Sciencemadness Discussion Board

A powerful,unreported new primary explosive--NiCC

littlesky - 15-7-2023 at 19:34

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

littlesky - 15-7-2023 at 19:35

Annex 4

Attachment: 5mgNiCC slow.mp4 (2.5MB)
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underground - 16-7-2023 at 07:30

What is the storage stability ?

littlesky - 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

underground - 16-7-2023 at 16:28

Cool. The copper/calcium/magnesium nitrate salt of CHZ could be a good secondary too

Hey Buddy - 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.

Sir_Gawain - 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.

littlesky - 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.

Vpatent357 - 16-7-2023 at 18:25

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

Capture.JPG - 17kB

Video YT :)

littlesky - 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

underground - 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]

Laboratory of Liptakov - 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:

underground - 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]

Microtek - 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.





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MineMan - 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.

Microtek - 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).

underground - 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]

Microtek - 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.

underground - 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]

Microtek - 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.

underground - 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

Microtek - 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.

underground - 27-7-2023 at 07:12

Interesting. Obviously i am not a chemist and i am still learning.

littlesky - 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

B(a)P - 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.

ManyInterests - 30-7-2023 at 15:23

Commenting on this now. I am in the process of making sodium chlorate and this seems really promising. I don't know where to get carbohydrazide in Canad (the prices on ebay for 100g are too high) but if I can get some, I can give this process a go some time.

Do you have information on its ability to detonate secondaries? Especially insensitive secondaries such as TNT or ammonium picrate?

Microtek - 4-8-2023 at 08:56

I have been doing a few tests on the copper variant (CuCP). It is indeed capable of powerful detonation, but seems to require more containment than NiCP. NiCP will detonate when heated over flame in a fold of Al foil, CuCP requires the foil to be folded so the ends are closed off. I have also tested the sensitivity in the apparatus described above. The sensitivity is practically identical: 2/5 at 93 cm.

I still need to test the ability of CuCP to DDT and also initiation ability (for both compounds). I won't be doing any tests of the power of gram amounts, since this is not useful for a primary. I also won't synthesize any chlorate analogues since I distrust them. I have not seen any indication that CuCP is any more unstable than NAP or NiCP, but I will continue to store only about a gram inside a large steel pot just in case (I have only had it for about two weeks so far).

underground - 5-8-2023 at 03:21

What about the nitrate salts

Microtek - 5-8-2023 at 08:37

I can certainly try them at some point, but I don't have high hopes; they are usually less impressive than perchlorate complexes. The low toxicity would be a plus though.

Microtek - 18-8-2023 at 08:34

CuCP DDTs about as well as NiCP or NAP; 10 mg is enough in light confinement. I have worked on testing initiating power and both NAP and NiCP initiates RDX in amounts as low as 10 mg. I haven't tested smaller amounts because reproducability becomes problematic if I go much lower (my scales are accurate enough to 1 mg, but it is difficult to press, say, exactly 5 mg into the cap since some will stick to the rod). Even 10 mg pressed onto a base charge is a thickness akin to apple skin, so I don't think there is much reason to use less.

IMO, a primary should have low sensitivity, be non-hygroscopic, have low toxicity and be capable of initiating a base charge of a moderately sensitive secondary. Power beyond this is of limited utility. Someone on SM once raised concerns about the possibility of producing nickel carbonyl when detonating nickel containing explosives. I think it's probably not a huge issue, but on the other hand detonating a negative OB explosive will probably produce a little CO and also atomized nickel. Given the exceptionally toxic nature of nickel carbonyl I figured it might be prudent to explore some other transition metal complexes.
For this reason, I have synthesized the cobalt analogue to NiCP, CoCP. It is a pink, non-hygroscopic material that seems on par with the nickel versions in terms of sensitivity and explosivity. I haven't done an exhaustive examination yet, though.

MineMan - 18-8-2023 at 18:31

Try the copper microtek.

Microtek - 18-8-2023 at 23:37

I did try the copper compound, it's the one I refer to as CuCP a couple of posts ago. It seems fine in terms of explosivity, sensitivity and ability to DDT, but the yield of the reaction is not so great. It seems to have a greater solubility in water, leaving the supernatant solution strongly coloured whereas the NiCP leaves a completely clear supernatant, indicating no nickel ions in solution.
One definite advantage that these carbohydrazide complexes have over aminoguanidine complexes is the stability of carbohydrazide versus aminoguanidine. Free aminoguanidine decomposes in solution, leaving a black residue.

