megalomania
June 21st, 2003, 11:22 AM
Microtek
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posted 03-18-2001 07:57 AM
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As we all know from recent discussions on this forum, the nitration of both glycerine and mannitol can be easily accomplished using only concentrated H2SO4 and AN or KNO3
etc.
I was wondering if the same could be done with pentaerythritol. There has been some debate on the subject but I haven't been able to find a definite answer.
In my opinion, PETN would be perfect with this method ( if at all possible ), as the ammonium sulfate that is produced along with the nitric, is water soluble. Litterature states that PETN is practically insoluble in water, so large amounts could be used to wash the product.
I have come in contact with a source that is willing to sell PE to me without reservation,
so I really need to know if this method is viable.
wantsomfet
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posted 03-18-2001 11:16 AM
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US Patent 1,660,651 describes the nitration of pentaerythrite by dissolving it in H2SO4 & adding this solution to nitric acid. If that is possible why shouldnt it work with only H2SO4 and nitrate addition?
I have some pentaerythrite, perhaps i'll try it sometime.
http://internettrash.com/users/altreal/petn.html
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Microtek
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posted 03-18-2001 11:39 AM
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I agree. If the H2SO4 doesn't interfere with the process, then it probably will work.
I'd really like to hear of any results if you decide to do this experiment.
PS. How did you obtain your PE ?
[This message has been edited by Microtek (edited March 18, 2001).]
Mr Cool
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posted 03-18-2001 12:50 PM
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Yeah, where do you get PE? I've been looking for ages for a good source of it, but everyone asks questions...
10fingers
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posted 03-18-2001 01:16 PM
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Pyrotek has it for $9.95 per lb. Are you in the U.K.? If so, shipping may be expensive.
wantsomfet
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posted 03-19-2001 06:13 AM
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I looked a long time, too - asked in many pharmacies but they either refused to order (almost any chemicals) or if they were willing they told me the next day that they can't sell it because PE is a coronar active substance. Mmmh, always thought only PE nitrates are that. They probaply mixed it up with PETN/PETriN but since i didn't want to raise more suspition i remained quiet.
I don't like the idea of ordering the PE (online), you'll sure raise someone's attention especially when ordering via Pyrotek.
I exchanged it for(?) some other chemicals.
And no, im not from the UK.
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wantsomfet
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posted 03-19-2001 07:52 AM
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Oh yes, before i try: What do you guys think would be better?
a.) dissolving the PE in H2SO4 and adding the nitrate to the solution
b.) dissolving the PE and nitrate in different portions H2SO4 and combining them ?
thanks in advance!
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wantsomfet
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posted 03-19-2001 02:17 PM
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OK, i couldn't wait and did it.
Patent 1,660,651 gives the following instructions:
" ... One part pentaerythrite is dissolved in six and one-half part
of concentrated sulfuric acid (90 - 95% strength). After all pentaerytrhrite
has been dissolved, the sulfuric acid solution is added slowly to six parts
strong nitric acid (90 - 100% strength), keeping the temperature of the
nitrated mixture between about 40 °C and 60 °C. Instead of strong
nitric acid, we may use, with equally good results, a mixed acid of relatively
low sulfuric acid content, for example, 80% HNO3, 12% H2SO4 and 8% H2O.
After addition of the sulfuric acid solution to the nitric acid is completed,
the mixture is agitated for a short period, for example, one half hour
in order to insure completeteness of reaction, after which the crystalline
pentaerythrite nitrate may be separated from the waste acid by filtration
or by drowning in water. ... "
- 1 part pentaerythritol / 5g
- 6 1/2 parts H2SO4 90% - 95% / 33g
- 6 parts nitric acid 90% - 100% / 30g
1.) In an erlenmeyer flask 5g pentaerythrite
(PE) were dissolved in 18ml (33g) H2SO4 96%. A light red solution was obtained
after heating the acid/PE to ca. 50 °C in a water bath. (At room temperature
not all PE dissolved.)
2.) In another erlenmeyer flask a mix
of 30 ml (55,2g) H2SO4 and 50,5g KNO3 was prepared, reacting to 31,5g HNO3
and 68g KHSO4 (H2SO4 + KNO3 --> HNO3 + KHSO4). A slight excess of H2SO4
was used, only 26,6 ml necessary. (1/2 mole)
3.) After waiting 60 minutes for the reaction
to complete, the HNO3 / KHSO4 was still very thick & syrup like. The
H2SO4/PE solution was added in little amounts over ca. 10 minutes with
constant light shaking the mix. (appears to be a bit difficult because
it's so thick) After another 10 minutes the shit was so thick that i could
put the erlenmeyer flask upside down without one drop lost. Agitating with
a glass rod solved this problem, it turned into a thick white paste.
I waited 60 minutes, stirring the mix
from time to time.
Because the mix was not pourable i diluted
it with the same amount distilled water and poured in a 600ml beaker. Then
i added additional 300ml distilled water. Unsoluble white foam was observed
on the surface of the milky solution and a white substance settled at the
bottom of the beaker. After cooling to room temperature i filtered the
solution through normal coffee filterpaper obtaining extremely fine white
crystals (similar to AP).
They are drying right now. After recristallizing
from acetone & drying i'll perform an impact sensitivy test.
I think the procedure works although it'll
be better to use ammonium nitrate instead of potassium nitrate because
of the better solubility of the byproducts.
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Microtek
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posted 03-19-2001 04:21 PM
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Sounds very promising; I can hardly wait to
read about your results!
Jumala
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posted 03-19-2001 09:47 PM
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Pentaerytritol is used in the plastic industry in large quantitys to make polymere. Perhaps there is a possibility to obtain some.
nbk2000
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posted 03-20-2001 06:22 AM
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A helpful hint for dealing with foams in reactions is to add the contents of a capsule of a gas relief medication containing simethicone, commonly available over the counter in GAS-X.
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Jumala
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posted 03-20-2001 09:51 PM
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Very interesting. When it works properly is is one of the best and easiest ways to make a strong HE.
I have an idea:
When you dilute the nitrate/H2SO4 mix with some common 70% nitric acid, so that the total amount of water arises not over 8% (like in the patent script said) it could keep the material in liquit condition.
Then it will be not so much sufate in the solution.
Could it work?
wantsomfet
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posted 03-21-2001 09:59 AM
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Jumala: That could solve the problem with the thick slurry...
