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PHILOU Zrealone
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Quote: Originally posted by idrbur  | I am wishing to make nitrobenzene for many weeks but in my area benzene is not available easily but yesterday i read on wikipedia that it can be
synthesised by reacting aniline and KMno4 in specific condition .can anybody explain me the whole procedure from A-Z.
And thanks in advance. |
Benzene can be done by dry distillation of Na benzoate and NaOH...
Same can be done form para-benzene-dioic acid (terephtalic acid) found in OTC PET (Polyethylene-terephtalate) from nearly all soda bottles upon
reaction of NaOH...
The Member publication section is thus very instructive for you:
Member publication
benzene
terephtalic acid
Then reaction of benzene with HNO3 (69%) should do the trick...H2SO4 will help to accelerate the reaction up.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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retrofit
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Erythritol blackened by black mold
A recrystallized sample of erythritol is being eaten by some organism. Not all crystals are affected yet. Some are still clear, others are black. It
is accompanied by a moldy smell.
I'm looking for tips on how to purify it again, since it's clearly contaminated. Would slow recrystallization from boiling be likely to kill and
exclude the organisms/waste products?
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Hawkguy
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What is this
Okay so some of you might have been around when I made my last Erythritol post. Erythritol I bought online (NowFoods brand, Amazon.ca) turned out to
be a different sugar I didn't bother to identify. It looks, smells like sugar, but tastes less sweet, and is a lot more soluble in water. I tried
nitrating it again today, and made a few observations.
- Not very soluble in Acid, made nitrations difficult.
- Lower nitrates of the sugar produced in first nitration would deflagrate very energetically once melted and exposed to flame. Left behind some
Carbon residue. Would decompose, releasing Nitrogen Oxides when heated somewhat gently.
- Second nitration yielded white solid with very low melting point (less than 100 degrees C). Explosive once melted, at a similar scale to DDNP. Would
explode after lower nitrates or unreacted sugar boiled off on heating. When melted it would be a yellow oil floating on surface of water. Would form a
waxy white solid when cool. If someone shows me how, I can post pictures.
So the point of this post? -> What is it? My interest is dying but some of you might find it cool.
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nitro-genes
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Sounds like erythritol although it could be that it is a mix with other low calory sweeteners, what does the package say? A nitration is not a very
effective way of identifying a compound. 
How was it nitrated?
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kecskesajt
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Lower nitrates could be because of Xylitol.
Try a warmer enviroment for nitration(20C°)
ETN has a very low MP(61C°),not a big surprise.
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James Ikanov
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I'd also speculate Xylitol.
It's the only sweetener I know of that would make sense; it's lower nitrates are less explosive IIRC, and they are also a liquid that tends to make a
solution or slurry of the higher nitrates.
However, the higher nitrates are mostly or entirely solid.
| Quote: |
Would explode after lower nitrates or unreacted sugar boiled off on heating.
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Sounds like that could've been bad.
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aga
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Nitrogen Narcosis is a lot less messy.
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Praxichys
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I have NOW Foods erythritol and it works fine for me. You have to use a lot of excess mixed acids to keep the nitration thin enough to stir, otherwise
you get incomplete nitration. Grind the crystals into a fine powder in a coffee grinder or a mortar first, then bake it at 100C for a few minutes,
spread thinly on a metal pan. It should be like flour when you add it to the acids. A good final consistency for the mixed acids and erythritol is
like that of creamed corn or porridge. Pre-chill some extra sulfuric acid. Use it to dilute the mix if it gets too thick and sticky. This soup needs
to sit at 15-20C for about an hour, with occasional stirring after adding all the erythritol for good results.
Crash it into five times its volume of ice water and filter immediately. Transfer the wet ETN directly into a saturated solution of sodium bicarbonate
and shake, venting often. Filter the crude product.
Wash the product thorougly in plain water after neutralization. The lower nitrates and erythritol are very soluble in water and are easily removed.
Recrystallize from warm acetone by making a saturated solution of ETN and acetone in a 50C water bath with stirring. Add acetone slowly at 2 or 3
minute intervals until everything is dissolved. It is extremely soluble so you will not have to use much. Crash the hot solution into fifteen times
its volume in ice-cold water, and filter immediately while cold.
I guarantee it's pure erythritol. It's food-grade and the only listed ingredient. They would be in big trouble if it wasn't.
http://www.nowfoods.com/Erythritol-1-lb.htm
[Edited on 29-7-2015 by Praxichys]
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kecskesajt
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My 6$/kg erythritol works just fine.
