Sciencemadness Discussion Board - Short question / quick answer - Thread

It's not interesting at all to make an ANNMAL cap, not to mention terribly unreliable. No, there's zero chance of it detonating from pressing it. RDX is probably the least sensitive material I would ever use in a detonator.

For me, it seems interesting since it allows to make a detonator safely at the last moment and 0.2g SADS can't do damages or very little.
The guy in the video was exploding 20g to more 100g boosters of activated ANNMAL directly with a single cap 200mg SADS.

Why you said "No, there's zero chance of it detonating from pressing it"? for what reasons then.. because i think this guy already made it

NeonPulse - 23-8-2014 at 19:32

I doubt it would work as you will have problems with critical diameter in a 1ml syringe. pressing ANNMAL is not likely to make it detonate. Also very small AN charges may not even detonate at all especially when pressed. The only other way is to give it a try.

bbartlog - 27-8-2014 at 20:58

Quote: Originally posted by hyfalcon

They also sell DampRid which is pure calcium chloride at most home stores.

Bit of a thead necro, but I just wanted to note that DampRid, despite its MSDS and labeling, contains some single digit percentage of some impurity. Probably irrelevant if you're just using it to dry something, but for metathesis reactions it may cause issues. I tried to synthesize 2 moles of CuCl₂ via CuSO₄ + CaCl₂ (as DampRid), with followup addition of a small amount of oxalic acid to clear the remaining CaSO₄ from solution. But boiling down precipitated several grams of an additional white substance that formed fibrous crystals. I'm guessing this is some anti-caking agent that is added to stop the DampRid from clumping. Not a showstopper but if you really want 99+% pure CaCl₂ you should use something else.

PHILOU Zrealone - 29-8-2014 at 10:21

@bbartlog,
So if I do understand correctly:
CuSO4 + CaCl2 --> Cu(2+) + 2Cl(-) + CaSO4(s)

But
CaSO4 <==--> Ca(2+) + SO4(2-) (at ambiant T° solubility is > 15g/L)

then you try adding oxalic acid to precipitate Ca oxalate and generate sulfuric acid...
HO2C-CO2H <==> 2H(+) + (-)O2C-CO2(-)
Ca(2+) + (-)O2C-CO2(-) <--==> Ca(C2O4)(s)
2H(+) + SO4(2-) <==> H2SO4

The problem is antagonist equilibriums...
H2SO4 is way stronger acid than oxalic.
Ca oxalate is weakly soluble much more than Ca sulfate.

So probably you get intermediate reactions because H2SO4 dissolution (acidity) forces oxalic acid to be present as the molecular species and not as the dianion.

Or you get a weird intermediary system with CaHSO4 and Ca(O2C-CO2H)2 because both H2SO4 and HO2C-CO2H are diacids...

[Edited on 29-8-2014 by PHILOU Zrealone]

Bert - 29-8-2014 at 17:59

Quote: Originally posted by bbartlog

Quote: Originally posted by hyfalcon

They also sell DampRid which is pure calcium chloride at most home stores.

Indeed!

Calcium chloride is a common garden soil supplement, used by gardeners & vegetable growers after heavy rains deplete soil of available Ca... Which can cause your tomato/pepper/squash plants to develop "Blossom End Rot"

Last year, I thought the same thing... Damp rid, which I had on hand, must be pure CaCl and would be just the thing to use when my garden plants showed signs of Ca shortage after a series of heavy rains.

Whatever the other chemical(s) in DampRid may be, they are not very water soluble. A whitish blanket of undissolved material remained after dissolving most of the DampRid in hot water, decanted the solution from this and used it anyhow. Didn't hurt my tomato and pepper plants, but I will buy garden supplement grade or ice melter grade calcium chloride for either chemistry or garden use in the future.

greenlight - 6-11-2014 at 06:58

I just found an MSDS for the Damprid brand moisture absorbers and in the composition/information on ingredients section it states:

1. Calcium chloride 60.00-100.00%
2. Sodium chloride 1.0%-5.0%
3. Potassium chloride 1.0%-5.0%

Shame they can't give you exact percentages. But this doesn't clear up the fact that the additional chem's added are not water soluble because obviously both Potassium chloride and Sodium chloride are.
Is there something else added they don't mention?