I dried the crystals. Before recrystalizing from acetone they weighed 9,7g.
Upon dissolving in boiling acetone (200ml @ 55 °C) not all crystals dissolved, the solution stayed milky and a small blob of lightly yellow substance formed at the bottom of the beaker. I filtered through coffee filter again obtainig a clear solution. This was dumped into 300ml cold distilled water, immediately extremely fine white crystals precipitated which were filtered out, washed with a little water and dried.
Total amount of dry substance: 6,5g.
- If a small piece is ingnited, it melts and then starts bunrnig quietly with a light green flame. (The same did the PETN i extracted from DILCORAN 75).
- It was not possible to set off small amounts placed on an anvil and smashed with a hammer.
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Microtek
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posted 03-22-2001 03:02 PM
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Could you try initiating some with HMTD or AP?
If it is the real thing, then our shaped charge needs will be met ( not to mention plastique filler and bursting charge needs ).
wantsomfet
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posted 03-22-2001 07:05 PM
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I'll make a cap (see my "ANNM/AL sensitized" post) with the substance supposed to be PETN.
We'll see if it can detonate some ANNM (without Al).
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Microtek
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posted 03-23-2001 08:06 AM
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When I test whether an explosive is functional or not, I compress it into a cap with an HMTD initiating charge.
I then tape about 10 iron nails together
( the ones with a square cross-section ),
so they form a "plate". Then I tape the experimental cap onto the plate in such a way that it crosses the nails ( 90 degree angle ). When you detonate the cap, you will be able to see how far the detonation travelled in the cap, by looking at whether the nail corresponding to that section of the cap was bent or not. It helps to mark the nails in some manner, if the tape is not strong enough to hold the them together.
For the supposed PETN I'd suggest a rather thin tube ( 3-4 mm ) as it should be sensitive enough.
wantsomfet
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posted 03-28-2001 02:31 PM
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OK, the shit works! I did some testing and ANNM (with & without metal sensitation and/or smokeless powder) can be detonated with ~1g @ 1,2g/ccm initiated by ~0,3g lightly pressed acetoneperoxide. Although 1g AP @ 0,9g/ccm alone did the job, too. (8mm glasstube)
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wantsomfet
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posted 05-29-2001 08:06 AM
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PETN without white nitric acid, a second attempt:
Calculated ratios of chemicals:
Pentaerythrite: 25g
H2SO4 96% to dissolve PE, 6,5 parts: 162,5g / 88ml
H2SO4 96% for nitration: 294,2g / 160ml (3 mol)
KNO3 for nitration: 303,3g (3 mol)
Again not all pentaerythrite dissolved at room temperature in the calculated amount H2SO4. I added ca. 30ml H2SO4 more -> everything dissolved when heated to ca. 50 °C in a water bath.
The nitration mix was prepared by slowly adding 304g dry KNO3 to 160ml H2SO4 in an ice/water bath. I used more H2SO4/KNO3 mix than necessary to ensure complete nitration (patent suggests 6 parts HNO3 to 1 part pentaerythrite, i used ca. 7,5 parts). After the mix had cooled down to room temperature, the pentaerythrite/sulfuric acid solution was added to the nitration mix in 4 equal portions over a time of ca. 10 minutes with constant stirring & no cooling.
After 60 minutes i diluted with twice the amount of distilled water, filtered with buchner funnel and "sucking flask" (?) and washed with ca. 300ml distilled water. The slightly wet cake was introduced in 800ml acetone held at 50 °C on a hotplate, 5g Na2CO3 was added and the mix stirred for ca. 10 minutes. The solution was filtered again, a clear solution was the result. This clear solution was dumped into the same amount of ice cold distilled water. Immediately large amounts of white substance precipated. Again it was filtered with buchner funnel and "sucking flask" and washed with ca. 100ml distilled water to remove remaining acetone.
It's drying now...
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Agent Blak
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posted 05-29-2001 10:05 AM
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What is the emperical formula for PE aswell as PETN. The fact that you can make a HE with the cutting power of PETN without hard to find HNO3 is awsome. Home made Coridt anyone?
I must say Cudos on that shit there.
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CodeMason
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posted 05-29-2001 06:41 PM
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Pentaerythritol, I believe, can be formed by mixing acetaldehyde and formaldehyde and letting all the liquid evaporate (much the same way you'd make hexamine), but I'd have to check up on that.
Acetaldehyde is a common industrial chemical, and you can make it by bubbling acetylene welding gas through water, perhaps with a catalyst.
Formaldehyde is also a common industrial chemical, and I think it can be made by heating paraformaldehyde.
Anthony
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posted 05-30-2001 05:25 PM
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If true that would be an easy way to get PE, as long as the catalyst for making acetaldehyde wasn't really exotic.
Isn't paraformaldehyde just anhydrous formaldehyde?
CodeMason
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posted 05-30-2001 06:13 PM
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Paraformaldehyde is the polymer of formaldehyde.
CodeMason
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posted 05-30-2001 06:33 PM
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quote:
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It's drying now...
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Famous last words.
Mr Cool
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posted 06-02-2001 06:36 AM
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Formaldehyde is CH2O. You can polymerise it to paraformaldehyde by breaking the C=O bond, thus allowing many to combine: n[CH2O] --> [-CH2O-]n. This paraformaldehyde can be used instead of formaldehyde in the reaction, which is good because a solid is easier to handle and weigh out. When you add paraformaldehyde to water, it depolymerises to a solution of formaldehyde.
To make PE, you react 224 grams of paraformaldehyde with 63 grams of acetaldehyde in 441 mL of water. To this mixture, slowly add 5 grams of Ca(OH)2, and heat with constant stirring to 65*C and hold it at this temperature, while stirring, for 45 minutes. After this time, cool the solution and precipitate the Ca(OH)2 with Na2CO3. Filter the solution, and evapourate the water off at 35*C under reduced pressure (or just let it evapourate or boil it off). Recrystalise the crystals formed from their weight of boiling water (this is untried by me, but came from a reliable source).