My procedure is like this:
Pour H2SO4 to the HNO3.Add a thermomether.Cool under 15 C°.Start adding erythritol 0.5 gramms per 2 mins, keeping the temp bellow 20 C°.After
adding,keeping the temp. at 20 C° for 2 hours.After it,keep the temp at 30C° for another hour.After this add to 3 times of volume ice-slush.Stir for
10 mins.Filter it,wash with water, saturated NaHCO3, water again.Let it dry for 3 days at room temp.After this,recrystalise from hot 80/20
Alcohol/Acetone solution.Add some NaHCO3.Pour it into 3 times of volume of ice-slush water.Stir rapidly for 5 mins.Filter it.It will make the volume
of ETN much bigger.
Use Alcohol or Alcohol/Acetone,ETN is highly soluble in acetone,will make your yield bad.
My yield is between 70-85%.
[Edited on 30-7-2015 by kecskesajt]
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Bert
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Threads Merged
30-7-2015 at 06:37 |
James Ikanov
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Related to the above two posts but not in the exact same line of question.
I recently nitrated an off the shelf erythritol sweetener that also contained small quantities of "Reb A". During the mixed acid process I noted that
the solution became very visibly... red/orangey.
I'm not sure if it's related but could the nitration of these trace ingredients affect the final product significantly?
I've noted that my crystals are generally flake like and yellow compared to granular and white as I've previously read them described.
If it's any help I used about 100g of powdered ammonium nitrate in 125ml solution of sulfuric acid with 35g of sweetener.
It's one of those generic brand "Stevia leaf" sweeteners.
I was perhaps foolish to assume that the other ingredients small percentage of the overall product would not affect the outcome.
While I'm at it, I'll just go ahead and ask a few "stupid" questions.
1) I see continuous references to oxygen balance and I think I roughly or conceptually understand that that equates to a more effective chemical
reaction for the same amount of reactants... but is there a specific advantage beyond this, such as more rapid gas production or greater explosive
brisance? Further, is there a reliable way to calculate the Oxygen balance of a given composition?
2) How reliable is RE factor of TNT? AN is listed on wikipedia as having a VOD of about 2500 IIRC, yet an RE of about 0.42, yet Blackpowder, with a
"VOD" (I use the term loosely) of only 600 has about a 0.55? Is it a difference in density or what? How does one even measure RE?
3) Aside from the stickied compendium of energetics, are there any other general reading resources related specifically to energetic materials?
For better or for worse I've found that I more easily absorb material explicitly related to energetics. I've found it as kind of a helpful carrot for
learning in small parts about chemistry, as most of the compounds are at least somewhat related and the reactions generally follow the same rough
pattern(rapid and literally explosive change to state of matter). I'm not looking to be spoon fed so much as a source relating energetics to the rest
of chemistry, though perhaps that is a tall order....
Thanks for any help you can give.
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Hennig Brand
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Not exactly sure how "small quantities" of impurity translates to a mass fraction or percentage, but in general pure reactants are always preferable
and some impurities can cause big problems for some reactions and product(s) even in small quantities. Erythritol can be obtained cheaply and in high
purity.
1) Taken from the Wiki page on oxygen balance:
"
Oxygen balance (OB, or OB%) is an expression that is used to indicate the degree to which an explosive can be oxidized. If an explosive molecule
contains just enough oxygen to form carbon dioxide from carbon, water from hydrogen molecules, all of its sulfur dioxide from sulfur, and all metal
oxides from metals with no excess, the molecule is said to have a zero oxygen balance. The molecule is said to have a positive oxygen balance if it
contains more oxygen than is needed and a negative oxygen balance if it contains less oxygen than is needed; the combustion will then be incomplete,
and large amount of toxic gases like carbon monoxide will be present. The sensitivity, strength, and brisance of an explosive are all somewhat
dependent upon oxygen balance and tend to approach their maxima as oxygen balance approaches zero.
The oxygen balance is calculated from the empirical formula of a compound in percentage of oxygen required for complete conversion of carbon to carbon
dioxide, hydrogen to water, and metal to metal oxide.
The procedure for calculating oxygen balance in terms of 100 grams of the explosive material is to determine the number of moles of oxygen that are
excess or deficient for 100 grams of a compound.
OB% = (-1600 / Mol. wt. of compound) * (2X + (Y/2) + M - Z)
where
X = number of atoms of carbon, Y = number of atoms of hydrogen, Z = number of atoms of oxygen, and M = number of atoms of metal (metallic oxide
produced).