[Edited on 6-11-2014 by greenlight]

[Edited on 6-11-2014 by greenlight]

Bert - 6-11-2014 at 08:08

There is an anti cakeing chemical added, as noted above.

There is also a formulation with scent added, I'd avoid that product.

CuReUS - 7-11-2014 at 02:26

just a quick question
could you make meta nitro benzoic acid by treating nitrobenzene with phosgene in the presence of catalysts like AlCl₃ or glacial acetic acid(they use acetic acid while brominating the ring to activate the bromine) and hydrolysing it

[Edited on 7-11-2014 by CuReUS]

Metacelsus - 7-11-2014 at 05:53

Why not just nitrate benzoic acid? The meta product will be predominant.

CuReUS - 7-11-2014 at 09:48

actually i came across this in my lab record from my undergrad days .i think we had a synthesis challenge at the end of the term and our teacher had given us nitrobenzene as the starting product.What i ended up doing back then was another nitration to get meta dinitro benzene which i selectively reduced using NH₄HS to get meta nitro aniline ,which i diazotised and treated with CuCN to get meta nitro benzonitrile which i finally hydrolysed to get meta nitro benzoic acid

looking back i think if you could just treat it with phosgene ,my work would have been much easier ( and i might have won the prize

) .IIRC ,the guy who ended up winning used a grignard approach.

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...

chemrox - 7-11-2014 at 13:57

IMHO a Grignard approach is usually indicated when making an aromatic acid barring other factors of course. Yield is usually excellent and the reactions are easy to run.

Metacelsus - 7-11-2014 at 15:46

Quote: Originally posted by CuReUS

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...

In my organic chemistry class we nitrated methyl benzoate to methyl m-nitrobenzoate. I can't imagine the acid to be much harder to nitrate than the methyl ester.

CuReUS - 7-11-2014 at 21:57

Quote: Originally posted by chemrox

IMHO a Grignard approach is usually indicated when making an aromatic acid barring other factors of course. Yield is usually excellent and the reactions are easy to run.

Quote: Originally posted by Cheddite Cheese

Quote: Originally posted by CuReUS

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...

In my organic chemistry class we nitrated methyl benzoate to methyl m-nitrobenzoate. I can't imagine the acid to be much harder to nitrate than the methyl ester.

chemrox-but aren't aromatic grignards very difficult to initiate
during my undergrad ,we once made phenyl magnesium bromide so that we could react it with methyl benzoate to make triphenylmethanol
we spent almost 45 minutes trying to react the magnesium with bromobenzene by scratching the magnesium at the bottom of the flask as our teacher had instructed
some people even made a hole through their flask and the magnesium ignited and caused quite a chaos that day

but the guy who won was damn smart :mad:

he used ethane 1,2 dibromide as an initiator to kick start the reaction ,and it worked like a charm.
maybe it was also because of the withdrawing nature of the nitro group

cheddite-the orsyn page that i linked uses methyl benzoate as the starting material .maybe the ester is a lesser deactivating group than the acid

Metacelsus - 8-11-2014 at 05:42

In my organic class, we also made triphenylmethanol, but from benzophenone and the Grignard reagent. The phenylmagnesium bromide formation went easily. We ground up the magnesium metal immediately before adding it to the reaction mixture.

[Edited on 8-11-2014 by Cheddite Cheese]

CuReUS - 8-11-2014 at 06:31

Quote: Originally posted by Cheddite Cheese

We ground up the magnesium metal immediately before adding it to the reaction mixture.

IIRC ,we used magnesium turnings for the reaction.
but dont you think using Mg powder or dust would be dangerous ,considering that metal dusts form explosive mixtures with air and there is copious amounts of ether around to add fuel to the fire

PHILOU Zrealone - 13-11-2014 at 08:14

Grignard with a nitroaromatic?
Would'nt the nitro group be reduced by the Mg into Ar-N=O, Ar-NH-OH, Ar-N=N(O)-Ar, Ar-N=N-Ar or Ar-NH2?

PHILOU Zrealone - 14-11-2014 at 08:37

About the activation of the Mg towards aromatic halide for Grignard's reaction, one may also use a tiny I2 cristal.

