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Author: Subject: Synthesis of oxidized cellulose paper
Σldritch
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[*] posted on 12-2-2018 at 08:13
Synthesis of oxidized cellulose paper


Does anyone know a way to make oxidized cellulose paper? I tried heating 100% cotton paper in a solution of 1:1 Sodium Persulfate to Sodium Carbonate but it did not seem to work.

H2O + Na2S2O8 + 2 Na2CO3 ---> [O] + 2 Na2SO4 + 2 NaHCO3

Note that i did not use Sodium Bicarbonate because it will ruin the papers structure when Carbon Dioxide evolves.


Here is the wikipedia page: https://en.wikipedia.org/wiki/Oxidized_cellulose
If possible i would like to use an oxidizer that leaves a lot of carbonyl groups with as strong as possible cellulose. It seems the paper i used did not want to soak up the solution very well, is there some way to help it soak up? Maybe boiling it in water first?
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aga
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[*] posted on 12-2-2018 at 12:35


I think those solutions would be somewhat basic, which reminds me of an old process to make oxalic acid with wood shavings (also cellulose) and NaOH with heating.

Perhaps something like that happened instead of what you expected.




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Σldritch
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[*] posted on 13-2-2018 at 00:31


I probably did hydrolyse it a bit, it had a somewhat slimy texture. However reading more on oxidized cellulose, maybe that was my product because oxidized cellulose is supposed to be soluble. Probably due to loss of hydrogen bonding between chains. If it is soluble, how will i get rid of the salts? Maybe hydrogen peroxide is better.

I think i will try with thinner paper, is regular printer paper lignin free?

[Edited on 13-2-2018 by Σldritch]
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Bert
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[*] posted on 13-2-2018 at 10:41


See liquid CO2 reference in the compressed wood thread?

Claims it oxidizes lignin and extracts the products, what's it going to do to the cellulose on longer contact? Also, could liquid CO2 be "doped" with one of your suggested oxidants?

What's the intended use for the material? Wikipedia was kind of uninformative.


Quote:

I think i will try with thinner paper, is regular printer paper lignin free?


Plain, white (unscented, no lotion or other additives) facial tissue or toilet paper works well for a number of other cellulose modifications (estrification, anyone?) About as close to pure cellulose as you can easily get OTC.

Quite asside from remaining lignin, most "writing" or "copier" paper has plenty of mineral and/or resin fillers along with other adjunts and modifiers, even ph buffers to prevent embrittlement from retained process chemicals in the fiber on aging.

[Edited on 13-2-2018 by Bert]
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Σldritch
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[*] posted on 13-2-2018 at 14:15


Maybe printer paper is not such a good idea, ill visit an art store and ask, anyway i made some oxidzed cellulose from cotton as a test.

Materials:
Cotton 10g
Hydrogen peroxide 100ml (12.5%)
Distilled Water 210ml + some for washing
Acetone
A pinch of ferrous sulfate

Procedure:
The cotton was loosly placed in a jar and 200ml of distilled water and 100ml Hydrogen Peroxide solution were added and stirred in with a glass rod. A pinch or two of technical grade Ferrous Sulfate were dissolved in 10ml of water and added to the cotton with stirring. This was left for about 8 hours at room temprature with occasional agitation with a glass rod to remove oxygen bubbles and submerge the cotton. After 8 hours the oxygen generation rate should have slowed down considerably and is decanted. The product is washed twice in cold tap water, twice in distilled water and once in acetone, pinced into small pieces and left to dry.

Observations:
After the reaction had progressed for some time some increased stability of bubbles on the surface was observed implying dissolved polymer. The pH of the solution was also tested at this time showing a pH of ~5.5 . The product is slightly yellow, some sources claim oxidized cellulose is pale yellow but the color could come from iron.

IMG_20180213_231217.jpg - 3MB

[Edited on 13-2-2018 by Σldritch]
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[*] posted on 13-2-2018 at 14:30


If you NEED it to be in normal, flat paper form, the thinnest tracing paper they can give you at the art store is probably your best bet for cellulose without extra goodies. This is what we use when making magician's flash paper-

The described washing step sounds a bit light to me, but I'm used to trying to remove acid from inside the (tubular!) cellulose fibers to prevent self catalyzing breakdown in storage, which takes rather more steps.

But what's it FOR? Just something you were interested in?
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[*] posted on 13-2-2018 at 14:34


I want to strenghthen cellulose by crosslinking it with urea, which is why i want it in paper form.

[Edited on 13-2-2018 by Σldritch]
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[*] posted on 13-2-2018 at 15:08


If you just want cellulose, use "Schweitzer's Reagent" or a zinc chloride solution.

Clearly the feedstock will determine how much work will be required to get 'clean' cellulose.

The zinc chloride route takes days, but still works.




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