this diluted HCI is added to the mixture with stirring until the mixture is acid tot litmus (turns blue litmus paper red). A good way to do this is to add 100 ml of the dilute HCI right away, and then after stirring and checking for acid condition is achieved. This will convert the calcium formate made in the reaction to formic acid and CaCL, and also knock out left over CaO. In these forms they are more easily gotten rid of.
Next the yellow color can be removed by adding 30 grams of activated charcoal powder (Norite brand is usually used in the lab) and stirring it around for a few minutes. Then the solution is once again filtered so as to remove the charcoal, and the filtrate is clear once all the charcoal has been succesfully filtered out. Until then it is black, and the pail is a holy mess. Get a clean pail. This step can be omitted, but a yellow product will result which will be more touchy to convert to PETN without the dreaded red gas being formed. It will also not keep so well.
Now the solution must be reduced in volume so that crystals of pentaerythritol can form. To do this the water and other assorted smelly gunk must be boiled away under a vacuum. Formic acid and the unreacted aldehydes will be eliminated in this process. The first step in this adventure is to get a large enough container to hold the reaction mixture for the boil down. 5-gallon(18,925 liters) flasks are not commonly available to the public, but a good substitute is one of those thick glass water jugs often seen in offices for the water cooler. This is about 5(18,925 liters) gallons in volume, and has a narrow opening which can be plugged with a onehole rubber stopper, and attached to the vacuum source (either aspirator or water bed pump).
To get this process going, put the reaction mixture into the glass jug along with a couple small pieces of a Dr. Scholl's pumice footstone (to ensure an even boil) and a chunk of paraffin wax the size of a small grape (to control frothing). The jug should be heated by means of steam, which can be supplied from a pressure cooker by filling it half of water, clamping a section of automotive hose to the outlet on the lid where the weighted pressure control usually sits, and piping the steam produced from heating the preasure cooker into a cowling surrounding te jug.
The jug should sit in a large pan and be lifted off the bottom an inch or so by use of a few wooden blocks. The steam hose is run under the jug so that the steam rises up around the jug to heat it. The cowling can be as simple as a plasic garbage bag draped around te jug. A drain hose should run from te bottom of the pan to a drain or sink to carry away the water formed from the condesing steam.
When the jug is reasonably warm, vacuum should be applied to it and the heating continued. The contents of the jug will begin to boil away. This should be continued until the volume of liquid in the jug is reduced from 3(11,355) gallons to one gallon.(3,785 liters) Then the heating is stopped, and when te boiling ceases, the vacuum is removed.
Now that the liquid has been concentrated, crystals of pentaerythritol can form. Just let the jug cool off in the refigerator overnight. In the morning, the crystals can be filtered out. The liquid that filters through contains more product. This can be obtained by boiling away until the volume of the liquid is halved, i.e., reduced to 2 quarts(1,8925 liters). Upon cooling, a new crop of crystals can be filtered out. Repeating the process again, and boiling away the liquiddown to one quart, upon cooling, another set of crystals. The remaining liquid can then be flushed down the toilet. The crude product should be purified before use in PETN production. To do this, its weighhed, and an equal weight of distilled water is put into a stainless steel pan, or large pyrex beaker. The volume of water will be about a pint. The water is heated up on a stove, and the crystals are put into the water, along with 10 ml of HCl. Mix them around until they dissolve, and boil a just a litlle bit. Upon cooling, a large mass of crystals will appear. Filter them out. The liguid should then be concentraded down to about half its starting volume, and the cooled. Another crop of crystals will appear. By repeating this process a cuople of more times about 350 grams of pure pentaerythritol will be obtained. It will be a somewhat yellowish, but will work for making PETN. This product should be spread out on wax paper and allowed to dry thoroughly before use.
<small>[ January 27, 2003, 09:28 AM: Message edited by: zylion ]</small>
Bitter
January 9th, 2003, 10:13 AM
Don't post new topics on your first post ! Good god, how many times do we have to tell you people ? It's the wrong section too...
nbk2000
January 9th, 2003, 02:16 PM
It's in the right section now.
And while your post was OK, it'd have been nice if it was something that we didn't already have in the form of the original book on the FTP.
We prefer ORIGINAL content, not simple copy/paste.
Anthony
January 10th, 2003, 02:39 PM
Since PETN is such a lovely material, pentaerythritol is quite important to us. Yet few, if any people synthesise their PE.
So let's see if this thread can't be salvaged.