About the activation by Br-CH2-CH2-Br...it may react via an unwished Wurtz coupling pathway or dehalogenation...
Ar-Mg-Br + Br-CH2-CH2-Br --> Ar-CH2-CH2-Br + Ar-CH2-CH2-CH2-CH2-Ar + MgBr2
Br-CH2-CH2-Br -Mg/ether-> Br-CH2-CH2-CH2-CH2-Br + (-CH2-CH2-)2 + (-CH2-CH2-)n + CH2=CH2 + MgBr2

[Edited on 14-11-2014 by PHILOU Zrealone]

CuReUS - 15-11-2014 at 20:27

Quote: Originally posted by PHILOU Zrealone

Grignard with a nitroaromatic?
Would'nt the nitro group be reduced by the Mg into Ar-N=O, Ar-NH-OH, Ar-N=N(O)-Ar, Ar-N=N-Ar or Ar-NH2?

this is quite interesting ,i didn't know that grignards could act as reducing agents

BTW,treating nitrobenzene with phosgene followed by subsequent hydrolysis works ,i checked it out

good yield of meta nitro benzoic acid is obtained ,although there is a little coupling as well

Chemosynthesis - 25-11-2014 at 07:10

I was always taught that deactivation only really becomes an issue after two deactivators on a ring.
Contrary to what some may have been led to believe, nitration of benzoic acid is commonplace, and there is a qualitative test based on it (Mohler's test).
In fact, dinitration is possible without complication (PMCID: PMC1197580 Biochem J. Oct 1951; 49(5): 700–704.)

CuReUS - 25-11-2014 at 22:22

Quote: Originally posted by Chemosynthesis

I was always taught that deactivation only really becomes an issue after two deactivators on a ring.

but i remember that one of my friends from that undergrad batch tried a friedel craft alkylation of nitrobenzene followed by KMnO₄ oxidation for getting meta nitro benzoic acid

she was ecstactic that she had worked out the shortest route among all of us (the grignard guy was sceptical though :mad:

)

sure enough ,she failed miserably and became the butt of all jokes for the remaining term

Chemosynthesis - 26-11-2014 at 07:33

Quote: Originally posted by CuReUS

Quote: Originally posted by Chemosynthesis

I was always taught that deactivation only really becomes an issue after two deactivators on a ring.

)

sure enough ,she failed miserably and became the butt of all jokes for the remaining term

You are comparing two very different things here. First, the theory means nothing without the data. You can apply the theory or extrapolate from a named reaction to a new substrate and impress a professor in lecture, but fail miserably to get a lab result due to the most substrate-specific molecular quirks.

The way this is often taught is that the nitronium ion is a very strong, rich electrophile relatively speaking. Nitration of bromobenzene, dinitration of benzene, FC alkylation of polybenzenes, and similarly deactivated benzenes (not nitro) have been reported in literature, to further support the notion that deactivation is a guideline rather than a rule (the first being a common undergraduate laboratory procedure in years past).

Contrast with FC acylation, for example, which often gives only or predominantly one acylation of benzene due to deactivation. It sort of makes sense that having the electron deficient Lewis acid catalyzed EAS alkylation mechanism work on a similarly deactivated benzene would fail.
The specifics get interesting: DOI: 10.1021/jo00299a051

DubaiAmateurRocketry - 13-12-2014 at 15:19

https://www.youtube.com/watch?v=RdYtd0rxxYk

I just wanted to post this video, beautiful effect of the explosive, looks like TNT.

VladimirLem - 21-12-2014 at 08:51

Hi

Does anyone have a synthesis for ETN using 95%< HNO3 + 95%H2SO4+ eritrol ?

I have a lot of synthesis pdfs for ETN, but they all just uses nitrate salts/65%HNO3+H2SO4
I dont think that i want to make it that way, cause i have enough RFNA atm and dont want to have a (partly) underitrated yield

Vlad

Turner - 21-12-2014 at 09:30

I have tried ETN synthesis with anhydrous nitric acid and sulfuric acid a few times and I am still not sure why but I could never get above 60% yields with any process.

This describes a synthesis of ETN with pure nitric and sulfuric acids:

http://energetics.chm.uri.edu/system/files/ETN%20Paper%20acc...

