Sciencemadness Discussion Board

LL8 from Dr. Liptakov

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MineMan - 24-2-2022 at 01:55

Quote: Originally posted by Laboratory of Liptakov  
It looks like there has been another breakthrough in the Lithex brisance. The unsuccessful reaction of TACP production from LiClO4 gave a change in color and consistency after 3 days. The dark blue turned to a light blue suspension. The light blue color is most likely copper hydroxide. Hydroxy-contaminated LiClO4 was dried. At 180 C. The hydroxide decomposed to CuO. (estimate) A sample of thus contaminated LiClO4 was mixed with hexamine in the usual ratio of 80:20. The maximum pressure was used when filling the cavity. A density of 1.818 g / cm3 was achieved. For an output segment weighing 400mg. The brisance at this density is the same as that of highly pressed ETN 400 mg.
Thus, the depth of the crater is 7.5 mm with a crater diameter of 19 mm. Because the tests are shot in lead, an error of at least 10% must be taken into account.
Anyway, MineMan had truth. If the Lithex can be compressed to high density, its brisance will be identical to ETN. Which has just been confirmed. The mixture thus prepared has, of course, excellent flame sensitivity. Therefore, it is not necessary to use a different chemical substance for ignition in the cavity. Lithex with CuO (xy%) works as a monopropelant with incredible brisance.



I am confused? Is this hydroxl lithium perchlorate or is this Lithex with a small amount of CuO?

Hexamine is a low density fuel at 1.37g/cc. I advise higher density and easy to obtain fuels for Lithex to achieve the holy 2.0g/cc. The fuels I have in mind are Melamine at 1.57g/cc and Azodicarbonamide, a widely avilable blowing agent with a density of 1.9g/cc. With the later I predict Lithex @ 2.1g/cc easily pressed with brisance between that of RDX and HMX.

MineMan - 24-2-2022 at 01:58

Quote: Originally posted by Laboratory of Liptakov  
It looks like there has been another breakthrough in the Lithex brisance. The unsuccessful reaction of TACP production from LiClO4 gave a change in color and consistency after 3 days. The dark blue turned to a light blue suspension. The light blue color is most likely copper hydroxide. Hydroxy-contaminated LiClO4 was dried. At 180 C. The hydroxide decomposed to CuO. (estimate) A sample of thus contaminated LiClO4 was mixed with hexamine in the usual ratio of 80:20. The maximum pressure was used when filling the cavity. A density of 1.818 g / cm3 was achieved. For an output segment weighing 400mg. The brisance at this density is the same as that of highly pressed ETN 400 mg.
Thus, the depth of the crater is 7.5 mm with a crater diameter of 19 mm. Because the tests are shot in lead, an error of at least 10% must be taken into account.
Anyway, MineMan had truth. If the Lithex can be compressed to high density, its brisance will be identical to ETN. Which has just been confirmed. The mixture thus prepared has, of course, excellent flame sensitivity. Therefore, it is not necessary to use a different chemical substance for ignition in the cavity. Lithex with CuO (xy%) works as a monopropelant with incredible brisance.



This makes sense. CuO is an incredible catalyst for perchlorates. It can allow certain flashpowders to DDT. Another little known catalyst is well, I will say it in private message

Laboratory of Liptakov - 24-2-2022 at 02:57

I estimate, that is it CuO. But his structure can be different against CuO pure powder, which is simply mixed into white Lithex. During reaction on TACP and follow within degradation after 3 days, maybe arised better form of CuO. Is it similar as for preparation for example NHN. Temperaure and entire procedure is important for better or best properties of NHN. Maybe for example 1% of some NH3/4 is bonded in molecule Lithex. I use method of observation. What it is or not, is not so important. Important is brisance. If is possible preparation make repeatedly with same results. St. Nicholas may be inside the Lithex molecule if it works. If St. Nicholas create better or biggest hole, let's leave him there...:cool:



ManyInterests - 27-2-2022 at 12:01

Quote:
Lithium perchlorate can be manufactured by reaction of sodium perchlorate (relatively easy prepare) with lithium chloride which can be cheap and available.


Is that like turning Calcium Ammonium Nitrate into Potassium nitrate by adding the CAN in solution with Potassium chloride and letting the potassium nitrate precipitate? if that is the case, can you give me the ratios please? Or a quick breakdown of the process.


AngelEyes - 28-2-2022 at 09:10

Quote: Originally posted by ManyInterests  
Quote:
Lithium perchlorate can be manufactured by reaction of sodium perchlorate (relatively easy prepare) with lithium chloride which can be cheap and available.


Is that like turning Calcium Ammonium Nitrate into Potassium nitrate by adding the CAN in solution with Potassium chloride and letting the potassium nitrate precipitate? if that is the case, can you give me the ratios please? Or a quick breakdown of the process.



Yes, but I don't think I'd want to do it that way.

Sodium Perchlorate is very soluble, which is good. And Lithium Chloride is pretty soluble too (83.5g / 100ml water @ 20C, according to wikipedia) but the resulting products are also pretty soluble themselves (Lithium Perchlorate 56g / 100ml @ 20C and Sodium Chloride 35g / 100ml @ 20C). You'd have to remove the NaCl and then boil the Lithium Perchlorate solution, cool it, filter it, boil some more etc.

Sounds like a PITA to me.

ManyInterests - 28-2-2022 at 10:21

Quote: Originally posted by AngelEyes  
Quote: Originally posted by ManyInterests  
Quote:
Lithium perchlorate can be manufactured by reaction of sodium perchlorate (relatively easy prepare) with lithium chloride which can be cheap and available.


Is that like turning Calcium Ammonium Nitrate into Potassium nitrate by adding the CAN in solution with Potassium chloride and letting the potassium nitrate precipitate? if that is the case, can you give me the ratios please? Or a quick breakdown of the process.



Yes, but I don't think I'd want to do it that way.

Sodium Perchlorate is very soluble, which is good. And Lithium Chloride is pretty soluble too (83.5g / 100ml water @ 20C, according to wikipedia) but the resulting products are also pretty soluble themselves (Lithium Perchlorate 56g / 100ml @ 20C and Sodium Chloride 35g / 100ml @ 20C). You'd have to remove the NaCl and then boil the Lithium Perchlorate solution, cool it, filter it, boil some more etc.

