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Author: Subject: Synthesis of Oxygen Absorbing Crystal (from cobalt)
SupaVillain
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[*] posted on 13-4-2015 at 07:48
Synthesis of Oxygen Absorbing Crystal (from cobalt)


Ok guys, that new crystal they discovered from cobalt is crazy useful, some number liters (prolly a few) can suck up all the oxygen out of a room and can hold three times as much as a high pressure oxygen tank.

so obviously i want to make it.

The name of it is:

"*If you must know, the chemical name of the salt is written out as {(bpbp)Co2II(NO3)}2(NH2bdc)2 * 2H2O, where “bpbp” stands for 2,6-bis(N,N-bis(2-pyridylmethyl)-aminomethyl)-4-tert-butylphenolato, and “NH2bdc2” stands for 2-amino-1,4-benzenedicarboxylato). Don’t ask us how to pronounce all that."

If you can tell me how to make this... i will make it and provide pretty pictures and advice on my experience. And if i can make a lot, I will certainly sell it to you. I have some experience with chemistry and hard determination to learn and accomplish but I start to get distant when the names are longer than my attention span LOL

even if i need industrial equipment i have a shop to make all that in
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Loptr
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[*] posted on 13-4-2015 at 07:59


Are you referring to this?

http://pubs.rsc.org/en/Content/ArticleLanding/2014/SC/C4SC01...
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SupaVillain
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[*] posted on 13-4-2015 at 08:16


Yes it is! i saw a patent but was going to find a day off from work to rent it and do a bunch of research on it. Most of the time synthesis is written out in patents, hopefully this one is too.

[Edited on 13-4-2015 by SupaVillain]
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cmos6667
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[*] posted on 13-4-2015 at 09:44


relevant username much?! don't make me regret this ;)


Edit(woelen): Cmos6667 asked me to remove downloadable file, due to copyright issues.

[Edited on 16-6-15 by woelen]
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SupaVillain
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[*] posted on 13-4-2015 at 09:56


LOL i dont know of much evil i can do with oxygen crystals. These may prove to help much in firefighting to starve fires of oxygen and make safer and cheaper oxygen tank setups for the firefighters.
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cmos6667
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[*] posted on 13-4-2015 at 10:01


right, that's what I thought! but seriously though, this could be useful for making inert environment for reactions
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Loptr
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[*] posted on 13-4-2015 at 11:13


Quote: Originally posted by cmos6667  
right, that's what I thought! but seriously though, this could be useful for making inert environment for reactions


And this is what I thought as I read the abstract. I was looking into different methods for deoxygenating various solvents a while back, and this might be something of interest.

EDIT: Also, possibly as a source of oxygen if the complex could readily release it in a controlled manner.

[Edited on 13-4-2015 by Loptr]
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Praxichys
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[*] posted on 13-4-2015 at 12:01


Might be a good media replacement for PSA-based oxygen concentrators, especially for generating near-100% oxygen. It could have applications in many industries - imagine a self-regenerating low pressure oxygen tank. Long-lasting rebreathers, self-regenerating welding equipment, oxygen storage for submersibles and hypoxic, high-altitude environments...



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Dr.Bob
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[*] posted on 13-4-2015 at 12:07


They show that they can release it simply by heating. The system does look great for both removing oxygen from gases for inert streams (like glove boxes), as well as oxygen concentrators, like what old people with CPOD and emphysema use to breath.
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cmos6667
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[*] posted on 13-4-2015 at 12:21


it takes upwards of 24h to absorb oxygen and that oxygen is released upon heating, so I highly doubt your idea for fire extinction.
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SupaVillain
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[*] posted on 13-4-2015 at 18:00


HMMMMMM okay well that sucks that means it cant be used to knock people in a room. Well as far as the 24 hour figure for absorption... how much are we talking???? I dont care if it takes 24 hours if over that span of time it could do a whole airgas truck of oxygen cylinders! Either way im sure i wont care sinve its way cheaper than an oxygen concentrator and the whole setup
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cmos6667
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[*] posted on 13-4-2015 at 23:50


Here's what you could do: you know how cigarettes have a lot of tar and ash? That's because of incomplete combustion - increase the oxygen and voilà, low tar cigarettes ;)
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Oscilllator
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[*] posted on 14-4-2015 at 02:44


Quote: Originally posted by cmos6667  
Here's what you could do: you know how cigarettes have a lot of tar and ash? That's because of incomplete combustion - increase the oxygen and voilà, low tar cigarettes ;)

I think this would cause the cigarette to burn vigorously even when you aren't sucking on it, rather than eliminate the tar. Still though, I imagine it would be amusing to try.
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Tsjerk
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[*] posted on 14-4-2015 at 07:16


Besides the sigaret vigorously burning, also the nicotine would burn...
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cmos6667
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[*] posted on 14-4-2015 at 07:21


or maybe isolate the nicotine, then nitrate the hell out of the cellulose, then put the nicotine back
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Metacelsus
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[*] posted on 14-4-2015 at 08:48


That's not how you make exploding cigarettes.



As below, so above.

My blog: https://denovo.substack.com
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MrHomeScientist
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[*] posted on 15-4-2015 at 05:40


Replace the tar with volatile {(bpbp)Co2II(NO3)}2(NH2bdc)2 * 2H2O! That sounds like a great idea!

