Florasol (R134a) extractions.

[Doctor Vapor]

Several members have asked that I start this thread to post more information regarding the method of cannabis extraction that utilizes "Florasol" or R134a instead of CO2, Butane or other solvents. This is an advanced topic and I speak from some experience.

I hope this thread will be a place to share information, pictures of our experiments, thoughts and questions about the process of using R134a to extract the Herb.

Let's begin with a review of the literature:

http://www.mmv.org/sites/default/files/uploads/docs/artemisinin/06b_HFC-134a.pdf

http://link.springer.com/article/10.1007/s11802-012-1948-0

http://en.wikipedia.org/wiki/1,1,1,2-Tetrafluoroethane

R134a is 1,1,12-Tetrafluroethane but be careful, there are fakes out there:

http://www.iicl.org/techcorner/bulletins/r134a_testing_procedures_1.pdf

Also some versions come with lubricant or dye in them and these are not suitable for our purposes.
You probably need a license or a friend who is a refrigeration tech to even get R134a

Your reservoir needs to have both vapor and liquid connections. The liquid connection uses a dip tube while vapor is at the top of the tank.

Something like this would be great:

http://www.ntxtools.com/network-tool-warehouse/ROB-34750.html

Don't even mess with the little cans you get at the auto parts store. Those have oil or dye in them.
Get together with your friends and buy a tank that is used to charge refrigeration systems. Remember to check for lubricants and dyes. Expect to pay around $200 for this.

You are going to need a "recovery pump" to compress the gas back into a liquid. The Appion G5 Twin is the one I reccommend:

http://www.ebay.com/itm/Appion-G5-Twin-Refrigerant-Recovery-Unit-/271172200126?_trksid=p2047675.m1850&_trkparms=aid=222002&algo=SIC.FIT&ao=1&asc=11&meid=6316257943167434329&pid=100011&prg=1005&rk=3&sd=170961977496&

Yes you can expect to pay around 500-600 dollars for this.

You've already spent $1000 and you don't even have an extraction vessel or a recovery vessel yet. Those are usually custom made. They MUST be made of stainless steel.

I'll be back in a while to post more about this, in the meantime your questions and comments are appreciated. -DV

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Thank you, Moderator. I will use edit in the future!

Mod note: When possible, please avoid making back-to-back posts in a thread. Use the Edit feature located at the bottom of your posts. Last 7 posts merged.

 

[scottio19]

wow, I have never heard of such a solvent. Is it a watched substance?

Is it an organic solvent like d-limonene, or a hydrocarbon, or neither? I am very interested

 

[Buildozer]

Thanks for sharing all the good info Doc.. that's some nice extract

 

[Doctor Vapor]

Here is a source for the proper R134a which is DuPont "Suva"

http://www.ebay.com/itm/DuPont-R-13...Parts_Accessories&hash=item4ac26caa0d&vxp=mtr

Here is another one

http://www.ebay.com/itm/R-410A-REFRIGERANT-25lb-NEW-SEALED-R410a-R410-R-410-/251100102431?_trksid=p2047675.m2109&_trkparms=aid=555003&algo=PW.CAT&ao=1&asc=142&meid=6324727994954274402&pid=100010&prg=1076&rk=2&sd=251245550830&

It looks like only the State of Wisconsin has really strict rules regarding sales to EPA certified technicians but it can't hurt to be more aware of the possible dangers to yourself and the environment.

http://www.epa.gov/ozone/title6/608/faq.html

Please keep in mind IT IS ILLEGAL TO VENT R134a TO THE ATMOSPHERE.
It's also not good for children, small animals and all future life on Planet Earth.

I said earlier not to bother with the small cans sold for recharging car A/C systems at home. This is an easy way to avoid the lubricant which is often added to lubricate the pumps in an automotive system. There may be a few of these kits that don't have lubricant but I would be very careful unless you want to inhale nasty stuff when you vape the end product. You could spend a lot of time finding something that works so, unless your time is worth nothing, you're better off getting the real thing in bulk. It looks like the price of R134a has actually come down in price since I last checked.

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What is Florasol Extraction?

It is more like a CO2 extraction and not so much like the simple BHO extractions we are familiar with. The difference here is that the pressures are much lower than the pressures required for CO2. We might use some stainless parts that are similar to what is used in high-end BHO extraction but that is where the similarity ends. This is also not a distillation process and it does not rely on elevated temperatures. Because the liquid must be recirculated, you will need a pump.

It's not going to be a quick process and it isn't cheap. Remember the engineering adage "GOOD, FAST, CHEAP, pick two".