Sounds like a PITA to me.


I'm very open to suggestions. Especially since I don't want my lithium perchlorate to be contaminated by sodium chloride. What would be a more efficient process? Or how would I remove the NaCl from the solution?

I guess that method is good when using it to make potassium nitrate, since the resulting product is quite pure and I've used it to make both the 65-70% azeotrope and the 99.5% fuming nitric acid (I got a specific gravity of 1.51 on my first attempt! It was still a bit red due to nitrogen dixode contamination, but those can clear up on their own after a while.

underground - 28-2-2022 at 15:04

Quote: Originally posted by ManyInterests  

I'm very open to suggestions. Especially since I don't want my lithium perchlorate to be contaminated by sodium chloride. What would be a more efficient process? Or how would I remove the NaCl from the solution?


Direct electrolysis of lithium chloride to perchlorate. Lithium chlorate 1st with a MMO anode and then to perchlorate with a Pt/LD anode. Liclo4 is much less soluble than Liclo3, so Liclo4 will ppt out of the solution.

[Edited on 28-2-2022 by underground]

B(a)P - 28-2-2022 at 16:27

Quote: Originally posted by underground  
[

Direct electrolysis of lithium chloride to perchlorate. Lithium chlorate 1st with a MMO anode and then to perchlorate with a Pt/LD anode. Liclo4 is much less soluble than Liclo3, so Liclo4 will ppt out of the solution.

[Edited on 28-2-2022 by underground]


Any reason you wouldn't go from LiCl to LiClO3 with Pt?

ManyInterests - 28-2-2022 at 16:36

Quote:
Direct electrolysis of lithium chloride to perchlorate. Lithium chlorate 1st with a MMO anode and then to perchlorate with a Pt/LD anode. Liclo4 is much less soluble than Liclo3, so Liclo4 will ppt out of the solution.


I got an MMO anode and a titanium cathode. So all I need to make a perchlorate is to get a platinum anode? How I do electrolysis is using a DROK voltage regulator and a 12V laptop power supply. Last time I did electrolysis I managed to get a voltage of 6 and 4.5 or so amps. My yields were... not good, but I did get get yields nevertheless. It also my first really pure yield of potassium chlorate at the time and I considered it good enough and I haven't dealt with chlorates since.

I found an online source for lithium chloride, but they only sell for 100 grams a package. I hope that'll be enough for a good long time!

Laboratory of Liptakov - 1-3-2022 at 01:14

Platinum requires relatively precise reaction conditions. Temperature, Ph, voltage, current. Otherwise, it will be destroyed within a few hours. I recommend the method of thermal decomposition NaClO3 = heat 600C = NaCl + NaClO4.
It's tried, easy and it works.
https://www.youtube.com/watch?v=1Ylt2ZKJlME&t=17s
Also you can try LiCl = electro cell = LiClO3 ....heat.... LiClO4 + LiCl....Unfortunately not tested.

S.C. Wack - 1-3-2022 at 16:51

...or 500C/20 min. Removing chlorate from the product is easy with K but will be difficult with Na.

BTW a hexamine reference I didn't note before:
https://www.sciencemadness.org/whisper/viewthread.php?tid=25...

Quote: Originally posted by AngelEyes  
You'd have to remove the NaCl and then boil the Lithium Perchlorate solution, cool it, filter it, boil some more etc.


I wonder how far from precisely that this was what was going on during the recent incident at BYU (google image: byu dorm room)...or did it involve sugar, or what exactly...If one was to convert the Na to the Li salt directly, it would be done hot, and the Li would simply be collected on cooling. Perhaps the recovery of the remainder of the Li (in any form) from the solution at that point would be an issue.

Laboratory of Liptakov - 2-3-2022 at 00:38

It will be easier to prepare perchloric acid and react it with lithium hydroxide. (Li + H2O = LIOH) Until neutral reaction to pH. It's simple, fast and tried. Pure LiClO4 and water are formed. There are no problems with the reaction. There is also no problem with the production of HClO4 when using the Adams method. https://www.youtube.com/watch?v=KXpGlgj9_uw&t=70s

It is still easier than counting and testing different solubilities and crystallization conditions and then being frustrated by the tragic yield.

Microtek - 2-3-2022 at 00:59

I hate to sound like a broken record, but if you are worried that your NaClO4 is contaminated with chlorate, one solution is to convert it to HClO4 by reacting with strong HCl (>35%). NaCl is practically insoluble in this and precipitates out. After filtering the NaCl off, you distill the filtrate to collect the excess hydrochloric acid. By raising the pot temperature to ca. 120-150 C, you ensure that any HClO3 present is thoroughly destroyed, and all HCl is driven off, while losing almost no HClO4. The product I made this way was found to be 50% w/w, gave no precipitate when added to dilute AgNO3 (so no chloride present), and did not react with sugar (I didn't have a more sophisticated test for chlorate than this, but I struggle to imagine ClO3- surviving in a strongly acid, hot environment for prolonged periods).

The only real issues here are access to strong HCl (if the concentration is too low, the solubility of NaCl increases) and whether you can filter such a corrosive mix. I use a glass frit Büchner funnel which are cheap and widely available.

Laboratory of Liptakov - 2-3-2022 at 02:43

The repetition this method is sure not unnecessary, it is important. It sounds a like simpl method. Simpler than Adams. Because NaClO4 is easer available and HCl also. Against NH4ClO4 and HNO3 for Adams method. You have some ratios for HCl 35% + NaClO4 (anhydride?) I estimate, that this method require outdoor conditions during a boiling HCl mixture at 150 C.

hcl.jpg - 117kB

Microtek - 2-3-2022 at 08:20

I have attached the paper were I read about this method. In summary, 25-30 ml HCl to 20 grams of NaClO4 (and then several 1 ml portions to wash the filter cake). Yield is more than 95%. My own results matched those in the paper. And yes, you definitely need ventilation when evaporating the excess HCl. I collected it by distillation because I didn't want to expose my fume hood pump to large quantities of HCl (and also it can be used for less demanding applications, such as cleaning glassware, etc.)