Oh, and I also tried the copper nitrate complex. It did give a precipitate but it was non-flammable and had no energetic properties as far as I could determine.

[Edited on 19-8-2023 by Microtek]

MineMan - 19-8-2023 at 00:48

Hmm


Is the toxicity of NAP really a concern if only 10mg is need for RDX

For the copper, the yields still seem high, only issue is I witnessed a sample go off with the smallest hammer tap (we’re talking like silver azide) after about 6 months.

Just seems hard to improve on NAP. I would be much more interested in seeing new research from you in the form of Urazine perchlorate at proper critical diameter and more strained TAG compounds and melem which hey buddy speaks highly of.

Or even a revisit to the DUAN melt cast. And a procedure to get it out of solution with ease, maybe even some dry ice cooling in methanol.

I haven’t checked the Carbohyrazide prices since 5 years ago. Back then it was about $50kg or far less in bulk.

littlesky - 19-8-2023 at 02:07

Sorry for not replying to you guys for a while. I have been working on new energetic materials recently, such as fox-7, DNOAF, TEX.
In fact, the content I initially published was only a small part of the full paper. I will place the full text through machine translation below.
Additionally, I will release content on DNOAF and FOX-7 in the near future. Thank you for your reply.
:P:P:P

littlesky - 19-8-2023 at 02:44

The following is a machine translated version, without careful inspection, there must be many errors.