VladimirLem - 21-12-2014 at 11:51

60% yields

this is really strange...

exactly like the text from the link: 2g Erytrol -> 3.6g ETN, isnt really good

i dont get it...most infos say, 1g Erytrol to 2g< ETN (and thats with using nitrate salts/65%HNO3+H2SO4)
how can there be less yield, using higher quality chemicals?
Is it like making TNP, that using over 80%HNO3 will oxidize the material? *confused*

DubaiAmateurRocketry - 25-12-2014 at 15:27

What are a list of journals that publishes articles on EM frequently ?

Hmtd as sensitizer in mixture with lead styphnate and potasium nitrate

otonel - 4-1-2015 at 12:15

I searching a sensitizer for a mixture of lead trinitrorezorcinate or lead picrate and potassium nitrate as replacement for tetrazene because I don`t have it and my searching favorites are : HMTD, cooper azide, silver acetylide.
This sensitive materials are very dangerous alone but if I used 5 % of composition work and delivered ignition when mixture is struck by a blow but what make me to post this topic is chemical stability of my mixture in time.
I prefer to use HMTD because is easy synthesized and work good but I don`t have information about selflife and chemical reactivity with lead styphnate and potassium nitrate plus the container surface will be painted cooper wall to prevent corrosive reaction with this
Please help me with some advices to find best replacement and don`t make a mixture who make boom without mechanical stimuli

[Edited on 4-1-2015 by otonel]

Bert - 4-1-2015 at 12:45

Quote:

Please help me with some advices to find best replacement and don`t make a mixture who make boom without mechanical stimuli

I advise you to stop using organic peroxides immediately, then learn more about such compounds reactivity & chemistry before attempting to make or use other explosives.

NO! DON'T mix Lead or other metallic compounds with HMTD. Don't contain HMTD in Copper metal, even if you have "painted" it.

You have been a member since 2005, I see. Almost as long as I have- What are you trying to do???

otonel - 4-1-2015 at 13:36

Bert , I`m not stupid to blow up my fingers but look at this Priming mixture patent
I don`t know if that mix what used , but if that was so dangerous why they patented , or it was a improvised solution for war ammo

[Edited on 4-1-2015 by otonel]

Bert - 4-1-2015 at 14:08

There were a number of such patents and attempts to use HMTD for primary explosive in military and industrial applications. Reactivity to common metals mostly put an end to these experiments.

If any got past testing stages, I do not know of it. Rosco or other professionals may correct me on that.

Mere existence of the patent doesn't mean it was practically used, or a good idea for one to try for their self.

Are you trying to make a priming compound for small arms?

Rosco Bodine - 6-1-2015 at 21:05

Bert , I`m not stupid to blow up my fingers but look at this Priming mixture patent
I don`t know if that mix what used , but if that was so dangerous why they patented , or it was a improvised solution for war ammo

[Edited on 4-1-2015 by otonel]

That was patented to scam money out of Remington

HMTD is not storage stable and nobody's patent makes it stable.

otonel - 7-1-2015 at 12:04

Are you trying to make a priming compound for small arms?

Yes I m trying )
Thanks for your answers , I tried to find an alternative solution for a sensitive compound but what I find as available for me is not good as chemical stability and have reactivity with metals, the mixture with hmtd works but my safety is more important them my research as hobbyist
I will return to traditional materials used as sensitive compound and right now I search some sources for aminoguanidine nitrate for synthesis tetracene or sodium hypophosphite.
For aminoguanidine synthesis I have urea , sulfuric acid and silica gel , and sodium hypophospite can be made from this stuff foliar fertilizer ?

low yields with ETN

underground - 11-1-2015 at 15:16

Quote: Originally posted by VladimirLem

60% yields

I also have tryed many ways of nitration of E and always the yeields are really poor. With 15gr of E i end with no more than 12gr of ETN.
I use a really boiled H2SO4 and really dry AN but the results are poor. Everything is really dry, well mixed and powdered.

[Edited on 11-1-2015 by underground]

VladimirLem - 12-1-2015 at 09:22

Quote: Originally posted by underground

Quote: Originally posted by VladimirLem

60% yields

i guess your H2SO4 has a bad a quality...