** Edit: the reaction needs 4 moles of acetaldehyde for every mole of formaldehyde. Actually, it might be the other way round I'll find out change it **
One way to make acetaldehyde that I have used is this: put 200 grams of K2Cr2O7 into a 2L flask. Add 600 grams of water, and 200 grams of pure ethanol (I actually used methylated spirits (that purple stuff) - 90% ethanol, 5% methanol, and 5% water, and it worked fine). Then slowly add 270 grams of 98% H2SO4, and quickly attach a liebig condenser to the flask. The reaction will heat itself up, turn green due to the reduction of the K2Cr2O7, and acetaldehyde will come off and be condensed. Gentle heating (c. 50*C) of the flask will make sure that all the acetaldehyde is distilled off. It is volatile, so keep it in a tightly sealed container in a cool place.
Maybe you bubble the acetylene through water with H2SO4? This is a common catalyst, but it might also be a heavy metal compound. I'll try and find out, because this method would be easier!
Paraformaldehyde can be bought as a fungicide, mildewcide, portable toilet cleaner, as one part of a two part glue (resorcinol glue? Used in making boats I believe), and from farming supplies as a sheep dip or disinfectant or something. You can also buy 37% formaldehyde solution as a cleaner/anti-microbial in many hardwear stores.
To all UK people here: I'll hopefully be making quite a lot of PE during the summer, so if I trust that you know what you're doing, you won't blow yourself up, and you won't do anything stupid, then I'll sell you some. The amounts will be limited however.
Memebers of the private UK forum can have as much as they want, because I trust them. I'm not sure how much it will cost though!
[This message has been edited by Mr Cool (edited June 03, 2001).]
Mr Cool
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posted 06-14-2001 02:26 PM
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It's four moles of formaldehyde, or the same weight of paraformaldehyde, to every mole of acetaldehyde. It makes formic acid which is neutralised by the calcium hydroxide.
I'm still trying to find out about making acetaldehyde from acetylene.
[This message has been edited by Mr Cool (edited June 14, 2001).]
10fingers
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posted 06-14-2001 05:19 PM
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*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mr Cool
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posted 06-14-2001 05:31 PM
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Catalytic oxidation of ethanol is what I posted.
the freshmaker
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posted 06-14-2001 06:22 PM
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Thats exactly what happens in your body after you have drinkin alot of beers- or other spiritus!
10fingers
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posted 06-14-2001 09:48 PM
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*
[This message has been edited by 10fingers (edited October 26, 2001).]
Mr Cool
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posted 06-16-2001 10:03 AM
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Well that's certainly a possibility. I can't see of any reason why it wouldn't work, except maybe that the larger acetaldehyde molecule would "thrash around" more at the high temp. and tear itself apart (the reason why sucrose caramelises at lower temperatures than glucose).
The method I posted works well though. You can use H2SO4 in as low a concentration as about 25% (see Mega's chemicals section), and K2Cr2O7 isn't very hard to find. There are several UK sources for it, the same is probably true in America.
I haven't been able to find another method for acetaldehyde (e.g. from acetylene), and I think doing a vapour-phase reaction would be more effort to set up efficiently.
pete
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posted 06-16-2001 06:23 PM
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What are your yields of ethanal, the process sounds like a good one. I have read about doing the same process, but adding the oxidizer and alcohol to hot sulphuric, so the ethanal distills of as it is formed. That however makes the process trickly, i messed it up most times i tried it. PETN is great material thought, once i aquired some PE (-; , from college. I made some PETN from it and white nitric acid, my notes, i make notes of all my reactions, yeilds, method etc. Tell me from 43 grams PE i got 66 grams of PETN, i remember up until then i had only used chemicals like nitrocelluose and nitrostarch. I decided to detonate the whole lot in one go, from previous experience i figured 30 meters would protect me. I always protect my ears, good job. I set the charge of, i was on my knees 30 meters back, the shock wave was somthing else, my skin actually went numb. When i stagged up i felt giddy and fell over, man it was something else. Thanks in advance for any information.
pete
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posted 06-17-2001 06:28 AM
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I have read that it is possible to oxidize ethanol with HClO, created from ethanoic acid and NaOCl, bleach. This could save us alot of money, i will research the topic some what further. On a site called Xrefer i have read that polymers of ethanal are used as slug pellets and as a stove camp fuel, and no they don't mean Hexamine. The etanal is easily depolymerized from such a source. The polymer of interest is metaldehyde, a relation of paraldehyde.
Mr Cool
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posted 06-17-2001 07:10 AM
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I know metaldehyde is used in slug pellets, and some solid fuel tablets, but I didn't know this could be depolymerised to acetaldehyde, I thought only paraldehyde could.
Does anyone else know anything about this?
I've never bothered to record my yields accurately with the H2SO4/K2Cr2O7 process. I get nearly 75 mL of crude acetaldehyde per 100 mL of ethanol. This should give you a rough idea of how efficient it is.
I forgot to say:
I'll try the NaClO/acetic acid method, but surely it'll decompose it into sodium acetate, water and chlorine? Or is acetic too weak to do this?
[This message has been edited by Mr Cool (edited June 17, 2001).]
pete
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posted 06-17-2001 08:13 AM
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Nice yield, the meta form is very similar to the para form, the only thing that separates the two in production is the temperature they are polymerized at. I will have a crack at depolymerization of ethanal from slug pellets if i can find some that contain it. As for the oxidization using HOCl, it was not complicated, but i think it would be a touchly reaction, so i will find the reference again and record it accuratly.
[This message has been edited by pete (edited June 17, 2001).]
Mr Cool
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posted 06-17-2001 09:36 AM
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It's not a bad yield, but remember that also contains some ethanol and acetal.
It would be great if you could find out the exact method for oxidising ethanol with NaClO, as that's probably quite easy.
More info on depolymerising paraldehyde, and probably also metaldehyde (thanks to Megalomania and his site!):
To depolymerize paraldehyde back into acetaldehyde, place the paraldehyde into a round-bottom 200-mL Florence
flask. Add 4-5 drops of concentrated sulfuric acid for every 20 g (20 mL) of paraldehyde in the flask. Set the flask up for
fractional distillation, use glass in the fractionating column. Use a 125-mL Erlenmeyer flask as the receiver; keep it cool by
immersing in an ice water (but not salt-ice) bath. Place a loose plug of cotton into the Erlenmeyer flask to help reduce
evaporation loss; it must be loose. Care must be taken to prevent the cotton from coming into contact with the distillate.
