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Author: Subject: A powerful,unreported new primary explosive--NiCC
littlesky
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[*] posted on 15-7-2023 at 19:34
A powerful,unreported new primary explosive--NiCC


Preface:Before introducing NiCC,let's first introduce a primary explosive that someone may know.
Nickel tricarbohydrazide perchloric(NiCP) is a less well-known primary explosive.But its excellent performance has attracted the attention of many Chinese enthusiasts.Powerful,easy to prepare,and environmentally friendly are its advantages.According to different preparation conditions,this is a kind of powder from light blue to dark blue.(Annex 1)

However,raw materials-perchlorate(especially sodium salt and ammonium salt)or perchloric acid are almost impossible to obtain and expensive.And its theoretical sensitivity is not high,but due to the presence of numerous edges and fractures in the crystal,its actual sensitivity is very high, similar to that of peroxide HMTD.(Annex 2)

About a year ago, when I was doing a test,I accidentally found that the mixture of nickel tricarbohydrazide nitrate and Potassium chlorate had strong explosive power.So, would it have a better effect if chlorate ions entered the molecule instead of simply mixing?

I have consulted many similar article,but there are no results.Only one article mentioned the Copper(II) chlorate complex Therefore, I believe that this compound and similar substances have not been synthesized by other researchers.

Later,I successfully synthesized this substance through experiments. After testing,I found that it indeed has strong detonation ability. Sensitivity similar to NiCP but lower.And after multiple experimental optimizations,more suitable preparation conditions were found.
Warning:This energetic material has not undergone strict sensitivity testing, and there is no data to prove its sensitivity. After my simple testing, I believe that its sensitivity is lower than NiCP, but some people have also made dangerous high sensitivity products. So it is not recommended to prepare in large quantities.
1.Preparation
Source of chlorate:I prepare it through Sodium chlorate.In China, Chlorate is difficult to obtain,but Sodium chlorate can be purchased as a water treatment agent(called COD).You can also get a more pure nickel chlorate solution by mixing Barium chlorate and Nickel(II) sulfate solution,filtering out Barium sulfate.
Nickel(II):I use Nickel(II)nitrate hexahydrate. After many experiments,I found that the solubility of nickel tricarbohydrazide nitrate mentioned above is very high.After the experiment of other enthusiasts, Nickel(II) sulfate hexahydrate is also feasible.
Carbohydrazide(CHZ):a chemical raw material that can be purchased directly.

Let's start preparing now
Weigh 0.79g CHZ and 1g NaClO3, and dissolve them together with 4ml of water.(No reaction,no need to worry)
Also weigh 0.85g Ni(NO3)2•6H2O and dissolve in 4ml of water.
Freeze 10ml of distilled water at the same time for subsequent washing.
Take Nickel(II) nitrate solution as the bottom solution, and drip Sodium chlorate CHZ mixed solution under magnetic stirring,and the solution turns blue.
Wait for a while, a small amount of sediment appears
Place the beaker in an ice bath(-5~-10℃)and stir continuously.At this time,a large amount of precipitates will precipitate and settle to the bottom.The upper clear liquid is light blue.
Place the beaker in the freezer to further cool down to increase yield. After filtration or suction filtration,wash with cold water 2-3 times.It is recommended to use suction filtration here,because this material has a large solubility and a fast dissolution rate,and can quickly reach the precipitation Solubility equilibrium when the temperature is slightly higher.Just ordinary filtration time can cause a significant loss of product.
It is difficult for the yield to exceed 80% during ordinary filtration.After preparing so many times,the highest yield is only around 78%,while suction filtration is estimated to exceed 85%
Dry naturally to obtain blue powder
This is the final product(Annex 3)
2.Test.
Mechanical sensitivity:After some testing,I feel that it is lower than the nicp,and capable enthusiasts can help me measure the specific data.
flame sensitivity:It can be directly ignited and detonated by KNSU charges(KNSU:60~65%Potassium nitrate,40~35%Sucrose),but this is unlikely to happen in NiCP.
Power test:Accurately weigh 5mg NiCC,Aluminum foil wrapping,fuel ignition.(Annex 4)

NiCP physical image change.jpg - 497kBNiCP appearance under electron microscope2.jpg - 33kBIMG_20230319_083731.jpg - 1.5MB
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littlesky
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[*] posted on 15-7-2023 at 19:35


Annex 4

Attachment: 5mgNiCC slow.mp4 (2.5MB)
This file has been downloaded 220 times

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underground
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[*] posted on 16-7-2023 at 07:30


What is the storage stability ?
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littlesky
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[*] posted on 16-7-2023 at 16:25


Quote: Originally posted by underground  
What is the storage stability ?

