LL8 from Dr. Liptakov

To diversify the thread, I attach the crystallization process of Cu(ClO4)2 x 6H2O. Procedure: 20g HClO4 68% + 60g dH2O + 20g CuCO3. The solution is boiled at about 100 Celsius for about an hour. An acidic solution is formed, filtered from exces CuCO3. After filtering slowly evaporation at 60 Celsius. After concentration, the crystals are filtered. Proceeds will be announced later.

This is a way of making Cu(ClO4)2.
This procedure yields a theoretical 11.6g CuII(ClO4)2 starting from 10g NH4ClO4. Not sure how pure your copper perchlorate needs to be, but this is pretty pure and easy. I hope it helps.

CuSO4*5H2O + 2NH4(ClO4) + XH2O=> (NH4)2SO4 + Cu(ClO4)2*xH2O

10.62 g CuSO4*5H2O
10.00 g NH4CLO4
50.00 ml dH2O
>100 ml Acetone

Heat dH2O up to boiling
Dissolve all CuSO4
Dissolve in all NH4ClO4
remove heat once all dissolved
Add at least =/> 100 ml Acetone and stir well. if you are above acetone bp, solution will boil when acetone is added and large clumps of sulfate will be produced instantly.
(NH4)2SO4 precipitates as a white sandy insoluble, it has a layer of copper II ions making it light blue on surface.
Filter off (NH4)2SO4 with copper contamination
Rinse with acetone
light blue filtrate collected contains CuII perchlorate, and should contain no solids at all.
Boil down this acetone/perchlorate solution to evaporate or just leave alone and allow evaporation.
When a white solid begins to appear around meniscus during boiling, remove from boiling and allow to cool.
Blue Cu II Perchlorate crystals will form on cooling.

This procedure can be doubled to 20 g NH4ClO4 & 21.24 g CuSO4*5H2O with only 50 ml of H2O (100ml H2O doubling is not necessary, less water helps to precipitate out the sulfate on addition of acetone).






[Edited on 12-12-2022 by Hey Buddy]

Very easy and interesting , thank Buddy....

Here are the first results.
Unfortunately, Cu(ClO4) 2 prepared from CuSO4 (and after adding 20% hexamine = called Cu8) shows poor detonation properties. Cu(ClO4)2 x6H2O should have a melting point of 82 C. This one clearly does not. It does not melt, but strangely enough it burns by itself, without the content of fuel, i.e. hexamine. The perchlorate prepared in this way contains many impurities, most likely from acetone. Therefore, it is flammable in itself. The preparation process will require optimization including recrystallization. However, this is a method that could lead to a simple preparation of neutral Cu(ClO4)2 in the future. Which has not yet been described anywhere. Which is a great benefit. Because HClO4 + CuCO3 produces an acidic version of crystals that cannot be neutralized with NaOH, KOH, LiOH, NH4OH. Due to impurities, this method of preparing copper perchlorate and hexamine (Cu8) achieves poor results. Which is evident from the pictures. This Cu8 substance has DDT properties. Which is good news. But it can't fire ETN. Only causes partial detonation. Small remnants of unexploded ETN were observed in the crater. The figure contains reference values for 0.3 g ETN full detonation and for 0.3 g Lithex full detonation. In the sense of a highly pressed output segment. Full power Cu8 is in this thread above. And should by basically same as Lithex. (page 2, shooting into alu brick)



[Edited on 12-12-2022 by Laboratory of Liptakov]

Quote: Originally posted by Laboratory of Liptakov

Here are the first results. Unfortunately, Cu(ClO4) 2 prepared from CuSO4 (and after adding 20% hexamine = called Cu8) shows poor detonation properties. Cu(ClO4)2 x6H2O should have a melting point of 82 C. This one clearly does not. It does not melt, but strangely enough it burns by itself, without the content of fuel, i.e. hexamine. The perchlorate prepared in this way contains many impurities, most likely from acetone. Therefore, it is flammable in itself. [Edited on 12-12-2022 by Laboratory of Liptakov]

During further tests, Lithex is shown to detonate consistently and reliably. The dosage was only 900 mg. Therefore, the crater is not as deep as from 1g ETN. Also, the density of Lithex was slightly lower, only 1.7 g/cc. A 3% addition of aluminum Alu - bright was used. However, the diameter of the crater is the same. This means that Lithex can fully replace ETN in many applications. His DDT is reliable and his brizance is very similar.