To step up to this process expect to spend more than BHO extraction but less than CO2.

If you don't have a few thousand dollars to spare, you need to at least be able to TIG weld and the welds must be inspected. It's possible to buy Stainless Tubing that you can make an extractor with but a lot less trouble to buy it already made.

Why would I even want to do a Florasol Extraction?

Before we get into details about the extraction vessel, the separator vessel and the molecular sieve (I'll show you how to make one), let's look at the reason why some of us want to build an extractor like this.

The end product speaks for itself. Need I say more? Say hello to Golden Taffy..

 

[Doctor Vapor]

wow, I have never heard of such a solvent. Is it a watched substance?

Is it an organic solvent like d-limonene, or a hydrocarbon, or neither? I am very interested

Please read the original post for the answer.

 

[mephisto]

Holy Crap! Its great being an A/C tech! Can't wait to see more of this ....Thanks for the info.

 

[Roger D]

Wow. Mad science here. Waiting to see the whole process. Good point that you don't have to throw any of the solvent. Pictures appreciated

 

[Puffers]

Thanks for making this thread DocVapor. I have many questions to pick your brain with if you are so willing.

So 134a seems to have a loading factor similar to a sub-critical CO2 extraction from what you mentioned earlier which is why this system has to be a closed loop for recirculating the solvent 10 or so times through the material. Is an extraction a lengthy process? I understand this obviously varies greatly particularly with regards to the temperature you perform your extraction having direct proportional affect on the pressure of your solvent which i assume also changes the loading factor of the solvent and the speed that it can move, not to mention the amount being extracted. You mentioned you use a co solvent for the waxes, is this a contolled product? If you omit this solvent is it basically an absolute extract?

Do you have to have rebuilld your recovery pump to work with the oil-less refrigerant? I have heard this has to be done with eventually for closed loop butane extraction systems.

One of those bottles you listed was 410a (the pink one) which is completely different 134a. I assume this was mislinked.....


Since time is money you may be interested in this guy. If the solvents speed and loading factor are changed with temperature this may be helpful: http://www.centurytool.net/MT69_CPS_Recovery_Submersible_Subcooler_p/cpsmt69.htm

 

[Doctor Vapor]

Thanks for making this thread DocVapor. I have many questions to pick your brain with if you are so willing.

So 134a seems to have a loading factor similar to a sub-critical CO2 extraction from what you mentioned earlier which is why this system has to be a closed loop for recirculating the solvent 10 or so times through the material. Is an extraction a lengthy process? I understand this obviously varies greatly particularly with regards to the temperature you perform your extraction having direct proportional affect on the pressure of your solvent which i assume also changes the loading factor of the solvent and the speed that it can move, not to mention the amount being extracted. You mentioned you use a co solvent for the waxes, is this a contolled product? If you omit this solvent is it basically an absolute extract?

Do you have to have rebuilld your recovery pump to work with the oil-less refrigerant? I have heard this has to be done with eventually for closed loop butane extraction systems.

One of those bottles you listed was 410a (the pink one) which is completely different 134a. I assume this was mislinked.....


Since time is money you may be interested in this guy. If the solvents speed and loading factor are changed with temperature this may be helpful: http://www.centurytool.net/MT69_CPS_Recovery_Submersible_Subcooler_p/cpsmt69.htm

Thank you for being here, Puffers. You are correct about the loading factor. For R134a it is about 10 in fact!

There are different ways to add the co-solvent and there are different solvents. One way is soaking the material in a liquid (like ethanol) another is adding a compatible hydrocarbon gas (like lab-grade propane).

The recovery pump does require re-building after a few hunderd hours of use. I think the important thing here is to not get a pump that actually uses the gas as a lubricant. Research on this from several years ago showed the Appion to be one of the few. There are also other, more expensive pumps available.

Dude, you're so right about the pink bottle. My bad. Gotta stop posting at 2AM
Too late now for me to edit it. NO, NOT THE PINK BOTTLE.

Cool link on the subcooler.

Did you know that Subcool (of TGA genetics) is the son of a refrigeration engineer? He's also a great photographer. If you don't know about Subcool check him out.

Wow. Mad science here. Waiting to see the whole process. Good point that you don't have to throw any of the solvent. Pictures appreciated

Roger, thanks for your reply. It helps to know who is reading this thread. Pictures are coming soon. A friend of a friend actually has one of these extractors. (FOAF, you know) Here is a quick look at it.

More pics will follow as we discuss the florasol extractor in more detail.