In the case of TNT (C6H2(NO2)3CH3),
Molecular weight = 227.1
X = 7 (number of carbon atoms)
Y = 5 (number of hydrogen atoms)
Z = 6 (number of oxygen atoms)
Therefore
OB% = (-1600 / 227.1) * (14 + 2.5 - 6)
OB% = −74% for TNT
Because sensitivity, brisance, and strength are properties resulting from a complex explosive chemical reaction, a simple relationship such as oxygen
balance cannot be depended upon to yield universally consistent results. When using oxygen balance to predict properties of one explosive relative to
another, it is to be expected that one with an oxygen balance closer to zero will be the more brisant, powerful, and sensitive; however, many
exceptions to this rule do exist. More complicated predictive calculations, such as those discussed in the next section of the explosive materials
article, result in more accurate predictions."
2) RE (Relative Effectiveness) depends on the application and can be a quick and easy way to get a good approximation of what would be a suitable
charge size to use in a certain application. It is a method used by the military and keep in mind they typically use a large excess of explosives per
shot.
3) Check out the forum library. A good place to start is "The chemistry of Powder and Explosives" which is free to download. There are many great
texts on explosives, many of which can be found online quite easily.
[Edited on 1-8-2015 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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James Ikanov
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Based on the labeling I'm estimating the amount of "Reb A" to be roughly 0.045 grams per gram of sweetener at maximum.... but, the labeling could be
misleading.
I reached this conclusion because the ingredients are listed as 2g per packet, with 2g of erythritol in each packet. The labeling usually goes out to
at least 0.1 grams, meaning that there is less than 0.1g per 2g of erythritol.
I am aware that there is much purer erythritol available, and there are a wide number of reasons I chose to use this particular sweetener, partly
logistical and also simply for curiosity's sake to see if it was possible. It might save me some trouble if I can simply go to the grocery store
rather than wait two weeks for each shipment. Perhaps even some money. That said if it negatively effects the end product then it's not really worth
it I suppose.
After doing some reading I found a rough look at what REB A consists of and I must say I'm very interested in a more proffesional analysis of what
might occur if it was nitrated.... everything about this structure based on my limited knowledge of chemistry screams that it's potentially something
that could cause serious interference or adopt it's own explosive properties....
https://en.wikipedia.org/wiki/Rebaudioside_A
And again, thank you for the information!
Edit: after drying my crystals I took a small sample and burned it under the tip of a propane blowtorch. Something interesting that I haven't seen or
heard specifically described happened: as the ETN deflagrated, the flame was a very distinct blue and then slowly flashed a bright, almost "aluminum
burning" white before disappearing entirely. It was more like watching a very fast thermite.
Is this a common occurrence or no? I'm curious if the small amount of Reb A may have actually significantly altered the properties of my ETN batch.
[Edited on 31-7-2015 by James Ikanov]
[Edited on 1-8-2015 by James Ikanov]
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kecskesajt
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I want to preform a reaction:
From the past days,I made quite a large amount of benzoic acid.
I want to sulphonate to benzene sulphonic acid.
If I add benzoic acid to cc. H2SO4, and heat it to 60 C°, will it get decarboxylated and sulphonated or just sulphonated to benzenesulphonic acid?
And add nitric acid of course to get nitrobenzene.
----------------------------------------------------
Is there any OTC ways to get higher nitrated form of benzene like di or tri nitro benzene?
I don't have dicromated nor TNT.
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PHILOU Zrealone
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@James Ikanov ,
Rebaudioside is <5% in stevia/erythritol. I use the 99% Erythritol - 1% Stevioside blend from Carrefour big departement store in Europe.
If rebaudioside is nitrated it will display the properties of nitrated suggar --> bad stability for storage.
If a few% in ETN, then stabilisation will be lower...and even 1% might be a trouble...yellow color may mean decomposition (NxOy). So recrystalization
is a must!
ETN is overoxygenated (positive OB) then it will burn blue to white since all the carbon and hydrogen in the molecule will find oxygen in the molecule
to fully burn. Aromatic fuels and explosives usually display negative OB and are underoxygenated...carbon/sooth usually remains after burning what
renders the flame yellow and fuliginous.
[Edited on 2-8-2015 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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battoussai114
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Would you rather boil a solution of acetate with excess acetic acid, or try to separate different acetates?
I've used excess acetic acid to get zinc acetate from some leftover zinc carbonate I had and now I need to get the acetate... but I'm still divided
between having my house smelling like vinegar or trying to exploit the solubility of the zinc and some other acetate to separate them.
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aga
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There are times when it's better to just let it go ...
