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Author: Subject: High Test Hydrogen Peroxide (catalytic)
symboom
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[*] posted on 16-6-2017 at 13:55
High Test Hydrogen Peroxide (catalytic)


Step 1
Concentration of 3% to 30 %
https://m.youtube.com/watch?v=5dPTtOimdzk

15%hydrogen peroxide
The clear outer liquid in a glow stick

30% hydrogen peroxide
Pharmacy
Hydroponics
Hair salon(beauty supply)

Step 2
Vaccum distillisation
IMG_20160125_181616.jpg-thumb.jpg - 16kB
The water goes into the one way valve at the end of the tube.
Hydrogen Peroxide is left behind

http://www.sciencemadness.org/talk/viewthread.php?tid=64146


Google search for anhydrous Hydrogen peroxide
Or High test Peroxide has interesting patents

Method 1
Extraction with p-cymene

http://www.prepchem.com/synthesis-of-hydrogen-peroxide/

80-90% hydrogen peroxide starting material can also be obtained by mixing 30% hydrogen peroxide solution with twice its amount of p-cymene.
____________________________
Method 2
Extraction with serine

https://www.researchgate.net/publication/232377047_Preparati...

The adduct of hydrogen peroxide and serine is unstable in these organic solvents
________________________
Method 3
Extraction with Boric acid alcohol ester

http://www.freepatentsonline.com/2386484.html
https://www.google.com/patents/US2386484

Experimental
As stated from
http://www.sciencemadness.org/talk/viewthread.php?tid=14750

Fairly concentrated H2O2 can be prepared by treating a thick suspension of zinc peroxide with H2S, then filter off the ZnS formed.

Another link
http://www.sciencemadness.org/talk/viewthread.php?tid=1325


Experimental

Urea/peroxide adduct
Add citric acid form
Hydrogen peroxide and urea citrate percipitate.

And urea citrate is supposedly insoluble and not destructive to hydrogen peroxide


Urea peroxide and citric acid is a solid and water is added to leach out the peroxide and drive to precipitation reaction of urea citrate

Not sure if this could work in absolute ethanol without reacting
Ethanol has a lower boiling point the pure hydrogen peroxide.

[Edited on 17-6-2017 by symboom]




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Natures Intellectual Organic Peroxide. >>Ascaridole <<
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Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
Sodium had its fame long enough time for Calcium
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[*] posted on 16-6-2017 at 19:20


The extraction with cymene seems quite interesting as apparently cymene can be prepared by boiling together limonene and sulfur, both of which are readily available. I've attached a paper that may help if someone wants to go down this route.


Attachment: cymene from limonene and sulfur.pdf (1.3MB)
This file has been downloaded 204 times

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[*] posted on 17-6-2017 at 07:12


needing alot of peroxide
Making this various inorganic peroxides
Peroxide is mixed with each to form the corresponding peroxide dont need high test peroxide for it but why not.

Lithium peroxide
LiOH
Magnesium peroxide
MgO
Calcium peroxide
CaCl2 +NH3
Copper peroxide
CuSO4 + NH3
Zinc Peroxide
ZnO

Finally a lead

Describing use of organic solvents to make anyhydrous solution so the using ethyl ether for extraction was actually true

First google search
ether and sodium percarbonate concentrated peroxide
Long link sorry

Titled safe use of hydrogen peroxide in the organic lab

PDF
https://www.google.com/url?sa=t&source=web&rct=j&...

Solutions of H2O2 in organic solvents: Hydrogen peroxide has good solubility in many organic
solvents and experimenters unable to access the highly concentrated (e.g., 90% or ~25-30M)
grades of H2O2 described in many procedures for synthesis of peracids or alkyl hydroperoxides,
15 have sometimes turned to "anhydrous" solutions available by extraction of 30 or 50% aq. H2O2
into ether or dichloromethane, followed by drying over Na2SO4 or MgSO4.
These solutions, which can be up to 3M in peroxide, should be considered inherently unstable. Our group has
frequently prepared these solutions, but rarely on volumes greater than 10 mL. Ethereal solutions of H2O2 should never be concentrated or stored, but immediately consumed or
quenched. A recent article describes safety issues related to generation and ignition of O2 head
gas within organic solutions of H2O2.
Attempts to further concentrate ethereal solutions of H2O2 through evaporation or distillation
represent needless hazard; distillations in particular have been shown to be ineffectual in
generating pure material. A recently described alternative involves dissolution of amino acid
perhydrates into organic solvents.


