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Bho Extraction And Recovery


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#1 Graywolf

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Posted 23 January 2011 - 09:28 AM

Wow, what a summer, fall and winter chock full of time dark holes and glad to be seeing what I hope is not a Mars light at the end of the tunnel. R&D projects fell behind relocating two pharmers and three grows, as well as other personal business, but I did make progress on a few things, that appear to be about two strokes short of total intellectual orgasm. The first is to design and build a butane extraction and recycle prototype, which I am in the process of shaking out as we speak. It was based on Foaf's excellent pioneering recovery work, though there are many design differences. So far everything checks out, except for a reliable column vacuum, despite some expensive trick gaskets, so I have one more set to try, and then if the column is still temperamental, I will chuck the heads in my lathe and cut o-ring grooves. The column is too long for my lathe, so I will have to take it out for re-facing. Attached is an AutoCad schematic, and a picture of the equipment. The concept is that the material is loaded into the 1 1/2" 304 SS Schedule 10 stainless column and the whole system pulled under vacuum. That removes the balance of the water from the plant material. Valves are then opened, which allows liquid butane from the liquid side of the 50# refrigerant recovery tank, to be push-pulled into the column and out the bleed valve at the top. The valves can be closed at that point and the material allowed to soak in the butane, or left open and the butane allowed to flow in the bottom of the column and up through the upper bleed valve, before heading down to the lower collection vessel. If it is allow to soak, rather than simply flow through, a 3/4" dump valve may be opened at the bottom of the column to do so rapidly into the collection vessel which is under vacuum. Regardless of which method is used, the butane is pumped from the lower collection vessel as a gas and recompressed as a liquid in the original refrigerant recovery tank, using an oil less refrigerant recovery pump. When the whole system is again under vacuum, all of the butane has been recovered, including that soaked into the plant material, and it automatically shuts off. The fully purged oil may then be recovered from the lower collection vessel. Everything that the oil touches is either electro-less nickel plated or stainless steel. More as this project shakedown progresses:

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#2 eloquentsolution

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Posted 24 January 2011 - 02:42 AM

this project has been in conception from the moment we pharmers first gathered. it is so exciting to see it come to fruition. never would have happened without jd! when this comes together, we will be recycling all solvents. the skunk pharm gone truly green! i love it, jd. thanks for all you do.
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#3 Graywolf

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Posted 05 February 2011 - 12:05 AM

Bingo! Successful shakedown trials!! Resurfacing the column heads and cutting o-ring grooves in the flanges worked slick and solved the vacuum reliability problem. Now that everything pulls down and cycles reliably every time, this weekend I will make a product run. Shake down did highlight that I need to follow though with heat for the lower vessel. It ices during recovery and slows down the process. For the purposes of proving the system, I simply stuck it in a make shift water bath. Here are some pictures of me filling the 50# refrigerant recovery tank with lighter butane, using a can tapper and of the frosting up of the process vessel.

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Edited by Graywolf, 05 February 2011 - 12:11 AM.

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#4 mediuse

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Posted 05 February 2011 - 08:57 PM

Bumpitty bump!...thanks GW...am saving this for further study...not got the grey matter firing too well today...but I will be back! muhhahaha muA
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#5 StEaLyOuRfAcE

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Posted 08 April 2011 - 01:31 AM

This setup is impressive....I have been studying extraction and recovery systems and designs for the last year, and this is truly beautiful for a DIY setup, great job Graywolf,I also noticed in a few posts on various sites that you have some rough designs for a co2 extraction system,any progress in that area?How is the butane system running?,I am in the process of aquiring materials to build something similar to your design, I have a friend who works for a large metal distribution company,he can provide the SS, cut ,weld and pressure test anything I can design,any tips or improvements you've made since this post woulld be greatly appreciated .Thanks and much love..Keep up the good work! flyingsmiley.gif
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#6 Graywolf

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Posted 08 April 2011 - 06:02 AM

I also noticed in a few posts on various sites that you have some rough designs for a co2 extraction system,any progress in that area?How is the butane system running?,I am in the process of aquiring materials to build something similar to your design, I have a friend who works for a large metal distribution company,he can provide the SS, cut ,weld and pressure test anything I can design,any tips or improvements you've made since this post woulld be greatly appreciated .Thanks and much love..Keep up the good work! flyingsmiley.gif


No further progress on the CO2 system, as I have been buried in more pressing projects! More on that later.

The butane recycle system works slick, but the recovery pump didn't last long, despite being oil less, so researching that some more now. Looking at commercial gas liquidification compressors, in addition to refrigerant recovery pumps. More on that later too, as I sort it out.

Ohmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!!!!!!!!!!!!!!!!!!1
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#7 eloquentsolution

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Posted 31 May 2011 - 12:43 AM

a quick bump to let you know the butane recovery system is working! with five runs on the same material, it looks worth the time to do subsequent runs.
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#8 mediuse

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Posted 31 May 2011 - 03:25 AM

GW...th@ can tapper you use...I cannot find one...could you perhaps post a link? muA
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#9 Graywolf

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Posted 31 May 2011 - 04:56 AM

a quick bump to let you know the butane recovery system is working! with five runs on the same material, it looks worth the time to do subsequent runs.