Of course it's safe.I synthesized this compound on June 22, 2022 and it has been stored at room temperature for over a year. So far, there has been no change in color or morphology. The explosion test is also quite perfect. In addition, I also prepared a solution of this compound and stored it in sunlight and in a dark place for one month without any color change. It should be possible to demonstrate the long-term storage stability of this substance

Fresh solution.jpg - 1.6MBOne month later.jpg - 1011kB
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[*] posted on 16-7-2023 at 16:28


Cool. The copper/calcium/magnesium nitrate salt of CHZ could be a good secondary too
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[*] posted on 16-7-2023 at 16:56


Does anyone know of a commercial source in USA of carbohydrazide/semicarbazide? Or of NaNO2 for that matter? I can only find it direct through the Chinese for last couple of years.
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[*] posted on 16-7-2023 at 17:00


Sodium nitrite can be bought from sporting goods stores as bait cure. I bought mine here. They're out of stock right now but they restock fairly regularly.



“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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littlesky
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[*] posted on 16-7-2023 at 17:04


Quote: Originally posted by underground  
Cool. The copper/calcium/magnesium nitrate salt of CHZ could be a good secondary too

Haha, chz complexes are very interesting. I have been studying copper complexes with chz for a year. Nitrates have various isomers. But without exception, they are very weak and unstable.
According to different preparation methods (temperature, solvent, etc.), dark brown, dark blue and Baby blue powders may appear. The dark blue isomer turns yellow and then green after less than a month of storage. Baby blue isomers will decompose spontaneously and slowly. The black isomer is relatively stable and has a high density, but the preparation conditions are very strict.
These three isomers cannot continue to burn on their own. Only when continuously under the flame can it burn, emitting a green flame. When heated and decomposed, the two blue isomers first melt and then burn and explode. It is obvious that melting is endothermic and cannot sustain combustion on its own. This makes it impossible for this substance to be applied in the field of primary explosives.I have tried to detonate copper nitrate of CHZ, but failed.
I also made Chlorate and Perchlorate of chz copper complex. The former is a Dangerous goods that is easy to self explode (which almost kills me), and the latter is an explosive with high sensitivity and cannot be used in the field of primary explosives.
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[*] posted on 16-7-2023 at 18:25


Synthesis of a new primary explosive:Nickle tricarbohydrazide perchlorate(NiCP)

Capture.JPG - 17kB

Video YT :)




Small blasting caps, fingers safe!
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littlesky
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biggrin.gif posted on 16-7-2023 at 18:43


Quote: Originally posted by Vpatent357  
Synthesis of a new primary explosive:Nickle tricarbohydrazide perchlorate(NiCP)



Video YT :)

I made this video:D:D
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[*] posted on 17-7-2023 at 05:19


What is the difference between the chlorate and perchlorate salt ?

Have you ever tried other complexes of CHZ with other metals like magnesium calcium cobalt etc

[Edited on 17-7-2023 by underground]
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[*] posted on 17-7-2023 at 09:08


Difference can be advantage use NaClO3 which is easily avaliable (produce) than NaClO4. But carbohydrazide availability as key precursor can be problem in a lot countries.
A like every new substance, also Nickel carbohydrazide chlorate (NiCC) require perpedicular test 1000 mg against lead brick or aluminium brick.
The test on a can of coca cola has no telling value.....:cool:




Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023)
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[*] posted on 17-7-2023 at 16:45


littlesky have you ever tried to nitrate CHZ ? Diaminodinitrourea may be formed

[Edited on 18-7-2023 by underground]
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[*] posted on 23-7-2023 at 11:02


I have experimented a little with the perchlorate variant. I found that preparation was easy and high yielding (89% with no effort to maximize yield except for using ice water to wash the product). NICP is a sky- or baby blue material. It can be air dried and doesn't seem hygroscopic, though I haven't tested that rigorously. If contacted by a flame when on a spatula, it sputters and flashes, but seems less inclined to take fire than NAP or lead styphnate.
If contained in a fold of aluminum foil and held over a flame, it detonates extremely violently, perhaps even more so than NAP. It DDTs in amounts as low as 5 mg from the spit of a thin (1.5 mm) BP fuse when compacted into a piece of PVC tubing, with the two ends closed with compacted Al-foil and tissue paper respectively.