Preface: Nickel perchlorate tricarbonylhydrazide (NiCP) is a high-performance, highly stable, and easy to prepare primary explosive. Its derivatives such as GTX and GTG have also been widely known. However, one of its raw materials, perchloric acid, is difficult to purchase and expensive, greatly limiting its potential for promotion. (Another good method is to use NaClO4 as a source of perchlorate, similar to the following method)
During a fire lead test, I accidentally discovered that a mixture of nickel tricarbonylhydrazide nitrate (XTN) and potassium chlorate had strong explosive properties, even surpassing NiCP in power. So, would it be better to introduce chlorate ClO3- directly into the molecule instead of simply mixing it?
I have tried to consult many similar literature, but have not mentioned this compound. Therefore, I personally believe that this compound has never been prepared by other researchers. Later, I successfully prepared this compound through experiments and found through testing that it indeed has strong explosive properties, but sensitivity and other aspects still need further research.
Warning: This energetic material has not undergone strict sensitivity testing and there is no data to prove its sensitivity. However, after a simple test (see below), I personally believe that its sensitivity is moderate, similar to the NiCP mentioned earlier, so it is not recommended to prepare too much.
1. Discussion on raw materials:
Reaction principle: 3CHZ+Ni2++2ClO3- (excess)=Ni (CHZ) 3 (ClO3) 2
① ClO3- Source: The best is of course the chlorate of Ni. However, it is almost impossible to obtain, and chlorates commonly used in the metathesis reaction ions (such as Ca2+, Ba2+, etc.) are also difficult to purchase. So, since it is no longer possible to prepare without introducing other ions and to precipitate NiCC, a high concentration of ClO3- needs to be used. The author used NaClO3 in the preparation, with an excess of about 1.5 times.
② Source of Ni2+: From previous experiments, it has been found that the solubility of nickel tricarbonylhydrazide nitrate (XTN) is relatively high, which may precipitate NiCC. Therefore, the author used nickel nitrate hexahydrate as the source of Ni2+. (Hexahydrate nickel sulfate can also be used, thank you for the experiment with @ Keto_RDX)
③ carbonylhydrazide (CHZ): It can be purchased directly as a chemical raw material.
2. Preparation
Weigh 0.79g CHZ and 1g NaClO3, and dissolve them together with 5ml of water. (No reaction, no need to worry)
Also weigh 0.85g Ni (NO3) 2 • 6H2O and dissolve in 5ml of water.
Attention: After multiple experiments (over ten times), I have found that when the solution concentration is too high, the product precipitates and the beaker becomes very viscous, showing a gelatinous appearance, making it difficult to filter. And the product appears in flakes and will stick to the filter paper, making it inconvenient to collect. A slightly higher amount of water can cause all the products to sink to the bottom (as shown in the figure below), and the production flow has good dispersion.
Freeze more than ten milliliters of distilled water by the way, and wash and use it later.
Using a nickel nitrate solution as the base solution, drip a mixture of sodium chlorate and carbazide under magnetic stirring, and the solution turns blue.
After a while, a small amount of precipitation precipitates.
Place the beaker in an ice bath (-5~-10 ℃) and continue stirring (manual stirring or magnetic stirring can be recommended). At this point, a large amount of precipitates will precipitate and gradually 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, as the solubility of this substance is high and the dissolution rate is fast. When the temperature is slightly high, the precipitation dissolution equilibrium can be quickly reached. Just ordinary filtration time can cause a significant loss of product.
It is difficult for the production rate to exceed 80% during ordinary filtration, and the highest rate for individuals who have done so many times is around 78%, while suction filtration is estimated to exceed 85%
After drying, it becomes a powder with excellent flowability.
3. Testing
① Sensitivity test (extremely rough)
Mechanical sensitivity:
1) Take a very small amount of sample on the aluminum foil, wrap it well, and use a hammer to strike it. Even if struck with force, it is difficult to explode.
2) Take a very small amount of sample onto the brick, stick it with tape, and use a hammer to strike it. Strong tapping can cause an explosion.
3) Same as above, use a hammer to vigorously rub and make a slight "crackling" sound.
Compare it with its brother NiCP:
1) Not done.
2) You can knock it out with a slight force. (subjectively speaking, NiCC is more difficult to be knocked out)
3) Basically the same.
Summary of mechanical sensitivity: NiCC has a moderate mechanical sensitivity, similar to its brother NiCP. Breaking my previous belief that explosives containing chlorates are unstable. In fact, due to crystal structure issues, the sensitivity of NiCP is much higher than expected. This is also why NiCP can only be used for amateur enthusiasts.
Flame sensitivity:
This initiating explosive can be directly ignited by a pen core tube containing KNSU (60-65% KNO3, 35-40% sucrose). The flame sensitivity is high.
3. Limit dosage test:
1) Hammer press 0.5g of 5-ATNO3 with a density of 1.38g/cm3 into an 8 * 6mm 6061 aluminum alloy tube
Insert circular paper slices and pour 60mg (uncompacted, loose) of NiCC onto the surface of the metal can, ignite and ignite.
Due to lack of compaction, the detonation effect is poor, and only the surface of the metal can is concave.
2) Ditto, 0.5g5-ATNO3, press and install using a vise, increase the density of the charge to>1.45g/cm3, use 40mgNiCC and compact with a wooden rod, and also stick it to the surface of the metal can to ignite and detonate.
A violent explosion occurred, and the back of the metal can was also pierced by debris.
The test results show that the initiating ability of this explosive is quite strong, and it can successfully detonate the high-density low sensitivity explosive 5-ATNO3 with a dosage less than 40mg. Based on experience and data estimation, the maximum initiating charge for RDX is less than 30mg, significantly stronger than commonly used initiating charges such as NHN and HMTD.
4. Inspection of chlorate in the product:
After the initial release of this article, it sparked discussions among some enthusiasts and experts, mainly questioning whether the product, especially the anion, is chlorate. I also have doubts about the authenticity of this substance, so in response to these doubts, I attempt to test it.
1) Principle: ClO3-+3NO2-+Ag+=AgCl ↓+3NO3-. Analysis: To precipitate Cl - with Ag+, the first step is to have Ag+, which cannot coordinate with chz, so chz must be oxidized and removed. The second step is to reduce chlorate to obtain chloride ions. The author inspired the idea through the experiment on "Inspection of Chlorine Elements in Matchhead" in the textbook "Experimental Chemistry" published by the Jiangsu Education Press. The use of nitrite to reduce chloride ions and the introduction of impurities (nitrite) are relatively simple to treat.
2) Experiment. Drugs: 1g NiCC, potassium permanganate (medicinal grade), dilute nitric acid (extremely dilute, pH ≈ 2), silver nitrate, sodium nitrite, sodium hydroxide, ethanol (all analytical pure)
Dissolve NiCC in 10ml of water and slowly add potassium permanganate solid under magnetic stirring, emitting a large amount of gas and gradually turning into a dark brown colloidal fluid.
Stop adding potassium permanganate when no gas is emitted. A small amount of ethanol can be added to reduce excess potassium permanganate. At this point, the pH is approximately 8. Add a small amount of sodium hydroxide, adjust the pH to 13-14, maintain strong alkalinity, filter to remove manganese and nickel species, and obtain a colorless treatment solution. Add dilute nitric acid to restore neutrality.
Afterwards, take a sample and add a silver nitrate solution acidified with dilute nitric acid. The solution becomes turbid, and after slight stirring, it dissolves and becomes clear. Suspected to be precipitated with silver chlorate or silver hydroxide.
Add solid sodium nitrite and dilute nitric acid to reduce chlorate. Immediately, a large amount of precipitation occurs, with a small amount of NO2 released, which should be due to the reaction between nitrite and acid. Due to the fact that silver nitrite is also a precipitate, to prevent interference, 30% H2O2 was added and stirred slightly to prevent the precipitation from dissolving.
Due to the hasty nature of the experiment, there was no time to take photos during the process, which will be supplemented in the future. Only one final sedimentation diagram is shown below.
5. Recrystallization
Weigh 0.3g of dried primary product ①, add 3ml of water, stir and dissolve in a water bath at~50 ℃, then place it in an environment at~5 ℃, wait for 2-3 days, and crystal products appear. The macro photos are as follows:
Due to equipment and time constraints, further detailed testing cannot be conducted yet. Detailed data on sensitivity and related explosion data cannot be provided. Further research is needed on this material.