I myself have a couple of questions:
First, why must the solution be reduced under vacuum and heated with steam? Heating with steam seems to be complicating things unecessarily, I think a water or oil bath would suffice.
PE doesn't even melt until 257*C, so boiling water will likely not harm it. Also, during the purification, it is stated to boil the PE in water. I wonder if the vacuum is required only to lower the BP to the point where steam heating can boil the solution. If this is true then I consider it another good reason to use an oil bath. Vacuum is a pain.
Secondly, zylion, what is your source of acetaldehyde?
Al Nobel
January 10th, 2003, 07:14 PM
As acetaldehyd has a flaming point below 0*C and a boiling point below 35*C it seems to be quite unpleasent to handle.Is there any alternative for it,or an alternative way to syntetisize pentaerythritol?
ALENGOSVIG1
January 10th, 2003, 08:16 PM
Boiling stones dont work under vacuum.
nbk2000
January 10th, 2003, 08:36 PM
To prevent bumping under vacuum, it's usually OK to use a capillary tube immersed in the boiling solution, and to have a slow stream of air (or inert gas) bubbling through it.
stanfield
January 24th, 2003, 05:27 PM
couldn't you rewrite your post with international units ? Liter, Kilogram,...
I converted some of the value of I think I'm wrong somewhere...
is this post writed in US units or UK units ?
mongo blongo
January 24th, 2003, 11:52 PM
Personally I agree. I hate imperial units (they make no sense to me) but that's how some people like to do it.
I remember a mars probe crashed into the atmosphere because two teams were using the two different units. Why can't we all just get along. :)
stanfield
January 25th, 2003, 09:38 AM
yeah, that's right... it's very annoying !
zylion, what the units ? US, UK ?
I'm translating the article in french, and it's really bugging me !
thanx...
Anthony
January 25th, 2003, 01:23 PM
I've never heard anyone in the UK use "quarts" so it's almost certainly America and thus 3.75L to a gal.
If you look at the synth, all the important measurements, e.g. reagent quantities are in gm or ml.
ALENGOSVIG1
January 25th, 2003, 01:45 PM
Im sorry but whats the hell is so complicated about converting the units of measurement yourself?
stanfield
January 25th, 2003, 03:34 PM
there are US gallon and UK gallon...
furthermore, 1 quart (UK system) = 2 pints = 1.136 Liter.
why the hell don't you use international chemistry system ? it's so easy for everyone...
a_bab
January 25th, 2003, 03:49 PM
As NBK2000 said, the Zylion's post it's just a copy/paste "work", hence the units. I guess it's taken from from some Uncle Fester book.
Anthony
January 25th, 2003, 04:30 PM
It's almost certainly an American authored book, so again it's almost certainly America units.
stanfield
January 25th, 2003, 05:39 PM
ok ok let's convert in US system ! :p
Polverone
January 25th, 2003, 10:15 PM
Or you could skip the unit conversion altogether and go straight to the prep that the American book probably imitated in the first place. All of the improvised bits are modifications that a moderately experienced home experimenter would naturally apply anyhow.
<a href="http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0425" target="_blank">http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0425</a>
Machiavelli
January 26th, 2003, 11:45 AM
IMHO we are a scientific board so we should use the units standardized by IUPAC (International Union of Pure and Applied Chemistry).
And that excludes this weird imperial stuff :p
zylion
January 27th, 2003, 09:57 AM
It was a section taken from Uncle Festers Home Workshop Explosives printed in the USA that's right. 4 quarts(liquid measure)= 1 gallon= 3.785 liters.
also browse section Chemistry Related with the topic : Tables weights and measures.
<small>[ January 27, 2003, 01:00 PM: Message edited by: zylion ]</small>
Trinitrotoluene
January 30th, 2003, 12:02 AM
In the future I may have to synthesize pentaerythritol in my lab. I was about to order it from pyrotek but they don't sell it no more. I then sent them an email and their reply was: you need an ATF permit to buy that stuff.I can't seem to find nowhere else that sells pentaerythritol in the United States.
<small>[ January 29, 2003, 11:03 PM: Message edited by: Trinitrotoluene ]</small>
ALENGOSVIG1
January 30th, 2003, 12:48 AM
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> don't sell it no more </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica"> </font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> can't seem to find nowhere </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Are you some kind of imbred hillbilly?
Finding a supplier for pentaerythritol isnt that hard. You just need to spend an hour or two poking around on google. If you cant find a supplier in the states, why not buy it from a euro/asian supplier? Theres lots of places in china that will be happy to sell it to you.