I "made" ETN, using 500ml HNO3(95%<

, 300ml H2SO4 and 100g Erytrit and i fucked it up
Result: 80g ETN :mad:

Check US Patent 1691954

I dissolved 100g E in 150ml H2SO4 (little bubbles visible). That mixture was like wood glue.
Then adding it to the HNO3...FUCK! the mixture was absolutly "insoluble"/hard to mix with the HNO3 that would have resulted in a EXREMELY low yield, so i just want to try the nitration with fine E powder and already mixed around 150ml of H2SO4 into my HNO3 but then i said, give it a try and added the E-H2SO4 mixture again and it become very good soluble into the H2SO4...

well....i added the mixture completely (around 10ml got lost) and have to say that nearly ZERO themerature have risen...i dunno if this is a good or bad (if i have to guess, bad LOL) sign but i was able to drow around 10ml of it at once into the HNO3+(only)150ml H2SO4

this was all done in around 15minutes lol...
so, then i thought that this was damn fast and i heated the whole acid mixture carefully in a waterbath up to 32C. the Acid now bacame clear as water. Only a few lumps of (i guess) undernitrated* ETN floating inside of the acids where visible and then cooling it down
*I added around 10g of fine powdered E to the acids after i added the around 90g E (from the E-H2SO4 mixture)

The whole nitration was around 20-30 minutes...i dont know if it was to short? I cant imagine, cause normaly i dont heat the acides (byside RDX) and the yield is VERY good (at least at mannitol, PE)...never did ETN syn before...

Can anyone say what went THAT wrong at my syn?

Vlad

otonel - 15-1-2015 at 11:36

I am back )
My last priming compound has made from :
-25% lead trinitrorezorcinate
-17% red phosphorus from matches box
-5% tetril
-53% Pb(NO3)2
- some glass powder , and calcium carbonate as anti acid from red phosphorus
I test that mixture and work good and I want your opinion about chemical stability and what can be improved
My source of inspiration was this patent https://drive.google.com/viewerng/viewer?url=patentimages.st...

Bert - 15-1-2015 at 12:05

I want your opinion about chemical stability and what can be improved

It is usual to use some kind of binder and a liquid to make pellets for primer use. How are you handling that?

The red phosphorus will slowly oxidize away in air- Match book striker material is an unknown, but certainly contains ground glass, adhesives, probably shreds of paper fibers and whatever binders/inks/fillers the paper is made with.

Red phosphorus with COATINGS will oxidize less & last longer than the raw or salvaged product, most likely.

https://www.google.com/patents/US8540828

Here's a coating process:

https://docs.google.com/viewer?url=patentimages.storage.goog...

And here's a nice long home made primer thread on a reloading/shooting forum. You may recognize some names there.

http://castboolits.gunloads.com/showthread.php?182089-can-yo...

otonel - 15-1-2015 at 12:23

Thanks, very useful your answer Bert

Trotsky - 24-1-2015 at 04:47

Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.

PHILOU Zrealone - 24-1-2015 at 09:09

Quote: Originally posted by Trotsky

Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.

-If Sucrose is C12H22O11
-Then Sucrose octanitrate is C12H14N8O27
-Assuming density between 1.5 and 1.7 g/ccm (based on density of nitrostrach (1.6) and nitrocellulose (1.67)
-Based on enthalpy of formation evolution from 11%N to 13.3%N nitrocellulose: enthalpy of formation must be between 0 kJ/mol and -1450 kJ/mol.

Entering datas into Engager's SMF detonation calculator utility program:
*With Hf°= -0.1 kJ/mol
if d= 1.7 g/ccm
VOD = 8784 m/s
PCj = 344 kbar

if d= 1.6 g/ccm
VOD = 8382 m/s
PCj = 304 kbar

if d= 1.5 g/ccm
VOD = 7980 m/s
PCj = 267 kbar

*With Hf°= -1450 kJ/mol
if d= 1.7 g/ccm
VOD = 7919 m/s
PCj = 161 kbar

if d= 1.6 g/ccm
VOD = 7567 m/s
PCj = 142 kbar

if d= 1.5 g/ccm
VOD = 7216 m/s
PCj = 124 kbar

Nitro-sugar is considered too unstable for practical use and stabilization is much harder than Nitroglycerin.

[Edited on 24-1-2015 by PHILOU Zrealone]

Dany - 24-1-2015 at 11:14

Quote: Originally posted by Trotsky

Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.

Trotsky,

According to [1], sucrose octanitrate is a solid with a melting point of 85.5°C. If heated slowly, sucrose octanitrate decomposes at about 135° and if heated rapidly deflagrates at about 170°C. The fused and solidified material has a specific gravity of 1.67 g/cm<sup>3</sup>.

