Author Topic: Microcrystalline Cellulose  (Read 288 times)

Douchermann

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Microcrystalline Cellulose
« on: February 02, 2009, 05:30:16 AM »
Microcrystalline cellulose has very limited use. That is, however, unless you're pressing pills/tablets. It is the most universal and quite possibly the best base excipient for making pills. It acts as a disintegrant, a tough binder, and a lubricant to a slight degree. Unfortunately it is also quite expensive to purchase, and even harder to find a legitimate supplier that will sell to residences. However, the process to make it at home is astonishingly simple. The reason for the high cost is due to the elaborate manufacturing process employed on an industrial level which becomes quite expensive since this material is bulky. Not to mention, previous processes for producing this were quite inefficient and/or required expensive starting materials.

Reaction:

There is no real reaction scheme, so I can't write up an equation. At first, a cellulose pulp is hydrolyzed with sodium hydroxide. This dissolves most of the pentosan, and hemicellulose and also converts some of the cellulose. It is washed free of this, then is hydrolyzed with hydrochloric acid to break down the amorphous and somewhat chaotic organization of cellulose, into a more crystalline form of cellulose - hence the name microcrystalline cellulose.

First, obtain roughly 100g of ordinary paper. Fresh computer paper is recommended, but you can use recycled paper. However, newspaper (or anything similar) is not recommended. If using ordinary computer paper, it will take between 20-25 sheets to obtain roughly 100g. Cut the sheets into 16ths and place in a blender with a little hot water. Blend it up until its quite smooth. This is your paper pulp. Depending on the dyes or bleaching agents used in the paper, it could be blue or purple - this will go away. Add roughly 1000ml of hot water to your 2000ml beaker, or teflon coated saucepan. Add to this, 50g of sodium hydroxide. Thoroughly dissolve the sodium hydroxide, then add the paper pulp from the blender. Heat this up and hold it at an average of 60C for 60minutes minimum. Stir it occasionally.

Once it's done cooking, flood it with water. Set up your strainer with the T-shirt pieces to make a coarse filter. Set the strainer up above the 5 gallon bucket. Pour the contents through this. The filtrate should be a milky color - similar to starch in water. The material in the filter is what you want. Put latex gloves on, and ring out the material in the filter. Get as much water out as possible. In a very large stock pot, add around 1 gallon of hot water. Add the filtered paper pulp to this, and stir it well. Filter this out. Repeat this two more times, and on the third time all the soluble products and remaining sodium hydroxide should be gone. The wash water in the bucket can simply be dumped down the drain.

Ring the pulp out well one last time, and add it again to the 2000ml beaker, or teflon coated saucepan. Add another 1000ml of hot water, then add 150-160ml of 31.45% hydrochloric acid (muriatic acid). Bring this up to an average of 90C and hold it there for at least 2 hours. Add more water if it boils away. Once done, again flood it with water, and set up your strainer over the 5 gallon bucket.

Pour the pulp through the filter/strainer. You will notice the pulp now has a subtle difference in it's properties. While waiting for it to drain, fill up the stock pot with 1 gallon of hot water. Do not ring the water out of the pulp this time. If you do, it will clump very tight and make it quite hard to wash it. Add it directly to the hot water and stir it well. Repeat that step two more times, making sure not to ring it out in between each wash. This product should now be completely free of acid and any soluble chemicals. After the final straining, ring it out very well. Get as much water out as possible, as it will quicken the drying process. The water in the bucket can simply be poured down the drain. When you unravel the t-shirt, you will notice it is now tightly clumped and very hard. These are the exact properties that make microcrystalline cellulose important. Place it in your blender to chew it up into finer particles - close to the consistency of crumbs. Spread this on a foil lined cookie sheet in a very thin layer. Throw it in the oven at 300F (150C) for 1-2 hours. When removed, it should be crunchy sounding, as opposed to the very soft feel of paper that we started with. Last time I did this, I obtained 56g of dried product.

