Caffeine extraction from green coffee with supercritical CO2 

Would be awesome if his voice sped up after 7:55 and the camera got super shakey.

An aqueous iron solution will turn opaque and black if tea or coffee are introduced. As it happens, that's a method of making ink, though I first learned about it by playing with 2L pop bottles of iron-rich well water adding a single drop of tea to make the whole volume slowly change. I don't know enough about the reaction to say whether it contributed, but I figured I'd mention it for completeness.

You are such a wonderful person, thank you!

how did i get here but hey cool! that remain m of walther white partner that make coffee extractor

Yeah but what happened when you snorted it?

First of all, let me say, that your videos are awesome. Now, I do not know your background but if already know this pass it, if not, her are some information. SFE occurs in different stages, first, the vegetal matrix absorbs the supercritical solvent, swelling its cellular structure, membranes and dilating the intercellular channels, leading to a drop in the resistance to mass transfer; in the meantime, dissolution of the extract occurs, and mass transfer take place from the inner matrix to its surface and solubilized compounds reach the external surface. These are finally transported from the surface to the supercritical solvent and removed from the solvent. So, this happens in various stages: 1- First there is a constant extraction rate period, where the external surface of the particles is covered with solute (easily accessible solute) and the convection (in the CO2) is the dominant mass transfer mechanism. 2- Secondly, there's a falling extraction rate where failures in the external surface oil layer appear and the diffusion mechanism starts, operating combined with convection; c) Lastly, there's a Low Extraction Rate or Diffusion-Controlled (DC) period, where the external layer of oil practically disappeared and the mass transfer occurs mainly by diffusion inside the solid particles. So, you're dependent on the biomass matrix itself, and you should grind the beans, increasing the surface area thus enabling a better impregnation of the biomass, increasing the solubilization of the target molecules and also insuring a better mass transfer from the biomass matrix to the CO2. In your case (maximum yield and lower extraction time possible) you should operate on the first to second phase. Oh and the extraction result isn't pure caffeine. Some tips: Water in the biomass increases the celular turgor and helps to increase the yield of the SFE by allowing a better impregnation of the biomass, but don't mistake it for cosolvent modifier, these are used to extract other type of molecules (hidrophilic/polar fraction) and these can also be used to manipulate selectivity of the extraction. Grinded coffee beans translates in increased yield. You could bubble the outlet of the extraction into an ethanol solution thus allowing better distillation afterwards. That bursts of CO2 you have on the outlet of the vessel when CO2 forms ice, blocking the pass, you could heat up that outlet zone with the electric heating mantle and that would decrease that. Cheers!

- Of course, I had to taste it :D

Just imagining people doing lines of purified caffeine

I bet this guy can make some WICKED hash oil!!!

4:29 "Time to get my GIANT PIPE WRENCH"

Yeah, I'm always floored by the work Ben does. This is incredibly interesting -- and I love the DIY angle.

It’s 2020 and I’m in quarantine. This channel is keeping me sane

Excellent video and channel! I guess by now someone must have had this idea, but... I guess the black solute in the extract is either iron carbonate or iron oxide. Maybe the water from the beans reacted with the CO2 to form carbonic acid, which in turn reacted with the steel pipe. That would explain why only some of the beans are dark; it´s probably those that were touching the wall. At work we need to purge lines when refilling CO2 tanks so no air moisture gets inside the tank because if it does time over time, internal corrosion takes place.

This is just awesome! I have worked with supercritical drying for my bachelor's and master's work and I remember fondly the pain in the ass that is drying aerogels and extraction if caffeine that my colleagues ran. CO2 freezing in the valve was a major problem, if you still run it try just heating it with the heating tape or air gun...And again, you are awesome for making this happen in at home. Congrats on the great content!

Supercritical fluid extraction can be more selective than other extraction means - but I would still expect it to extract all other free base alkaloids from the coffee beans as well. This might also change the taste of the decaffeinated beans beyond just the taste component given by caffeine - AND it also means your extracted caffeine is not 100% pure - I would still be very curious what purity grade that is (and whether or not it is high - like 80-100% or much lower). Do you know anything about that?

can you do this for nicotine or THC?

They actually make black printer ink with coffee

Sooooo who wants to talk about fractionating cannabis products?

What happens to the water when the CO2 goes supercritical?

how do you know that white powder is all caffiene ? Coffee beans would also contain chlorogenic acid that could be in there also.

graah!! white fiberglass from hell! *itch* *scratch*

Out of curiosity could this process be used to extract thc from marijuana?

@bkraz333 you are probably the master of extracting thc from the herb.

by the way i am on your side , i seen nothing rong with heating your vessel with a torch , you obviously no what your doing and a torch aint all that hot , where do you order your parts from bro, im having trouble sifting threw all the massive piles of web sites

hey friend im shure you thought of this but have u considerd draning the co2 by using the valve on top first, to say 50 psi , imnot shure but i dont think dry ice will form at this pressure , then you coulddrain your most awsome coffee ever......

