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Rosin Technique....Easy DIY Solventless

heady blunts

Well-Known Member
does the ability to edit posts expire after some amount of time? i wanted to add this picture of the burritos.

12142416_1093280270682609_1021009276_n.jpg


hmm i wouldn't disagree with those generalities rufio made. but i have gotten pull-and-snap and sap and shatter all at 220. i think terpene profiles play a big role in consistency. if i have high levels of certain terpenes which are non-polar solvents i assume the product will probably be sappier.

rosin seems increasingly complex for such a straightforward process. that's probably what's keeping me so interested! the bio assay isn't bad either :razz:

10853004_755725594533024_1305669512_n.jpg


11420931_1286157958077085_1348890725_n.jpg


12141833_968203359893311_1686626457_n.jpg
 

BoogerMan

Well-Known Member
Grabbed this from the Rosin Facebook group, gives some insight into the effect of pressure and heat on the bud:

k3yLati.png

That's interesting about going over 3,000 psi and getting smaller yields. He does say though it is caused by too much pressure too fast. So I wonder if you increase pressure (over 3,000 psi) at a slower rate would it work okay? Hmmmm maybe?

I only go up to about 2,500 psi so idk??
 

heady blunts

Well-Known Member
sunfire has also found a point of dimishing returns as you increase pressure. i've heard 2000psi seems to be ideal from several experienced heads.

i think warping and denting start to play a role at high pressures.

even minor changes to the evenness of the pressing surfaces will drastically change yield efficiency IME.
 
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ixtapa

Well-Known Member
sunfire has also found a point of dimishing returns as you increase pressure. i've heard 2000psi seems to be ideal from several experienced heads.

i think warping and denting start to play a role at high pressures.

even minor changes to the evenness of the pressing surfaces will drastically change yield efficiency IME.
So it dawned on me that extraction of oils from plants is a very old problem, and agriculture has been evolving for many centuries. I did a little digging into the agricultural world and found a few interesting things (the technogy is referred to as "expeller pressing"). Rather than pressing as discussed in this thread, commercial oil extracting operations use a screw press to generate both heat and pressure. They are very expensive and are only practical at the hundreds of pounds and up levels, and are thus not directly relevant here. However, some of the results should at least transfer in part, and are worth considering.

In particular, this paper http://ainfo.cnptia.embrapa.br/digital/bitstream/item/61565/1/Anna-Rossano-Tech-Oil-presses.pdf mentions a formula relating oil yield as a function of pressure, time under pressure, and viscosity (which can be looked at as a proxy for temperature).
wqeSY4G.png

For the non mathematically inclined, I'll explain the upshot here. According to this model, diminishing returns are seen in pressure, time under pressure, and increased viscosity. To double your current yield using pressure alone will require using 4 times more than your current pressure. To double your yield by increasing time alone will require over 4000 times longer than your current time under pressure. To double your yield using viscosity alone will require a decrease between 16 and 4000 times in viscosity, depending on the material being pressed.

I'm not sure there is anything new here other than what I've seen determined experimentally by people on this thread. Pressure matters, but the returns are diminishing. Time matters, but the returns are diminishing. The interesting variable to me is viscosity. Pressure is easy enough to come by as witnessed by the numerous creative approaches seen here. I'm not convinced, however, that we are getting all the viscosity practically possible using heated plates.

But I have also come to realize based on this formula the diminishing returns available in solving this problem. Large improvements in viscosity will only generate modest improvements in yield, less so than equivalent improvements in pressure. Despite this, I'm still going to continue to think about ways to improve viscosity. I can't come to terms with a process that yields nearly as much on a second pressing as the first pressing - I can't help but think a better methodology would get the second press yield out in the first press! And just throwing more pressure at the problem has experimentally shown not to be the solution. So for the time being, it seems like viscosity is probably the most important technical problem to improve.

One last quick point: this paper http://library.uniteddiversity.coop/Food/Food_Production_and_Processing/oil_extraction.pdf states that increasing pressure slowly is important. The idea is that you push it down a little and some oil flows, then push some more, and all that oil plus some new oil flows, etc. By going directly to maximum pressure, some channels will be blocked, thereby decreasing yield.
 
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randomtoker

Well-Known Member
Great vids, pics, and info going on here on this page of posts.