After setting up, heat the flask gently. The temperature of the distillate must not be allowed to rise above 35 °C as it will
only repolymerize. The acetaldehyde is now ready for use.
If you depolymerise too much, you can store it by polymerising it like this:
To polymerize acetaldehyde for storage, place it in a dry test tube and cautiously add 1 drop of concentrated sulfuric
acid per 2 mL of acetaldehyde in the tube. Mix thoroughly, the polymerization will begin to take place. Some gentle
warming can hasten the reaction. After some minutes add 3-4 mL of water per 2 mL of acetaldehyde, an insoluble
precipitate of paraldehyde will form.
Edit: You can use paraformaldehyde instead of formaldehyde in the reaction for PE, so you could probably also use paraldehyde instead of acetaldehyde. This would be easier, and safer due to the lack of toxic acetaldehyde fumes.
[This message has been edited by Mr Cool (edited June 17, 2001).]
pete
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posted 06-17-2001 10:33 AM
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Slug pellets are only 3 percent metaldhyde, what the hell is the rest, it does not say. Perhaps the polymer can be separated from the rest of the filler, some sort of solvent extraction seems like the best method to do the job. Is metaldehyde soluble in water, i think that it must be as it is used to poison slugs, and most organic poisons are water soluble. I will find out about the HClO oxidization ASAP, (-:
10fingers
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posted 06-17-2001 09:03 PM
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From U.S.Patent #6,121,498, The manufacture of Acetaldehyde from Acetic Acid. The following was some background info. Theres some other good information there. "Acetaldehyde has been produced commercially by the reaction of ethanol with air at 480 C in the presence of a silver catalyst". That doesn't sound too difficult.
The other process, acetylene reacting with water, uses mercury salts as a catalyst. This process is no longer used because of the toxicity problems. They did not give any other details such as temperature or pressure.
[This message has been edited by 10fingers (edited June 17, 2001).]
Microtek
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posted 06-20-2001 06:06 AM
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Regarding the oxidation of ethanol to acetaldehyde, could the K2Cr2O7 be replaced by KMnO4 and if so, what would the proper amounts be?
Mr Cool
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posted 06-20-2001 08:12 AM
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I was also wondering about KMnO4, but I couldn't find any information on it and I haven't tried it.
I bet the rest of the slug pellets would be chalk or something similar, a bit of soluble adhesive, and blue dye, but without messing around with a few I have no way of knowing. The slug pellets I have in my shed are aluminium sulphate!! ARRRGHHH!!!!
PHILOU Zrealone
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posted 06-21-2001 09:06 AM
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Of course KMnO4 can be used instead of K2Cr2O7
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Mr Cool
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posted 06-21-2001 09:24 AM
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I thought so, but I didn't want to risk losing the rest of my reactants if it didn't work. I thought it might oxidise it to ethanoic acid or something.
PHILOU Zrealone
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posted 06-22-2001 10:46 AM
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They can both do the job to acetic acid and even to carboxylic acid, formic acid and formol; everything is a question of concentration of temperature and of pH.
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PHILOU Zrealone
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posted 06-22-2001 10:48 AM
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I forgot time of reaction; the distillation is there to take the volatile acetaldehyde off the reacting media.
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Mr Cool
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posted 06-24-2001 11:19 AM
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Yes I know both could do it, I just thought that maybe the KMnO4 could do it faster, so that it was oxidised to ethanoic acid (etc) before it could be distilled off.
Microtek
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posted 06-27-2001 05:43 AM
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Could any of you give a few pointers as to how it should be done with KMnO4.
I'm not that good at chemistry I'm afraid.
PHILOU Zrealone
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posted 06-27-2001 10:17 AM
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Take the same procedure but instead of K2Cr2O7 200g use KMnO4 how much grams?
200g/Molar Mass of K2Cr2O7 *Molar Mass of KMnO4= 200g* MM KMnO4/MM K2Cr2O7
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10fingers
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posted 06-27-2001 12:28 PM
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This is good information. I would like to know if this works for anyone. I have seen potassium permanganate for sale in 5 lbs. containers for around $12.00. It was in a DIY store and it was used as some type of rinse for water filters. The least I have seen potassium dichromate for is around $7.50 per lb. from skylighter.
[This message has been edited by 10fingers (edited June 27, 2001).]
Mr Cool
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posted 06-27-2001 01:06 PM
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Yes, KMnO4 is commonly used for killing algae in water containers.
Shit, I was going to work out the amount of KMnO4 needed, but I can't remember the R.A.M. of manganese. I'll find out and tell you all how much KMnO4 is needed.
Anthony
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posted 06-27-2001 04:03 PM
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RAM of Mn = 55
so KMnO4 = 39+55+(16x4) = 158
jin
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posted 07-17-2001 04:38 PM
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i was wondering if metatformaldehyde was used in some brands of solid fuel tablets.
has anybody tested paraldehyde as a seditive drug and anaesthetic
[This message has been edited by jin (edited July 17, 2001).]
PYRO500
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posted 07-18-2001 12:05 AM
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As I recall paraldehyde is poisonous and can cause skin burns, I dont think you wanna inhale that or make someone inhale unless you want to kill them. Sure it probably would knock them out but any oxyagen displacing gas/liquid will do that. I beleve I once read about someone that kidnapped someone by jamming the straw of a PC duster can in someonesmouth ant spraying. From what I hear PC duster has little smell and will knock you flat on your ass
jin
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posted 07-18-2001 01:22 AM
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acetaldehyde also polymerizes when treated with concentrated sulphuric acid.at room temperature paraldehyde,(ch3cho)3 is formed,this is a liquid used as an anaesthetic and seditive.metaldehyde(ch3cho)4
is formed at 0 c.
www.rxmed.com/monographs/paralde2.html
i think its used in alcohol drinks to knock pepole out but it has a bad smell so it may be hard to use
[This message has been edited by jin (edited July 18, 2001).]
jin
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posted 07-25-2001 08:07 PM
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are there any other chemicals used in fuel tablets other than hexamine and metaldehyde i was thinking you could just use metaldehyde(ch2cho)4 fuel tablets and formaldehyde to make pentaerythirtol and save time making the ethanal.
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posted 03-18-2001 07:57 AM
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As we all know from recent discussions on this forum, the nitration of both glycerine and mannitol can be easily accomplished using only concentrated H2SO4 and AN or KNO3
etc.