(this not a reference to farting in a lift)
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iloveloli
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I have a question about lead(ii) azide. I mix lead(ii) nitrate solution and potassium azide solution together. The potassium azide solution contain a
little bit N2H4. Then i get a pink powder.
I took really little of the power and burn it. it explode and make a loud sound.
I didn't dry it as it is too terrible........
what is it? i don't thing it is just PbN6.
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PHILOU Zrealone
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| Quote: Originally posted by iloveloli | I have a question about lead(ii) azide. I mix lead(ii) nitrate solution and potassium azide solution together. The potassium azide solution contain a
little bit N2H4. Then i get a pink powder.
I took really little of the power and burn it. it explode and make a loud sound.
I didn't dry it as it is too terrible........
what is it? i don't thing it is just PbN6. |
What makes you think that it is more than just Pb(N3)2?
Did you tried it alone as comparison?
N2H4 doesn't complexate with lead (Pb(2+)) like it does with Ni(2+), Zn(2+), Co(2+), Cu(2+),... with such cations unsoluble sensitive complexes may
form like Ni(N2H4)3(NO3)2.
N2H4 nitrate (N2H5NO3) is very soluble and deliquescent.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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nitro-genes
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Never seen a pinkish colour for lead azide, what was the source of the potassium azide and lead nitrate? Since you mention hydrazine present, I assume
it was synthesized? The pH was presumably much higher when free hydrazine or KOH was present, which might have precipitated a form of basic lead azide
(Does it exist?), alternatively, it may have formed a double salt  . The
obtained yield may give some information, or careful destruction of a well measured amount using acidified nitrite and measure nitrogen gas formed. If
a double salt has formed, start some extensive testing of the compound and patent it ASAP!
[Edited on 11-8-2015 by nitro-genes]
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Antoine
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nitroglycerin from h2so4 and kno3
Hi, I've got a little question, it is possible to make nitroglycerin from potassium nitrate and sulfuric acid instead of nitric acid?
sorry for my poor english
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kecskesajt
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It was discoussed many times in this webpage.
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gdflp
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Search the website, this has been discussed many times in this thread.
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Bert
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Threads Merged
18-8-2015 at 09:06 |
Bert
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Does anyone have hands on experience with a mixture of 70:30 Potassium chlorate:cupric thiocyanate?
It is said to be a flame sensitive primary explosive, is there a VoD published anywhere?
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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PHILOU Zrealone
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| Quote: Originally posted by Bert | Does anyone have hands on experience with a mixture of 70:30 Potassium chlorate:cupric thiocyanate?
It is said to be a flame sensitive primary explosive, is there a VoD published anywhere?
|
Good finding Bert,
I have like 50kg of KSCN and NH4SCN... I knew it was of a certain value for energetic materials.
I don't know the VOD nor the power; I haven't done it yet.
From what I know:
-Cyanides and thiocyanates are good ways to store energy thus energetic fuels. Energy output will be greater than with other more common fuels.
-Stoechiometric intimate mixes of chlorates with those must be brisant especially with the non hygroscopic ones (unsoluble) and/or with heavy metal
ones (Ag, Cu, Hg).
-Copper may be an activator of sensitivity of chlorate...I had chlorate based black powder stabilised with CuCO3, Cu(OH)Cl and/or CaCO3/CuCl2 smelling
chlorine after a while; the basic nature of those compounds was to catch acidity of the sulfur and avoid formation of HClO3; the copper was for
green-blue flame color.
--> So Cu(2+)/Cu(+) may be catalyst of decomposition; lowering the activation energy.
--> Great care must be taken with handling, with quantities and with storage (never in hard casing like hard plastic, glass or iron)! Check on a
regular basis the smell and look of it.
If stored, store away from chemicals, flamable compounds or damageable valuable stuffs ... just in case of a bad event!
Maybe the unstability comes from Cu(ClO3)2?
Copper chlorate tread
Cu(ClO3)2
About the stability of the ingredients...
It seems Cu(SCN)2 is in the line of Cu(CN)2 and unstable towards water...
Cu(CN)2
Cu(SCN)2
[Edited on 21-8-2015 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Bert
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I asked this question as some 15 year old devices composed of this were among a store of old special effects supplies I removed from a venue for safe
destruction off site-
The devices are essentially an electric match head coated with this composition, bound with a nitrocellulose lacquer. They were designed to initiate
shock tube, such as NonEl or NoMatch.
I believe they have degraded due to age (and probably atmospheric moisture, they were not stored in a sealed container with dessicant).
A couple went BANG! very nicely, most just give a sad little spit.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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