From my limited experience, my thoughts and observations match up with what people are talking about. I seemed to get a great return recently by pressing for a minute going from 180f and heating up to 220f over time (just by unplugging and plugging in my hair straightener). I also slowly closed the grip clamp over 20 seconds going from zero pressure to whatever max I could get out of the 600lb clamp. My max pressure isn't near what's required, so that's why I was seeing a near equal return on my 2nd presses doing the same method but going up to 240f over 1.5 minutes.

I'm looking forward to making a little bottle jack press with some plates and heaters so I can do this better in a single press. My clamp experiment and everyone's posts have taught me a lot.
 

Monsoon

Well-Known Member
Anyone here try BlackLabelPaper parchment yet? Supposedly they made it specifically with concentrate use in mind and they sell it cut and folded to size and in different weights. I'm probably going to order some soon to use for when my plates arrive next month. The 35lb seems to be what's recommended for rosin pressing but they also have 50lb which might be better for high pressure testing.
 

BoogerMan

Well-Known Member
I got my titanium foil in today.

I'm going to rule it out.

The bud was very hard to remove and came apart in chunks. Collection was not super easy either. I had to use a flat tip tool to scrape it up. The stamp and eraser method did not work on Ti foil.

@Monsoon that looks interesting! Let us know how it goes. I don't understand what the weight of the paper means though? :huh:
 

BoogerMan

Well-Known Member
@Pyr0 @Monsoon thanks!

Has anyone tried some thicker PTFE yet? I remember talks of it but not sure if anyone tried it.

Sorry about my previous post. I was so vaked that I forgot to upload pics. I uploaded them to photobucket and everything. Just forgot to attach them to the post :wave: ha.

Anyways here they are.

Before press
C29DB7EA-E352-4F9B-85C1-99E442157935_zps7rytdfcn.jpg


After press (it pooled up nicely, but bud removal and collection failed lol. The rosin didn't seem to flow out as far away from the bud as it does on parchment).
BD0E02DC-F1E9-4636-A25D-13994B2AE4EA_zpsppfkgoxf.jpg


And after my attempt to remove the bud
30018D5D-46D3-48BD-A5A5-86332B827135_zpsbzk9ul11.jpg


I guess it is not as non stick as I thought :\ well at least it's not after 2,500 psi :lol:
 

CrazyDiamond

Crosseyed & Painless
@BoogerMan leads the way again! The oil looks watery too...thank you for spending the time and money on all that you do...agreed, Ti paper a big out!

@ixtapa I'm not sure we can equate viscosity and temperature. Viscosity is, in very simple terms, how thick or thin a liquid is. I think in our case, how much does it flow is an issue too. If it's too viscous, it will just pool on top of the flower. So I think we need to look at the mechanism that makes the oil flow out of the flower. Someone mentioned an interesting thing about those microchannels the oil flows through and out of the flower...too much pressure crushes those and the oil doesn't flow nearly as well. @BoogerMan has demonstrated diminishing returns above a certain psi/tonnage...there is definitely a sweet spot for pressure as well as temperature. Myself and others have shown great results between 180 (more sappy) to 220 and a little above for more shatter consistency (I prefer around 210-215 for my setup since I get the more snappy/pull). I really believe @farscaper is on it with the steam concept. Because of the pressure, I believe that your plates do not have to be at the boiling point of water, but there is a fine line of too low a temp and not getting the "steam" effect for lack of a better term. Again, just my thoughts and ymmv.
 

Monsoon

Well-Known Member
@Pyr0 @Monsoon thanks!

Has anyone tried some thicker PTFE yet? I remember talks of it but not sure if anyone tried it.

Sorry about my previous post. I was so vaked that I forgot to upload pics. I uploaded them to photobucket and everything. Just forgot to attach them to the post :wave: ha.

Anyways here they are.

Before press
C29DB7EA-E352-4F9B-85C1-99E442157935_zps7rytdfcn.jpg


After press (it pooled up nicely, but bud removal and collection failed lol. The rosin didn't seem to flow out as far away from the bud as it does on parchment).
BD0E02DC-F1E9-4636-A25D-13994B2AE4EA_zpsppfkgoxf.jpg


And after my attempt to remove the bud
30018D5D-46D3-48BD-A5A5-86332B827135_zpsbzk9ul11.jpg


I guess it is not as non stick as I thought :\ well at least it's not after 2,500 psi :lol:
Well thanks for trying it and sharing the results. Random thought, I wonder if it would be possible to coat the metal sheets in the same silicone coating used on parchment?