The experimental heat of formation (HOF) taken form [2] is HOF= -1364 kJ/mol.

Sucrose octanitrate has a slightly negative oxygen balance (OB%= -9.1) so the BKW thermochemical code [3] with RDX set of parameter is suitable for the calculation of the detonation performance (D_CJ & P_CJ).

Based on the experimental density of 1.67 g/cm<sup>3</sup> and HOF of -1364 kJ/mol we have:

D_CJ= 7821 m/s
P_CJ= 264 kbar.

References:

[1] TENNEY L. DAVIS, The Chemistry of Powder and Explosives, p.p 242.

[2] P.J. Linstrom and W.G. Mallard, Eds., NIST Chemistry WebBook, NIST Standard Reference Database Number 69, National Institute of Standards and Technology, Gaithersburg MD, 20899, http://webbook.nist.gov.

[3] Mader, C. L. 2008. Numerical Modeling of Explosives and Propellants. 3rd ed. Boca Raton, FL: CRC Press.

Dany.

Trotsky - 25-1-2015 at 01:22

You're not kidding about difficulty stabilizing it. I washed 3x with bicarbonate until it measured neutral with my ph paper. Let it sit in a glass jar for 3 hours while I napped. Came back afterwards and found that it'd completely decomposed to a black mass that reaked hard of nitrous oxides. Glad it wasn't worse.

I'm gonna give it another go, but I'll leave it sit in a saturated bicarbonate solution until I'm ready to use it.

otonel - 1-2-2015 at 10:22

If I have a lot of lead acetate cam make lead nitrate using alkaline nitrate without using nitric acid?

roXefeller - 1-2-2015 at 12:37

If I have a lot of lead acetate cam make lead nitrate using alkaline nitrate without using nitric acid?

Its technically a question for the general chemistry forum, but you can use gibbs energy methods to determine this. I don't have the entropy of lead(II) acetate but here is what I have.

lead(II) nitrate H -451.7kJ/mol, S 217.9J/K mol, G -256.9 kJ/mol
lead(II) acetate H -960.9kJ/mol
sodium nitrate H -467.9kJ/mol, S 116.5J/K mol, G -367.0kJ/mol
sodium acetate H -708.8kJ/mol, S 123.0J/K mol, G -607.2kJ/mol

It looks unfavorable based on the enthalpies of formation at least at room temperature.

Hennig Brand - 1-2-2015 at 14:51

If I had lots of lead acetate I would just use that as my soluble lead salt, in place of lead nitrate. At least for my purposes it normally wouldn't make much difference which salt was used.

otonel - 2-2-2015 at 13:03

Quote:

If I had lots of lead acetate I would just use that as my soluble lead salt, in place of lead nitrate. At least for my purposes it normally wouldn't make much difference which salt was used.

I understand that , but for making lead hypophospite and double salt is necessary lead nitrate.
Lead acetate was made from old car battery by boiling lead dioxide with acetic acid, is not very pure but is workable ,and I have same lead sulfate with impurities
If I boil lead acetate with sodium or potassium nitrate what will result will be lead nitrate and sodium acetate but both are soluble .
From this concentrated solution lead nitrate can precipitate due to his low solubility?

roXefeller - 2-2-2015 at 19:11

It is quite an unfavorable enthalpy hole to dig yourself out of, theoretically. If you have a pile of reactants, give it a try, this is science after all. If you can play with solubilities (find a solvent that only lead nitrate is insoluble) you may be able to help yourself since some unfavorable reactions become favorable due to precipitation effects.

Hennig Brand - 2-2-2015 at 19:16

A while back I too took lead dioxide from an old car battery, but I didn't try and react the lead dioxide with acetic acid and I am not sure that it would even work. I made sure the lead dioxide was well rinsed of sulfuric acid then I put it in an old steel soup can with a loose fitting steel cover. I then put the steel can on/in a bed of hardwood coals in my wood stove and opened the draft to let more air/oxygen in and make the coals hotter. The soup can was held at bright red/orange (ca. 650-800C) for 10-15 minutes or so at which point the can was removed and cooled. The lead dioxide was nearly all converted to yellow lead monoxide. Yellow lead monoxide can be easily converted to lead acetate or nitrate with the corresponding acid.