Special note: Final product should be colorless and odorless. If it is to be used in consumable pills/tablets, it must be completely white - no tints of the rainbow. Also, if it is pharmaceutical grade, you must use all glass cooking materials. The first time I performed this experiment, I used a teflon coated aluminum saucepan. The teflon coating was eaten away in some places, so the aluminum dissolved to a small extent and I was left with a slightly gray product. This is of course from aluminum hydroxide, which isn't specifically poisonous, but it's not always the visible things that can harm you...


lqdtrance

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Re: Microcrystalline Cellulose
« Reply #1 on: February 03, 2009, 12:41:52 AM »
Awesome information!!!! Welcome to the Vespiary!!

xxx

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Re: Microcrystalline Cellulose
« Reply #2 on: February 20, 2009, 07:45:30 PM »
Stupid question but... Can I nitrate it? I assume its still cellulose therefore nitrateable but just need to know.

Vesp

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Re: Microcrystalline Cellulose
« Reply #3 on: February 20, 2009, 11:10:32 PM »
Yes you could, it is Cellulose.

Good write up on how to make Microcrystalline Cellulose by the way. Have any pictures of it? :)
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Douchermann

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Re: Microcrystalline Cellulose
« Reply #4 on: March 04, 2009, 08:10:04 AM »
Actually, I don't.  My good camera broke before I obtained a solid method of performing this, and my other camera just turns the white pulp into a gigantic spotlight each time (where-as you can't see it if the flash is turned off).  I have a decent camera on my phone now, so perhaps I'll do this procedure one last time for novelties sake, taking pictures along the way.  Actually, it probably wont be for novelty, I'm sure I'll make mescaline tablets when I synthesize it.

Paddywhacker

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Re: Microcrystalline Cellulose
« Reply #5 on: March 08, 2009, 06:59:30 AM »
Would this make a good column chromatography material?

Column stationary phases seem to be uniformly overpriced.  I have long considered making my own.

Vesp

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Re: Microcrystalline Cellulose
« Reply #6 on: March 08, 2009, 07:05:26 AM »
I doubt it would work very well, but I honestly don't know I've never really thought about it. It could work though, after all there is a thing called Paper chromatography.

Normally the use silica gel. You can make your own silica gel adding an acid to a solution of sodium silicate. Sodium silicate can be bought as water glass, or you could produce it by heating sand and sodium hydroxide together. I've done this reaction before and it is easy very easy to do. You will want clean sand however.
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Paddywhacker

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Re: Microcrystalline Cellulose
« Reply #7 on: March 08, 2009, 10:45:58 PM »
Cellulose is an excellent chromatographic medium, but whether or not the microcrystalline variety would be superior is the question.

Column packings aren't just a load of powder.  That will cake up and block.  The material has to be granular.  Commercial materials specify a mesh size for their granules.

Making a packing from alumina or silica dust (available from pottery supply houses) or from microcellulose like this would require a bit of skill.  I was thinking ... make a paste with the material, water, and a binder such as plaster of paris.  Dry it out and grind up roughly.  Sieve out the large granules with a course seive and the dust with a fine seive and you would have your material.  But would it work?

I guess this deserves a separate thread.

Vesp

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Re: Microcrystalline Cellulose
« Reply #8 on: March 08, 2009, 10:51:34 PM »
Yeah, I don't think it would be to hard to try this on a small scale and if it worked do it on a more useful scale. I think it could work and you probably could it get where all the particles were about the right size.
I would be very interested in hearing about your attempts at this, so if you do it please let us know how it goes.
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myCH3

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Re: Microcrystalline Cellulose
« Reply #9 on: March 21, 2012, 03:45:21 AM »
could this be made food safe through the use of pickling lime instead of naoh, and a more food safe acid, possibly fumeric?

Vesp

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Re: Microcrystalline Cellulose
« Reply #10 on: March 21, 2012, 04:27:09 AM »
The HCl and NaOH wont cause much of a problem food-safe wise - Especially if you do an extra good job at cleaning it with clean distilled water.

Remember, HCl is stomach acid, and NaOH is used to make the food lutefisk and soaps. I believe HCl was also used as an acid a long time ago for lemonade.

Fumeric acid is not a strong enough acid, and pickling lime (calcium hydroxide?) is likely not basic enough and has very pour solubility.
Additionally, if the two mix, I suspect it will form insoluble(?) calcium fumerate which would be impossible to separate from the cellulose.


IIRC the MCC produced using this procedure does not work well for pressing pills.
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myCH3

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Re: Microcrystalline Cellulose
« Reply #11 on: March 21, 2012, 10:46:46 PM »
^funny your thoughts went there ;) thank you tho.