You should know that Teflon tape does not seal the pipe, its purpose is to facilitate (as a dry lubricant) the screwing of the taper pipe threads, thus allowing for a better seal.

that "hmm, not bad!" look at 7:57 is priceless

Ben you've got some fascinating videos. Kudos, the world needs more people like you.

This guy could make Industrial-Grad Lab Equipment, (Extraction-Units), just like APEKS-Supercritical, or Eden-Labs.

Love the detail you go into explaining the process, also how excited you sound at the beginning of the video.

Did you try extracting THC using this nice device? :D This look perfect for making oil!

How much pressure have you taken it to before?

Methylene Chloride, I'm so used to hearing it called 'Dichloromethane' (DCM) in the lab. Old school naming schemes always baffle me.

You could use this process for super clean honey oil. I wonder if people have tried yet?

I find this experiment and household application of chemistry and thermodynamics to be quite interesting. I was wondering if you have an estimate on how much this scale experiment costed, where you got liquid CO2 from, and what safety precautions you had to take? I would have been quite frightened to have the pressure exceed the the working pressure of the sight glass.

Your video is great. Do you know is there any commercial scale supercritical co2 extraction plant working on decaffeination for green beans in the world currelty? Thank you

Man, brewing coffee like this seems intense :P

could this be done with weed? (supercritical skuff)

This is really cool. What is the efficiency of this process is w.r.t. yield?

isn't caffeine in high concentration poisonous?

This was very interesting. I didn't understand most of it though XD

Swedish chemist Scheele likely died because he had a practice of tasting the compounds he made.

3000psi...on a sightglass.... Pucker factor => EXTREME!!!! 😳

The water may help with the extraction by allowing the CO2 to form carbonic acid (H2O+CO2->H2CO3) because caffeine is basic?

Is this the patent you're basing all of this off of? patents.google.com/patent/US4996317A/en *Edit:* Nevermind, I just saw you showed a SS of it. It's this one: patents.google.com/patent/US5288511A/en

Can you make some cannabis product using the super critical CO2 process I need a super critical CO2 vessel that can hold one oz of flower so I can use the end product to make safe Cancer medicine THC kills Cancer an THCa hemp flower is 50 state legal in USA so I wanted to know if you can see if you can make it and build me one out of stainless steel so it's safe for cancer patients.

With the pressure vessel you made from aluminium and acrylic, would the liquid CO2 leak out over large time scales? or is it reasonably stable? IE: could I make one and have a really cool workshop ornament?

well, see, the thing is, brewing coffee with hot water is not the best way to get the caffeine out of it, a lot is left in the grounds. Also, the caffeine in a pound of coffee is diluted with around 256 ounces of water, if brewed according to the label. This dilutes the caffeine even farther, slowing its absorption by the body. In its pure form, only a very small amount of caffeine is required to cause serious problems to the body.

Why does there need to be water in the system? Is the solubility of caffeine that low in supercritical CO2? I was expecting a pipe with beans that got half filled with liquid CO2, turn it supercritical and in order to extract the solid all you would need to do would be to evaporate the CO2 leaving you with a pile of caffeine. Can supercritical CO2 not dissolve a significant enough g/ml in them compared to water?

No. Did you just make that up on the spot? From wikipedia: "Part of the reason caffeine is classified by the Food and Drug Administration as GRAS (generally recognized as safe) is that toxic doses (over 1 gram for an average adult) are much higher than typically used doses (less than 500 milligrams)."

I don't know where you got that from. It's not illegal. Caffeine is an unscheduled drug. I don't see why there would be a legal distinction between pure and impure controlled substances. Cut cocaine is just as illegal as pure cocaine.

did the water become acidic via carbonic acid which cause the steel create the black residue? i seem to remember playing with acids and iron and it turning black, but for the life of me cant remember much more then that. ps, love your work

I like how you just ended up "resorting to a hydrocarbon extraction" at 8:24 as if it were nothing. I complain about how long it takes to boil water when I make mac and cheese and you purify caffeine via hydrocarbon extraction. Sheesh.

@sabamacx Well since he based the procedure off a patent it's a pretty safe bet. I'd imagine that the patent proved that the product was caffeine (i.e. through chemical analyses such as qualitative features, TLC, mass spectrometry, or NMR spectroscopy).

I have a simple design for equipment to make carbon nanotubes and carbon nanowire. Are you interested in developing these designs with me?

@bkraz333 that may be a bit dangerous it you end up with a extremely high percentage of pure caffeine. And how much did that shop cost to construct and what do you do for a living as i am hoping to go into the biology field?

what was the other solvent used to extract the caffeine from the black solution? you mention hydrocarbon filter,

soooo.... ok ill ask, have you ever expertimented with more nefreious substances in that lab of yours... i mean... all these chemicals all this know how... have you ever made any illegal substances?