I know you said that you don't have nitric acid, but you must be able to get or make at least low concentrated nitric acid. Even 10% nitric acid can be used, it just means removing more water to concentrate the lead nitrate solution later on. Add an excess of yellow lead monoxide to fairly warm or hot nitric acid and then filter out what does not dissolve before concentrating the lead nitrate solution. There are a few more details, but that should get you started.

[Edited on 4-2-2015 by Hennig Brand]

Hennig Brand - 5-2-2015 at 13:21

Oh, here is a neat tip with regards to lead dioxide calcination in a steel soup can. Keeping the can at bright red/orange for 10-15 minutes will cause some rust to form on the inside of the can and flake off into the lead dioxide/oxide. When I first saw this I was not pleased, since the idea of picking little bits of rust out of lead monoxide sounded tedious and possibly unhealthy even. I remembered that iron oxide formed at high temperatures like this is normally magnetite, (Fe3O4), and judging by the very dark color of the rust it did appear to be mostly magnetite. Just as the name sounds, magnetite is magnetic. Gently stirring the yellow lead monoxide and Fe3O4 mixture with the magnet end of a small magnetic pickup tool quickly collected almost all of the rust contamination. I was once again happy.

otonel - 6-2-2015 at 12:43

You have right Henning Brand, my synthesis was inspired by this article homemade lead acetate and I forgot step with lead oxide because I make this a couple of months ago.
I boil lead acetate with potassium nitrate and I have some white precipitate to dry, I don`t know right now what exactly is.

[Edited on 6-2-2015 by otonel]

Hennig Brand - 6-2-2015 at 13:07

I also read that very good article a while ago. I didn't rinse the battery for a full hour, but I more or less followed his procedure other than that.

Might as well post the pdf, just in case the link isn't around at some point.

Attachment: Homemade Yellow Lead Oxide & Lead Acetate.pdf (358kB)
This file has been downloaded 893 times

what is the fuel of USSR rocket Katyusha in WW2

smithdotyu - 9-2-2015 at 19:56

Hi everybody：
I have try KNDX、KNSU、KNSB as rocket fuel， but i found this rocket fuel enthalpy is low，I know USSR invent a good rocket named Katyusha in ww2，I think this rocket fuel may be AN（NH4NO3），Is there any document about this rocket fuel？

Bert - 9-2-2015 at 20:19

It was double base propellant. Nitrocellulose and nitroglycerin.

http://en.m.wikipedia.org/wiki/RS-82_%28rocket_family%29

http://www.airwar.ru/weapon/anur/rs82-132.html

[Edited on 10-2-2015 by Bert]

smithdotyu - 9-2-2015 at 20:43

It was double base propellant. Nitrocellulose and nitroglycerin.

http://en.m.wikipedia.org/wiki/RS-82_%28rocket_family%29

http://www.airwar.ru/weapon/anur/rs82-132.html

[Edited on 10-2-2015 by Bert]

Thank you.I used to thought that the rocket fuel is AN ,Russia use nitroglycerin is crazy！ It is hard and dangerous for me to make this fuel

kclo3 + ZnS make primer

smithdotyu - 9-2-2015 at 21:05

I want't make some primer. In our country ，we have use kclo3 + As2S3（realgar）.but this reaction product is （As2O3）Arsenic is poisonous。so I want use ZnS instead ，Is it possible？

Bert - 9-2-2015 at 22:25

Describe what you want to ignite?

How you want to trigger the ignition. Friction? Impact? Shock wave? Electrically heated wire? Shooting primer with LASER beam through a fiber optic cable? Adiabatic heating? Ionizing radiation???

How long does the primer need to be stored and still work 100%- A week? A year? 10 years?

smithdotyu - 10-2-2015 at 01:21

er，i want make stab composition instead mercury fulminate

Bert - 10-2-2015 at 07:43

The Potassium chlorate:Arsenic sulfide mix is only used for friction igniters in fireworks novelties, as far as I know. Mercury fulminate primers have a poor storage life.

Antimony sulfide is commonly used for stab and percussion primers.