Good point, sorry for falling behind!

After replacing the Microvac II refrigerant recovery pump with an Appion G5 Twin, as well as replacing our broken digital vacuum gauge with a simple analog one, the process has run smoothly by the numbers.

After shakedown using fan leaves, we made one 300 gram run using prime U of Dub bud, with a yield of around 10% using four runs with a 3 minute soak and the fifth run at 5 minutes.

I just made two more columns, to augument the existing 1 1/2" X 48" original. I made a 12" and a 24" for the smaller runs that are more typical of our individual patients needs. Yesterday I boiled out the 12" column in hot soapy water, in preparation for trying it out today.

More on the new column results after testing, but the 48" 300 gram column took 41 minutes to vacuum dry,so ostensibly the 12" will hold around two ounces and will do a final vacuum cycle in the neighborhood of 10 to 15 minutes.

We did discover that our analog gauge loses its zero and requires recalibration between cycles.

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Edited by Graywolf, 31 May 2011 - 05:00 AM.

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#10 eloquentsolution

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Posted 31 May 2011 - 11:56 AM

that was amsterdam flame, jd. of little interest but it was cut early for real estate appraisal.
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#11 Graywolf

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Posted 01 June 2011 - 06:04 AM

GW...th@ can tapper you use...I cannot find one...could you perhaps post a link?




muA



I bought mine off E-Bay and the link is now closed. I did however see a splended aray at the local refrigeration supply firm where we pick up misc parts.

I will look for the invoice and forward the info, if I can find it.

that was amsterdam flame, jd. of little interest but it was cut early for real estate appraisal.



My mistake! I sometimes forget and mispell strains!
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#12 Graywolf

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Posted 21 July 2011 - 06:17 PM

Here is the decarboxylation graph I promised.

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#13 mediuse

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Posted 21 July 2011 - 06:32 PM

Thanks GW :lol: muA
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#14 Dudz

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Posted 21 July 2011 - 09:12 PM

I want your extraction machine! LOL Getting tired of wasting money on butane that could be recycled and used again.
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#15 Strider555

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Posted 22 July 2011 - 01:16 PM

I want your extraction machine! LOL

Getting tired of wasting money on butane that could be recycled and used again.


you outta see it in action its pretty cool stuff man..... :)
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#16 Graywolf

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Posted 20 August 2011 - 09:25 AM

Hi ya'll! We have refined our butane extraction and recycle system to the point of producing thin film vacuum purged BHO and have developed thin film vacuum purging of the ethanol that we use when we convert from a raw oleoresin to an absolute. Butane recovery is approximately 100%, or what ever level we choose. An absolute as many of ya'll know is a raw extract with the non active ingredients removed, leaving the cannabinoids and the turpenoids. Picture attached: The system has three different length columns, a 12", a 24", and a 48". Using the 24", the full cycle time is about 1 hour and our best run on bud was 22.2% oleoresin. To achieve that, we pulled a 29.9"Hg vacuum on the system and then flooded the column with liquid butane. We stopped flooding when liquid butane flowed out the top of the bottom flood column, as evidenced by the instantaneous chilling of the stainless vent tube. We recorded the time it took to do so and considered that one column volume. Using the refrigerant recovery pump, we again pulled a vacuum on the lower end of the system and when it reached -10" Hg vacuum, we again flooded one volume through the column. We repeated that step every time the vacuum level fell to -10". At the end of 30 minutes flooding and reflooding, we open the lower valve and dump the column out the bottom. At that point we have run about 10 to 12 volumes of butane through the material, with soaks in between. We then pump the system down using the refrigerant recovery pump, until we hold at -25" Hg, at which point we switch to the high vacuum pump and pull the system below 29.9" Hg for the final purge. Because reclaiming 100% of the butane requires about another 30 minutes of pumping and the wear on the recovery pump running essentially dry at those vacuum levels, we have now compromised on reclaiming approximately 90/95%. The heating cable wrapped around the bottom of the recovery vessel keeps the system from freezing up from the refrigeration created by boiling off the butane under reduced pressure. Attached is a picture of a thin film purged BHO oleoresin before removal from the recovery pot. We recover it from the pot by re-dissolving it in hot ethanol, which we filter and then place in the freezer for three or four days. That causes the waxes and plant lipids to clump together and drop out of solution, so that they can be filtered out. After filtration, we remove the alcohol by simple evaporation, heat, or by pouring a shallow pool of the oil/alcohol solution in a 6" Petri dish and setting that in a vacuum desiccator, which we evacuate to 29.9" Hg to insure complete alcohol removal. Picture attached: I have also attached a scan of the hand corrected copy of my original Auto Cad drawing. Alas my Auto Cad 2002 won't run on my new 64 bit processor and I can't justify $2K for a new version in retirement. I'll replace the drawing with a more professional one when I resolve that issue. The principle advantages of this system is that it is the cheapest extraction method that we have found yet and produces a pristine absolute. From a potency and quality standpoint, it bows to none of extracts displayed as the best of the best on international forums. It is much faster than the Tamisium extractors and my cost to build the 300 gram prototype was about the price of the smallest Tamisium unit. Because it uses a non polar solvent, relatively non soluble in water, it avoids picking up most of the water solubles associated with alcohol extracts and our later winterizing step removes the plant waxes that are picked up. The resulting absolute is milder in flavor and much smoother than a raw oleoresin when used orally or by vaporization. In addition, removing the waxes eliminates wax coating the lungs if it is vaporized.