 

[Doctor Vapor]

I got a minute to post a few more pictures of the extractor a FOAF has. This is the original prototype extractor and there are now some by newer designs that are more automated. This should give you a better idea of what a homebrew Florasol Extractor looks like. This one requires the constant attention of an operator. The guy who ran this is a helicopter pilot so you can get an idea of the skill level of the operator. We'll go into the details as time permits. Questions and Comments are welcome.

Here is what a commercial unit looks like.

 

[OO]

You are the man.

You are bringing actual science to the table on this forum, and it is much appreciated.

 

[Doctor Vapor]

Thank you for the encouragement, OO. I'm not sure how many people are actually interested in this thread so anyone who checks in or likes the posts here will have a motivational effect. There is some effort involved in breaking down the information for more people to access.

Those of you who have experience in refrigeration, AC and other closed-loop processes do have a big advantage because you already understand some of the physics at work here. The more advanced, re-circ Butane extractors also use some similar ideas but operate at 1/10 the pressure of R134a. If you're thinking of using stainless parts from butane extractors, be certain they can handle the pressures we will be working with. If any of you have the facility to actually do some experiments, please don't hesitate to post your results here.

I will do my best to explain the process in a way that makes sense to more people and try not to rely too heavily on mathematical equations. That said, there are some basic concepts you will want to be familiar with. Let's start with how a refrigeration system works.

Here is some recommended reading.



http://www.fridgesolutions.com/basics.shtml
http://www.buzzle.com/articles/how-does-a-refrigerator-work.html
http://en.wikipedia.org/wiki/Refrigeration

Here are some videos.

Have a look at the pictures of the FOAF extractor in my previous post and find the similarities to a classical refrigeration loop. The expansion valve and compressor are clearly visible.


I'm sure there are many more examples that illustrate the closed cycle refrigeration system. We're not building a refrigerator but need to understand the basics of operation since we will be working with a refrigerant gas.

Did you know that Butane can be used as a refrigerant gas?

http://en.wikipedia.org/wiki/Einstein_refrigerator
http://io9.com/5706535/the-story-of-einsteins-refrigerator

One of the inventors is a rather famous individual.

 

[Puffers]

snip

Thanks for all the pictures Doc, can you shed some light on what equipment is being used in the pics above. I see what looks like a large recovery pump (blue marked s s extractor), the extractor itself (closeup of vessel with t handle). Is the the kenmore appliance an insta-hot (electric tankless hot water heater)? What are the two large columns some sort of condenser for use in conjunction with the water heater

 

[Doctor Vapor]

This should help.

1. Compressor Pump (in this case a really expensive explosion proof one)
2. Reservoir (this has both gas and liquid ports and a dip tube)
3. Extraction vessel (put the herb in here, liquid flows through it. note the sight glass)
4. Molecular sieve (removes water)
5. Expansion valve (allows liquid to flow at a steady rate to change to gaseous phase)
6. Collection vessel (in this case with a water jacket to improve performance)
7. Water heater (for the water jacket on the collection vessel)
8. Water pump (circulates the hot water through the water jacket)
9. Vacuum pump (to evacuate the system before and after use)

 

[kushcabbage]

This should help.

taking it to another level, very impressive! We appreciate the info and thoroughness! How's the high or dab compared to a bho solvent extract?

 

[Doctor Vapor]

Thank you kushcabbage. The information wants to be free. I'm taking some criticism here from people who think this should be a deep dark secret. (not in the forum but in my circle of friends) I believe that we can all benefit from a more open discussion. Not eveyone is going to want to build one of these but it will help patients appreciate the ways medicine can be made.

As for comparison with BHO, it always depends most on your starting material. However, this process has some advantages in that it does not require elevated temperatures so the delicate terpenes and other low boiling components remain in the extract. The terpenes have been clearly shown to moderate the action of cannabinoids at the receptor sites so their value should not be underestimated for therapeutic purposes.

The FOAF who built this extractor was motivated by the desire to help cancer patients far more than the desire for profit or even recreational use.

Having said that, I think the terpene rich extractions have more flavor by far and also provide a nicer 'head change'.

 

[kushcabbage]

then you sir, are the man! Hoping these methods can be scaled down and utilized safely for people who are in states that are behind. (like mine) Thank you for your time in educating us. In bho I try to go "low and slow" to preserve terpenes. This seems like the holy grail.

 

[Puffers]

Right after I posted I realized the long vessel was probably the extractor and the other a collection vessel. So the heat in the water jacket is used to help draw everything to the collection vessel? How hard is the remainder of the solvent to purge left in the oil? If the co solvent is left out does it just omit the waxes? If that's the case what's the use of the co solvent? Is it contained with minimal loss in the closed system also?