Go North to Liuyang...

ecos - 10-2-2015 at 12:36

Quote: Originally posted by smithdotyu

Thank you.I used to thought that the rocket fuel is AN ,Russia use nitroglycerin is crazy！ It is hard and dangerous for me to make this fuel

think about this propellant:

Bert - 10-2-2015 at 14:00

ecos-

Somehow, a combination of NO mention of diphenylamine or other acid scavengers in that mixture, along with the storage stability given as "can be stored for many years" does not inspire confidence in the information.

Could you list title & author?

Trotsky - 10-2-2015 at 17:10

Right, but since I assume "many years" is less than a decade, that might not be so bad. Assuming suitably washed NC, at least a few years probably isn't too unlikely, it's only 25% NC. I've had some NC that I made almost exactly three years ago stored in a pill bottle that still burns leaving very little residue (probably more than when I first made it, admittedly, but it's not that different from very produced NC) and hasn't yellowed or filled with red vapor yet.

This doesn't seem to be a new document by any stretch. I wonder when it was made and what sort of stability testing they did at the time. Some of these older documents describe propellants and explosives that seem to have just been invented and compare them to things that today seem hard to imagine.

ecos - 12-2-2015 at 02:00

you can find the mixture in a patent : https://www.google.de/patents/US3753810?dq=nitrocellulose+am...

regarding the screenshot :
reference : Preparatory-Manual-of-Black-Powder-and-Pyrotechnics -- first edition
page 88

Bert - 15-2-2015 at 07:26

ecos-

The patent does suggest use of diphenylamine or similar stabilizers.

Quote:

The powder preferably contains a conventional stabilising agent, such as diphenylamine or 2- nitrodiphenylamine, in a quantity of l to 2 percent by weight based on the ammonium nitrate and nitrocellulose.

However, this is stated to be useful as a gun propellant- Specifically, use in the secondary charges (increments) of mortar rounds. I believe your interest is in rocket propellants?

If you put an Aluminum fueled propellant in a rifled gun, accuracy will be destroyed VERY quickly. Aluminum oxide is a good abrasive.

PHILOU Zrealone - 15-2-2015 at 09:15

If you put an Aluminum fueled propellant in a rifled gun, accuracy will be destroyed VERY quickly. Aluminum oxide is a good abrasive.

Except if they finally do C-diamond thin layer coating inside the canon

or alternatively
-Tungsten carbide (WxCy)
-Carborundum (SiC)

[Edited on 15-2-2015 by PHILOU Zrealone]

otonel - 15-2-2015 at 09:32

What do you think about using lead chlorate instead of potassium chlorate, lead chlorate drawback is its toxicity but lead chloride I don`t think is corrosive.
I have not found much documentation about this on the internet about them and I have a curiosity if can be used in non-corrosive percussion mixtures

PHILOU Zrealone - 15-2-2015 at 10:17

What do you think about using lead chlorate instead of potassium chlorate, lead chlorate drawback is its toxicity but lead chloride I don`t think is corrosive.
I have not found much documentation about this on the internet about them and I have a curiosity if can be used in non-corrosive percussion mixtures

It might be interesting, some heavy metal chlorite are shock-heat sensitive explosive so maybe Ag, Hg and Pb chlorate are good candidate for percussion mixes.
Beware that some of those heavy metal chlorate are moisture sensitive...this tendency increases from the unsoluble halide to the very soluble perchlorate passing through hypochlorite, chlorite and chlorate oxydation state.

otonel - 6-3-2015 at 13:00

I don`t have success to make lead chlorate, first time I obtain lead dioxide using sodium hipoclorite and sodium chlorate solution from bleach , next try was with a solution of lead acetate and potassium chlorate but the result was not i want
I need your help to obtain lead chlorate because my experiments failed

jock88 - 6-3-2015 at 15:34

Quote: Originally posted by PHILOU Zrealone

If you put an Aluminum fueled propellant in a rifled gun, accuracy will be destroyed VERY quickly. Aluminum oxide is a good abrasive.

Except if they finally do C-diamond thin layer coating inside the canon

or alternatively
-Tungsten carbide (WxCy)
-Carborundum (SiC)

[Edited on 15-2-2015 by PHILOU Zrealone]

Rhenium too I think

Molecular Manipulations - 6-3-2015 at 18:07

otonel, all transition metal chlorate and perchlorates are very soluble. I don't think there's a very easy was to make it, try chloric acid with lead oxide, hydroxide or carbonate.

PHILOU Zrealone - 7-3-2015 at 05:38