And the guy at pyrotek was lying to you. You dont need any permit.
<small>[ January 29, 2003, 11:49 PM: Message edited by: ALENGOSVIG1 ]</small>
Polverone
January 30th, 2003, 02:32 AM
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">If you cant find a supplier in the states, why not buy it from a euro/asian supplier? Theres lots of places in china that will be happy to sell it to you.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I see lots of places that are willing to sell chemicals by the ton. It's considerably harder to find small scale suppliers. Or are you suggesting he use the old "evaluation sample" trick?
The BATF doesn't regulate pentaerythritol, but I am sure Pyrotek was serious about wanting to see a permit. Fine-mesh aluminum powder isn't regulated either, but a number of suppliers still want to see some sort of explosives manufacturing permit before they let you purchase large quantities of it.
Mr Cool
January 30th, 2003, 02:56 PM
"Or are you suggesting he use the old "evaluation sample" trick?"
Well, I'm sure it beats paying for the stuff <img border="0" title="" alt="[Wink]" src="wink.gif" /> . You'll probably have to pay for postage though, it'll cost quite a lot to send 1.5kg from China to America...
Trinitrotoluene
June 30th, 2003, 03:03 PM
I had found a supplyer in China, after 5 minutes of searching on google. But my concern is woulden't it look a bit suspisious? They don't have any other use for that chem except in some paints, and for heart treatment.
Mr Cool
June 30th, 2003, 03:47 PM
It's been done by people before. Just take some care in the composition of your e-mails to them. Don't try to come up with an excuse for wanting it unless they ask you what it is for, otherwise it may look a bit odd.
Although I personally have never got any PE through a sample scam, I have got some things which I consider to be even more interesting/fun, and certainly a lot more dangerous/suspicious.
bobo
September 4th, 2003, 06:59 AM
I am wondering about the use of PE for the synthesis of dendrimers (symmetric starburst polymers). It is a molecule with symmetry in four equal hydroxyl groups, so it fits the profile for dendritic core somewhat. While I am sure there are compounds better suited as core for dendrimers, could this perhaps be a valid application?
The main issue here would be to have a reaction that attacks the -OH groups and is 100% complete and nonselective, as well as introducing at least two functional groups at the outside of the molecule. I can't think of such a reaction, perhaps someone has one?
Trinitrotoluene
October 10th, 2003, 10:32 PM
If anyone's looking for a source of pentaerythritol someone from ebay sells it, just use the search. The amount sold is 200grams. Another company located in Canada sells pentaerythritol in 1 kg.
knowledgehungry
October 11th, 2003, 10:01 AM
I wouldnt buy that from Ebay, youll get attention from the feds, not because of its use in explosives but because of its use in drug manufacture.
Mumble
October 12th, 2003, 02:25 PM
The one who sells it on Ebay is the same one who runs the company in Canada. I've been looking into buying a thing or two from them, but they seem to be a bit on the shady side of things. Also, shipping is outrageous, but the prices seem pretty good. I guess it all evens out, but something about that has trap written all over it. A month or two ago they sold Red Phosphorous.
nbk2000
October 12th, 2003, 03:25 PM
"Companies" that sell only "forbidden" chemicals like red phosphorus and PE are either A) traps ran by the government to snare dope cooks and terrorists or B) morons who are drawing police heat and who'll gladly hand over their client list to get a reduced sentence. :(
Use 'em while you can, but always use cut-outs and drop boxes to remove yourself from them.
Hang-Man
October 12th, 2003, 05:09 PM
www.expeditedchemicals.com
what do you think NBK?
I think I am going to put an order in for 500g of Penta. I've been in contact with the company and they seem legit. I dont know. I don't think I can pass up a chance to get potassium Chlorate, AN, Hexamine, Pentaerythritol, Urea, and potassium perchlorate in one place, and they are only charging me $10 shipping because I'm in Canada. Are these chemicals illegal to own? or do they have to me made into explosives before they are illegal?
DBSP
October 12th, 2003, 05:15 PM
Not that I'm very paranoid but thats mostly things that pyros use. Had it been in my own country I wouldn't have worried about it. But since it's Canada which I maby wrongly compare with the US I must say I get a bit worried. I wouldn't buy anything from them.
As I said it may be wring to compare Canda with the US but still, it is a but suspicios...