Attachment: Mathers_JACS_1910.pdf (377kB)
This file has been downloaded 89 times

[Edited on 2-3-2022 by Microtek]

Laboratory of Liptakov - 2-3-2022 at 13:33

Mathers method seems to be the easiest way to prepare HClO4. HClO4 is, of course, the basic and starting precursor for the research of perchlorates energetics mixtures. HClO4 is actually responsible for the discovery of a mixture of CuClO4 + hexamine=Cu8. And subsequently for the discovery of LiClO4 + hexamine = Li8 = Lithex. It is almost certain that whoever has HClO4 can easily come up with another discovery of primary-secondary material.

Microtek - 2-3-2022 at 13:40

Yes, there is a huge number of perchlorate salts and complexes with nitrogen rich counterions and/or ligands waiting to be discovered. Many of them will undoubtedly be very powerful, and maybe there will be some that combine high performance and low sensitivity.

S.C. Wack - 2-3-2022 at 14:50

Quote: Originally posted by Laboratory of Liptakov  
It will be easier to prepare perchloric acid and react it with lithium hydroxide.


If one is going to use LiOH, they might as well make AP from crude perchlorate and add the hydroxide to a solution of AP and remove the ammonia by distillation. It would be interesting to substitute with carbonate.

If one is going to use perchloric acid and distillation of HCl, they might as well add LiCl to the acid and get even more HCl, which is presumably recycled to make more perchloric acid.

Microtek - 4-3-2022 at 00:42


Quote:

If one is going to use LiOH, they might as well make AP from crude perchlorate and add the hydroxide to a solution of AP and remove the ammonia by distillation.


But then you might not get rid of any chlorate that was in the crude perchlorate. IMO, the increased peace of mind is easily worth the effort.

S.C. Wack - 4-3-2022 at 14:51

The solubility of sodium (per)chlorate is much higher than AP. The 23rd ed. CRC Handbook (1939) sitting here says AP's solubility at 0C is 10.74 g/100 ml water. The only common (per)chlorates less soluble are the K salts and silver chlorate. Perhaps barium chlorate by mole fraction. Ammonium chlorate is "very soluble".

Quote: Originally posted by Microtek  
I hate to sound like a broken record, but if you are worried that your NaClO4 is contaminated with chlorate, one solution is to convert it to HClO4 by reacting with strong HCl (>35%). NaCl is practically insoluble in this and precipitates out. After filtering the NaCl off, you distill the filtrate to collect the excess hydrochloric acid. By raising the pot temperature to ca. 120-150 C, you ensure that any HClO3 present is thoroughly destroyed


I didn't bring up heating HCl with the thermal product for the same reason (plus others) I wouldn't recommend chemical oxidation (in sulfuric acid) of Na chlorate (but this concern is more avoidable for the K salt, where the process works better in every way, even though technically it should be chloric acid all the same) to perchlorate: chlorine dioxide and its tendency to explode at concentrations higher than 10%. (2KClO3 + 4HCl = 2KCl + Cl2 + 2ClO2 + 2H2O)

ManyInterests - 8-4-2022 at 21:37

Quote: Originally posted by underground  
Quote: Originally posted by ManyInterests  

I'm very open to suggestions. Especially since I don't want my lithium perchlorate to be contaminated by sodium chloride. What would be a more efficient process? Or how would I remove the NaCl from the solution?


Direct electrolysis of lithium chloride to perchlorate. Lithium chlorate 1st with a MMO anode and then to perchlorate with a Pt/LD anode. Liclo4 is much less soluble than Liclo3, so Liclo4 will ppt out of the solution.

[Edited on 28-2-2022 by underground]



Quote: Originally posted by B(a)P  
Quote: Originally posted by underground  
[

Direct electrolysis of lithium chloride to perchlorate. Lithium chlorate 1st with a MMO anode and then to perchlorate with a Pt/LD anode. Liclo4 is much less soluble than Liclo3, so Liclo4 will ppt out of the solution.

[Edited on 28-2-2022 by underground]


Any reason you wouldn't go from LiCl to LiClO3 with Pt?


http://www.chlorates.exrockets.com/litpat.html

I've seen this patent that did describe the lithium chloride to perchlorate directly. They did mention Pt anodes for use, but they claimed that even a graphite anode (which I won't use) would work. I wonder if an MMO anode would work to convert the chloride directly to perchlorate. I have 100 grams of chloride and given how soluble it is in water, I need to be careful when I try to make it, least I lose everything in one go. I can actually run that experiment within the next two weeks if an MMO anode will do and not need to shell out a lot of cash for an additional platinum anode (which is a different size to my cathode).

LL8 will be an interesting challenge to make. I actually forgot that lithex isn't LL8. :D But I will be following Liptakov's experiments with lithex very well. If he finds another new energetic that can be used as a primary then I will be trying it... besides, I gotta use my lithium chloride on something!

[Edited on 9-4-2022 by ManyInterests]

Laboratory of Liptakov - 9-4-2022 at 00:24

For LiCl on LiClO4 you will need PbO2 anode. I recommend all setup from link: https://www.ebay.com/itm/174251053308?hash=item28922c10fc:g:...
Or similar cheaper, necessary find it.
MMO works only on LiCl = LiClO3
For Oxygen 4 in molecule is necessary platinum or PbO2 or Carbon rod.
Carbon rod is almost always decomposed on carbon powder in solution.
Best way as price / power is professional PbO2 anode.

ManyInterests - 9-4-2022 at 08:56

Quote:


For LiCl on LiClO4 you will need PbO2 anode. I recommend all setup from link: https://www.ebay.com/itm/174251053308?hash=item28922c10fc:g:...
Or similar cheaper, necessary find it.
MMO works only on LiCl = LiClO3
For Oxygen 4 in molecule is necessary platinum or PbO2 or Carbon rod.
Carbon rod is almost always decomposed on carbon powder in solution.
Best way as price / power is professional PbO2 anode.


Those are quite pricey, but I guess I am determined to do it. This will be something I will do a bit later, since I want to try to make ammonium perchlorate first.

I saw your videos on making sodium perchlorate (which can be used to make ammonium perchlorate by reacting the sodium with ammonium chloride). I saw that you used a lot of heat to turn the sodium chlorate into sodium perchlorate. Would this process also destroy all the chlorates in the crucible? All of the work I read on making ammonium perchlorate warn heavily to make sure that no other chlorates are present in the starting perchlorate otherwise it would convert into the highly unstable and danger ammonium chlorate.