Some photos were not uploaded. If necessary, please contact me and I can send them to your email.

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Microtek - 24-8-2023 at 00:14

Quick update: I tried initiating RDX with CuCP. It failed at 10 mg but succeeded at 20 mg, so the minimum required amount is probably somewhere in the 10-20 mg range. Note that I didn't do a statistically significant number of repetitions, so there is still some uncertainty.

Next will be CoCP, the cobalt analogue.

MineMan - 24-8-2023 at 02:06

Quote: Originally posted by Microtek  
Quick update: I tried initiating RDX with CuCP. It failed at 10 mg but succeeded at 20 mg, so the minimum required amount is probably somewhere in the 10-20 mg range. Note that I didn't do a statistically significant number of repetitions, so there is still some uncertainty.

Next will be CoCP, the cobalt analogue.


Does it compare to NiNQPerchlorate?

More stable less sensitive?

Can ammonium perchlorate be used to make it?

underground - 24-8-2023 at 04:45

I have made NiPerc from Ammonium Perc by this method.
Ca cloride + NaOH --> CaOH (insoluble)
CaOH + NH4 perc --> Ca Perc (stay in solution, unreacted CaOH filtered out)
Ca Perc + Ni Sulphate --> Ni Perc (solution) + Ca Sulphate (insoluble)

Copper Sulphate can also be used for Copper Perch.

Ba Perc can also be used since Ba Sulphate is insoluble too.


Since NiCP seems to be very insoluble in water, maybe it can also be prepared from K perch.
For example: Ni Carb Nitrate + K perc --> KNO3 + NiCP

[Edited on 24-8-2023 by underground]

Microtek - 24-8-2023 at 09:42

I made it from NaClO4, so I'm sure NH4ClO4 would work as well. As stated above, CuCP is a little less powerful than NAP while NiCP is close enough that I can't tell the difference. In terms of sensitivity, check out my examinations above. The objective here is to find a primary that is comparable to NAP in terms of power and insensitivity, but less likely to generate hyper-toxic gases on detonation. I'm sure that using nickel based primaries outdoors would be unproblematic, but I do a fair number of indoor tests, and given that nickel tetracarbonyl is toxic at concentrations of just a few ppm, I would like to not gamble that the equilibria doesn't favour the formation.

Microtek - 29-8-2023 at 08:54

OK, a new update:

The cobalt derivative CoCP seemed very promising at first. Low sensitivity (like the others) very high power when heated in Al foil, non-hygroscopic, sensitive to flame from fuse and DDTs in small amounts with little containment. However, when I did initiation tests, it didn't perform so well. I had multiple failures from ca. 20 mg loadings on 5mm coloumns of RDX.