I shall have to do this in my 2L Grade 1 Titanium Autoclave at work. I am sure my bosses will not mind too much. Plus it has a working pressure of 10K Psi. Let's not talk about the value on it....

Seems counterintuitive to soak them first. since the caffeine is water soluble aswell as taking up space between the cellusose and lignin whereas the co2 cant reach. Maybe im wrong.

right on w your success!!! you must not over fill the vessels w plant matter. A plug can occur between the gauge and or valves and when you open this plugged vessel, the final threads will fail sending the top off like a cannon. the pressure difference of the blast is very lethal and anyone w in that radius is in danger. be careful and try employing safety relief valves for G.P.

so weird it came out black. did you scrub out the pipe? maybe some of the black oxide coating was dissolved in the process

Thinking caffeine as a toxic substance, all the caffeine removed from coffee must be quite valuable.

Judging from the past of human interaction with plants, somehow we will make a drug out of most plants out there. so yes(: it will cus caffiene is also a stimulant like cocaine lawl

Freeze dry green coffee then crush it into a fine power & solvent extract the powder with a hydrocarbon solvent in a buchner funnel or better //

FYI robusta coffee beans contain more caffeine than arabica beans. Btw you're set up is awesome. I've tried the crystallized caffeine, it has a rather nasty taste.

@Ammoniummetavanadate Sorry, it is grade 2, not grade 1. We do work with sulphides and chlorides, pure Ti is one of the only things that can reliably stand up to them.

I did a caffeine extraction @ 2,000psi. and 65C. Came back from the lab a marginal extraction. So I will post a video showing the process being done @ 10,000psi. Caffeine is water soluble, CO2 is non-polar so its almost doing nothing as far as a soluble solvent. Its just used for pressure.

no, it's quite very not. 1 person could ride that train out. it would be unpleasant, there would possibly be some vomiting, but the subject would not die.

@IDRadam You'll get quite active, nothing more .. :] It's not as good as amphetamins, and it won't work if you smoke weed with it, but it does give energy :]

Ahhh yes, your speaking about ice plugs @ about 7:24. I will do a extraction @ about 10,000 psi and water. I do believe the non compressible fluid is really blasting through the beans and it makes its caffeinated water w 680 bar assistants.

any thoughts if it was black and colored becasues of residue from the metal pipe?

coming up.... from Ben - One RTG battery using just pipe fittings. I'm pretty confident you are going to end up the richest DIY guy on this planet...

Nice, you could make some money selling the caffeine.

just want to say a lot if not most of the black color is from the pipe used i use to work with the black iron pipe and water alone will go black.

would the black staining have anything to do with a reaction with the iron in the fittings? perhaps stainless steel might rectify this problem.

The inventors of that patent are from the same small towns in PA I used to live in. I didn't think much science was happening there

I wonder how it would taste if you prepared the bean water like a normal cup of coffee? Would it also work with tea, perhaps?

Appreciate your efforts to upload your experiments. Great stuff!

this process is made industrial, what sense hase it to meke it DIY

What happened to the aluminum mesh-like insert? Did it react with the supercritical CO2 as well - like in your aerogel experiment?

@bkraz333 i dont mean to sound rude, but where do you get the money for all this? and where do you find the time? do you have a job?

Why? Emil Fisher did this extraction with water and you can modify it with alcohol and put that extract directly on the HPLC :)

Could the black ink possibly be the steel pipe? like making a pancake on a brand new pan, the first one always comes out black..

Next time, just get decafe coffee.

What the government don't want you to know...also another reason why good people die so young, too much caffeine kills .

If you snort it, you'll get a caffeine high quicker than if you ingest it orally and it'll go away quicker as well.

I did a bitter kola extraction w water and co2 @ 7,000 psi. The extract was red , hard like a jolly rancher candy, and very translucent.

It would be cool to send it in to get it tested via HPLC or something similar to see how pure it is.

Is it really worth the risk of these pressures to get "caffeine". Its bloody dangerous, especially when you use SOFT pipe steel!!!!!

1:27 look a Apple vacuum cleaner! I NEED IT :O

hey I didnt know apple makes fire extinguishers

Can you do some real drugs? What I mean is can u extract sugar from sugar cane?

Cool setup and video. Can I ask why you did all of this?

can any one tell me what is the price of co2 super critical chamber?

good thing you didn't OD on caffeine. It can happen!

Awesome channel. have you made a grinder?? 😁

Green coffee contains a lot of pesticides and fungicides.

hey seriously let me know if you'd ever want to sell me one of these id totally buy one!

Is this process is safety rather than swiss water process or sparkling water process?