I've got a bunch of OilSlick Sheets so I'll probably be trying those out as well. I may just end up using it for the outer collection sheet and then use parchment for the enchilada/burrito.
 

poonman

Well-Known Member
So I tried my clothes' iron with the steam/spray button
and it worked like a charm . I was able to re-hydrate both
sides of the chips with an even application of moisture in
short time . Ya the 2nd presses provided a much darker yield .
I'd also tested with some fresh nugs , and visually it looked
like slightly more return and slightly darker .

So currently , we are experimenting with some .
1. adding pressure as we press .
2. ramping up the heat as we press .
3. rolling/moving press to squeeze out ala toothpaste .
4. adding moisture to assist in extraction . ( maybe during press )
5. different parchment/foil .


@BoogerMan
Thank you again , for experimenting .
Why didn't your bud stay intact after pressing like usually ?
Why did it break apart ?
 

BoogerMan

Well-Known Member
@BoogerMan leads the way again! The oil looks watery too...thank you for spending the time and money on all that you do...agreed, Ti paper a big out!

Yeah the oil did turn out sappy/wet. But on parchment, this is the same strain the gets super shattery. Interesting right?

Something is going on with the moisture/steam if I were to guess. The Rosin did not flow out as far like it does on parchment. I think more moisture stayed around or something :shrug:

Well thanks for trying it and sharing the results. Random thought, I wonder if it would be possible to coat the metal sheets in the same silicone coating used on parchment?

I've got a bunch of OilSlick Sheets so I'll probably be trying those out as well. I may just end up using it for the outer collection sheet and then use parchment for the enchilada/burrito.

Yeah a more nonstick coating on the Ti foil may help. Hopefully we find something better and more reusable soon. I feel like that is the last missing puzzle piece!

what about chucking a nug in one of the little mesh bags in the titanium sheet? Maybe that way you wouldn't have to worry about peeling it off the titanium in bits?

I really don't like the mesh bags for small runs. It absorbs too much of the oil. I can see how they would work well for fine material or hash and for large amounts of nug, but I only do 0.5g at a time (and that's just about my limit with the small size plates I use) so they aren't ideal for me.

I would try it to see if it would work better with the Ti foil, but I sold the little mesh bags when I sold the D nail press. Sorry man!

So I tried my clothes' iron with the steam/spray button
and it worked like a charm . I was able to re-hydrate both
sides of the chips with an even application of moisture in
short time . Ya the 2nd presses provided a much darker yield .
I'd also tested with some fresh nugs , and visually it looked
like slightly more return and slightly darker .

So currently , we are experimenting with some .
1. adding pressure as we press .
2. ramping up the heat as we press .
3. rolling/moving press to squeeze out ala toothpaste .
4. adding moisture to assist in extraction . ( maybe during press )
5. different parchment/foil .


@BoogerMan
Thank you again , for experimenting .
Why didn't your bud stay intact after pressing like usually ?
Why did it break apart ?

I have a couple guesses.

Not all of the oil got pushed out of the bud so the stickiness made it not come off in one piece.

The Ti foil is not as non stick as we thought. Maybe that is why the oil stuck onto the bud and didn't flow out as far as normal.

The Ti effected the heat which effected how the steam plays a role with the rosin flow.

I'm excited to hear how all of those turn out, specifically #3 :tup:
 

ixtapa

Well-Known Member
@ixtapa I'm not sure we can equate viscosity and temperature. Viscosity is, in very simple terms, how thick or thin a liquid is. I think in our case, how much does it flow is an issue too. If it's too viscous, it will just pool on top of the flower. So I think we need to look at the mechanism that makes the oil flow out of the flower. Someone mentioned an interesting thing about those microchannels the oil flows through and out of the flower...too much pressure crushes those and the oil doesn't flow nearly as well. @BoogerMan has demonstrated diminishing returns above a certain psi/tonnage...there is definitely a sweet spot for pressure as well as temperature. Myself and others have shown great results between 180 (more sappy) to 220 and a little above for more shatter consistency (I prefer around 210-215 for my setup since I get the more snappy/pull).