[Edited on 17-6-2017 by symboom]

[Edited on 17-6-2017 by symboom]




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Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
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[*] posted on 17-6-2017 at 07:23


I wonder if there is any possibility of creating undesirable amounts of phosgene if extracting with DCM.



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[*] posted on 18-6-2017 at 20:38


hydrogen peroxide from glow sticks is desolved in an organic layer it doesnt want to react with anything I even added permnganate to it Its like the organic compound protects the peroxide from attack also it doesnt free the peroxide easily I added it to bleach added it to copper sulfate still no reaction
Unless the concentration is very low
It was bubbling but only at the boundary layer


Next up add hydrogen peroxide to it maybe I can absorb the hydrogen peroxide out of a 3% solution and see if I can get urea to desolve in it to form urea peroxide Also need a solvent to blend the two layers together maybe I will add ethanol or ethylene glycol

I appologize my post are long I want to be covering as much as I can experimently as well as cover the topic completely

This photo is my attempt to use the hydrogen peroxide from the glow stick to make copper peroxide blue solution is tetramine copper peroxide
IMG_20170618_211949.jpg - 3.8MB

Quoting nitro-genes
http://www.sciencemadness.org/talk/viewthread.php?tid=971&am...

yield of hydrogen peroxide on basis of percarbonate is not that high, but the precess works, even with 30% percarbonate laundry cleaner. Basically, you neutralize the percarbonate with 37% sulfuric acid at room temperature in a large container while stirring, until most of the percarbonate has dissolved, liberating the hydrogen peroxde. Then you filter out the undissolved carbonate/percarbonate and add an equal volume of ethanol or methylated spirits and put it overnight in the freezer, this will precipitate almost all of the sodium sulfate as a hydrate (the loss of hydrogen perxoide due to forming an adduct with the sodium sulfate is unknown, but probably existent). It is important that the solution is near neutral (or better, slightly acidic to stabilize the H2O2), since sodium hydrogen sulfate will refuse to precipitate and the ethanol will just form an unmixed layer on top of the HSO4 solution. After some mixing and overnight cooling, the massive amount of sodium sulfate hydrate formed is filtered out and the solution boiled to drive off most of the ethanol. The hydrogen peroxide solution formed can probably be used for most reactions, long term stability unknown.



IMG_20170619_164516.jpg - 2.8MB IMG_20170619_185341.jpg - 2.7MB

Adding 3% hydrogen peroxide to the organic layer of the hydrogen peroxide glow stick as you can see the organic layer did not absorb the hydrogen peroxide solution the peroxide solution from the glow stick went into the hydrogen peroxide layer I think more concentrated hydrogen peroxide formed there is a bit of turbity in the water layer so I boiled some water in a mug then put the test tube in it it cleared up the turbity tgen I shoock the test tube again I see bubbles forming the boiling water should not have been used should have used hot water I see a precipitate formed between the boundary of the organic and water layer not sure what it is. my next try is freezing the mixture did not freeze organic layer thickened
In the picture half of the organic layer is gone I presume that hydrogen peroxide has been leached from the organic layer

>> update organic layer soluble with ethanol (alcohol)

Also when organic layer is added to water the water floats on top of the organic layer they do not mix when only when ethanol is added they mix together no separation occurs
These solutions seem to react with manganese dioxide slowly

Next test distilled water and organic layer

[Edited on 20-6-2017 by symboom]

Cant seem to pull the hydrogen peroxide out something is desolved in the aqueous phase


Because I got it to desolve in ethanol I figure ill use urea to form urea peroxide this is my last thing ill try with the glow sticks.