If is Ca(ClO4)2 easy available, is it maybe best way for preparation Cu(ClO4)2. Good idea, thanks.


Interesting fact: Lithium perchlorate with hexamine (Lithex) has a special property after drying at 175 Celsius. Its structure and behavior is very similar to talc. A very fine powder is always formed which is partly slippery. Like crushed the talc.

[Edited on 27-1-2023 by Laboratory of Liptakov]

Quote: Originally posted by Laboratory of Liptakov

As already indicated, at least 2 crystalline barriers must be overcome when drying LiP. At 80 and 120 C. The melting point of completely dry LiP is 236 C. Boiling point - decomposition 400 C. For this reason, there is no need to worry about decomposition during drying to the anhydride. Caution, do not use Teflon for drying. LiP immediately reacts with Teflon at 80 ° C and begins to blacken. Even the stainless steel surface is not perfect. When LiP is melted, there is a slight browning of pure factory LiP. The same effect is observed when the Li8 mixture is dried. After drying, the mixture is slightly gray. However, its energy properties will not affect it for the worse. [Edited on 24-1-2022 by Laboratory of Liptakov]

Quote: Originally posted by underground

Are not all perchlorate salts need a metal cavity to go DDT, just like ETN ? Are any of these capable to DDT into a plastic straw like other primaries, for example HMTD ?

The easiest of the way of acids is ETN and SA-DS in plast confinement. The easiest of perchlorate way, is the Lithex and metal confinement...

Quote: Originally posted by Microtek

I question the statement that ETN is not sensitive.

Due to next research was developed an interest substance. ( working title Brightelite) Which is not full power material for use as initiation for secondary material. But his properties are interest. S a base of mixture is formula: AP 80 + CuO 4 hexamine 8 in part by weight. (No. 4). This substance is of course weak, with very positive oxygen ballance, but any way, brisantion is there. Lab. preparation is 20g dH2O on stainless surface, + 4g AP + 0.2g CuO + 0.4g hexamine. Boiling solution, evaporate and gringing on very fine powder. Operation without accident at 80 C on surface friction. Second step is adding nitrocellulose commerce grade 12.4 N 0.35g + Aluminium bright powder 0.35g. + 2g Acetone for dilluting of NC. This mixture has OB + 2.0 on CO2. Mixing on porridge at 20C, evaporate and grain 1x1 mm. And is more power. (No. 1 +2) . There is enough power for full initiation of ETN now. (No.3). For last test (No.5) was used nitrocellulose with over 13% N. Resluts show clear bigger brisantion. Mixture (grain) is pH neutral, no-hygroscopic with good manipulation properties. For all test was used output segment 300 mg, ETN density 1.65. Brightelite density 1.5 g /cm3. As itself is weak, but can provide easy way for (maybe even reliable) of initiation ETN in solid metal cavity. Friction and impact test show on almost same properties as CHP. Also his burning speed is similar with similar color of flame.

Well, THAT is quite snappy for a mixture of common pyrotechnic materials. Have you tried zapping it with a piezoelectric spark yet?

Could you describe containment, ignition used? What does it do if ignited in the open...

I would expect substitution of a commercial high nitroglycerin smokeless propellant such as "Bullseye" for the higher nitration nitrocellulose of test 5 might yield similar or even greater brissance.
L



[Edited on 2-12-2023 by Bert]

Quote: Originally posted by Herr Haber

Reading your recent research I'm so glad I didn try those pyrotechnic compositions I was thinking about a few years ago... I was going for ammonium perchlorate, hexamine and CuOCl the first two being quite "neutral" in terms of color production.

