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ManyInterests
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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?
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Microtek
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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).
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underground
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What about the nitrate salts
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Microtek
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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.
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Microtek
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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.
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MineMan
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Try the copper microtek.
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Microtek
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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]
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MineMan
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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.
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littlesky
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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.
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littlesky
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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.
Attachment: phpzCAI6L (247kB)
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Attachment: phpBacTwT (268kB)
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Microtek
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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.
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MineMan
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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?
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underground
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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]
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Microtek
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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.
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Microtek
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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.
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littlesky
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| 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.
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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.
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littlesky
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| 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.
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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.
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Laboratory of Liptakov
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If the factories are using zinc carbohydrazide perchlorate, it will probably be a good choice.....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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Microtek
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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.
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smithdotyu
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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.....
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smithdotyu
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I think this compound should have a Chinese short name:
GTN ---- gao tan nie
LTN ---- lv tan nie
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littlesky
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| 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.....
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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.:
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littlesky
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Haha,You are right. NiCP＝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.
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smithdotyu
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| 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.: |
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.
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littlesky
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| 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.....
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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.: |
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.
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