Process desolve organic layer in ethanol then add urea to form urea peroxide

[Edited on 20-6-2017 by symboom]




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Natures Intellectual Organic Peroxide. >>Ascaridole <<
2020 year of science
Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
Sodium had its fame long enough time for Calcium
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[*] posted on 20-6-2017 at 04:59


:-( failed extracting hydrogen peroxide from glow stick by mixing it with ethanol then adding urea to form urea peroxide
It crystalized out but did not for the urea peroxide
Unfortunately only urea crystals formed
Hopefully someone can succed where I failed on the extraction of hydrogen peroxide from glow stick

IMG_20170620_054518.jpg - 2.6MB IMG_20170620_104340.jpg - 2MB

Whats up next to try

A water in insoluble desicant
activated charcoal
Added rapid bubbling also did that with just water
So not sure if it decomposing

Calcium sulfate
It formed an insouble precipitate cloudy suspension
The calcium sulfate has settled to the bottom
Haven checked if concentration increased yet

Silica beads
molecular sieves
Has anyone tried it
Also instead of evaporation in the open dessicant it
Using something like sodium hydroxide

>Concentrating hydrogen peroxide by borate ester
Boiling off the azotropic ethanol which should remove 5% water
Just as the hydrolysis removes more water.
>Extraction of sodium percarbonate with sulfuric acid
>Concentration >extraction with cymene

[Edited on 20-6-2017 by symboom]




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Natures Intellectual Organic Peroxide. >>Ascaridole <<
2020 year of science
Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
Sodium had its fame long enough time for Calcium
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[*] posted on 18-7-2017 at 02:47


Interesting videos
Vacuum distillisation
https://m.youtube.com/watch?v=jurYOOHDjx0
Evaportaing
https://m.youtube.com/watch?v=_L2ecuDZwlA
Desicant method
https://m.youtube.com/watch?v=1OiAm65hAoo

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[*] posted on 29-7-2017 at 08:33


The peroxide is usualy in the glass vial in the middle, should start there.
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[*] posted on 29-7-2017 at 15:16


Yea i dont know why people think that i used hydrogen peroxide to test both solutions it was the outside vial the dye in the glass vial reacted with the peroxide demostrating that it contains no peroxide also tested with copper sulfate
Hydrogen peroxide does not like to be alone haha
In water it is hard to pull out of the mixture with water
In organic solvent with glow stick water wont pull it out

A vacuum desiccator seems to be the second best method behind vacuum distilization


[Edited on 30-7-2017 by symboom]

[Edited on 30-7-2017 by symboom]
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[*] posted on 29-7-2017 at 15:34


Cymene is fairly easy to obtain and can be extracted from cumin and thyme. I would definitely give the cymene route another look.



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[*] posted on 8-3-2018 at 12:52


Here is a better vacuum distillation setup using glass tubing
Vacuum produced by a asperator adaptor
https://m.youtube.com/watch?v=tYLlkTDstmo
Room temperature boiling water with asperator if it was hydrogen peroxide the water would boil off.
or a hand pump vacuum see picture above

IMG_20180308_124048.jpg - 2MB

Hot water could be in the wine glass providing some heat

Hard plastic tubing may work since it is low temperature or room temperature and only water is passed over

When I say better I mean better than my original post there is no receiving flask only a long hose with a one way valve and the water collects in there

Also thanks for the info However, standard Erlenmeyer flasks are not designed to be used under pressure. A filtering flask without a side arm should be used - these are able to withstand a vacuum.


Or even using two vacuum flasks
The main objective is to figure out a cheap way to do vacuum distillation

[Edited on 8-3-2018 by symboom]

[Edited on 8-3-2018 by symboom]




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Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
Sodium had its fame long enough time for Calcium
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[*] posted on 8-3-2018 at 13:03


Anything with a conical flask in it is not a "better" vacuum setup.
(Except in the unusual circumstances of it being a vacuum rated flask.)
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biggrin.gif posted on 26-10-2018 at 22:15
Self concentrating hydrogen peroxide making device


Concentration success a self sealing bell jar with a shot glass of desicant. It is working No heat was applied it may dedicate faster if heated then closed. The bonus is the descant can be seen through the glass.
The self sealing action is great because it shows if you have a good seal makes a pop sound as the pressure drops inside due to the descant absorbng the moisture.


After a good concentration then I'll test on cottonballs



IMG_20181026_230508.jpg - 1.4MB



[Edited on 27-10-2018 by symboom]

[Edited on 27-10-2018 by symboom]




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Oxone
Used for the production of --> CH2O/Cl2/ClO2/Br2/I2
------------------------------------->>Hydrogen Peroxide <<
Sodium had its fame long enough time for Calcium
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[*] posted on 27-10-2018 at 17:16



Do you really want to combine those in a sealed jar like that?
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[*] posted on 27-10-2018 at 19:32


OK then thanks for changing my mind :)
Link to pdf
n Thursday May 28, 2009, at approximately 7:30 p.m., a 56-year-old chemist received
chemical burns over 65% of his body when he mixed sodium hydroxide with hydrogen
peroxide.