I have since turned towards the iron derivative, FeCP. It behaves a little strangely during synthesis, and I suspect that the iron(III) ions that I have been using are oxidizing the carbohydrazide. The iron(II) that is formed is probably what is precipitating as the energetic complex in the form of (suprisingly) white, needle shaped crystals. I have only done very preliminary testing, but it seems very powerful indeed. It detonates in sub-milligram amounts in the open on flame contact. I can't comment on sensitivity yet, but will report when I have new findings.

littlesky - 29-8-2023 at 19:24

Quote: Originally posted by Microtek  
OK, a new update:

The cobalt derivative CoCP seemed very promising at first. Low sensitivity (like the others) very high power when heated in Al foil, non-hygroscopic, sensitive to flame from fuse and DDTs in small amounts with little containment. However, when I did initiation tests, it didn't perform so well. I had multiple failures from ca. 20 mg loadings on 5mm coloumns of RDX.

I have since turned towards the iron derivative, FeCP. It behaves a little strangely during synthesis, and I suspect that the iron(III) ions that I have been using are oxidizing the carbohydrazide. The iron(II) that is formed is probably what is precipitating as the energetic complex in the form of (suprisingly) white, needle shaped crystals. I have only done very preliminary testing, but it seems very powerful indeed. It detonates in sub-milligram amounts in the open on flame contact. I can't comment on sensitivity yet, but will report when I have new findings.

Do not try iron (III) compounds as they are extremely dangerous. It has been reported that related compounds may cause self explosion accidents. When synthesizing other compounds, efforts should also be made to avoid mixing iron (III) ions, otherwise it can lead to extremely serious accidents.

littlesky - 29-8-2023 at 19:27

Quote: Originally posted by Microtek  
OK, a new update:

The cobalt derivative CoCP seemed very promising at first. Low sensitivity (like the others) very high power when heated in Al foil, non-hygroscopic, sensitive to flame from fuse and DDTs in small amounts with little containment. However, when I did initiation tests, it didn't perform so well. I had multiple failures from ca. 20 mg loadings on 5mm coloumns of RDX.

I have since turned towards the iron derivative, FeCP. It behaves a little strangely during synthesis, and I suspect that the iron(III) ions that I have been using are oxidizing the carbohydrazide. The iron(II) that is formed is probably what is precipitating as the energetic complex in the form of (suprisingly) white, needle shaped crystals. I have only done very preliminary testing, but it seems very powerful indeed. It detonates in sub-milligram amounts in the open on flame contact. I can't comment on sensitivity yet, but will report when I have new findings.

haha,Cobalt salt is indeed not a good choice. Currently, there are detonator factories using zinc salt as the primary explosive. Zinc salt is weaker than nickel salt, but safer. All of these compounds have strong initiation ability.

Laboratory of Liptakov - 29-8-2023 at 22:48

If the factories are using zinc carbohydrazide perchlorate, it will probably be a good choice.....:cool:

Microtek - 29-8-2023 at 23:01

My procedure for preparing and testing energetics is not vulnerable to accidental or even spontaneous detonation at any point. Therefore, I will not refrain from experimenting based on anecdotal "evidence", especially since your last warning was false, but I will of course treat it as carefully as any other untested (by me) primary.
Also, I don't have a lot of confidence in the professional chinese energetics community given all the recent papers with obvious, serious errors and lack of basic understanding.

smithdotyu - 5-9-2023 at 03:05

I made some NiCC for my home made strontium chlorate.

when strontium chlorate is pure the product color is blue-white.

when strontium chlorate not pure the product color is blue like sky.

both them can DDT when use a green fuse. but some time can't DDT, the success rate maybe 90%. high than CuNH4NT

CuNH4NT is more cost time to make.....


smithdotyu - 5-9-2023 at 03:08

I think this compound should have a Chinese short name:

GTN ---- gao tan nie

LTN ---- lv tan nie

littlesky - 6-9-2023 at 06:50

Quote: Originally posted by smithdotyu  
I made some NiCC for my home made strontium chlorate.

when strontium chlorate is pure the product color is blue-white.

when strontium chlorate not pure the product color is blue like sky.

both them can DDT when use a green fuse. but some time can't DDT, the success rate maybe 90%. high than CuNH4NT

CuNH4NT is more cost time to make.....