So many questions..... thanks for fielding them all Doc, this is the stuff my Mechanical/Cannabis Science wet dreams would be made of

 

[Doctor Vapor]

Scale is a relative concept. I thought the system we are discussing was already 'scaled down' by comparison to this one...

My lab looks like this.

© 2012

So yes, I guess it is more 'scaled down'.........


I'm leaving on a business trip for about a week so won't be able to post much. I'll check the thread and answer questions as much as possible while I'm away from my office. Thanks for the props and please post your comments whenever possible. I appreciate members who spot the mistakes here as well. My ego isn't so fragile that I can't accept constructive criticism. But, please don't flame me, I bite. If there is anyone out there lurking, feel free to add your thoughts to this discussion. Vape on!

~ Doctor Vapor

 

[Doctor Vapor]

Right after I posted I realized the long vessel was probably the extractor and the other a collection vessel. 1) So the heat in the water jacket is used to help draw everything to the collection vessel? 2) How hard is the remainder of the solvent to purge left in the oil? 3) If the co solvent is left out does it just omit the waxes? 4)If that's the case what's the use of the co solvent? 5) Is it contained with minimal loss in the closed system also?

So many questions..... thanks for fielding them all Doc, this is the stuff my Mechanical/Cannabis Science wet dreams would be made of

1) yes
2) easy
3) for the most part
4) I like wax. Is that a good answer?
5) You can expect to lose about 10% of the gas/co-solvent mix due to vacuum purging.

I suggest keeping a detector around to measure leaks. (refrigeration dudes use these a lot)

I've seen simple ones on ebay for under $100

Also it's a good idea to use soapy water on the seals to see if there are any bubbles. Otherwise you will lose even more gas due to leakage.

 

[smokum]

Just piping in to thank you for sharing your knowledge and process even though this appears wayyyyy out of my range of education & $$

Regardless, it makes for a very nice knowledgeable read, and learning something (new) is never a bad thing eh.

Again... thanks for sharing & educating !! Sure would be lovely in the future if something like this progressed to the level to allow a small set up and general use of us 'common folk'. But until then.... it's BHO for me

 

[Puffers]

1) yes
2) easy
3) for the most part
4) I like wax. Is that a good answer?
5) You can expect to lose about 10% of the gas/co-solvent mix due to vacuum purging.

I suggest keeping a detector around to measure leaks. (refrigeration dudes use these a lot)

I've seen simple ones on ebay for under $100

Also it's a good idea to use soapy water on the seals to see if there are any bubbles. Otherwise you will lose even more gas due to leakage.

Leaks would be easiest to diagnose by pumping the system full of a dry gas like nitrogen then using micro-leak detecting soap bubbles. Given that some of those refrigerant gas detectors can detect under a .25oz of refrigerant leaking per year (like the one I have) would they be better for judging a full purge? If purging is easier then butane though this would probably overkill. Just thinking out loud there.
So if the co solvent is omitted is the oil basically an absolute, would winterizing be useless?

 

[Doctor Vapor]

Leaks would be easiest to diagnose by pumping the system full of a dry gas like nitrogen then using micro-leak detecting soap bubbles. Given that some of those refrigerant gas detectors can detect under a .25oz of refrigerant leaking per year (like the one I have) would they be better for judging a full purge? If purging is easier then butane though this would probably overkill. Just thinking out loud there.
So if the co solvent is omitted is the oil basically an absolute, would winterizing be useless?

Leaks can occur while the system is in operation. I found a $20 leak detector on ebay.
http://www.ebay.com/itm/Halogen-Gas...106?pt=LH_DefaultDomain_0&hash=item25741dec8a
It is sensitive but the leaks can be pinhole size or smaller. Even the $20 one can detect 14gr/yr leaks. If you are leaking south of the extraction vessel you are losing more than gas so it pays for itself quickly if a leak should develop. Since people here are talking about scaling down and saving money I thought I would suggest this as a way to find leaks before they become a real problem.

Nitrogen testing is a good idea but doing that every time adds an extra step to an already tedious process. We did the Nitrogen test once, when the apparatus was first built, to test for leaks before filling it with R134a but we don't do it every time the machine is used. I certainly recommend doing this to test for leaks the first time. If you have good seals and everything holds tight up to around 250Psi, you're good to go.