I was wondering if the same could be done with pentaerythritol. There has been some debate on the subject but I haven't been able to find a definite answer.
In my opinion, PETN would be perfect with this method ( if at all possible ), as the ammonium sulfate that is produced along with the nitric, is water soluble. Litterature states that PETN is practically insoluble in water, so large amounts could be used to wash the product.
I have come in contact with a source that is willing to sell PE to me without reservation,
so I really need to know if this method is viable.
wantsomfet
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posted 03-18-2001 11:16 AM
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US Patent 1,660,651 describes the nitration of pentaerythrite by dissolving it in H2SO4 & adding this solution to nitric acid. If that is possible why shouldnt it work with only H2SO4 and nitrate addition?
I have some pentaerythrite, perhaps i'll try it sometime.
http://internettrash.com/users/altreal/petn.html
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Microtek
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posted 03-18-2001 11:39 AM
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I agree. If the H2SO4 doesn't interfere with the process, then it probably will work.
I'd really like to hear of any results if you decide to do this experiment.
PS. How did you obtain your PE ?
[This message has been edited by Microtek (edited March 18, 2001).]
Mr Cool
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posted 03-18-2001 12:50 PM
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Yeah, where do you get PE? I've been looking for ages for a good source of it, but everyone asks questions...
10fingers
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posted 03-18-2001 01:16 PM
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Pyrotek has it for $9.95 per lb. Are you in the U.K.? If so, shipping may be expensive.
wantsomfet
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posted 03-19-2001 06:13 AM
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I looked a long time, too - asked in many pharmacies but they either refused to order (almost any chemicals) or if they were willing they told me the next day that they can't sell it because PE is a coronar active substance. Mmmh, always thought only PE nitrates are that. They probaply mixed it up with PETN/PETriN but since i didn't want to raise more suspition i remained quiet.
I don't like the idea of ordering the PE (online), you'll sure raise someone's attention especially when ordering via Pyrotek.
I exchanged it for(?) some other chemicals.
And no, im not from the UK.
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wantsomfet
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posted 03-19-2001 07:52 AM
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Oh yes, before i try: What do you guys think would be better?
a.) dissolving the PE in H2SO4 and adding the nitrate to the solution
b.) dissolving the PE and nitrate in different portions H2SO4 and combining them ?
thanks in advance!
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wantsomfet
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posted 03-19-2001 02:17 PM
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OK, i couldn't wait and did it.
Patent 1,660,651 gives the following instructions:
" ... One part pentaerythrite is dissolved in six and one-half part
of concentrated sulfuric acid (90 - 95% strength). After all pentaerytrhrite
has been dissolved, the sulfuric acid solution is added slowly to six parts
strong nitric acid (90 - 100% strength), keeping the temperature of the
nitrated mixture between about 40 °C and 60 °C. Instead of strong
nitric acid, we may use, with equally good results, a mixed acid of relatively
low sulfuric acid content, for example, 80% HNO3, 12% H2SO4 and 8% H2O.
After addition of the sulfuric acid solution to the nitric acid is completed,
the mixture is agitated for a short period, for example, one half hour
in order to insure completeteness of reaction, after which the crystalline
pentaerythrite nitrate may be separated from the waste acid by filtration
or by drowning in water. ... "
- 1 part pentaerythritol / 5g
- 6 1/2 parts H2SO4 90% - 95% / 33g
- 6 parts nitric acid 90% - 100% / 30g
1.) In an erlenmeyer flask 5g pentaerythrite
(PE) were dissolved in 18ml (33g) H2SO4 96%. A light red solution was obtained
after heating the acid/PE to ca. 50 °C in a water bath. (At room temperature
not all PE dissolved.)
2.) In another erlenmeyer flask a mix
of 30 ml (55,2g) H2SO4 and 50,5g KNO3 was prepared, reacting to 31,5g HNO3
and 68g KHSO4 (H2SO4 + KNO3 --> HNO3 + KHSO4). A slight excess of H2SO4
was used, only 26,6 ml necessary. (1/2 mole)
3.) After waiting 60 minutes for the reaction
to complete, the HNO3 / KHSO4 was still very thick & syrup like. The
H2SO4/PE solution was added in little amounts over ca. 10 minutes with
constant light shaking the mix. (appears to be a bit difficult because
it's so thick) After another 10 minutes the shit was so thick that i could
put the erlenmeyer flask upside down without one drop lost. Agitating with
a glass rod solved this problem, it turned into a thick white paste.
I waited 60 minutes, stirring the mix
from time to time.
Because the mix was not pourable i diluted
it with the same amount distilled water and poured in a 600ml beaker. Then
i added additional 300ml distilled water. Unsoluble white foam was observed
on the surface of the milky solution and a white substance settled at the
bottom of the beaker. After cooling to room temperature i filtered the
solution through normal coffee filterpaper obtaining extremely fine white
crystals (similar to AP).
They are drying right now. After recristallizing
from acetone & drying i'll perform an impact sensitivy test.
I think the procedure works although it'll
be better to use ammonium nitrate instead of potassium nitrate because
of the better solubility of the byproducts.
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Microtek
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posted 03-19-2001 04:21 PM
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Sounds very promising; I can hardly wait to
read about your results!
Jumala
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posted 03-19-2001 09:47 PM
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Pentaerytritol is used in the plastic industry in large quantitys to make polymere. Perhaps there is a possibility to obtain some.
nbk2000
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posted 03-20-2001 06:22 AM
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A helpful hint for dealing with foams in reactions is to add the contents of a capsule of a gas relief medication containing simethicone, commonly available over the counter in GAS-X.
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Jumala
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posted 03-20-2001 09:51 PM
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Very interesting. When it works properly is is one of the best and easiest ways to make a strong HE.
I have an idea:
When you dilute the nitrate/H2SO4 mix with some common 70% nitric acid, so that the total amount of water arises not over 8% (like in the patent script said) it could keep the material in liquit condition.
Then it will be not so much sufate in the solution.
Could it work?
wantsomfet
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posted 03-21-2001 09:59 AM
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Jumala: That could solve the problem with the thick slurry...
I dried the crystals. Before recrystalizing from acetone they weighed 9,7g.