So Bert's assumption was correct. Composition: 80 AP + Hex 8 + CuO 4 + Al 7 + Shotgun powder 8 parts..(No. 6) ..show basically same brizantion as composition with homemade nitrocellulose 7 parts of weight. (No.5) Diameter is only slightly less. Precision repeatedly measurement are No.5 2.7 + 12.5 mm. And for shotgun powder 2.7 x 12.2 mm. Exact results of course require minimal 3+3 tests for both formula, but for orientation results is it enough. Both formulas has sufficient brizantion for initiation ETN. next:
¨
Test on confinement in alu foil 5 layer , candle heated causes only puffy and rocket effect.
Test on electric spark was without ignition of Brightelite. (directly pour 0.1g into the lighter hole, 10x sparks)
Burning Brightelite with shotgun powder has slightly slower burning on free heap. Than with homemade NC.



Now I remembered: the homemade nitrocellulose used was prepared by double nitration. Commercial fibrous NC was re-nitrated. The PLM method was used for its cleaning and stabilization....
https://www.youtube.com/watch?v=oVZkPWxj5WE
Thus 4 years old, but good stabilized NC with nitrogen content maybe over 13.5 %.

[Edited on 13-2-2023 by Laboratory of Liptakov]

During the experiments, it became clear that CuO can be replaced by CuCl2. In water heating process, this creates Cu(ClO4)2 + NH4Cl. Given presence of hexamine in solution, perhaps something else as well. Which, according to the result, contributes to brizantion. Other values are the same as in the experiments described above. So density of output segment is 1.5g/cc per 300mg. The crater depth of 3.1 mm is largest of all investigated variants. Which is interesting result.

Brightelite

Since Brightelite is non-wetting and essentially just an ordinary pyrotechnic compound, it was re-examined. This time to transfer detonation from basic detonator to booster. Test was successful. Output segment of basic detonator (300mg cavity 6) had same density as booster, i.e. 1.5g/cm3 (1g cavity 8). VoD at booster output is estimated at 3 - 3.5 km/s. Which is quite a bit for a booster. But, for example, for secondary mixtures based on TACN, this brisance and power of initiation is sufficient. From which it follows that some more sensitive secondary EMs can be initiated only with this common pyrotechnic composition. Brightelite thus provides advantage that its brisance may be sufficient for some secondary materials itself.

Quote: Originally posted by yobbo II

What perchlorate do you get when you add copper sulphate to barium perchlorate (in solution) and get a ppt of insoluble barium sulphate with copper perchlorate in solution. Is it I or II, CuCl04 or Cu(ClO4)2 Barium Perchlorate is Ba(ClO4)2 Yob

Verification experiments were carried out on stability of newly developed substances. Brightelite appears to be stable after one month of manufacture and cavity filling. And it can initiate ETNs. Lithex is also stable after 2 months from production and filling. Lithex requires a hermetic seal against moisture after filling. For example, insulation from polyisobutylene rubber (PIB), as in this case.

Quote: Originally posted by Laboratory of Liptakov

Since Brightelite is non-wetting and essentially just an ordinary pyrotechnic compound, it was re-examined. This time to transfer detonation from basic detonator to booster. Test was successful. Output segment of basic detonator (300mg cavity 6) had same density as booster, i.e. 1.5g/cm3 (1g cavity 8). VoD at booster output is estimated at 3 - 3.5 km/s. Which is quite a bit for a booster. But, for example, for secondary mixtures based on TACN, this brisance and power of initiation is sufficient. From which it follows that some more sensitive secondary EMs can be initiated only with this common pyrotechnic composition. Brightelite thus provides advantage that its brisance may be sufficient for some secondary materials itself.