I have tested sensitivity with my oblique impact machine, which combines impact and friction testing by striking the sample at a shallow angle with a steel pendulum (see attached picture). The sample is spread evenly on a small piece of 100 grit sand paper and clamped to a steel plate on the base of the apparatus. Then the pendulum (550 g) is raised to a certain height and released. This is repeated 5 times at a given height and the number of positive tests is recorded.
For NICP 90 cm (4.86 J) gave 2/5 (2 go and 3 no go the positives are number two and three from the bottom) while 95 cm gave 1/5. For comparison, NAP gave 2/5 at 110 cm.





IMG_20230723_141205_V2.jpg - 886kB

IMG_20230723_141452_V2.jpg - 2.4MB
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[*] posted on 25-7-2023 at 03:46


Just can’t beat NAP. Nor would I expect one too. Aminoguanidine is a very good and stable molecule.
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[*] posted on 25-7-2023 at 16:31


Well, I'm not quite certain about that. It is true that NAP is slightly less sensitive, but both of them are very insensitive for primaries. As I see it, NAP has the disadvantage that due to the air sensitivity of free aminoguanidine, it is destroyed by contact with liquid water. NICP has the disadvantage that carbohydrazide is not as easy to find or prepare.

I am thinking of experimenting with some other combinations of ligands and (transition) metal ions to see if I can find other promising materials (as other members have too).
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[*] posted on 25-7-2023 at 17:51


I am pretty sure most Ni chlorate/perchlorate complexes are primaries. CHZ can be bought from Alibaba at relatively good price. 2kg of CHZ would be enough lifetime supply for expiramenting.

CHz is a nitrogen rich compount, i believe other insensitive CHZ complexes would be good secondaries too. Maybe magnesium copper calcium nitrate complexes.

[Edited on 26-7-2023 by underground]
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[*] posted on 26-7-2023 at 03:09


I prepared the copper analogue to NICP. It is a very visually pleasing reaction yielding a beautiful midnight blue product. I have only tested its reaction to flame and indirect heating, and in these tests it doesn't seem very impressive. Of course, that is hardly conclusive.
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[*] posted on 26-7-2023 at 04:00


Try to detonate a few grams and compare it with ETN.

Magnesium complex in theory will outperform all the rest complexes due to the low molar mass of magnesium metal compared to other metals.

[Edited on 26-7-2023 by underground]
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[*] posted on 26-7-2023 at 16:43


It will be some time before I have an opportunity to test anything else, but yes, more experiments with the copper complex will be undertaken.

Magnesium is not great at making complexes with nitrogen rich ligands. It has an affinity for hard oxygen ligands such as water or hydroxylates. For this reason I think transition metals such as iron, zink or cobalt are much more promising.
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[*] posted on 26-7-2023 at 17:18


Quote: Originally posted by Microtek  
It will be some time before I have an opportunity to test anything else, but yes, more experiments with the copper complex will be undertaken.

Magnesium is not great at making complexes with nitrogen rich ligands. It has an affinity for hard oxygen ligands such as water or hydroxylates. For this reason I think transition metals such as iron, zink or cobalt are much more promising.


What about Calcium
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[*] posted on 27-7-2023 at 03:38


Same as with magnesium. It is related to the concept of hard and soft acids and bases, which is in turn related to charge distribution and polarizability of the metal ion. Small, "hard" metal ions (Lewis acids) such as all of the group one and two elements form stronger complexes with "hard" bases such as those containing oxygen (eg. water). If you look at the wikipedia article about HSAB theory, you can find an overview of which metal cations are considered hard and which are soft. This being chemistry, it is a spectrum of hardness rather than definite categories, so exceptions to these rules do exist.

Nevertheless, this is the reason I think that the transition metals are a better group to look towards for complexation centers in energetic compounds.
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[*] posted on 27-7-2023 at 07:12


Interesting. Obviously i am not a chemist and i am still learning.
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[*] posted on 28-7-2023 at 23:28


Ok,guys.Do not try to synthesize Chlorate/Perchlorate of chz copper complex, they are extremely unstable dangerous compounds.I once synthesized Chlorate of chz copper, and this substance blew itself up in the middle of the night
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[*] posted on 29-7-2023 at 13:16


Quote: Originally posted by littlesky  
Ok,guys.Do not try to synthesize Chlorate/Perchlorate of chz copper complex, they are extremely unstable dangerous compounds.I once synthesized Chlorate of chz copper, and this substance blew itself up in the middle of the night


Did you test and have the same issue with the perchlorate salt? Or are you assuming chlorate and perchlorate will be the same? They will generally have very different properties.
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