Upon dissolving in boiling acetone (200ml @ 55 °C) not all crystals dissolved, the solution stayed milky and a small blob of lightly yellow substance formed at the bottom of the beaker. I filtered through coffee filter again obtainig a clear solution. This was dumped into 300ml cold distilled water, immediately extremely fine white crystals precipitated which were filtered out, washed with a little water and dried.
Total amount of dry substance: 6,5g.
- If a small piece is ingnited, it melts and then starts bunrnig quietly with a light green flame. (The same did the PETN i extracted from DILCORAN 75).
- It was not possible to set off small amounts placed on an anvil and smashed with a hammer.
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Microtek
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posted 03-22-2001 03:02 PM
--------------------------------------------------------------------------------
Could you try initiating some with HMTD or AP?
If it is the real thing, then our shaped charge needs will be met ( not to mention plastique filler and bursting charge needs ).
wantsomfet
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posted 03-22-2001 07:05 PM
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I'll make a cap (see my "ANNM/AL sensitized" post) with the substance supposed to be PETN.
We'll see if it can detonate some ANNM (without Al).
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Microtek
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posted 03-23-2001 08:06 AM
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When I test whether an explosive is functional or not, I compress it into a cap with an HMTD initiating charge.
I then tape about 10 iron nails together
( the ones with a square cross-section ),
so they form a "plate". Then I tape the experimental cap onto the plate in such a way that it crosses the nails ( 90 degree angle ). When you detonate the cap, you will be able to see how far the detonation travelled in the cap, by looking at whether the nail corresponding to that section of the cap was bent or not. It helps to mark the nails in some manner, if the tape is not strong enough to hold the them together.
For the supposed PETN I'd suggest a rather thin tube ( 3-4 mm ) as it should be sensitive enough.
wantsomfet
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posted 03-28-2001 02:31 PM
--------------------------------------------------------------------------------
OK, the shit works! I did some testing and ANNM (with & without metal sensitation and/or smokeless powder) can be detonated with ~1g @ 1,2g/ccm initiated by ~0,3g lightly pressed acetoneperoxide. Although 1g AP @ 0,9g/ccm alone did the job, too. (8mm glasstube)
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wantsomfet
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posted 05-29-2001 08:06 AM
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PETN without white nitric acid, a second attempt:
Calculated ratios of chemicals:
Pentaerythrite: 25g
H2SO4 96% to dissolve PE, 6,5 parts: 162,5g / 88ml
H2SO4 96% for nitration: 294,2g / 160ml (3 mol)
KNO3 for nitration: 303,3g (3 mol)
Again not all pentaerythrite dissolved at room temperature in the calculated amount H2SO4. I added ca. 30ml H2SO4 more -> everything dissolved when heated to ca. 50 °C in a water bath.
The nitration mix was prepared by slowly adding 304g dry KNO3 to 160ml H2SO4 in an ice/water bath. I used more H2SO4/KNO3 mix than necessary to ensure complete nitration (patent suggests 6 parts HNO3 to 1 part pentaerythrite, i used ca. 7,5 parts). After the mix had cooled down to room temperature, the pentaerythrite/sulfuric acid solution was added to the nitration mix in 4 equal portions over a time of ca. 10 minutes with constant stirring & no cooling.
After 60 minutes i diluted with twice the amount of distilled water, filtered with buchner funnel and "sucking flask" (?) and washed with ca. 300ml distilled water. The slightly wet cake was introduced in 800ml acetone held at 50 °C on a hotplate, 5g Na2CO3 was added and the mix stirred for ca. 10 minutes. The solution was filtered again, a clear solution was the result. This clear solution was dumped into the same amount of ice cold distilled water. Immediately large amounts of white substance precipated. Again it was filtered with buchner funnel and "sucking flask" and washed with ca. 100ml distilled water to remove remaining acetone.
It's drying now...
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Agent Blak
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posted 05-29-2001 10:05 AM
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What is the emperical formula for PE aswell as PETN. The fact that you can make a HE with the cutting power of PETN without hard to find HNO3 is awsome. Home made Coridt anyone?
I must say Cudos on that shit there.
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CodeMason
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posted 05-29-2001 06:41 PM
--------------------------------------------------------------------------------
Pentaerythritol, I believe, can be formed by mixing acetaldehyde and formaldehyde and letting all the liquid evaporate (much the same way you'd make hexamine), but I'd have to check up on that.
Acetaldehyde is a common industrial chemical, and you can make it by bubbling acetylene welding gas through water, perhaps with a catalyst.
Formaldehyde is also a common industrial chemical, and I think it can be made by heating paraformaldehyde.
Anthony
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posted 05-30-2001 05:25 PM
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If true that would be an easy way to get PE, as long as the catalyst for making acetaldehyde wasn't really exotic.
Isn't paraformaldehyde just anhydrous formaldehyde?
CodeMason
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posted 05-30-2001 06:13 PM
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Paraformaldehyde is the polymer of formaldehyde.
CodeMason
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posted 05-30-2001 06:33 PM
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quote:
--------------------------------------------------------------------------------
It's drying now...
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Famous last words.
Mr Cool
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posted 06-02-2001 06:36 AM
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Formaldehyde is CH2O. You can polymerise it to paraformaldehyde by breaking the C=O bond, thus allowing many to combine: n[CH2O] --> [-CH2O-]n. This paraformaldehyde can be used instead of formaldehyde in the reaction, which is good because a solid is easier to handle and weigh out. When you add paraformaldehyde to water, it depolymerises to a solution of formaldehyde.
To make PE, you react 224 grams of paraformaldehyde with 63 grams of acetaldehyde in 441 mL of water. To this mixture, slowly add 5 grams of Ca(OH)2, and heat with constant stirring to 65*C and hold it at this temperature, while stirring, for 45 minutes. After this time, cool the solution and precipitate the Ca(OH)2 with Na2CO3. Filter the solution, and evapourate the water off at 35*C under reduced pressure (or just let it evapourate or boil it off). Recrystalise the crystals formed from their weight of boiling water (this is untried by me, but came from a reliable source).