Hang-Man
October 12th, 2003, 05:22 PM
yes, that is what scares me; the only chems they are selling are dangerous ones. ones that only have applications in explosives.
wrench352
October 16th, 2003, 12:16 PM
I cant say about the red phosphorus,but,the rest are unlisted chemicals with legitamit uses.I always thought the issue was liability.As long as the chems are unlisted whats the big deal?I hate that my secret stash is being advertised here now.
Mumble
October 16th, 2003, 05:37 PM
Its just that Pentaerythritol that throws it for me. All the other ones I could easily use in pyro or pyro related proceedure. Soap in a case of a few. I know Pentaerythritol can be used to make paint and some cosmetics, but how many home creators of paint are there actually? I think I'll try to get a few things before I go for the PE. Mostly just to see shipping time and some things like that. That would at least make me feel safer about ordering it. In anycase I'll see about sending it to an alternate location if I do infact get anything.
grendel23
October 17th, 2003, 08:41 AM
I have purchased pentaerythritol from Expedited chemicals. I have had good luck with them. Most of what they sell is pyro chemicals, legal to order and own in the US, if a bit suspicious. If you don't attract attention locally, I doubt that small acquisitions will bring the JBTs.
The drug nazis are the ones you really need to fear, they will hunt you down for small quantities of certain chemicals. Pentaerythritol is not a DEA list I or list II chemical, those are the ones you need to be very carefull about, some more than others. I was amazed to see red phosphorus on e-bay, what idiot would buy it?
bobo
October 17th, 2003, 02:42 PM
This list from Rhodium contains some very common compounds. Ibuprofen for some reason:) A friend of mine eats trays full of ibuprofen, and gets it without prescription.
http://www.rhodium.ws/chemistry/watched.html
markgollum
November 6th, 2004, 01:04 AM
Lately I have been thinking about formaldehyde, and the way it reacts with molecules containing electron withdrawing functional groups (nitros, aldehydes, ketones, and probably halides).
While re-reading the chapter on acrolein in “The War Gasses” I thought why cant PE be made from acrolein?.
(1) CH2CHCHO(g) + H2O(g) – (Heat 120-150°C)--> HOCH2CH2CHO ( I know that this reaction happens at 100°C but I don’t know the rate, perhaps it will be faster in an acidic environment?)
(2) 2 HOCH2CH2CHO + 6 CH2O + Ca(OH)2 --> 2 (HOCH2)4C + Ca(HCOO)2 + 2 H2O ( I am positive that this step will work because when PE is made from acetaldehyde, the product from reaction 1 is an intermediary step)
Alternately, if reaction 1 occurs too slowly to be of use then there is a slim chance these two reactions could be used instead.
(3) CH2CHCHO + HCl > ClCH2CH2CHO (Again I know this rxn occurs but don’t know the rate, I assume that it would be high, even at room temp)
(4) ClCH2CH2CHO + NaOH > HOCH2CH2CHO + NaCl
Actually, scrap this last rxn the strong base would probably convert the aldehyde to a carboxylic acid instead.
akinrog
November 7th, 2004, 06:48 AM
http://rzv073.rz.tu-bs.de/bib/dir1/Books/booknews.htm
The above link contains Organic Syntheses Volumes. One of the volumes contains how to make pentaerythritol from scratch (involving reacting Formaldehyde with Acetaldehyde in presence of a base catalyst.
Marvin
November 7th, 2004, 08:10 AM
akinrog,
There is allready a link to the organic syntheses method in the thread. markgollum is trying to avoid acetaldehyde I think.
The method seems to hold water by my understanding, including the anti markovnikov addition. The true test would be trying it, and finding out at the same time how long its going to take. Acrolein is very nasty though and also very toxic. Its not very forgiving of furthur steps and the last time I made any my yeilds were apalling and I had a lot of charred material.
I think I'd find it easier to make acetaldehyde and it would probably be a lot safer.
mp5
November 24th, 2004, 04:23 PM
Few months ago I had about 10kg of booty for selling.
Now its all been sold off, but I can sell it again.
EMail me: dumbbutnaughtyass@yahoo.de
I sell my man-gina mainly in Germany and rest of Europe.
Until now there were no problems shipping it to Swizerland, Denmark, Norway...etc.
Also if you need my mouth, I can sell you some time in it.
The_Rsert
November 26th, 2004, 07:33 AM
MP5: Don't be so stupid to sell anything through the forum so official!
Maybe next time you will be banned for life from the forum.
freaky_frank
November 26th, 2004, 08:24 PM
Does anyone know how to prepare a polymer of pentaerythritol.
At school we are going to make our own pentaerythritol and then we need to make a polymer out of it...
