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Nano Cellulose

Production from mcc using 63.5% sulfuric acid in 2h at 30% yield. They hydrated the cellulose in water and added acid dropwise to prevent clumping. [1] [txt]

Regenerated cellulose

This paper adds water to the cellulose dissolved in phosphoric acid (says phosphoric acid needs to be 80% for cellulose to dissolve). [2] This next paper says that cellulose only soluble in phosphoric acid between 82%-85% phosphoric acid. [3]

Here is how I do it. -NatureHacker It is not fully dissolved, but almost all dissolved and what is left has been broken down:

  1. Take 10g Microcrystalline cellulose (MCC) and moisten with 5mL water. Mix this well.
  2. Add 100mL 85% phosphoric acid. Mix well and it should be paste like and not have many lumps (since the hydrating with water helps). Add a stirbar. Heat this to around 60c+ then stir.
  3. Reheat and restir this several times over the course of a couple hours (or if you have a heated stirplate, keep the temp around 60c and stir a couple hours). Don't get too hot because cellulose will burn (not a big deal though if it does). If it turns a yellowish color that is normal. It should be foggy but very slightly translucent when you are done. Of course you can add more phosphoric acid to get it to turn clear, but that is expensive.
  4. Add about 300mL of water while stirring. This regenerates the cellulose that you dissolved. This 300mL can contain a silicate or silicic acid solution you prepared earlier which will create silica doped cellulose.
  5. Centrifuge this. For a resuspension buffer preferably you can use 700mL of water with 30g of KOH added in (or ammonia if you desire). This will help neutralize the pellets as you resuspend them and re-centrifuge. Do this step a few times until the supernatant is neutral or alkaline.
  6. The pellets are now your regenerated/nano cellulose!

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