The stuff I also read on lithium perchlorate synthesis is that it can also be produced by reacting lithium hydroxide with ammonium perchlorate, which will precipitate the lithium perchlorate while converting the hydroxide into ammonium hydroxide. This process seems much simpler since lithium hydroxide is extremely easy to make.

Laboratory of Liptakov - 9-4-2022 at 13:12

Here is method how obtain pretty pure TACP from impurite NaClO4. And then is possible do it decompose on pretty pure NH4ClO4 + CuO.
https://www.youtube.com/watch?v=kUec6kHHxeM&t=3s
Thus TACP preparation in video works a like purification process 2 in 1.
You obtain directly pretty pure TACP. If you need pure NH4ClO4, (for preparation CHP) you can TACP decompose in boiling water on NH4ClO4 + fine powder (black) insoluble CuO. After evaporate water (separe CuO) you obtain pure ammonium perchlorate.

B(a)P - 9-4-2022 at 13:15

Quote: Originally posted by ManyInterests  

I saw your videos on making sodium perchlorate (which can be used to make ammonium perchlorate by reacting the sodium with ammonium chloride). I saw that you used a lot of heat to turn the sodium chlorate into sodium perchlorate. Would this process also destroy all the chlorates in the crucible? All of the work I read on making ammonium perchlorate warn heavily to make sure that no other chlorates are present in the starting perchlorate otherwise it would convert into the highly unstable and danger ammonium chlorate.


Most of the chlorate is converted. You can remove the remained with a recrystallisation using acetone.

ManyInterests - 9-4-2022 at 15:11

Quote: Originally posted by Laboratory of Liptakov  
Here is method how obtain pretty pure TACP from impurite NaClO4. And then is possible do it decompose on pretty pure NH4ClO4 + CuO.
https://www.youtube.com/watch?v=kUec6kHHxeM&t=3s
Thus TACP preparation in video works a like purification process 2 in 1.
You obtain directly pretty pure TACP. If you need pure NH4ClO4, (for preparation CHP) you can TACP decompose in boiling water on NH4ClO4 + fine powder (black) insoluble CuO. After evaporate water (separe CuO) you obtain pure ammonium perchlorate.


Quote:
Most of the chlorate is converted. You can remove the remained with a recrystallisation using acetone.


I downloaded both those videos. I guess I am all set (mostly). I just need to watch and study them thoroughly. I ordered some CuO from aliexpress to make sure I have enough for CHP and LL8. I know I could have made some, but I wasn't in the mood. Might do the same for 28% ammonium hydroxide, but I will make some in the future at home at a later date.

One question about the crucible with sodium chlorate. Is it possible to do it directly on the stove top? I don't have a heat gun (though I don't mind getting one) and the setup that you use with the cinder block is a bit cumbersome for me to use. Is a stove top enough? If I need to use a heat gun, would a different kind of support work while putting the heat gun on the ground? Does this produce dangerous gasses and need to be done outside or can I do it indoors?

I am looking at your video for ammonium perchlorate from TACP. I did see that you made the TACP using ammonium nitrate. Would HNO3 work instead? I don't have access to ammonium nitrate straight off, so I will need to make some for this experiment. Something I was planning on doing anyway.

Laboratory of Liptakov - 10-4-2022 at 00:27

You can use any setting for heating ceramic cup. Stove top, PB - flame, electric snare. Question is, whats happen when cup crack.
Heating can run indoor, is without smell, arises oxygen without chlorine.
Prepare NH4NO3 from HNO3 + ammonia water is slightly luxury, but yes.

ManyInterests - 10-4-2022 at 00:50

Quote:
You can use any setting for heating ceramic cup. Stove top, PB - flame, electric snare. Question is, whats happen when cup crack.
Heating can run indoor, is without smell, arises oxygen without chlorine.


By cup, I assume you mean the crucible? I'll have to monitor it as closely as possible and be ready with the crucible tongs to remove it. I bought a ceramic crucible a while ago.

https://www.amazon.ca/gp/product/B06XKHZKWQ/ref=ppx_yo_dt_b_...

This is the product that I have. I think they might have sent me the wrong size since it seems too small for 500ml. I might need to order another one off aliexpress since now that I look at it, I don't think it is good enough for perchlorate fabrication. I originally got it to make nitrite, which doesn't need as much heat as perchlorate synthesis.

Or am I wrong? What kind of crucible did you use? Is it of similar material?

Quote:

Prepare NH4NO3 from HNO3 + ammonia water is slightly luxury, but yes.


I have seen that done with the common 6% household solution (There is a brand in my area that is 6% ammonia and nothing else. Just ammonia and water. No other additive. I also have had someone else on this forum suggest that I can make ammonium nitrate directly from potassium nitrate and anhydrous magnesium sulfate. I bought some magnesium sulfate but I haven't dried it in my oven yet. I think I'll do that and make it that way, which seems much more economical than getting it from HNO3 which is, as you put it, a slight luxury.

I mean getting 70ml or so of 70% HNO3 requires quite a bit of KNO3. I don't want to waste my precious nitrates! I have spent a lot of time and money to replenish my supply. I will even make more when I order more potassium chloride, since for some reason most stores in my area no longer stock salt substitute, meaning I need to get it from a chemical supplier.

Edit: Actually I think might not need to do any of that. I think there is a brand of cold pack that I can get online that has ammonium nitrate there. Not calcium ammonium nitrate, but just straight up ammonium nitrate (with a nitrogen content less than 28%) is that sufficient for CHP/LL8/Ammonium perchlorate synthesis?

[Edited on 10-4-2022 by ManyInterests]

Laboratory of Liptakov - 10-4-2022 at 12:12

Yes, pure Ammonium nitrate from cold pack should by works for any reactions. My ceramic cup is old quality material. Cup from link is for high temerature melting gold, silver. It will works. 88 x 36 is good size. My cup is smaller 40x 50 mm.