We just have to make a polymer out of A sugar, doesn't matter what IF it is a sugar, so starch also counts as one.
Anyway does anyone have any idea's about sugar based polymers?
Myrol
January 7th, 2005, 03:04 PM
Ok, this thread discusses the synthesis of Pentaerythrite......but whats about DIpentaerythrite?
I have around 1,5kg of Pentaerythrite at Home and I dont want to make just PETN with it! ;) Dipentaerythritol Hexanitrate could be a VERY nice substitute for PETN because it's MELT-CASTABLE.
DIPEHN is a little less brisant (7500m/s max.) and dense (1,63g/cc) than PETN but it has significant more "power" than PETN. It produces 878Liters Gas on Detonation wich give us an Energydensity of 125mt whilst PETN has 123mt.
With this high Energy it could be a very nice Idea to mix it with MHN to a high-brisant powerful crushing Explosive especially against metal targets :)
Could it work to produce Dipenta if I heat Pentaerythritol to sufficient temperatures for a while? Some answer's were great!
kafrboomer
January 15th, 2008, 11:45 PM
I have recently order 200g of Pentaerythritol off of a website called lg-outdoors which is a hunting supplier. Seemed a little shady at first because of the process used to obtain your payment and information provided, but we will find out in a week or so if I actually get it. They also sell in 1lbs bags. Seems like a lot of PETN to me :) www.lg-outdoors.com was the site
cyf531
January 20th, 2008, 09:05 PM
I would not buy from LG-outdoors, PE is the only chem they sell and under uses it says "PETN" Looks like a setup...
gaussincarnate
January 22nd, 2008, 09:53 PM
I do not think that the government would be dumb enough to try that as a trap. They might as well sell miniguns with a sign on them that says "for killing people." I am not one to believe highly in the intelligence of our elected officials, but that seems a little dumb, even for them. Even still, it would probably not be a good idea. I still cannot believe that they actually listed it as a reagent for producing PETN.
Charles Owlen Picket
January 23rd, 2008, 09:45 AM
I do not think that the government would be dumb enough to try that as a trap.
No, they just did that with red phosphorus for years on end. They have just done that exact thing so many times, people are paranoid about accruing no-knock warrants for surfing.
.... I have little doubt that people would receive the product. Learn the term: "honey-pot snare" for the public on the internet. A few minutes learning about meth cook's issues buying precursors and you would not have ever thought that.
A source for acetaldehyde is more productive, [to synth it from available OTC materials.] Most everyone knows that getting a source of acetaldehyde is smarter and once that's done the "formalin" (any source of formaldehyde) cost penny's. Although there needs to be chemistry work there (it should be fun anyway) the cost would actually be less than $20 a lb !
totenkov
January 23rd, 2008, 10:15 PM
If you're looking for PE its not nearly as hard to find as you would have thought. I was cruising ebay a few weeks back and I just typed it in, and holy shit! There was a seller getting rid of 200g and 1lbs quantities.
I seized the opportunity and bought 1 pound. It looks really nice with the other fuels in my lab :) And no doubt, that will be a shitload of PETN, I when back and noticed that it was gone, and it said there was 45 lb bags avalible, so I think ebay may have taken the listing off, in any case, keep an eye on it.
kafrboomer
January 23rd, 2008, 10:37 PM
I actually just received my 200 grams today in the mail. I figured it would be a little less suspicious if i ordered the smaller amount. So far no problems at all. I plan to make my PETN this weekend :D
Aristocles
January 23rd, 2008, 10:45 PM
I have recently order 200g of Pentaerythritol off of a website called lg-outdoors which is a hunting supplier. Seemed a little shady at first because of the process used to obtain your payment and information provided, but we will find out in a week or so if I actually get it. They also sell in 1lbs bags. Seems like a lot of PETN to me :) www.lg-outdoors.com was the site
Send out some sort of warning if they kick your door in, after making bail, of course. :D It appears reasonably legit but alas that is exactly what they'd want you to think. It appears they have a bit of up and down reviews on ebay.
Did you order through their website directly or via ebay?
megalomania
January 26th, 2008, 05:03 PM
If something goes boom in your neighborhood that destroys property or harms someone, expect a visit from law enforcement, as well you should. If you are conducting harmless experiments, constructive engineering, or not even making explosives at all, then law enforcement has no business or reason to bother you. Unfortunately there are also jack booted thugs who wear the uniform of law enforcement, but murder, rape, and steal at every opportunity.
