The Science & Economics of CO2 Extraction and Oil Manufacturing
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What are you extracting for, and to what scale? This talk explores scientific methodologies to optimize your extract manufacturing by using univariate and multivariate DoE techniques.
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The Science & Economics of CO2 Extraction and Oil Manufacturing
- 1. www.outco.com Blake Grauerholz Extraction Manager OutCo, San Diego 1 The science and economics of CO2 extraction and oil manufacturing
- 2. www.outco.com • Production Yield • Production Costs • Extract Constitution/Quality • Legal Aspects 2 What is the best extraction system?
- 3. www.outco.com For what: • Yield per Run YpR • Yield per Week YpW • Cannabinoid Conc. CC • Terpene Content TC • Extraction Efficiency EE 3 Optimizing your extraction process With what: • Temperature T • Pressure P • Time t • Flow Rate FR • Particle Size PS
- 4. www.outco.com For what: • Yield per Run YpR • Yield per Week YpW • Cannabinoid Conc. CC • Terpene Content TC • Extraction Efficiency EE 4 Optimizing your extraction process With what: • Temperature T • Pressure P • Time t • Flow Rate FR • Particle Size PS
- 5. www.outco.com For what: • Yield per Run YpR Optimizing your extraction process With what: • Time t 0 100 200 300 400 0 5 10 15 20 25 30 35 40 YieldTHC(g) Time (t) Optimizing Run TimeExperiment t (h) YpR (g) 1 4 53 2 8 103 3 18 263 4 34 367 Raw n/a 500
- 6. www.outco.com For what: • Yield per Run YpR • Yield per Week YpW • Cannabinoid Conc. CC • Terpene Content TC • Extraction Efficiency EE 6 Optimizing your extraction process With what: • Temperature T • Pressure P • Time t • Flow Rate FR • Particle Size PS
- 7. www.outco.com For what: • Yield per Run YpR Optimizing your extraction process With what: • Particle Size PS Experiment PS (mm) YpR (g) 1 6 215 2 4 230 3 2 235 4 1 253 210 220 230 240 250 260 0 1 2 3 4 5 6 7 YpR(g) PS (mm) Optimizing Particle Size
- 8. www.outco.com Chemometrics is the science of relating measurements made on a chemical system or process to the state of the system via applications of mathematical or statistical methods. The design of experiments (DoE) is used to gather as much useful information about the influence of factors on a certain response in an effective and economical way. 8 Introduction of Chemometrics and Design of Experiment
- 9. www.outco.com 1. Defining the problem • Extracting Cannabis with a 20L, 2000psi SFE 2. Determine the response • Yield THC • Percentage Terpenes 3. Determine the factors • Temperature and Pressure 4. Additional things to keep in mind • Comparison • Replication • Blocking • Orthogonality 9 Designing the first Design of Experiment
- 10. www.outco.com Temperature (˚C) Pressure (psi) Yield THC (g) 34 60 1100 1900 47 1500 0 Executing the DoE Critical Point: 304.25 K & 72.9 atm Factor No. Factor Lower Level Upper Level Unit 1 Temperature 34 60 ˚C 2 Pressure 1100 1900 psi Expt. No. Temp. (˚C) Pres. (psi) A 34 1100 B 34 1900 C1 47 1500 C2 47 1500 D 60 1100 E 60 1900
- 11. www.outco.com Executing the DoE Critical Point: 304.25 K & 72.9 atm Factor No. Factor Lower Level Upper Level Unit 1 Temperature 34 60 ˚C 2 Pressure 1100 1900 psi Expt. No. Temp. (˚C) Pres. (psi) THC (g) % Terp. A 34 1100 2.00 63.4 B 34 1900 334 6.30 C1 47 1500 17.9 39.5 C2 47 1500 18.1 36.0 D 60 1100 0 0 E 60 1900 144 10.2 Temperature (˚C) Pressure (psi) Yield THC (g) 34 60 1100 1900 47 1500 0 400
- 12. www.outco.com A Taylor expansion describes the response surface. Matrix algebra solves the Taylor expansion. Y=bX b=(X’X)-1X’Y a=bX 12 Calculating response surface of DoE 𝒚 = 𝜷 𝟎 + 𝒊 𝜷𝒊 𝒙𝒊 + 𝒊 𝜷𝒊𝒊 𝒙𝒊 𝟐 + 𝒊 𝒋 𝜷𝒊𝒋 𝒙𝒊 𝒙𝒋
- 13. www.outco.com a= - 47.95 xT + 119.05 xp - 46.95 xTxp 13 Analyzing the DoE, THC yield
- 14. www.outco.com a= - 14.875 xT - 11.725 xp + 16.825 xTxp 14 Analyzing the DoE, %Terpene
- 15. www.outco.com • Having enough material • Separator conditions uncontrolled • Chiller trouble • Unstable conditions • Machine breakdown 15 Problems with DoE
- 16. www.outco.com • Sub-critical • More factors, more focus • MORE DATA 16 Future plans
- 17. www.outco.com 17 Rest of OutCo science team: Taylor Trah, Dr. Markus Roggen OutCo Cultivation: Dr. Allison Justice, Chris Cortina, Rick Padilla OutCo Management: Lincoln Fish, Austin Birch, Ben Ballard, Alex Bryan Thank You
- 18. www.outco.com 18 ●Solubility of THC and other cannabinoids in supercritical CO2 • J. of Supercritical Fluids 52 (2010) 6 • J. of Supercritical Fluids 55 (2010) 603 ●Introduction to Design of Experiment • Fisher, R.A., The Design of Experiments. Vol. Second Edition. 1937: Oliver and Boyd • Stansbury, W.F., Development of experimental designs for organic synthetic reactions. Chemometrics and Intelligent Laboratory Systems. 36 (1997) 199 Further Reading:
Editor's Notes
- In this talk I want to discuss our efforts at OutCo of optimizing our extraction processes to deliver the best product to the costumer at the best value for both them and us as the manufacturer. I will present how we applied design of experiment principles to optimize our extraction process. And now that it is late in the day and we already listened to so many great talks, I thought it might be time we finally get to do some math and solve a second order Taylor expansion. I hope this talk can serve as guide for everyone to apply to their process.