ManyInterests - 11-4-2022 at 07:20

Quote: Originally posted by Laboratory of Liptakov  
Yes, pure Ammonium nitrate from cold pack should by works for any reactions. My ceramic cup is old quality material. Cup from link is for high temerature melting gold, silver. It will works. 88 x 36 is good size. My cup is smaller 40x 50 mm.


That's perfect. The crucible I have was also advertised for gold/silver melting. I am thinking of getting an actual cup (the one I have is shaped as a bowl) and made of graphite. That one is also rated for gold and silver, so I think it would work (it also comes with a lid. Meaning much better heat retention and no need for a foil cover).

I hope that the cold packs are just ammonium nitrate and not calcium ammonium nitrate, otherwise I will need to fiddle around a little to get the ammonium nitrate. I don't know the exact nitrogen content, so I hope it is not only good for CHP/LL8 but also for using to make nitric acid. Because you can never have enough nitric acid!

And since I'm posting, can I redirect your attention slightly towards the thread Det Cap Strategies? I had some questions to ask regarding plasticizing and binding. Since PiB is one of the best binders, I wondered if it is possible to extract the PiB from chewing gum in the same way you extracted it with tape. As in, using gasoline (even lighter fluid works as you said) to get it out. Chewing gum is much more available than SCAPA 2501.

Herr Haber - 11-4-2022 at 09:16

I'd use the ceramic crucibles that come with a small lid for that kind of procedures.
I often use them either to incinerate filter papers (I have one dedicated for filters from silver and PGM recovery) or for when heating in the open air would be detrimental.

They're cheap and I never had one cracking on me with a butane torch. They easily glow white. A pair of pliers or an unfolded paper clip are enough to remove the lid and have a peek inside.
If it serves, I always underestimated the volume I needed with those things.


Laboratory of Liptakov - 11-4-2022 at 13:11

Chewing gum require experiments. Dissolving in gasoline, filtration solid parts and similarly. Not tested. Important : Graphite is carbon. Can easy react with any oxidizer. Especially with super hot oxidizer 400 C or about.

ManyInterests - 12-4-2022 at 08:17

Quote:

I'd use the ceramic crucibles that come with a small lid for that kind of procedures.
I often use them either to incinerate filter papers (I have one dedicated for filters from silver and PGM recovery) or for when heating in the open air would be detrimental.

They're cheap and I never had one cracking on me with a butane torch. They easily glow white. A pair of pliers or an unfolded paper clip are enough to remove the lid and have a peek inside.
If it serves, I always underestimated the volume I needed with those things.


Quote:
Chewing gum require experiments. Dissolving in gasoline, filtration solid parts and similarly. Not tested. Important : Graphite is carbon. Can easy react with any oxidizer. Especially with super hot oxidizer 400 C or about.


Duly noted about the crucible. I will get another ceramic one and make sure it comes with a lid. You did mention in a previous thread that any petroleum distillate will work. I also heard that regular gasoline from the pump won't work. Also it feels off to go to a gas station and ask for a small bottle of gasoline. So I will get a small bottle of Zippo lighter fluid (that is white petrol).

ManyInterests - 15-4-2022 at 20:18

Maybe I should start a thread with my finding later, but I might as well write it here.

I've begun experimenting with extracting rubber from bubble gum. Since as you know I did hear that most bubble gum uses a food safe PiB. Right now I've frozen around 154 grams of bubble gum and then washed them to get rid of the flavorings and other stuff. After rising it i ended up with around 47.5 grams of gum from the 154 (wow, that much sweeteners and stuff). The smell of the gum was very faint and it looked like well-chewed gum. I put the gum in a jar and added 200 grams of charcoal lighter fluid (it is also a petroleum distillate. I wanted to use zippo lighter fluid but I didn't find any). I swirled it around but the gum still likes to stick to the bottom.

The liquid then turned milky white. Maybe there is still something in the gum?

At any rate, Liptakov has kept his tape in the gasoline for 2 days. I will swirl it from time to time but also keep it for a day or three before seeing if anything seems to separate.

The brand of gum is excel extra white. Sugar free.

Herr Haber - 16-4-2022 at 06:02

I'd have gone for tablets such as Wrigley's Big Red, Hollywood etc. rather than dragee for reasons that seemed obvious to me.
Oh well...

ManyInterests - 16-4-2022 at 22:25

Quote: Originally posted by Herr Haber  
I'd have gone for tablets such as Wrigley's Big Red, Hollywood etc. rather than dragee for reasons that seemed obvious to me.
Oh well...


Another experiment for another time. :) Bubble gum is cheap. Zippo lighter fluid is also very cheap.

So far the gum appears to be completely dissolved and is settled at the bottom. The top layer of the liquid is mildly discolored, but is very liquidy.... I think I will need to filter out everything tomorrow. I attached a photograph of it so far.

I am also trying to find some cheaper self-adhesive tape. I would order Scapa 2501, but the price tag is quite high for me. I am seeing stuff on aliexpress like butyl rubber tape. Also some other sealing material that is all made of rubber. Sounds like I might need to shell out more cash and experiment!





Liquid.jpg - 1.5MB

Laboratory of Liptakov - 17-4-2022 at 03:25

It looks like I'm going to open an online store with concentrated PIB solutions ...:D And special plastificators.

ManyInterests - 17-4-2022 at 08:08

That would make things much, much easier! :D All guides and people say 'I used PiB' but they never say how to get it or correctly extracted.

Your plasticizer basic video is literally the only one that I have seen that does that!

Laboratory of Liptakov - 17-4-2022 at 22:33

For example, this tape ( is much cheaper ) looks like a good PIB source, but it is not. During dissolution, it dissolves in its entirety, including the black carrier. So far, the only tape in the world that provides clean and quality PIB is SCAPA 2501.

PIB tape.JPG - 140kB

ManyInterests - 17-4-2022 at 23:50

Well I will be trying. So far I need to buy a pan to test the liquid I got to see if it has PIB. Because now I still have the gum in the large amount of petrol.

I ordered this BTW: https://www.aliexpress.com/item/1005002488805666.html?spm=a2...

In the end of the day I might end up getting SCAPA 2501... but that will be a while from now. The 50$ price tag is really pricey and I want to try with other things.

There HAS to be another way. Lots of energetics guys get PIB and not all from scapa.