The formula I cited refers to kinematic viscosity, which is a function of temperature. Lowering viscosity is exactly the factor that would increase flow. So from a purely flow (yield) point of view, higher temperatures are better. In practice, however, increasing temperatures is of limited use, as we start losing desirable volatiles, THC converts to CBN, let alone the consistency of the end product as you mentioned. So there clearly is an ideal temperature in our use - as hot as possible without decarbing, boiling off terps, and leaving the desired end product (from sap to shatter). I am not proposing 300C pressings! I am simply curious if there is a better method for heating than hot plates, which are very inefficient at transferring heat to non-thermally conductive material in a short time.

I really believe @farscaper is on it with the steam concept. Because of the pressure, I believe that your plates do not have to be at the boiling point of water, but there is a fine line of too low a temp and not getting the "steam" effect for lack of a better term. Again, just my thoughts and ymmv.
I will begin by saying I absolutely do not know what is happening between the plates when pressure is applied. That said, the steam theory doesn't seem plausible to me. Hear me out. People have gotten great results with high pressure below the boiling point of water - you mention 180F. But remember, boiling points go UP under high pressure - that's the other end of the stick that allows purging solvents out under a vacuum. There is no steam at 180F. There is no steam at 210F. Under high pressure, there is no steam at 250F. But we see good results at all of these temperatures. This forces me to think that the steam theory, while a good one, is not the prime factor here. The only possible way steam was generated at 180F is if the pressure created friction to the tune of 32F within the plant matter itself. If you squeeze a bud with no heat at all, would it be hot to the touch? If so, the steam theory is still alive. If not, I just can't see where the steam comes from.
 

shark sandwich

"shit sandwich"
Accessory Maker
I will begin by saying I absolutely do not know what is happening between the plates when pressure is applied. That said, the steam theory doesn't seem plausible to me. Hear me out. People have gotten great results with high pressure below the boiling point of water - you mention 180F. But remember, boiling points go UP under high pressure - that's the other end of the stick that allows purging solvents out under a vacuum. There is no steam at 180F. There is no steam at 210F. Under high pressure, there is no steam at 250F. But we see good results at all of these temperatures. This forces me to think that the steam theory, while a good one, is not the prime factor here. The only possible way steam was generated at 180F is if the pressure created friction to the tune of 32F within the plant matter itself. If you squeeze a bud with no heat at all, would it be hot to the touch? If so, the steam theory is still alive. If not, I just can't see where the steam comes from.

We know from experimentation that moisture does affect yield, so work is definitely being done by water vapor, and the pressure and flow it creates.

Water does not have to be boiling to create vapor pressure. Water will evaporate at room temperature, and although boiling water vaporizes faster, it's still far from an instantaneous process.

The chart below shows how vapor pressure ramps up with temperature. It shows that 80c water produces about half as much vapor pressure as boiling water, and should vaporize roughly half as quickly.

80c is 176f, and when we press at that temperature, the moisture content will work just the same as it does at higher temperatures, just half as quickly. This is why press times must be increased when using lower temperatures.

SaturationVaporPressure3.gif




Edit:

I've come up with a way to press using a vacuum, and achieve a completely raw extraction!

According to skunkpharm, thc boils at 62.6f / 17c in a 100 Micron vacuum. Terpenes are more volatile and will boil sooner.

This means a 100 Micron vacuum will allow us to collect rosin at room temperature. This is achieved by using the pressure of the press to break open trichomes, vaporizing their contents using vacuum, then recondensing and collecting the vaporized fraction.


Here are the mechanics of it:

A vacuum pump is attached to the outlet of a cold trap like this:

z174238-large.jpg


The cold trap is packed in dry ice, and the inlet of the trap is connected to a flexible silicone tube stuffed full of flowers, maybe even to the point it is stretched out. This stuffed tube is what will be pressed.

A good silicone tube option may be a 4 inch length of 3/4" ID Tygon. There's a special chemical-resistant formulation of Tygon that's made without any plasticizers.