** Edit: the reaction needs 4 moles of acetaldehyde for every mole of formaldehyde. Actually, it might be the other way round I'll find out change it **
One way to make acetaldehyde that I have used is this: put 200 grams of K2Cr2O7 into a 2L flask. Add 600 grams of water, and 200 grams of pure ethanol (I actually used methylated spirits (that purple stuff) - 90% ethanol, 5% methanol, and 5% water, and it worked fine). Then slowly add 270 grams of 98% H2SO4, and quickly attach a liebig condenser to the flask. The reaction will heat itself up, turn green due to the reduction of the K2Cr2O7, and acetaldehyde will come off and be condensed. Gentle heating (c. 50*C) of the flask will make sure that all the acetaldehyde is distilled off. It is volatile, so keep it in a tightly sealed container in a cool place.
Maybe you bubble the acetylene through water with H2SO4? This is a common catalyst, but it might also be a heavy metal compound. I'll try and find out, because this method would be easier!
Paraformaldehyde can be bought as a fungicide, mildewcide, portable toilet cleaner, as one part of a two part glue (resorcinol glue? Used in making boats I believe), and from farming supplies as a sheep dip or disinfectant or something. You can also buy 37% formaldehyde solution as a cleaner/anti-microbial in many hardwear stores.
To all UK people here: I'll hopefully be making quite a lot of PE during the summer, so if I trust that you know what you're doing, you won't blow yourself up, and you won't do anything stupid, then I'll sell you some. The amounts will be limited however.
Memebers of the private UK forum can have as much as they want, because I trust them. I'm not sure how much it will cost though!
[This message has been edited by Mr Cool (edited June 03, 2001).]
Mr Cool
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posted 06-14-2001 02:26 PM
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It's four moles of formaldehyde, or the same weight of paraformaldehyde, to every mole of acetaldehyde. It makes formic acid which is neutralised by the calcium hydroxide.
I'm still trying to find out about making acetaldehyde from acetylene.
[This message has been edited by Mr Cool (edited June 14, 2001).]
10fingers
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posted 06-14-2001 05:19 PM
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*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mr Cool
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posted 06-14-2001 05:31 PM
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Catalytic oxidation of ethanol is what I posted.
the freshmaker
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posted 06-14-2001 06:22 PM
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Thats exactly what happens in your body after you have drinkin alot of beers- or other spiritus!
10fingers
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posted 06-14-2001 09:48 PM
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*
[This message has been edited by 10fingers (edited October 26, 2001).]
Mr Cool
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posted 06-16-2001 10:03 AM
--------------------------------------------------------------------------------
Well that's certainly a possibility. I can't see of any reason why it wouldn't work, except maybe that the larger acetaldehyde molecule would "thrash around" more at the high temp. and tear itself apart (the reason why sucrose caramelises at lower temperatures than glucose).
The method I posted works well though. You can use H2SO4 in as low a concentration as about 25% (see Mega's chemicals section), and K2Cr2O7 isn't very hard to find. There are several UK sources for it, the same is probably true in America.
I haven't been able to find another method for acetaldehyde (e.g. from acetylene), and I think doing a vapour-phase reaction would be more effort to set up efficiently.
pete
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posted 06-16-2001 06:23 PM
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What are your yields of ethanal, the process sounds like a good one. I have read about doing the same process, but adding the oxidizer and alcohol to hot sulphuric, so the ethanal distills of as it is formed. That however makes the process trickly, i messed it up most times i tried it. PETN is great material thought, once i aquired some PE (-; , from college. I made some PETN from it and white nitric acid, my notes, i make notes of all my reactions, yeilds, method etc. Tell me from 43 grams PE i got 66 grams of PETN, i remember up until then i had only used chemicals like nitrocelluose and nitrostarch. I decided to detonate the whole lot in one go, from previous experience i figured 30 meters would protect me. I always protect my ears, good job. I set the charge of, i was on my knees 30 meters back, the shock wave was somthing else, my skin actually went numb. When i stagged up i felt giddy and fell over, man it was something else. Thanks in advance for any information.
pete
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posted 06-17-2001 06:28 AM
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I have read that it is possible to oxidize ethanol with HClO, created from ethanoic acid and NaOCl, bleach. This could save us alot of money, i will research the topic some what further. On a site called Xrefer i have read that polymers of ethanal are used as slug pellets and as a stove camp fuel, and no they don't mean Hexamine. The etanal is easily depolymerized from such a source. The polymer of interest is metaldehyde, a relation of paraldehyde.
Mr Cool
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posted 06-17-2001 07:10 AM
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I know metaldehyde is used in slug pellets, and some solid fuel tablets, but I didn't know this could be depolymerised to acetaldehyde, I thought only paraldehyde could.
Does anyone else know anything about this?
I've never bothered to record my yields accurately with the H2SO4/K2Cr2O7 process. I get nearly 75 mL of crude acetaldehyde per 100 mL of ethanol. This should give you a rough idea of how efficient it is.
I forgot to say:
I'll try the NaClO/acetic acid method, but surely it'll decompose it into sodium acetate, water and chlorine? Or is acetic too weak to do this?
[This message has been edited by Mr Cool (edited June 17, 2001).]
pete
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posted 06-17-2001 08:13 AM
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Nice yield, the meta form is very similar to the para form, the only thing that separates the two in production is the temperature they are polymerized at. I will have a crack at depolymerization of ethanal from slug pellets if i can find some that contain it. As for the oxidization using HOCl, it was not complicated, but i think it would be a touchly reaction, so i will find the reference again and record it accuratly.
[This message has been edited by pete (edited June 17, 2001).]
Mr Cool
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posted 06-17-2001 09:36 AM
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It's not a bad yield, but remember that also contains some ethanol and acetal.
It would be great if you could find out the exact method for oxidising ethanol with NaClO, as that's probably quite easy.
More info on depolymerising paraldehyde, and probably also metaldehyde (thanks to Megalomania and his site!):
To depolymerize paraldehyde back into acetaldehyde, place the paraldehyde into a round-bottom 200-mL Florence
flask. Add 4-5 drops of concentrated sulfuric acid for every 20 g (20 mL) of paraldehyde in the flask. Set the flask up for
fractional distillation, use glass in the fractionating column. Use a 125-mL Erlenmeyer flask as the receiver; keep it cool by
immersing in an ice water (but not salt-ice) bath. Place a loose plug of cotton into the Erlenmeyer flask to help reduce
evaporation loss; it must be loose. Care must be taken to prevent the cotton from coming into contact with the distillate.
After setting up, heat the flask gently. The temperature of the distillate must not be allowed to rise above 35 °C as it will
only repolymerize. The acetaldehyde is now ready for use.