The name source of NiCC: Ni, nickel element, the first C stands for carbohydrazide, and the second C stands for chlorate ion. This is named after the NiCP analogy. According to this rule, your compound should be named SrCC. My friends and I have never tried alkaline earth metal complexes. You can do more experiments and participate in the discussion.::D

littlesky - 6-9-2023 at 07:05

Quote: Originally posted by smithdotyu  
I think this compound should have a Chinese short name:

GTN ---- gao tan nie

LTN ---- lv tan nie

Haha,You are right. :DNiCP=GTN=高氯酸(三)碳酰肼合镍.
Among this compounds, "G" stands for "高氯酸根(gao lv suan gen, ClO4-)", "T" stands for "碳酰肼(tan xian jing, CHZ)" and "N" stands for "镍(nie,Ni)". But I don't know why, I think the name LTN is very strange, so I use NiCC for analogy with English abbreviations.

smithdotyu - 6-9-2023 at 18:43

Quote: Originally posted by littlesky  
Quote: Originally posted by smithdotyu  
I made some NiCC for my home made strontium chlorate.

when strontium chlorate is pure the product color is blue-white.

when strontium chlorate not pure the product color is blue like sky.

both them can DDT when use a green fuse. but some time can't DDT, the success rate maybe 90%. high than CuNH4NT

CuNH4NT is more cost time to make.....


The name source of NiCC: Ni, nickel element, the first C stands for carbohydrazide, and the second C stands for chlorate ion. This is named after the NiCP analogy. According to this rule, your compound should be named SrCC. My friends and I have never tried alkaline earth metal complexes. You can do more experiments and participate in the discussion.::D



I just use strontium chlorate replace sodium chlorate. The strontium chlorate produced by use MMO anode electrolysis. first time i use KClO3 to make NiCC. it's failed. I got some blue powder. burn fast but can't DDT. than i start to electrolysis make strontium chlorate. after a few days later i got some strontium chlorate . than the make the steps is same as yours.

littlesky - 6-9-2023 at 19:46

Quote: Originally posted by smithdotyu  
Quote: Originally posted by littlesky  
Quote: Originally posted by smithdotyu  
I made some NiCC for my home made strontium chlorate.

when strontium chlorate is pure the product color is blue-white.

when strontium chlorate not pure the product color is blue like sky.

both them can DDT when use a green fuse. but some time can't DDT, the success rate maybe 90%. high than CuNH4NT

CuNH4NT is more cost time to make.....


The name source of NiCC: Ni, nickel element, the first C stands for carbohydrazide, and the second C stands for chlorate ion. This is named after the NiCP analogy. According to this rule, your compound should be named SrCC. My friends and I have never tried alkaline earth metal complexes. You can do more experiments and participate in the discussion.::D



I just use strontium chlorate replace sodium chlorate. The strontium chlorate produced by use MMO anode electrolysis. first time i use KClO3 to make NiCC. it's failed. I got some blue powder. burn fast but can't DDT. than i start to electrolysis make strontium chlorate. after a few days later i got some strontium chlorate . than the make the steps is same as yours.

oh,sorry,I misunderstood you earlier. l think that strontium ions will also coordinate with CHZ, resulting in impure products, which may be the reason for the failure of DDT. But you can also try chlorate of CHZ strontium (or other alkaline earth metal salts), which I guess is very interesting.

littlesky - 7-9-2023 at 02:42

In my test, nicc showed more power than NiCP(GTN) and NaCuNT. These are three test videos. Obviously, the order of strength is NICC > NICP (GTN) > Nacunt. I didn't synthesize NH4NT but NaNT, so I only did the test about NaCuNT. However, the strength of these two compounds should be similar, and even Na salt will be more powerful than ammonium salt, because NH4+ ion decomposition will absorb heat.

Attachment: GTN test.mp4 (2.9MB)
This file has been downloaded 168 times

Attachment: NiCC test.mp4 (3MB)
This file has been downloaded 174 times

Attachment: NaCuNT test.mp4 (839kB)
This file has been downloaded 153 times


littlesky - 7-9-2023 at 02:45

I will test AgNT in the same way these days.AgNT is more powerful than NaCuNT (or NH4CuNT).

Microtek - 7-9-2023 at 03:43

Well, from reading some more papers, it appears that at least magnesium (and probably other alkaline earths) does indeed form a complex with CHZ contrary to my admittedly limited understanding of complex chemistry.