There is also the rubber cement method. That one works, but I want to try to make PIB first since it is better than rubber cement.

MineMan - 18-4-2022 at 06:09

For this effort you could probably synth an energetic binder with far better performance.

ManyInterests - 18-4-2022 at 08:37

Quote: Originally posted by MineMan  
For this effort you could probably synth an energetic binder with far better performance.


I'm listening. Please tell me how it is done, because I can't find any information on it.

Laboratory of Liptakov - 18-4-2022 at 11:58

Scapa 2501 show on my browser 8.75 USD... 10 meters / 38 mm
It is a huge amount of tape. Very good price.
https://www.tme.eu/en/details/scapa-2501-38/self-amalgamatin...

ManyInterests - 18-4-2022 at 22:26

I was not aware of that site. The only site I checked for Scapa 2501 was ebay, which did sell for 50$ USD. That site you showed is much, much cheaper. I think I'll order a roll from there some time. :)

Edit: https://amzn.to/3jQed1J

I forgot to mention this. Lip gloss base appears to have all sorts of nice plasticizers in it. The ingredient list shows PIB as well as other stuff you used in styrofan (like styrene?)

[Edited on 19-4-2022 by ManyInterests]

ManyInterests - 20-4-2022 at 17:20

So a bit of notes on my bubble gum PIB extraction... I think there is definitely PIB in the bubble gum. But I believe I may have made a mistake in dissolving them. As in, I used too much lighter fluid. So when I put the fuel in the pan and evaporated the fuel (I need to check the flash point of that stuff, because while I did see white fumes, I was afraid it'll ignite and start a fire. Thankfully nothing of the sort happened).

I might have dried the stuff too much. Because while all the fuel did evaporate, what was left was a very, VERY sticky layer of glue-like substance. I've seen your video on the plasticizer and it much stickier than the stuff you handled.

I will need to try again.


Microtek - 21-4-2022 at 03:10

The stickiness is dependent on several factors, such as degree of polymerisation (of the PIB)and the nature and amount of plasticizer. The polymer and plasticizer may have different solubilities in your chosen solvent, and that could easily alter the polymer/plasticizer ratio in you extract. This would then change the properties of the remanence.

[Edited on 21-4-2022 by Microtek]

[Edited on 21-4-2022 by Microtek]

ManyInterests - 21-4-2022 at 20:52

Yeah. I will need to experiment more with it. But I'm not finding the time for it.

I did do one experiment with the rubber cement and bar and chain oil. I used around 5 grams of victor brand rubber cement and perhaps around 0.5 grams of all-season bar and chain oil (give or take 0.1 grams). I used Darian Ballard's method. I used 9.1 grams of cake flour as a test.

I could not fully dry them because the 2nd hand hair dryer I bought for this purpose broke after a bit of use (It was really cheap so I don't care. I'm sure I can pick up another 2nd hand one soon). So I just tried to mix and work with them until they did form a putty. It has the consistency of playdough (thought I can't really tell. I haven't played with playdough since I was a child) or a very soft eraser. I think I will to put in a little more rubber cement next time. I had a hard time measuring because my mixing bowl was too heavy for my scale. so there was some inaccuracies.

But overall it is a fine first attempt when using rubber cement based plasticizer. I hope my next attempts will be better. Scapa 2501 amalgamates a little better I heard (from people who used both rubber cement and Scapa 2501) but overall the rubber cement should be sufficient for my purposes.

I will still do something with the chewing gum, because why not? also spirit of experimentation and all that.

also I might try to work with makeup grade latex to see if I can make a rubberized substance. Lots of people make plastic explosives here, but I don't see that many showing off sheet explosives.


Laboratory of Liptakov - 22-4-2022 at 07:11

Most from researchers here focus on the most difficult and crucial task. So to create a reliable detonator, the production of which is maximally safe, simple and so on. The production of plastic explosives (eg 100g) is much more expensive than the research of new detonators, which usually contain 1g HE. Testing of new plastic HEs is also problematic due to noise.

MineMan - 22-4-2022 at 13:43

Quote: Originally posted by ManyInterests  
Yeah. I will need to experiment more with it. But I'm not finding the time for it.

I did do one experiment with the rubber cement and bar and chain oil. I used around 5 grams of victor brand rubber cement and perhaps around 0.5 grams of all-season bar and chain oil (give or take 0.1 grams). I used Darian Ballard's method. I used 9.1 grams of cake flour as a test.

I could not fully dry them because the 2nd hand hair dryer I bought for this purpose broke after a bit of use (It was really cheap so I don't care. I'm sure I can pick up another 2nd hand one soon). So I just tried to mix and work with them until they did form a putty. It has the consistency of playdough (thought I can't really tell. I haven't played with playdough since I was a child) or a very soft eraser. I think I will to put in a little more rubber cement next time. I had a hard time measuring because my mixing bowl was too heavy for my scale. so there was some inaccuracies.

But overall it is a fine first attempt when using rubber cement based plasticizer. I hope my next attempts will be better. Scapa 2501 amalgamates a little better I heard (from people who used both rubber cement and Scapa 2501) but overall the rubber cement should be sufficient for my purposes.

I will still do something with the chewing gum, because why not? also spirit of experimentation and all that.

also I might try to work with makeup grade latex to see if I can make a rubberized substance. Lots of people make plastic explosives here, but I don't see that many showing off sheet explosives.



LL is right. Generally it’s not interesting unless the binder is energetic. The procedures are well known. It’s just a matter of finding the right tape.

ManyInterests - 22-4-2022 at 15:47

You guys are right. I should keep any posting in this thread on the primaries being made here (which I do plan on making. I'm going to break out my chemistry kit for a bit of boring reagent making). If it's all about dissolving the tape in gasoline and extracting the stuff then... yeah. I guess it's already done.

But MineMan, I would like to speak to you about those energetic binders. I did look into them slightly, do you have any resources that could guide me further? Some of the stuff I did read did seem to point to a gelignite type explosive.

