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Author: Subject: Cyanoacrylate (Superglue) production/synthesis - possible for home chemist?
RogueRose
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[*] posted on 8-5-2017 at 22:51
Cyanoacrylate (Superglue) production/synthesis - possible for home chemist?


One of the most useful substances I have in my house, with as many applications as imagination allows. I would think that this would be one substance which would be very handy to be able to make - especially once one has found a lot of uses for it. $1 for .015 oz is kind of expensive and at that price is $67/oz and almost $1100 per lb.

So, does anyone know how to make this?
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Corrosive Joeseph
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[*] posted on 8-5-2017 at 22:56


You might like this...............

http://www.chm.bris.ac.uk/motm/superglue/superglueh.htm


/CJ




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RogueRose
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[*] posted on 8-5-2017 at 23:31


Quote: Originally posted by Corrosive Joeseph  
You might like this...............

http://www.chm.bris.ac.uk/motm/superglue/superglueh.htm


/CJ


Thanks CJ, I saw that page and it seemed that the synthesis step was a little lacking in details such as temps, pressures, atmospheric conditions, reaction times, etc. IDK if these factors are not very important in this synthesis and I've seen many synthesis written that seem simple but when the conditions necessary are listed, it is a whole other deal.
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JJay
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[*] posted on 9-5-2017 at 23:29


That page lists several references that likely have more information, in particular: Clayden, J., Greeves, N., Warren, S., Wothers, P., Organic Chemistry, 1st Edn, Oxford University Press, (2001) pp. 703

I have been working on a methodology for determining reaction conditions for named reactions. Basically, I just search for a lot of applications of the same named reaction and look at exactly what transformations/etc. are being made, what functional groups might cause problems, what reaction conditions are used, and how the authors of the article or book discussing the syntheses worked around problems. Obviously this won't tell you much about reaction conditions that no one has ever tried before, and I've had some pretty low-yielding experiments, but it's a vast improvement over taking wild guesses like I did previously.




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Deathunter88
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[*] posted on 9-5-2017 at 23:37


Quote: Originally posted by RogueRose  
One of the most useful substances I have in my house, with as many applications as imagination allows. I would think that this would be one substance which would be very handy to be able to make - especially once one has found a lot of uses for it. $1 for .015 oz is kind of expensive and at that price is $67/oz and almost $1100 per lb.

So, does anyone know how to make this?


Why not buy 16oz of almost pure cyanoacrylate on eBay for like 40 dollars?
http://www.ebay.com/itm/BIG-16OZ-BOTTLE-FLEXIBLE-THIN-HYPERBOND-CA-SUPER-GLUE-Cyanoacrylate-FLEX-/351971924500?hash=item51f3295a14:m:mumTQbPDdZ8HRgBfC mHByCw
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Dr.Bob
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[*] posted on 12-5-2017 at 18:29


The challenge with cyanoacrylates is that they polymerize very easily, thus forming glue/goo on any surface. You would need to keep an inhibitor in the material, then distill and likely add a trace of inhibitor to keep it good until sealed. And each container to hold it has to be immaculately clean, or any traces of impurity will likely polymerize it in the container. That is what you are paying for in a small tube, not the chemical inside.
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halogen
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[*] posted on 13-5-2017 at 23:30


Glue! I wonder if glue expressed from the devil's hoofs themselves has an activity of superglue. It seems probable.



F. de Lalande and M. Prud'homme showed that a mixture of boric oxide and sodium chloride is decomposed in a stream of dry air or oxygen at a red heat with the evolution of chlorine.
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jack44556677
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[*] posted on 9-4-2019 at 11:34


It would be cool if someone could supply the procedure for synthesis...

Short of that, I was very pleased with the superglue-like substance I made recently.

I had a very specific use case, where the adhesive needed to work well glass on glass, be completely non-toxic and foodsafe, and be able to routinely withstand heating and cooling from room temperature to 235C. Because I could find no commercial glue that ticked all those boxes, I decided to do some home experiment.

I found a research paper from 2 years ago "Egg Albumen as a Fast and Strong Medical Adhesive Glue" 2017 that outlined the process and I was shocked by the results (both theirs and my own).

First you air dry the albumen (egg white) in a fume hood / fan desiccator until it is as dry as possible ( according to the paper this was a 110fpm fume hood and the albumin was added by pipette to petri dishes that sat overnight ). I made mine with a computer fan and a Rubbermaid container. When completely dried, the albumen will be a light yellow and have a crystalline appearance. It will fleck off easily and will be hard like silica/quartz flecks, it will not be deep yellow and moist / bendy / sticky in any way (that would indicate there is more drying to do). This dried albumin ( measured at 5% of its original water content) should then be pulverized by mortar and pestle into a light yellow powder that appears more white as it becomes more ground. This pulverized material is then vacuum dried, held under vacuum at room temperature, for some time to further purge as much water as possible and the powder is declared EAA (egg albumin adhesive).

The proportion suggested in the paper was 0.875g of EAA to each ml of water for the ideal "gel superglue" like consistency, but they were also concerned with it's ability to be squirted through a syringe (which is a GREAT way to apply superglue by the by). Personally I used a small amount of the EAA and mixed a few drops of water in (drop at a time) until I got something I could work with. Ultimately the consistency I used was more like rubber cement, and formed sticky little balls/clumps with itself readily.

I used heptane (Bestine brand Solvent / Thinner) to clean both sides of the broken glass ( clean break, sides match pretty perfectly ) which seems to help a great deal when using any superglue then applied a very small amount of EAA mixed with water ( it really didn't seem like enough) on one side of the glass and pushed the two pieces together with some wiggling to ensure sliding / even application in the broken joint. Within a minute or so it seemed attached enough to stop holding it with my hands, and after about 5 minutes I had the courage to try putting the glass into position and begin heating it ( opposite to superglue, this glue cures as the water leaves it ) to get it to cure faster. So far the joint is performing well (it is air sealed and mechanically solid) but the paper didn't do much in the way of long term / duration stress-testing.

A little of the EAA got stuck to my finger and after the water dried the feeling and effect on my skin was barely discernible from superglue. In fact in terms of my experience using it, from the visible look of it, to the viscosity, to handle-ability it seemed functionally the same as gel superglue. If this stuff is this effective ( and biomedically seems ideal ) then the superglue syndicate may need to find a new scam.

It is recommended to keep the EAA powder fully desiccated and in the freezer until you are ready to mix up a batch for single use, or do so from fresh egg each time. It is still perishable and can harbor deadly disease. When used bio-medically it was sterilized under UV before use.
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