It does work unfortunately very well :( but the decomposition of the hydrogen peroxide does worry me now so vacuum desication I do not like due to the dangers associated with it.
Calcium chloride descant is more suited for this

[Edited on 28-10-2018 by symboom]
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[*] posted on 30-10-2018 at 04:00


A 'cool' way to concentrate H2O2, to quote:

"The freezing points of H2O2 and H2O are very similar, so this is tedious, but it is quite effective. Put the solution in the freezer and skim off ice crystals as soon as they form. The ice crystals, if small, will be nearly pure water. This will increase the H2O2 concentration of the unfrozen portion."

Source: https://www.quora.com/What-is-the-easiest-to-way-purify-H2O2...
--------------------------------------------------

Perhaps of only theoretical interest, very 'High Test Hydrogen Peroxide' can be formed, at least in small amounts, to quote a source (see 'The gas phase reaction of singlet dioxygen with water: A water-catalyzed mechanism' by Xin Xu, Richard P. Muller, and William A. Goddard III, in PNAS March 19, 2002 99 (6) 3376-3381; https://doi.org/10.1073/pnas.052710099:, link: http://www.pnas.org/content/99/6/3376):

"Recently, Wentworth et al. (1, 2) from the Scripps Research Institute reported the surprising result that Abs, regardless of source or antigenic specificity, have an ability to catalyze the generation of H2O2 in a highly efficient manner and by a mechanism that involves the oxidation of H2O by singlet oxygen molecules, O2 (1Δg). ..... To understand how Abs can carry out this remarkable and unexpected chemistry, we need to understand how 1O2 can interact with H2O to produce H2O2. Preliminary mechanistic investigation (2)§ suggested that 1O2 might be able to convert H2O to H2O2 via the formation of hydrogen polyoxides, H2O3 and H2O4."

where one might call H2O3 and H2O4 high test grades of hydrogen polyoxides.

Note: working with small quantities is a very good idea when working with potentially energetic materials.

[Edited on 30-10-2018 by AJKOER]
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[*] posted on 30-10-2018 at 07:13


ABS as in ABS plastic?
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[*] posted on 1-11-2018 at 06:51


Quote: Originally posted by Jackson  
ABS as in ABS plastic?


No, apparently the reference to Abs (or singular Ab), upon research I believe refers to either sticky protein structures, see to quote https://www.scripps.edu/news/old/press/021308.html:

"the proteins that stick together are amyloid-beta (Ab), proteins that do not affect the heart. TTR protein, which is made in the liver to transport vitamin A and the thyroid hormone through the bloodstream, has rarely been sighted in brain tissue. But there have been scattered research studies over the past 15 years that have found TTR can bind with Ab, thereby preventing Ab molecules from clumping together."

or possibly more generally, micro structures, like discussed in this article associated with a virus platform: https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4039020/ .

I will leave the final word to any resident microbiologist.

[EDIT] See also comments at https://www.ncbi.nlm.nih.gov/pubmed/26855676 . To quote:

"A pathway for the formation of both O3 and hydrogen peroxide (H2O2) was previously proposed, beginning with the antibody or amino acid-catalyzed oxidation of water by singlet oxygen ((1)O2) to form hydrogen trioxide (H2O3) as a key intermediate. A key pillar of this hypothesis is that some of the H2O2 molecules incorporate water-derived oxygen atoms. However, H2O3 decomposes extremely readily in water to form (1)O2 and water, rather than O3 and H2O2. This article highlights key literature indicating that the oxidation of organic molecules such as the amino acids methionine, tryptophan, histidine, and cysteine by (1)O2 is involved in ozone formation. Based on this, an alternative hypothesis for ozone formation is developed involving a further reaction of singlet oxygen with various oxidized organic intermediates. H2O2 having water-derived oxygen atoms is subsequently formed during ozone decomposition in water by known reactions."

See also full text available at https://core.ac.uk/download/pdf/33115718.pdf which discusses the action of (1)O2 on water as proceeding either by one of two pathways:

(1)O2 + 2 H2O = 2 H2O2

Or:

2 (1)O2 + 2 H2O = 2 H2O2 + (3)O2

[Edited on 2-11-2018 by AJKOER]
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