MineMan - 22-4-2022 at 19:07

Yah many interests. You kind of high jacked this thread I would recommend posting about the binders else where. I don’t except out of all of the ones available there must be one that is doable.

mysteriusbhoice - 4-5-2022 at 23:56

I have an alternative way of making copper perchlorate and it hinges on the fact that both copper chloride and sodium perchlorate are both highly soluble in ethanol but sodium chloride is not.
I will soon make a video on this.
Btw on preparing copper perchlorate with membranes you must use KClO4 and heat the cell below 80C and above 50C because it would otherwise be very difficult to seperate copper perchlorate from sodium perchlorate

Laboratory of Liptakov - 5-5-2022 at 07:24

Great message, thanks...:cool:...I have both compound for attempt.
I am curious.


[Edited on 5-5-2022 by Laboratory of Liptakov]

mysteriusbhoice - 5-5-2022 at 08:50

Quote: Originally posted by Laboratory of Liptakov  
Great message, thanks...:cool:...I have both compound for attempt.
I am curious.


[Edited on 5-5-2022 by Laboratory of Liptakov]


sadly as for trying to mix CuCl2 and NaClO4 in ethanol and it forms a complex which is deep green in color and doesnt crash NaCl out probably Na2Cu(ClO4)4 and I used anhydrous ethanol and 99% pure NaClO4 from solvent extraction.


I have also prepared before calcium perchlorate from ethanol, calcium chloride and sodium perchlorate. This can then be reacted with copper sulfate to form calcium sulfate and copper perchlorate.

I wonder if LL8 can work with somewhat purified Cu(ClO4)2 with slight contamination of NaClO4.

If we are talking about slightly contaminated Cu(ClO4)2 then the most incosequential one would be starting with NH4ClO4 in the membrane electrolysis stage as the electrolyte.
the membrane electrolysis with heated KClO4 is probably the only thing left to try.

[Edited on 5-5-2022 by mysteriusbhoice]

Laboratory of Liptakov - 5-5-2022 at 10:11

Yes, for example 5% NaClO4 in Cu(ClO4)2 will works sure. (+ hexamine) Neutral Cu(ClO4)2 is problem. Always were problems with acidity in him. (from HClO4 prepared) Preparation neutral Cu(ClO4)2 from NaClO4 + somethig, require exact verifycated method. Not found yet. Exact weights, temperatures, times etc.

MineMan - 6-5-2022 at 16:26

LL, any update on increased density? I can give you a mix with large density that will DDT, you already played around with it. It’s very similar to dragons tail. Basically if you do dragons tail and the ratios I suggested a few years ago and add two catalyst it DDTs :) at the density of a paste

mysteriusbhoice - 7-5-2022 at 01:31

Quote: Originally posted by Laboratory of Liptakov  
Yes, for example 5% NaClO4 in Cu(ClO4)2 will works sure. (+ hexamine) Neutral Cu(ClO4)2 is problem. Always were problems with acidity in him. (from HClO4 prepared) Preparation neutral Cu(ClO4)2 from NaClO4 + somethig, require exact verifycated method. Not found yet. Exact weights, temperatures, times etc.


I have done a lot of membrane electrolysis runs to produce Cu(ClO4)2 from NaClO4 and copper sacrificial anode.
it is then left to evaporate and ethanol is added just enuf which doesnt dissolved all of the NaClO4 and isolates somewhat pure Cu(ClO4)2 but to get the weight you have to dry it again..... carefully and find it out with scale.


IMG_20200716_224238.jpg - 2.7MB

the seperation power totally depends on your membrane and setup an in that pic was the old PVC + Sand but I have made better castable membranes for easy setup like the ionomer concrete.
mix of sand + OPC cement + CaSO4 9:3:1 ratio.
The CaSO4 can be substituted for cation exchange resin from the water filtration section of any hardware store.
be sure to grind the cation exchange resin in a blender first.
Anion exchange resin is only for anion permeation IE making H2SO4 and other processes.

Overall the thing which happens here is.
Cu + e = Cu2+ (anode)
NaClO4 + Cu2+ = Cu(ClO4)2 + Na+ (anode side)
Na+ + H2O = NaOH + H+ (cathode side)
H+ +e = H2 (cathode)

overall
NaClO4 + Cu + H2O = NaOH + Cu(ClO4)2 + H2



[Edited on 8-5-2022 by mysteriusbhoice]

Laboratory of Liptakov - 7-5-2022 at 10:30

That container looks a little mad. But if it works, it's ingenious equipment. Copper sheets, NaClO4, porous ceramic membrane. After all, we are on a science madness. Interesting thanks.

[Edited on 7-5-2022 by Laboratory of Liptakov]

mysteriusbhoice - 8-5-2022 at 03:04

I have seperated out the copper perchlorate from NaClO4 somewhat from this mix as it does form that green complex but it seems to settle out.

IMG_20220508_112402.jpg - 3.4MB

IMG_20220508_145435.jpg - 2.7MB

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mysteriusbhoice - 9-5-2022 at 04:26

NaClO4 is annoying because its hard to seperate Cu(ClO4)2 from NaClO4 using any solvent.
going ahead and using KClO4 membrane heated to 60C and it seems to be working fine.
hopefully I can create a seperable copper chlorate with less contamination with this.

Using NH4ClO4 is really ideal as NH4ClO4 contamination wont be a big issue.

Laboratory of Liptakov - 9-5-2022 at 07:54

Interesting. Relatively pure neutral Cu(ClO4)2 is not some easy.

mysteriusbhoice - 9-5-2022 at 12:36

Quote: Originally posted by Laboratory of Liptakov  
Interesting. Relatively pure neutral Cu(ClO4)2 is not some easy.



if you think that is annoying I also get orange copper 1 perchlorate!! :*((( if I let it run for too long.
This weird bright orange precipitate eventually appears coating the anode and settles out and its odd because its energetic!! when mixed with fuel after washing then dry.
edit: after looking at other images of copper 1 oxide, it may perhaps just be that mixed with some perchlorate residue but IDK honestly will have to isolate some of it in the future.
The same happens when making copper chloride where white copper 1 chloride is also made somewhere further along the electrolysis.
This bright orange precipitate looks different from copper 1 oxide which is a more dark brown.

I will keep messing about with membranes to try to get the KClO4 Cu(ClO4)2 mix which I believe I had success with this one since KClO4 settles out in the freezer and is not soluble as much in ethanol or water if its cold.