A vacuum pump is used to evacuate the system before introducing gas. This is a common practice in refrigeration applications also. Once the run is completed, it is a simple matter to purge in the heated collection vessel at a gentle temperature of >180F for about 20 minutes. If you don't use a co-solvent, yields will be smaller but when you take the product out and subject it to a wash and second purge it comes out as an absolute. No winterizing required.

It is best to start with kind bud. Close trim and shake produce an inferior product IMHO. There are wide variations in color, wax content and aroma from strain to strain. That's what makes it interesting. I have seen cases where the wax was desirable for making whipped concentrates and other cases where it is preferable to remove the wax. To some degree it is a matter of personal taste.

Would you call the product pictured earlier in this thread "an absolute"? I think it qualifies. The term comes from the science of fragrances as you know.
http://en.wikipedia.org/wiki/Absolute_(fragrance)

I was serious when I stated that this is already a scaled down system. I'm not even sure if it would work with a smaller setup. To make it worthwhile some friends of mine made a bigger system that holds 1kg of plant material at one time. It takes so long to do no matter what the size that it just makes sense to do the largest batch you can. Pooling resources and money would be one way to do this.

I'm not exactly dirty rich myself, just resourceful. If you live near Silicon City like I do, you would be surprised what you can find as industrial surplus. Maybe this is more of a project for a collective than for an individual. Some NASA trained engineers and a few Aerospace guys helped build the systems I have seen.

I want to say again that this IS the small system. While a smaller one might be possible I doubt it would be practical in terms of the value spent vs value recieved. Making an oz of good herb into 2 grams of concentrate and taking hours to do it with a $2000 system? Not my idea of a good investment.

The pump and the R134a are fixed in price and you need them no matter how small your set-up is. The same pump can be used to make more extract in each run by just using a larger vessel.

If you are looking for a small hobby system you can make and run by yourself it is much better to just make some BHO! I'm sure there is sufficient information on other threads in this forum if you are not already an expert.

If you make BHO, make it in a stainless or glass apparatus. You realize that PVC leaches into the butane and is carcinogenic. I can't believe we used to do it in a plastic tube with crappy cans of stinky butane. Well, that was more than 10 years ago. Now we know better.

The problem is it's really difficult to get pure butane. None of the stuff you buy for lighters, 8x distilled or not, is pure enough for human consumption. By law, it must have methyl mercaptin added as an odorant to detect leaks if it is shipped on the highways of the USA. DOT rules.

If you go down to the local specialty gas store and try to order chemically pure n-butane they have already been warned that people use it to make "drugs". Unless you actually do have a legitimate lab, you're painting a big target on yourself. That puts you in between a hard rock and a place.... so to speak.

The desire not to make patients even sicker is a major motivation for using the florasol process.

I have a larger florasol extractor to show you later in the thread. Let's first go over the operation of this small one just to get a basic grasp of the process.

 

[Roger D]

If you make BHO, make it in a stainless or glass apparatus. You realize that PVC leaches into the butane and is carcinogenic. I can't believe we used to do it in a plastic tube with crappy cans of stinky butane. Well, that was more than 10 years ago. Now we know better.

The problem is it's really difficult to get pure butane. None of the stuff you buy for lighters, 8x distilled or not, is pure enough for human consumption. By law, it must have methyl mercaptin added as an odorant to detect leaks if it is shipped on the highways of the USA. DOT rules.

If you go down to the local specialty gas store and try to order chemically pure n-butane they have already been warned that people use it to make "drugs". Unless you actually do have a legitimate lab, you're painting a big target on yourself. That puts you in between a hard rock and a place.... so to speak.

That's why I can't afford making concentrates. I don't joke with purity. Here there is only expensive or homegrown herb. With the available resources I got it seems more logical to use the herbs directly thru hi end vaporizer and glass. I wish I could make a batch of quality for the convenience and experience

Can't wait to see it all ! I love gear

 

[FLskwat]

1st: Using 0 impurity commercial tane + glass or ss apparatus + vacuum purging/heat, makes an end product with a merc. level totally consumable and less harmful then 90% of the chemicals used to grow our "bomb commercial" weeds...
2nd: we in Europe can get pretty easily N-tane without drawing a target as we do not have that concentrate market blooming...
3rd: to the OP, how can your end product be free of wax/lipids and have a taffy consistency...I see this as impossible (as all the end products I have seen free of lipides= liquid concentrate or crystallized and powdery)?
4th: your pictured product looks exactly the same as 90% of the end results we picture in the Oil extravaganza & my stash threads... so no IMO that picture does not show at all the "superiority"of florasol extracts...
Don't get me wrong I'm really interested in your posts but I don't want mis-information to be spread!