- But first, what is the best extraction system? Everyone has the best method, everyone makes the best concentrates. But what is the definition of the best? Do we want to get the highest yields? Last week we juiced the fresh leaves and got about 40% yield. But it was green water, with a few pieces of fiber. Not really what we want. Do we want low production costs? Extracting stems in a pipe with a lighter stuck on the top is really cheap. Also not desirable. So I think we should concentrate on Extract Constitution/Quality. We can agree that an oil of high THC concentration with lots of terpenes is desirable. Although, we always should keep laws and regulations in mind.
- Let’s assume that we chose an extraction method, bought the machine, now what? How do we go about optimizing the process. First we have to decide what we are actually looking for. My offers are: Yield YpR: yield of oil recovered per run Important if you have limited resources Yield YpW: yield of oil produced per week Important if you have unlimited resources / This is different then YpR, as it is a measure of time, not batches. Cannabinoid Concentration CC: percentage of total oil If we are honest, that is what most people care about Terpene Content TC: percentage of total oil This is what people should care about Extraction Efficiency EE: percentage of cannabinoids removed Again important if you have limited resources And we can change these factors: Temperature T: Set point of chiller Pressure P: Set point of extractor pressure Time t: Run time Flow Rate Operator ID: person loading and unloading the extractor Particle Size PS: Grind/screen size
- We naturally chose to change the run time from run to run, but hold everything else the same. Therefore the pressure and temperature settings, and the rest, are not important right now.
- And with just four experiments we already can see that if we run the extractor longer we get more THC out. As we also tested the starting material, we know that even after 34 hours we still have not extracted all THC out of the plant. So lets keep going?! But, wait, maybe if we increase the pressure we can extract faster? It turns out we can (see reference), but then we have to do the run time experiment again. And what about temperature? And the other factors? That will be quite some work to zero in on the optimal conditions.
- Lets look at something most of us might not think about at first. The effect the particle size of the raw material can have on extraction yields.
- 2kg plant matter, 6 hours run time. We used a Fritsch Mill to grind all trim to a consistent size. And we saw very quickly that the smaller the particle, the faster we can extract. We did not observe chlorophyll ‘wash out’
- Math: yeah! Statistics: yeah! Basically, this approach will allow us to test many different factors, like temperature, pressure and time, at the same time. Afterwards, with the help of mathematical analysis we can figure out how every factor influences each other and the response, be it the THC yield.
- Let’s start designing this DoE Defining the problem Extracting Cannabis with a 20L, 2000psi SFE Determine the response Yield THC Percentage Terpenes Determine the factors Temperature and Pressure Constant: Time, flow rate, Additional things to keep in mind Comparison: Ensure that every experiment is done on the same conditions, e.g. particle size, extract weight, extract type, operator Replication: Rerun experiments to evaluate variance and standard deviation Blocking: Do the experiments in one sweep to mitigate unexpected trouble Orthogonality: Chose factors that complement each other, not overlay, like time and flow rate
- Considering all these points, we arrive at a design with the following limits: Temperature 34 to 60˚C and pressure 1100 to 1900 psi. Please note the choice of units, both metric and imperial. Take it as a stand in for the current state of cannabis: Still torn between worlds. To cover the whole space of possible pressure and temperature combinations we chose a star design. We replicated the central point conditions.
- Here are the results
- The Taylor expansion includes second order behavior, namely the correlation between temperature and pressure and their influence on the system. All factors are paired with a coefficient ß to scale their influence on the system. Y is the result (response) matrix, X is the parameter (factor) matrix, and b is the coefficient matrix.
- a is the Taylor expansion, showing a strong correlation between pressure and THC yield, and an inverse correlation between temperature and THC yield. This can be explained by the effects that pressure and temperature have on CO2 density. And here is the response surface. We can clearly see that the best conditions are at the highest pressure and lowest temperature of your test area. We are now boxed in as we cannot go lower in temperature, as we are near the supercritical point, and our instrument does not allow for higher pressures.
- The Taylor expansion for the Terpene percentage in the extract looks very different. One cannot generalize a relationship between terpene percentage and temperature or pressure. The Response Surface shows that a low pressure and temperature is optimal for high terpene percentage in the extract.
- Problems with DoE Having enough material 4kg per run, 6 runs plus 1 spare, 28kg of the same material. The solution: Kitchen sink Separator conditions uncontrolled The temperature of the separator is passively influenced by extractor pressure and temperature. Variation between runs! Chiller trouble Chiller started to break down Unstable conditions We observed that the pressure and temperature did fluctuate around the set point. That makes these tests results very difficult to reproduce on other systems Machine breakdown The day after the last experiment for this DoE the machine broke down. And as it was the holidays, it took ages to get going again. Unfortunately, I do not have any further studies to present.
- That brings me to the question of what is next. We want to repeat this two factor design (temperature and pressure) in the sub-critical / liquid CO2 space. Maybe the optimal conditions lie there. The presented response surfaces seem to point towards it. After we are done with these two small scale DoEs, we will run a larger study, including at least 5 factors to really find the best conditions. That study will need at least 34 experiments and well over identical 100kg of trim.
- Thank to all Vertical integration