marc121
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Ratio HNO3 H2SO4 for PETN
Hello, I am new and I would need information about the synthesis of the PETN, in particular on the ratio HNO3 (90%) and H2SO4 (98%) and PE, taking as
example 10 gram of PE.
I'm afraid I'm wrong.
thank you
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NeonPulse
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You really need to search this forum. I highly doubt you will be spoon fed such easy to find information. It's all here. Just put PETN synthesis into
the search engine and you will find the solution.
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marc121
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In reality I searched and explored all the subjects but I did not find anything about the conc HN03 90%, that is why I allowed myself to post this
request
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Praxichys
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Use a 10-20% molar excess of HNO3 to ensure complete conversion. The amount of sulfuric acid doesn't really matter all that much. It's only acting as
the solvent and to help remove water. Start with 1.5:1 molar ratio with the nitric and if it gets too thick, add some more.
[Edited on 11-5-2017 by Praxichys]
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marc121
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Thanks for the advice, so it's better too HN03 than not enough.
I will do a test
thanks
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Praxichys
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Rereading that I suppose I should clarify the figure to 1.5:1 sulfuric:nitric; add more sulfuric if necessary. Adding excess of either acid will work,
but sulfuric is typically cheaper.
[Edited on 11-5-2017 by Praxichys]
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marc121
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I think I got this, is that it seems correct to you.
HN03 90% 60 Gram
H2SO4 98% 65 grams
PE 99% 10 Gram
HNO3
ACS reagent
Vapor density 1.3 (vs air)
Vapor pressure 6.6 mmHg (20 ° C)
8 mmHg (20 ° C)
Assay ≥90.0%
Dilution test passes test
ign. Residue ≤0.002%
Color colorless to yellow
Bp 120.5 ° C (lit.)
Density 1.48 g / mL at 20 ° C (lit.)
H2S04
0.0001 hPa (20 ° C)
Density 1.84 g / cm 3 (20 ° C)
Mp -20 ° C
PH 0.3 (49 g / l, H₂O, 25 ° C)
Shipped in ambient
Storage temp. Storage temperature: no restrictions.
Specifications Assay (alkalimetric): ≥ 97.5%
thanks
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NeonPulse
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This was the 3rd result in my search
Quote:
Verified efficient method of preparing PETN from diluted HNO3
use
32,7 ml of 70% HNO3 (75% excess)
18,9 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------
or
34,0 ml of 65% HNO3 (66% excess)
24,8 ml of 96% H2SO4
10,0 g of Pentaerythrite
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or
34,8 ml of 58% HNO3 (48% excess)
36,3 ml of 96% H2SO4
10,0 g of Pentaerythrite
------------------------
Nitration:
1. Cool nitration mixture during mixing of acids, thus minimalize even minimal decomposition of HNO3. Nitration mixture must be cooled before
nitration process to temperature of 10°C.
2. While stiring, add pentaerythritee in small portions (1-2g) to nitration mixture, always after previous batch is dissolved. Nitration mixture
gradually thicken as PETN forming in solution.
3. Constantly monitor reaction temperature and maintain it in 10-15°C range. Interval of adding pentaerytritol conform to reaction temperature, must
not rise over 15°C, leave beaker in cold water.
4. Stir with mixture for next 5 minutes after all pentaerythrite is added and dissolved. Mixture is now thick, but stirring is going well. During
nitration process must not be developed any brown fumes of NOx!
5. Now put beaker with mixture into water bath and maintain temperature at 50°C, continuously stir with mixture. During 20 minutes at this
temperature, all of possible sulfoesters come into PETN for maximal yield of nitration.
6. While maintaining mixture at higher temperature, mixture must be monitored for developing of NOx fumes. Only light brown colour can be in shrouded
beaker. Raised development of NOx pointing to higher temperatures used (even during previous nitration) or insufficient chmemicals purity and further
heating may end up in uncontrolled reaction and oxidation of formed PETN. In this case it is better to do not heat at all and end just after nitration
(if brown fumes apperas during nitration), the yield will be lower. In case of accidentally runaway reaction during heating, immedialtely pour mixture
into cold water, don't try stop reaction by cooling beaker, it will not help.
7. When heating after 20 minutes pass off, pour reaction mixture into cold water and follow standart procedure of filtration, neutralization and
purifying of PETN.
Yield was 22,1g of PETN from 10g of pentaerythrite, ~95% of theoretical yield (with 65% HNO3 used).
This procedure is result of my research of most effective method preparing PETN from diluted HNO3. Acid ratios are precisely calculated on data from
PETN nitration graph published by T. Urbanski in his book vol. IV. Generaly said, PETN is forming to maximum 30% of water portion in nitration
mixture. But, when also H2SO4 is contained in nitration mixture, minimum ammount of water must be keep, or oxidation with small yields occur. With
this acid ratios 20% of H2O is minimum. So, this nitration mixture has 20% of water on nitration start and 30% at the end, area for most effective
nitration, but again only with this ratios. For other acid ratios must be all recalculated. Excess of HNO3 is used to controll ammount of reaction
water. Only ammount of nitration mixture can be extended for lower mixture thickness, but it lower utilization of acids and overall efficiency. But it
isn't necessary.
I hope there is no major mistakes in my translation to english ;-)
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CalAm
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Quote: Originally posted by marc121  | I think I got this, is that it seems correct to you.
HN03 90% 60 Gram
H2SO4 98% 65 grams
PE 99% 10 Gram
HNO3
ACS reagent
Vapor density 1.3 (vs air)
Vapor pressure 6.6 mmHg (20 ° C)
8 mmHg (20 ° C)
Assay ≥90.0%
Dilution test passes test
ign. Residue ≤0.002%
Color colorless to yellow
Bp 120.5 ° C (lit.)
Density 1.48 g / mL at 20 ° C (lit.)
H2S04
0.0001 hPa (20 ° C)
Density 1.84 g / cm 3 (20 ° C)
Mp -20 ° C
PH 0.3 (49 g / l, H₂O, 25 ° C)
Shipped in ambient
Storage temp. Storage temperature: no restrictions.
Specifications Assay (alkalimetric): ≥ 97.5%
thanks |
Are you ordring your acid's from trade india ?
https://www.tradeindia.com/fp3432199/Nitric-Acid-98-.html
Because with the current lot of events playing out in the new's lately it wouldn't seem very smart to be ordering the acid's or PE from online sources
in case of interception at mail depots.
Especially when PETN has been used in past events for nefarious deeds. Also wouldn't you dilute your 98% HNO3 to the 70% conc and just use H2SO4
instead of dicking around with WFNA unless you are doing this industrially there is no real advantage.
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