Charles Owlen Picket
January 27th, 2008, 10:55 AM
Getting a common and continuous source for acetaldehyde is actually not that big of a deal. All it really takes is a condenser or condenser design apparatus and some thought. Have you ever made mercury fulminate? It's certainly one of the easiest primaries to synthesis. If you channel the gas from the fulmination process.....you've got acetaldehyde!!!! True enough, that is a large percentage of the gases when mercury fulminate is mfg.
The process calls for capturing the gas that pours from your fulmination and condensing same. It can be done in a distillation rig! Then you have a combination of acetaldehyde and ethyl nitrate which can be separated via a sep-funnel very quickly. both items very useful.
Your return is very high on this: volume wise you get the same condensation as initial ethanol for the fulmination process.
I know for a fact this works quite well: as I am looking at the acetaldehyde in a sep-funnel from last evening. I've actually done this before as using acetaldehyde to mfg fulminate in and of itself is a seemingly more efficient way to get well formed crystals of that material.
This way you keep the whole sourcing of materials "in house". The actual industrial use of pentaeythritol is limited and certainly limited outside of hobby chemistry. It would take a creative soul to think up a plausible reason for using same at home.
Emil
January 27th, 2008, 02:13 PM
I don't know if I would buy Pentaerythritol off ebay even if I could.
Called me paranoid but I don't think I would like to live with the fact eBay have records of all sales, and for some materials they may even be required to dish them out to LEs.
PETN sounds like a great explosive, but I don't see myself ever synthesizing any. The process for making PE can be easily done, but it isn't one I would like to perform in my area, with all the stink it gives off.
There's always pros and cons of energetic materials, but I think I will be sticking with RDX. Hexamine is alot cheaper and easier to obtain than PE, even though RDX is a bit more picky on which Nitric acid is used.
At least hexamine doesn't raise any eyebrows, and my WFNA can be made from OTC products.
Of course for you blokes over in the USA, things are always more available, so if you can find a legit supply of PE then good on ya!
Charles Owlen Picket
January 27th, 2008, 02:45 PM
I think you may have hit the nail on the head. However there are those that will blow a gasket at anything outside of a fine winter day and think their duty to get into the business of those around them. If that's the case, they may consider the stench from Brimstone within Black Powder to be the coming of the Apocalypse.
For some the purchase of hexamine may raise eyebrows - depends on the location. However, the smell from PE synth is formaldehyde and IF dispersed well, is not too evil.... (?)
Heating fuel within common sourcing for hexamine has rested within one supplier in the US (that I've seen thus far). There is a lot of Trioxane available but hexamine is rarer here. Speaking only for myself, the fun is being able to work from the ground up with various synthesis. I once tried the formaldehyde +ammonia route to hexamine and got enough for quite some time. But there I nailed an enormous amount of ammonia fumes through out the sky. However the yield was stupefying. I would imagine that finding a means to work trioxane to hexamine would be satisfying - as one can find Trioxane heating fuel at surplus dealers for pennies.
Emil
January 27th, 2008, 05:26 PM
I am quite suprised that hexamine is somewhat hard to find in your area, but I suppose these days they will jump at the chance to replace materials which have uses more than its "Intended" use. It all revolves around the big web of limiting our freedom but we won't go into that now.
In a slightly more remote area I would be happy to carry out more experiments and procedures, but of course one has to know the boundaries between acceptable, and pushing his luck.
Hell, if there was ever a way to convert Erythritol to PE then we'd really be rolling.
kafrboomer
January 27th, 2008, 10:08 PM
Did you order through their website directly or via ebay?
I ordered it directly from the website. The only chemical I really am willing to buy off ebay is KNO3. Besides that I am skeptical.
Emil
March 15th, 2008, 07:57 PM
I was recently looking at the production of acetaldehyde, as it is something which is pretty much impossible to buy, and even if you could you would have to have deep pockets judging from the prices I have seen listed.
I was recently looking at a synthesis which involves using Sodium Dichromate, water, Ethanol etc.
This led me to search for some Sodium Dichromate. On my searches I came across this supplier. Now get this. This chemical suppier is located in the UK and is possibly the first company I have ever came across, where in their "About" section, they state that they are more than happy to supply to "individuals, hobbyists, schools, amateur chemists, farmers or businesses".
This alone seems a little suspicious. Not only that, there prices are pretty damn high and they seem to have every chemical a meth cook could dream of. Ephedrine Hydrochloride, Red phosphorous, Hypophosphorous Acid, Hydrogen preoxide, Iodine :eek: :D
Is it just me or is this screaming "TRAP"???