Problem is I killed my membrane because I decided to run some PbO2 to oxidize copper 1 perchlorates and oxides and yea I let that run too long and perchloric acid fucked up my polymer membrane since the substrate is polyurea cleaning cloth and not fiberglass which explains the ammonia smell in the cathode chamber XD.

I am making an ionomer concrete membrane which hopefully will be better.

[Edited on 9-5-2022 by mysteriusbhoice]

ManyInterests - 21-6-2022 at 12:20

OK... while this is not the CHP thread. I am making good on my promise to start making the stuff for a few CHP synthesis. I spent a month (or almost a month) to make 500 grams of sodium chlorate (of varying purity) and am now trying to turn that chlorate into perchlorate via heat composition. Just as LL did in his video.

In the crucible pictured. I added 60 grams of slighly impure sodium chlorate and it has been on my stovetop at the highest heat for almost 3 hours. The color of the chlorate has become considerably darker, but has not begun to melt or turn into a slurry. I did not wrap anything in aluminium foil. Am I losing too much heat or what?


EDIT: I took a measurement with a candy thermometer (which broke when I tried to cool it down too fast... goodbye mr. candy thermometer!)

It was well above 200 degrees celsius, which is as far as the thermometer will allow (and it continued to go farther). So I know I am getting good heat from there. But maybe not as hot as needed?

ceramic.jpg - 1.6MB

[Edited on 21-6-2022 by ManyInterests]

ManyInterests - 21-6-2022 at 13:40

So I put it back on the heat with it being wrapped like this. I hope it will be hot enough to turn the chlorate into perchlorate.

Ceramic2.jpg - 2.4MB

Laboratory of Liptakov - 22-6-2022 at 10:06

Good luck. But the cup on hot wires looks a like really science madness....:D



[Edited on 22-6-2022 by Laboratory of Liptakov]

ManyInterests - 22-6-2022 at 17:29

OK, so I have tried to make it hotter by putting another larger pot on top of it. The stuff didnt melt, but it did get RED HOT in the crucible. Would I have some perchlorate there?

Edit: no. I only ended up with 0.2 grams! I need a stronger heat source.

[Edited on 23-6-2022 by ManyInterests]

ManyInterests - 27-6-2022 at 14:29

I think I am going to have to ask for a bit of advice in making perchlorates. No matter my efforts I cannot make it work through thermal decomposition.

Edit: Just after a private message talk with LL. I realize that I should have recrystalized and tried to purify my sodium chlorate before commencing with the heating. While I did order electrodes, I had to order another crucible since my previous one broke. What I will do in the meantime is make more chlorates and purify my entire supply via methanol crystalization and hopefully try again via the propane torch method.

I will need to make sure everything is pure because even using platinum electrodes requires very pure sodium chlorate to work. So it is a must anyway.

Everything should be ready for the next batch of tests in three weeks or so.

[Edited on 28-6-2022 by ManyInterests]

markx - 30-6-2022 at 10:22

Quote: Originally posted by ManyInterests  


I will need to make sure everything is pure because even using platinum electrodes requires very pure sodium chlorate to work. So it is a must anyway.

Everything should be ready for the next batch of tests in three weeks or so.

[Edited on 28-6-2022 by ManyInterests]


No you do not strictly need superbly purified chlorate to convert it into perchlorate on platinum anode. In fact I have never engaged in any sort of purification activities prior to perchlorate conversion....and even worse I routinely go with Pt straight from chloride to perchlorate in the same cell. Takes a while, but truly the lack of need to babysit and interfere with the process really makes it worth even if the anode lifespan is compromised. I put chloride into the cell.....fire it on and forget for a month...unless the anode dies before full perchlorate conversion I only have to add deionised water to top up once in a while. Or saturated chloride solution if I would like to receive "really thick stuff" in the end.
With electrochemical perchlorate production the key element is to be able to have knowledge and possibility to find or make replacement anodes. Because anything less than a solid brick of Pt is going to be an expendable asset. It will wear out, passivate and disintegrate in a few conversion runs at best. All the monstrously work and time consuming efforts of starting with "purified and chloride free" feedstock are not really going to make a noticeable difference in the end. It may make sense to some degree on an industrial scale, but on tabletop reactor realm it is wasted effort.

The "really thick stuff d=1,6g/cm3" not willing to mix with added water on top of it:
https://www.youtube.com/shorts/d7erWvS6JK0

The "expendable Pt anode" resuming work on the perchlorate conversion after being replaced:
https://www.youtube.com/shorts/37r58o5kB_Y


[Edited on 30-6-2022 by markx]

ManyInterests - 1-7-2022 at 16:18

Glad my information on making chloride straight to perchlorate would work.

Thing is, I've already started my latest and greatest chlorate run. Over 450 grams of chloride in 1350ml of water, plus 9.73 grams of calcium chloride for pH modification... I also put in 10 grams of magnesium sulfate by accident, but that shouldn't impact the yield. I already see white precipitate on the bottom of the big jar. It's quite early in the project. But I don't think it'll need more than 10 days to complete.

I am making more chlorates since I was told by someone I am in communication with that I don't have enough chlorates (assuming 100% purity) for a decent perchlorate run. I just hope to make to one very good sodium perchlorate run, and then convert all I can to ammonium perchlorate.

Then I can make the CHP and the LL8 and lithex that this whole thread was originally about. I did promise LL and Mineman I would make CHP after all.

But I am not going to give up on NHN. I liked making it and I plan on making more of it once I got some nitric acid made.

Theoretic - 4-7-2022 at 15:22

Quote: Originally posted by mysteriusbhoice  


I have done a lot of membrane electrolysis runs to produce Cu(ClO4)2 from NaClO4 and copper sacrificial anode.
it is then left to evaporate and ethanol is added just enuf which doesnt dissolved all of the NaClO4 and isolates somewhat pure Cu(ClO4)2 but to get the weight you have to dry it again..... carefully and find it out with scale.


If the compartments are physically separate, perhaps it's unnecessary to let sodium perchlorate be in the copper compartment? If you just put tap water there, it will provide enough initial conductivity until the perchlorate ions get through the membrane. In the meantime, copper will be turning into insoluble copper hydroxide until the perchlorate gets there. But that byproduct will be much easier to separate than NaClO4 surely

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