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UndermineBriarEverglade
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Synthesis 9
With my improved cooling setup, I also tried KFeNAT's sulfonation method. Rather than adding KNO3 to POE in an excess of sulfuric acid, I
combined POE with sulfuric acid and then dripped that into the nitration mix. The yield was about the same as my last run, with greater acid
consumption, a slower and more complicated procedure, and additional losses from what was left behind in the beaker of POE/acid. I can see how
sulfonation would be better for larger-scale reactions though, since temperature was very easy to manage.
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Target: 1 part = 0.0157 mol DNPOEN = 4.289 grams
1 part phenoxyethanol
5 parts potassium nitrate
10 parts sulfuric acid for nitration mix
2.7 parts (2.5mL / 4.5g 93.2%) sulfuric acid for the sulfonation
6.7 parts sulfuric acid added to keep it stirrable
Yield: .81 parts DNPOEN (3.51g)
Procedure:
In ice bath (no salt), KNO3 was added to sulfuric acid, with temp kept below 30°C or so.
In a separate beaker in the ice bath, POE was added dropwise to 4.5g H2SO4 with light stirring. Temperature was kept below
10°C. The mixture developed a very slight pink sheen and thickened.
Under heavy overhead stirring, the POE-acid mix was pipetted into the mixed acids. This was only slightly exothermic, taking 19 minutes with
temperature kept below 10°C. The mixture formed a white cream that was thinned with about 6mL of sulfuric acid.
The water-ice bath was replaced with 30°C water and held for 20 minutes. A speck of mixture stuck to the side of the beaker turned purple. The
main reaction mix went from bright white to off-white.
The mixture was rinsed into ~900mL water and filtered to yield a bright white filter cake and a very slightly yellow filtrate.
The filter cake was dissolved in 12mL of acetone, separating into two layers. As before, the top layer was clear and the bottom was an oily
yellow. The top layer, which smelled of acetone, was pipetted into water to yield a small crop of fine crystals. When additional acetone was added to
the remaining yellow solution, it did not form a separate layer.
The yellow bottom layer was poured into water, filtered, and added to warm ethanol. The partial solution was heated in a beaker until the
undissolved DNPOEN had just barely melted. Acetone and heat were applied until all the DNPOEN had dissolved. Then, the beaker cooled to 10C, a seed
crystal was added, and mild stirring was applied to precipitate a mat of fine white crystals. An excess of cool water was added to complete
precipitation.
3.51 grams of small white needle-like crystals were obtained by vacuum filtration.
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KFeNAT
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Quote: Originally posted by UndermineBriarEverglade  | | Nice work! I think it's time for a wiki page. I am curious about the performance of DNPOEN once melt-cast to a higher density, and of oxygen-balanced
mixes. Have you done any sensitivity testing? I will do a few more small syntheses before testing and scaling up. |
It is significantly less sensitive than TNP and Tetryl, even in its molten state.
It can explode when struck forcefully on a rail with a hammer, making it more sensitive than nitroguanidine.
It detonates relatively easily at lower pack densities; in my Hess test, I successfully made it work using a detonator packed with 0.8g of ETN.
Since the critical diameter of its cast products is likely similar to that of TNT (>30mm), I currently do not have enough samples to manufacture
pure DNPOEN ingots to verify whether its detonation performance matches the description in the book.
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UndermineBriarEverglade
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DNPOEN seems insensitive even while melted. I can detonate ETN by dropping a 2lb hammer about 5 inches onto a sample on a 1/4" steel plate. In the
same conditions, I have been unable to detonate nitroguanidine or DNPOEN even with a very hard hammer blow. I heated the plate to melt the DNPOEN and
still could not get it to detonate. I have decided that it is insensitive enough to handle with while molten. Unfortunately, I haven't been able to
get quantitative data. I tried to muffle my drop hammer apparatus, but positive tests are still too loud to attempt more than a handful of runs.
I melted 1g of DNPOEN and added low-density nitroguanidine needles. The NQ did not react or appreciably dissolve. The DNPOEN filled the spaces between
the needles to form a solid mass upon cooling, but I was only able to add about 0.2g of NQ. Good mixes will need high bulk density NQ.
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