None of it appeals to me, I'm not a meth cook or a terrorist, but it just strikes me beings as the UK is a terrible place to get chems, then all of a sudden you find a shop willing to supply all the chemicals which are almost impossilbe to aquire.
Check it out see what you think... http://www.thechemicalcloset.co.uk/
On another note, I have been looking for a source of Pentaerythritol and have found almost nothing. You guys buying off of that LG outdoors place should be a little bit warey I think, seems suspicious. There are loads of chemical companies in China who supply PE, but they never seem interested unless you are some legit company. I'm not to sure about having PE delivered in from another country anyway, I think customs might look upon a general member of the public buying some chemical which has almost no "Home" use a tad suspicious. Besides most of these Chinese companies only supply in bulk (25kg and over). I don't think they are going to go to the hassle of supplying someone thousands of miles away with a kilo lol.
I suppose I have fell victim and given in to the reported yields of PETN opposed to RDX. Now I am possibley interested in making some Acetaldehyde, then making some PE, then some PETN. I was going to buy some Sodium Dichromate off that site, but don't think that would be a good idea :rolleyes:
Charles Owlen Picket
March 16th, 2008, 04:11 PM
Personally, I would not buy from that place. .....Just my opinion.
I would offer this statement to one I considered a friend: "NO FUCKING WAY".
Here's how that shit works: the 3 letter agencies want to deal with super labs. They could make an effort to find them but may is beautiful Mexico need supplies. More so Mexico than many other places, due to availability of substitutes - this hook is tailored for the US & fabulous Mexico. I don't have to tell you to stay away....it's common sense, but the idea of getting pitched that Email would make me (personally) a bit paranoid.
Nitro
March 16th, 2008, 04:21 PM
Acetaldehyde can be made by dry Destillation of Calciumacetat with Calciumformiat.The most Aldehyds can be made by destillation of Calciumsalts from Carbonicacids with Calciumformiate.
ChippedHammer
March 17th, 2008, 05:42 AM
Personally, I would not buy from that place. .....Just my opinion.
I would offer this statement to one I considered a friend: "NO FUCKING WAY".
Safrole
Ephedrine Hydrochloride
Iodine
Hypophosphorous acid
Methylamine
Phenylacetic acid
Phosphorous Acid
3 necked round bottom flasks
12,000ml boiling flask
12,000ml boiling flask mantle
What the fuck? A store run for meth labs......
Anyone wanna be the lab rat and make a order?
Emil
March 17th, 2008, 07:36 AM
lol that is exactly what I thought. They haven't got any "standard" basic glassware that people might want to buy, like a 600ml beaker. Instead they have 12,000ml boiling flasks... hmmmm.
Well they deliver worldwide so come on now people don't shy away.... haha.
It did make me laugh slightly. the scary thing is I found their site through a piece of junk mail that was in my email inbox. It does make me wonder how it got in there :confused:
The bit that makes me chuckle the most is where they say they supply to "hobbyists". O yeh I almost forgot there are plenty of hobbyist meth cooks out there :rolleyes:
Zajcek
March 17th, 2008, 08:19 PM
If you have some friends interested in buying PE, you can join your wallets and order in bulk from a china supplier. It always works for us when we order potassium nitrate.
Ordering bulk quantities is cheaper than buying or even making a kilogram of that product.
If you know someone who ownes a company can be very helpful.
You should first calculate the cost of the final product (PETN) per gram (kilogram) and compare that to RDX. And then decide if it's worth the trubble. I think that RDX will be cheaper than PETN made from selfmade PE.
Do not be fulled by the yield of the final product.
It is not a good idea to order from sites that are not well known and confirmed by someone you know/trust.
Barnacles
March 18th, 2008, 01:23 AM
I don't know what country you are in where you can do that, but I doubt most people here are going to be buying barrels of Penterythritol anytime soon... Or barrels of anything for that matter. No offense intended.
Charles Owlen Picket
March 18th, 2008, 10:52 AM
You would need to live in a town with large commercial manufacturing of two specific products to find Penterythritol in bulk that was not some bizarre "sting" or looked like one. I had heard of the various web sites that sold it (Penterythritol) and there was something just out of place in it's sale that gives me the creeps. - Sites that sell camping equipment don't have any need for a product that is used in production of xxx on a factory scale.