Quote:

But I don't know why, I think the name LTN is very strange, so I use NiCC for analogy with English abbreviations.


That is much appreciated. It can be very confusing with acronyms that don't match the words you use. A case in point is the DPT thread where DNU means hexamine dinitrate...

I tested ZnCP for sensitivity in my oblique abrasive impact test, and got 1 positive in 5 attempts at 100 cm. This is almost exactly the same as NAP. ZnCP is not very flame sensitive and while it does burn, it does not flash like most of the other complexes.

[Edited on 7-9-2023 by Microtek]

B(a)P - 7-9-2023 at 12:29

Quote: Originally posted by littlesky  
In my test, nicc showed more power than NiCP(GTN) and NaCuNT. These are three test videos. Obviously, the order of strength is NICC > NICP (GTN) > Nacunt. I didn't synthesize NH4NT but NaNT, so I only did the test about NaCuNT. However, the strength of these two compounds should be similar, and even Na salt will be more powerful than ammonium salt, because NH4+ ion decomposition will absorb heat.


How much test material do you have in each of those little sleeves for each of your tests?

littlesky - 7-9-2023 at 15:29

Quote: Originally posted by B(a)P  
Quote: Originally posted by littlesky  
In my test, nicc showed more power than NiCP(GTN) and NaCuNT. These are three test videos. Obviously, the order of strength is NICC > NICP (GTN) > Nacunt. I didn't synthesize NH4NT but NaNT, so I only did the test about NaCuNT. However, the strength of these two compounds should be similar, and even Na salt will be more powerful than ammonium salt, because NH4+ ion decomposition will absorb heat.


How much test material do you have in each of those little sleeves for each of your tests?

This is a test method from an expert in the field of high-energy materials. Use a capillary tube with one end sealed (internal diameter 0.9mm-1.1mm) for explosion test.
Charge length:
GTN 2.2CM
NiCC 2.0CM
NaCuNT 2.3CM
I didn't weigh the specific charge weight, because my electronic scale is not accurate in micro-weighing. You can estimate for yourself.

littlesky - 7-9-2023 at 15:30

Who can help me measure the density of NiCC under different pressures?:D

littlesky - 4-10-2023 at 17:02

Has anyone made any progress?

MineMan - 5-10-2023 at 03:19

Idk. Hey buddy disappeared….

Microtek - 5-10-2023 at 22:14

I have tested ZnCP and found that it DDTs nicely when fired by fuse (and so presumably electric match) but not by the flash of gun cotton, and not by electric arc. It does not flash in the open. It is not significantly less sensitive in the oblique abrasive impact test than NiCP, NAP or CuCP.

For the specific niche of repeated indoor testing, I have concluded that CuCP is most desirable, the only drawback being the apparently higher water solubility which means that the yield of the reaction is maybe not quite as high as it could have been. I have not examined the yield quantitatively, it is just based on the observation that the mother liquor was strongly coloured after addition of carbohydrazide addition and precipitation of CuCP (after cooling overnight).

underground - 8-10-2023 at 05:35

Microtek could you also give a try for Chlorate salts? Barium Chlorate is much easier to buy and cheaper too than perchlorates. Barium sulphate is insoluble so any chlorate salt can be made. ZnCC CuCC CoCC are few that comes to my mind. Ni salts are super toxic and nasty, i really dont want to deal with.

Microtek - 10-10-2023 at 04:46

Hmm, I don't think I can buy barium chlorate (or any other chlorate for that matter), but I can prepare some sodium chlorate by thermal disproportionation of hypochlorite. I don't like working with chlorates but I could probably examine a small amount of these complexes.

Hey Buddy - 15-10-2023 at 16:19

Quote: Originally posted by MineMan  
Idk. Hey buddy disappeared….


Sorry, CPU died and I lost my password. Found it on a piece of paper today...

--So what are the thoughts on this material? My initial thought is carbohydrazide could be a good fuel if its preparation is easy... Ive never attempted to synth it. I dont know of any OTC sources of carbohydrazide. I believe it used to be used as an oxygen scavenger for boilers. I have searched a little in hardware stores and havent had any luck finding it in anything. In that case synthesis is important. So is there any successful methods for lab scale synthesis? Has anyone tried the numerous patent procedures? AGu is slightly annoying from reduction of NQ but not really that bad... Is CHZ easy?