Guanidine Nitrate preparation

in this video we prepare guanidine nitrate from ammonium nitrate,urea and silica gel.
the three chemicals are dried,mixed and heated for several hours with the resultant cake of solids extracted with water and crystallized. we then filtered with some difficulty after spending the night in the fridge.
we recrystallized the crude product ready for the next step.
we will turn this into Nitroguanidine and then use zinc metal in glacial acetic acid in a reduction process to Aminoguanidine.

[@MehranAzari-hn8ut]

In this test, there is a total of 160 grams of urea or 220 grams because 60 grams are added in the last step. If as you show in the video, 100 grams of urea should be mixed first and the remaining 60 grams should be added in the last step. Otherwise, a total of 220 grams. Urea should be used. Thanks for your advice

[@mandra3768]

According to SM it is 160 total, so 100 + 60

[@vivekkumarsingh4226]

Awesome job

[@schinderiapraemeturus6239]

thanks for sharing. the problem with this method is yield sucks, 20-30% of theoretical because large amounts of NH3 and CO2 (potential product) is wasted/evolved in the heating process a better method is US patent 3,009,949 (1961) which describes heating ammonium metaphosphate (DAP) with urea (1 to 1.2 ratio) at 250-280C for approximately an hour. the residue is a moiety of guanidine ortho&pyro phosphates that is extracted in hot water, filtered-then filtrate is reacted with the corresponding mineral acid to produce the desired guanidine salt. Cheers

[@karolus28]

cool. though isnt DAP ammonium ortophosphate? and where do i get and how do I make ammmonium metaphosphate(or is it the same as polyphosphate?)

[@fudes587]

at what temperature can it explode?

[@laboratoryofliptakov8157]

Is possible use instead silica gel for example glass microballoons, or white pure sand ? Are some a next variants for this physically inert catalyseur ? Thanks.:-)

[@accipiternisus649]

Treat water glass with sulfuric acid

[@arachnidadocumentary6159]

What if the ammonium nitrate isnt dry?

[@cobalt7530]

But wouldn't it be possible to use other ammonium salts like ammonium chloride to avoid the risk of explosion? Wouldn't you get guanadinium chloride then?

[@sazxcdewq123]

There is no other ammonium salt which melts instead of sublimating or decomposing.

[@Preyhawk81]

I prefer the Oxydation of dicyandiamid with HNO3 and HCL. You only Need 50 % nitric acid and ist much safer than melting an explosive.

[@AllChemystery]

Ulrich Hager the point of making this was a precursor to aminoguanidine bicarbonate. This is further reacted to make 5-amino tetrazole. If I had dicyandiamide I would just use this with NaN3 instead.

[@Preyhawk81]

You ve made in an other Video calciumcyanamid. You can make your Dicyandiamide from it. :)

[@midwestchem368]

Great video loved it! What is the name of the song that started towards the beginning of the video??

[@cannagorilla]

I thought you needed sulfonic acid?

[@astreliousrx6662]

i have tryed this pretty much , but everytime was no satisfacting yield

[@realedna]

Have you tested the product somehow? (e.g. melting point)
What is your source of information for this procedure? (SM, patent, paper, ...)

[@AllChemystery]

realedna there’s a patent here: www.google.com/patents/US4390726
And a thread from an SM member which was eventually put in the prepublication section. :I www.sciencemadness.org/talk/viewthread.php?tid=12938#pid184212
followed these as a guide so my product had to be The guanidine nitrate. The only test was that it was dehydrated to nitroguanidine later which was easily identified by its crystal structure and a M.P test on that product which came very close to a pure product.

[@markharder3676]

What''s the function of the silica gel? Is there a method by which you can buy guanidine and begin with that instead of urea? By acidifying with HNO3 for example?

[@joshenns2957]

You can just buy aminoguanidine bicarbonate directly from a supplier. If tetrazoles are your end goal that is. I got 500 grams for 50 bucks and that saved me lots of time preparing it.

[@markharder3676]

@@joshenns2957 Thanks, Josh.

[@cannagorilla]

Can you use silica gel from dsilicate that you get with new shoes.

[@AllChemystery]

cannagorilla sodium silicate- water glass. If you add sulfuric acid to this you will get silica which needs to be dried. I used crystals of silica cat litter. It's cheaper.

[@cannagorilla]

AllChemystery Thank you!

[@namenloseheld1469]

Is Guanidine Nitrate hygroskopic?

[@AllChemystery]

No. Not noticeably anyway.

[@namenloseheld1469]

@@AllChemystery Are there any "easy" ways to synthesize Guanidine Carbonate, mainly also based on Urea?

[@michaelf7093]

What is your thermocouple probe in?

[@AllChemystery]

Michael F an easy ld glass pipettes which I sealed at one end with a blow torch.

[@michaelf7093]

Good idea!

[@sargon6000]

Will ammonium sulfate work instead of ammonium nitrate?

[@AllChemystery]

Yes it should. You will get guanidine sulfate instead of nitrate though.

[@sargon6000]

Well, I mainly need a guanidine source, not a specific salt of it.

[@cannagorilla]

Chemical Engineer check out NerdRage's channel. I got my Guanidine Carbonate his way. 4$ for 20g

[@aritsa3946]

How to convert guanidine sulphate into nitroguanidine?

[@Glucoperon]

@@aritsa3946 add it into an ammonium nitrate sulfuric acid mix and let stir for 12 hr at room temp. pour the solution into cold water and it should drop out.

[@amarissimus29]

Frit abuse. That's painful.

[@sazxcdewq123]

Will silica cat litter work?

[@AllChemystery]

I need a better username this is what I used. Works well.

[@sazxcdewq123]

Question: Did you ever filmed TNT synthesis? I remember a video with pretty white crystals.

[@AllChemystery]

I need a better username yes. It's on my Vimeo channel.

[@JW-zs9bk]

:)

[@andrej552]

Try to make nitroguanidine nitrate

[@jangisgand6140]

Брюс Ли are you fucking stupid?

[@turningnull2538]

Bro, ANQN Vod=9551m/s. Very energetic

[@mahamimran1424]

It is the sweetest substance in the world that 300,000 times sweeter than sucrose.

[@marciaosullivan3200]

No it fucking isn't