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Edited by Graywolf, 20 August 2011 - 09:31 AM.

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#17 teddys head

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Posted 21 August 2011 - 05:20 AM

now your sucking diesel GW ,thats some job m8 :oldhippy:

thanks so much for this :)


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#18 Luc

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Posted 21 August 2011 - 02:12 PM

Hi Greywolf

That absolute is absolutely beautiful! Your absolute would make great tasting edibles. When can we expect the video of the process :) How much does this setup cost?

Have you done anymore work on your Supercritical Co2 fluid extraction?

Thanks
Luc

Hi ya'll!

We have refined our butane extraction and recycle system to the point of producing thin film vacuum purged BHO and have developed thin film vacuum purging of the ethanol that we use when we convert from a raw oleoresin to an absolute.

It is much faster than the Tamisium extractors and my cost to build the 300 gram prototype was about the price of the smallest Tamisium unit.

The resulting absolute is milder in flavor and much smoother than a raw oleoresin when used orally or by vaporization. In addition, removing the waxes eliminates wax coating the lungs if it is vaporized.


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#19 mediuse

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Posted 21 August 2011 - 03:49 PM

Th@ is just awesome, GW! :) :) :D heheheh muA
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#20 eloquentsolution

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Posted 21 August 2011 - 06:51 PM

the resulting oils have been used in my fruit infused truffles. they are to die for. unfortunately, they (so as not to shoulder blame...i told them the dose) have overdosed a few people.... hard to resist another! my sister and moms part time caregiver bit the dust! mom loves them though. i usually just eat them plain and do my medication in sub lingual drops of holy shit. no one has commented on the 22.2% return of pristine absolute! that is huge! it was done with outdoor grown buds. talk about a smooth vapor....wow! the system was built using many discards, as well as well as some newly purchased pumps, so cost is floating. graywolf can fill you in.
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#21 Dudz

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Posted 21 August 2011 - 07:18 PM

no one has commented on the 22.2% return of pristine absolute! that is huge! it was done with outdoor grown buds. talk about a smooth vapor....wow!

A 22.2% return is amazing and unheard of using butane, especially since butane doesn't strip the chlorophyll and waxes as much as alcohol does.
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#22 mediuse

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Posted 21 August 2011 - 07:55 PM


no one has commented on the 22.2% return of pristine absolute! that is huge!

MUhahahahha...I harvested last week for the first harvest of the year...my excuse is I been stonenened :) hehe


muA
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#23 Graywolf

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Posted 22 August 2011 - 06:36 AM

Hi Greywolf

That absolute is absolutely beautiful! Your absolute would make great tasting edibles. When can we expect the video of the process :) How much does this setup cost?

Have you done anymore work on your Supercritical Co2 fluid extraction?

Thanks
Luc


I picked up an HD camera and we actually did a video of this process and are refining it for presentation. More on that later.

Cost is under $1500, though I spent about $2000 building and sorting it out. The two pumps together are around $1000. My first refrigerant recovery pump was not suitable and required replacing.

I haven't pursued CO2 any further at this point, after reading the patents on the process and realizing how really slow the process is. I can also find no data suggesting that the Co2 extraction is in any way superior, justifying an all day process.

It is still on the project list, but is no longer perceived as the great panacea.

Edited by Graywolf, 22 August 2011 - 06:37 AM.

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#24 eloquentsolution

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Posted 22 August 2011 - 06:19 PM

A 22.2% return is amazing and unheard of using butane, especially since butane doesn't strip the chlorophyll and waxes as much as alcohol does.


these stats calculated after winterizing to remove the waxs and sunburning the chlorophyll for degradation products, so very pure. wish i could afford labs, but i can guarantee it is not the 6% thc that the refluxed extractions are producing. the more average percentage is for concentrates is 60% i'm told. it is that long boil that degrades the thc to cbn.....full decarboxilation. it is no wonder the refluxed extraction makes great sleep meds. cbn cannabinoids are sedative.
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#25 Luc

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Posted 22 August 2011 - 08:22 PM

Greywolf, thanks for sharing this really cool info and answering our/my questions.

I hope to see the video soon, don't put loud background music during narrations.

Luc

I picked up an HD camera and we actually did a video of this process and are refining it for presentation. More on that later.
Cost is under $1500, though I spent about $2000 building and sorting it out. The two pumps together are around $1000. My first refrigerant recovery pump was not suitable and required replacing.
I haven't pursued CO2 any further at this point, after reading the patents on the process and realizing how really slow the process is. I can also find no data suggesting that the Co2 extraction is in any way superior, justifying an all day process.
It is still on the project list, but is no longer perceived as the great panacea.


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