The other end of the silicone tube is connected to a digital vacuum regulator like this:

8701-1331-901_701_detail.jpg


The regulator is set to about 100micron. As the pump pulls a vacuum, the regulator will maintain the vacuum level. The air the regulator allows in will create flow inside the apparatus, from the regulator, through the material, and to the cold trap. This flow should provide the same utility that water vapor does in an open system, facilitating the transportation of the rosin.

The silicone tube would collapse under vacuum, so it must be adequately filled to facilitate flow. With this setup it may be possible to progressively "mash" the material in the tube while turning it, to break open as many trichomes as possible while inhibiting flow as little as possible.

To operate, the cold trap would be chilled, and the silicone tube would be filled then closed/sealed. Next a vacuum is pulled, and once established, the material is pressed. When condensate collection tapers off, the vacuum is let off and the silicone tube is refilled. The cold trap could be used for multiple pressings, and will only need to be emptied when full/desired.
 
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farscaper

Well-Known Member
anyone tried super low temp pressing...

under vacuum?
:cool:


Concerning @farscaper's vacuum question, pressing under vacuum would increase the amount of yield lost due to evaporation. @Joel W. has measured and quantified this loss- nearly 10% of the original weight, and that's at normal air pressure!

Terpenes and even thc will boil and evaporate at room temperature under vacuum. If we're at temperatures where actives are already boiling off, and we apply a vacuum, the loss will increase significantly. It would be interesting to use either a pressurized environment, or chilled collection sheets try to minimize that 10 percent loss. If joel is getting 10 percent loss and 20 percent returns, that means 30 percent should be achievable when the loss problem is solved.

We know from experimentation that moisture does affect yield, so work is definitely being done by water vapor, and the pressure and flow it creates.

Water does not have to be boiling to create vapor pressure. Water will evaporate at room temperature, and although boiling water vaporizes faster, it's still far from an instantaneous process.

The chart below shows how vapor pressure ramps up with temperature. It shows that 80c water produces about half as much vapor pressure as boiling water, and should vaporize roughly half as quickly.

80c is 176f, and when we press at that temperature, the moisture content will work just the same as it does at higher temperatures, just half as quickly. This is why press times must be increased when using lower temperatures.

SaturationVaporPressure3.gif




Edit:

I've come up with a way to press using a vacuum, and achieve a completely raw extraction!

According to skunkpharm, thc boils at 62.6f / 17c in a 100 Micron vacuum. Terpenes are more volatile and will boil sooner.

This means a 100 Micron vacuum will allow us to collect rosin at room temperature. This is achieved by using the pressure of the press to break open trichomes, vaporizing their contents using vacuum, then recondensing and collecting the vaporized fraction.


Here are the mechanics of it:

A vacuum pump is attached to the outlet of a cold trap like this:

z174238-large.jpg


The cold trap is packed in dry ice, and the inlet of the trap is connected to a flexible silicone tube stuffed full of flowers, maybe even to the point it is stretched out. This stuffed tube is what will be pressed.

The other end of the silicone tube is connected to a digital vacuum regulator like this:

8701-1331-901_701_detail.jpg


The regulator is set to about 100micron. As the pump pulls a vacuum, the regulator will maintain the vacuum level. The air the regulator allows in will create flow inside the apparatus, from the regulator, through the material, and to the cold trap. This flow should provide the same utility that water vapor does in an open system, facilitating the transportation of the rosin.

The silicone tube would collapse under vacuum, so it must be adequately filled to facilitate flow. With this setup it may be possible to progressively "mash" the material in the tube while turning it, to break open as many trichomes as possible while inhibiting flow as little as possible.

To operate, the cold trap would be chilled, and the silicone tube would be filled then closed/sealed. Next, a vacuum is pulled, and once established the material is pressed. When condensate collection tapers off, the vacuum is let off and the silicone tube is refilled. The cold trap could be used for multiple pressings, and will only need to be emptied when full/desired.

I knew we would get there eventually, the hardest part was waiting.
;)
 

shark sandwich

"shit sandwich"
Accessory Maker
@farscaper

Thanks for digging up those posts, and for asking a great question!

It's cool to see the solution laid within the original problem, and just needed to be extrapolated and engineered. I may have been lacking vision when I composed my initial response, but the idea stuck with me, as you can see!
 
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