I would be amazed if someone could make this at home.
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SupaVillain
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[*] posted on 15-4-2015 at 06:02


Im really confused here, the main chemical discussed is {(bpbp)Co2II(NO3)}2(NH2bdc)2 * 2H2O, but only synthesis for ones ending with 18, 12, 11, 15, 5H20's and a MeOH one are included. Are these more useful variations of the crystal? Which one is the most useful for oxygen purposes? Or am I supposed to know how to further turn these things into {(bpbp)Co2II(NO3)}2(NH2bdc)2 * 2H2O????????
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SupaVillain
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[*] posted on 15-4-2015 at 19:31


Pls halp
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Steam
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[*] posted on 16-4-2015 at 05:46


Supa Villan, a more detailed documentation of synth is on the last two pages of document. Here is the beginning of it. You are going to need bpbpH which I think stands for bipyrrolidine, but I am not 100% sure. You could easily look it up, after all you have access nearly infinite information right at your fingertips! :)



Screen Shot 2015-04-16 at 8.40.50 AM.png - 123kB




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SupaVillain
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[*] posted on 16-4-2015 at 11:47


My issue is that each of the bold text names on the synths are different compounds, unless Im wrong, I dont know which one to choose but I guess I'll just go with the easiest one, they said also that two of them are slower to absorb oxygen than the rest.

At least cobalt nitrate hexhydrate is cheap and easy to obtain off of ebay.
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Consequence
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[*] posted on 16-4-2015 at 15:20


Sorry I can't login as SupaVillain, password issues and not receiving emails within temp password....:(

anyways I've found the synthesis for bpbpH,(aka Hbpbp?) which is necessary for pretty much all the syntheses.


bpbpH SYNTHESIS

2,6-Bis{[bis(2-pyridylmethyl)amino]methyl}-4-tert-butylphenol,
Hbpbp
4-tert-Butylphenol (1.994 g, 0.0133 mol) and p-formaldehyde
(1.55 g, 0.0517 mol) were suspended in ethanol (25 cm3
). A
solution of N,N-bis(2-pyridylmethyl)amine (10.0 g, 0.0503 mol)
in H2O (50 cm3
) was added and the slightly yellow suspension
was stirred at reflux temperature for 3 d. The two-phase reaction
mixture was allowed to cool to room temperature and was
then partitioned between CH2Cl2 (200 cm3
) and H2O (100 cm3
).
The aqueous phase was extracted with CH2Cl2 (3 × 50 cm3
) and
the combined organic phase dried over anhydrous Na2SO4.
After removal of the solvent, the resulting brown oil was chromatographed
on a silica gel column using acetone as eluent
affording the crude product (5.86 g, 77% yield) as a slightly
yellow solid (m.p. = 122–126 8C). Recrystallization from diethyl
ether–light petroleum resulted in the pure product as white
crystals (60% relative to the crude product, m.p. = 123 8C). 1
H
NMR (250 MHz): d 1.27 (s, 9 H), 3.82 (s, 4 H), 3.90 (s, 8 H),
7.08 (m, 4 H), 7.19 (s, 2 H), 7.48–7.61 (m, 8 H), 8.52 (m, 4 H),
10.80 (s, 1 H). 13C-{1
H} NMR (62 MHz): d 31.57 (s), 33.85 (s),
55.12 (s), 59.88 (s), 121.81 (s), 122.84 (s), 123.16 (s), 125.85 (s),
136.33 (s), 140.79 (s), 148.83 (s), 153.43 (s), 159.39 (s) (Found:
C, 75.49; H, 7.04; N, 14.67. Calc. for C36H40N6O: C, 75.23; H,
6.96; N, 14.48%). FAB mass spectrum: m/z 572 (0.5, M1), 93
(100%, C5H4NCH2
1)

(from "Dinuclear iron(III)–metal(II) complexes as structural core models for
purple acid phosphatases †"
Morten Ghiladi, Christine J. McKenzie, Anke Meier, Annie K. Powell, Jens Ulstrup, and Sigrid Wocadlo
J. Chem. Soc., Dalton Trans., 1997, Pages 4011–4018)
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DFliyerz
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[*] posted on 8-6-2015 at 07:59


I've recently started work on synthesizing one of these crystals, and I think that I've figured out a pretty good method. I have yet to test it since I'm waiting on my distillation apparatus to arrive so I can make nitric acid, but the general idea of the synthesis is simple. The two more complex chemicals required for the easiest synthesis in the document are disodium terephthalate, which can be made by the "PET to terephthalic acid" method by Chromium, and cobalt nitrate, of which the synthesis is pretty obvious. I have some pieces of PET bottle cut up and ready to process, and I'll make cobalt nitrate from cobalt carbonate as soon as I can make nitric acid. I'll be sure to report back here once I do it. A synthesis for a possibly better crystal could be done by nitrating terephthalic acid and reducing the nitro group. I'll likely test both, but definitely the one with disodium terephthalate first. EDIT: Forgot about the bpbpH! I'll look into that.

[Edited on 6-8-2015 by DFliyerz]
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Mrinny
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[*] posted on 15-12-2017 at 10:17


Hey @DFliyerz

Any progress with the synthesis? How far did you come along? Did you stop midway? Any updates will be cool.
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Xiomy
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[*] posted on 20-1-2018 at 09:06


Hello, I need to make the synthesis of these crystals in the university, all the information here has helped me a lot to know where to start, but I would like to have more help from you if possible.

Thank you, good day.
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