Emil
March 18th, 2008, 01:40 PM
Zajcek:
Like Barnacles said, I'm not sure which country you are from, but your idea doesn't really sound to practical, at least for me. For starters it is going to look a bit suspicious due to the fact I do not know any company I could order through, meaning I would have to order myself. This is going to raise eyebrows in the modern day society. At least in my country.
Also I was not just thinking of the yield against cost. I know making PE and then PETN would work out more expensive than making the same ammount of RDX. However If I could cut the PE synthesis out, it would be quite the opposite.
It's not too much of a problem, it's not like I'm planning on making heavy ammounts of explosive, so I'll probably just go the long route and synth the PE. Should be an interesting lab overall.
Anyway rather than discuss our headaches obtaining materials, how about we get this thread moving a bit. A good place to start would be discussing the production of Acetaldehyde. All the sources I have read so far, regarding the production of PE, have made it sound like Acetaldehyde is down your local hardware stores in gallon quantities, which couldn't be more unnacurate.
I've searched for Acetaldehyde suppliers, and could only find a couple in the USA. This is no good beings as they won't ship. Not to mention the prices listed for the stuff would be enough to make an established company blush. One price I saw listed for a litre of the stuff was $735! Maybe this could of been a high grade product but even so.
There is a synthesis which Mega has written, it is based around using Sulfuric acid, Sodium Dichromate, water and Ethyl Alcohol. Has anyone tried this before?? if so what were the results like? I will probably be looking to try this myself sometime in the near future.
Zajcek
March 20th, 2008, 08:34 AM
I am very sorry about that I wrote. I never meant to insult anyone, but let me explain.
I guess I am lucky I can access to almost any chemical that is not drug a percursor.
Anything our chem supplier won't sell me I get from a friend who frequently goes to Italy and imports it from there.
Suspicious stuff is almost always ordered to a guys address I know, he knows nothing about chemistry and asks no questions as long as he gets some profit. (I went to primary school with this guy and he is a drug addict, he hates cops, I know him for a long time and I know I can trust him)
Acetic anhydride was pain in the ass to obtain and red phosphorus impossible.
I live in a very small country. We have a pyrotechnic forum and when there are a lot of people searching for one particular product, we make an arrangement, gather money, order greater quantity and at the end we split the product.
Acetaldehyde at our local chemical supplier costs about 35.1€ per 2.5l canister.
There has to be a chem supplier in the US that sells it at almost the same price. Has anyone tried to order from Sigma-Aldrich? They sell acetaldehyde from Fluka for 172.00 USD for liter and 338.00 USD for 2.5 L.
I ordered a lot of stuff from them (from their distributor for our country)
Or what about Alfa Aesar? (does anyone know that company, I have no experiences with it, maybe some day...)
I just searched Ebay, they sell 2x 500ml acetaldehyde, but the stuff is probably just about 20%, but can be distilled. And since you need a small amount just to make some PE with it, it may be just fine since you don't need a lot of it, and just for gathering experiences in synthesizing new chemicals.
By searching some internet and info how could I help you, I noticed that chemicals in the US are a lot more expensive than in europe.
There is a thread on another forum that sounds promissing.
http://www.sciencemadness.org/talk/viewthread.php?tid=55
I will try to find some more info, and even try to make some acetaldehyde at home myself and post the results here, even tho I dno't need it, maybe I will some day when my resources run out and our laws get more strict.
Charles Owlen Picket
March 20th, 2008, 10:48 AM
Frankly, I agree with Zajcek, in that it can be done. I would feel more comfortable relying to a PM on specifics but IF you take certain steps, getting chemicals that are not drug precursors is not too difficult. What is fascinating is that commercially, RDX is indeed cheaper than PETN; even though RDX needs fairly pure, high grade HNO3 for it's mfg.
I saw a procurement supply cost analysis and the cost of RDX is substantially lower than PETN due to the low cost of the main precursor (ammonia & formaldehyde= hexamine). However the bulk supply of Pentaerythritol is of no great cost if the material is looked at in light of the cost of IT'S precursors.
What is often forgotten is that laboratory chemical suppliers are NOT the best ones to get technical-grade materials from. And if you buy reagent-grade chemicals you are paying for something that you may really not need. ...There IS reagent grade Pentaerythritol available that is almost ridiculously high priced. But the cost of tech-grade is quite nominal.
However if anyone has sources [or methods directed to sources]; please keep them in a PM. Too many wonderful avenues have been closed down due to unthinking dolts - using the same techniques that a few have sought & worked very hard to achieve.
vBulletin® v3.7.2, Copyright ©2000-2008, Jelsoft Enterprises Ltd.