If you depolymerise too much, you can store it by polymerising it like this:
To polymerize acetaldehyde for storage, place it in a dry test tube and cautiously add 1 drop of concentrated sulfuric
acid per 2 mL of acetaldehyde in the tube. Mix thoroughly, the polymerization will begin to take place. Some gentle
warming can hasten the reaction. After some minutes add 3-4 mL of water per 2 mL of acetaldehyde, an insoluble
precipitate of paraldehyde will form.
Edit: You can use paraformaldehyde instead of formaldehyde in the reaction for PE, so you could probably also use paraldehyde instead of acetaldehyde. This would be easier, and safer due to the lack of toxic acetaldehyde fumes.
[This message has been edited by Mr Cool (edited June 17, 2001).]
pete
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posted 06-17-2001 10:33 AM
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Slug pellets are only 3 percent metaldhyde, what the hell is the rest, it does not say. Perhaps the polymer can be separated from the rest of the filler, some sort of solvent extraction seems like the best method to do the job. Is metaldehyde soluble in water, i think that it must be as it is used to poison slugs, and most organic poisons are water soluble. I will find out about the HClO oxidization ASAP, (-:
10fingers
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posted 06-17-2001 09:03 PM
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From U.S.Patent #6,121,498, The manufacture of Acetaldehyde from Acetic Acid. The following was some background info. Theres some other good information there. "Acetaldehyde has been produced commercially by the reaction of ethanol with air at 480 C in the presence of a silver catalyst". That doesn't sound too difficult.
The other process, acetylene reacting with water, uses mercury salts as a catalyst. This process is no longer used because of the toxicity problems. They did not give any other details such as temperature or pressure.
[This message has been edited by 10fingers (edited June 17, 2001).]
Microtek
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posted 06-20-2001 06:06 AM
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Regarding the oxidation of ethanol to acetaldehyde, could the K2Cr2O7 be replaced by KMnO4 and if so, what would the proper amounts be?
Mr Cool
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posted 06-20-2001 08:12 AM
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I was also wondering about KMnO4, but I couldn't find any information on it and I haven't tried it.
I bet the rest of the slug pellets would be chalk or something similar, a bit of soluble adhesive, and blue dye, but without messing around with a few I have no way of knowing. The slug pellets I have in my shed are aluminium sulphate!! ARRRGHHH!!!!
PHILOU Zrealone
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posted 06-21-2001 09:06 AM
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Of course KMnO4 can be used instead of K2Cr2O7
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Mr Cool
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From: None of your bloody business!
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posted 06-21-2001 09:24 AM
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I thought so, but I didn't want to risk losing the rest of my reactants if it didn't work. I thought it might oxidise it to ethanoic acid or something.
PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-22-2001 10:46 AM
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They can both do the job to acetic acid and even to carboxylic acid, formic acid and formol; everything is a question of concentration of temperature and of pH.
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-22-2001 10:48 AM
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I forgot time of reaction; the distillation is there to take the volatile acetaldehyde off the reacting media.
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Mr Cool
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Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-24-2001 11:19 AM
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Yes I know both could do it, I just thought that maybe the KMnO4 could do it faster, so that it was oxidised to ethanoic acid (etc) before it could be distilled off.
Microtek
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From:
Registered: JAN 2001
posted 06-27-2001 05:43 AM
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Could any of you give a few pointers as to how it should be done with KMnO4.
I'm not that good at chemistry I'm afraid.
PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 10:17 AM
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Take the same procedure but instead of K2Cr2O7 200g use KMnO4 how much grams?
200g/Molar Mass of K2Cr2O7 *Molar Mass of KMnO4= 200g* MM KMnO4/MM K2Cr2O7
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
10fingers
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From: USA
Registered: SEP 2000
posted 06-27-2001 12:28 PM
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This is good information. I would like to know if this works for anyone. I have seen potassium permanganate for sale in 5 lbs. containers for around $12.00. It was in a DIY store and it was used as some type of rinse for water filters. The least I have seen potassium dichromate for is around $7.50 per lb. from skylighter.
[This message has been edited by 10fingers (edited June 27, 2001).]
Mr Cool
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Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-27-2001 01:06 PM
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Yes, KMnO4 is commonly used for killing algae in water containers.
Shit, I was going to work out the amount of KMnO4 needed, but I can't remember the R.A.M. of manganese. I'll find out and tell you all how much KMnO4 is needed.
Anthony
Moderator
Posts: 2383
From: England
Registered: SEP 2000
posted 06-27-2001 04:03 PM
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RAM of Mn = 55
so KMnO4 = 39+55+(16x4) = 158
jin
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Posts: 113
From: uk
Registered: SEP 2000
posted 07-17-2001 04:38 PM
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i was wondering if metatformaldehyde was used in some brands of solid fuel tablets.
has anybody tested paraldehyde as a seditive drug and anaesthetic
[This message has been edited by jin (edited July 17, 2001).]
PYRO500
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From: somewhere in florida
Registered: SEP 2000
posted 07-18-2001 12:05 AM
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As I recall paraldehyde is poisonous and can cause skin burns, I dont think you wanna inhale that or make someone inhale unless you want to kill them. Sure it probably would knock them out but any oxyagen displacing gas/liquid will do that. I beleve I once read about someone that kidnapped someone by jamming the straw of a PC duster can in someonesmouth ant spraying. From what I hear PC duster has little smell and will knock you flat on your ass
jin
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Posts: 113
From: uk
Registered: SEP 2000
posted 07-18-2001 01:22 AM
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acetaldehyde also polymerizes when treated with concentrated sulphuric acid.at room temperature paraldehyde,(ch3cho)3 is formed,this is a liquid used as an anaesthetic and seditive.metaldehyde(ch3cho)4
is formed at 0 c.
www.rxmed.com/monographs/paralde2.html
i think its used in alcohol drinks to knock pepole out but it has a bad smell so it may be hard to use
[This message has been edited by jin (edited July 18, 2001).]
jin
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Posts: 113
From: uk
Registered: SEP 2000
posted 07-25-2001 08:07 PM
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are there any other chemicals used in fuel tablets other than hexamine and metaldehyde i was thinking you could just use metaldehyde(ch2cho)4 fuel tablets and formaldehyde to make pentaerythirtol and save time making the ethanal.