Supercritical CO2 Extraction

extraktLAB’s supercritical CO2 extractors are highly efficient and increase overall extraction yield. They are also capable of decreasing your yearly operating costs and leave scale up opportunities.

No, the material does not need to cure. Our methods complete the final drying step in a vacuum oven to bring the water content down from 10% to the 1% – 1.5% range for efficient CO2 extraction.

There are several drying methods used by growers to accelerate drying, but this is outside our scope of solutions. We recommend researching the agricultural methods to find what works best for you.

Harvest drying methods are outside the scope of our solutions; however, you want to dry the biomass to roughly 10% water content for quality storage to prevent mold or mildew.

Typically flowers and leaves – no stems or stalks. Some producers will sort out the flowers and process them separately, but most processing includes the leaves and flowers.

Yes, ethanol can become contaminated during ethanol extraction. It is important that you address the contamination with testing and reuse protocols. guidance for solvent reviews have been published by the FDA in 2010. Please refer to the many articles in this blog for more information on cross-contamination with extraction.

Hemp and cannabis biomass is an extremely absorbent material.  As a consequence, a large amount of solvent volume must be added to the biomass to first solvate the biomass and then fluidize it. For ethanol extraction, approximately one gallon of ethanol is required to extract 1 lb of hemp. Solvent loss comes from the incomplete recovery of that solvent from the hemp.

The following table details the estimated solvent loss from ethanol extraction as a function of volume of hemp processed:

Lbs processed per day	Daily requirement of  ethanol  (gallons)	Daily Loss of ethanol (gallons) at 90% recovery of ethanol	Max Cost of Solvent Loss per day: $16-30/gal food grade ethanol $6-8/ gal denatured Calculated at $30/gal
500	500-1500	50-150	$1,500-45,000
1000	1000-3000	100-300	$3,000-9,000
2000	2000-6000	200-600	$6000-18,000
10000	10000-30000	1000-3000	$30,000-90,000

 

 Another source of solvent loss is incomplete recovery of solvent from the CBD hemp oil. 

Processing a ton of hemp per day into extracts  can be an energy-intensive process depending on how the hemp is extracted. The following table compares the energy expense for ethanol extraction versus the energy expense for CO₂ extraction:

Energy cost for Ethanol Extraction for 1 ton per day at 1 gallon ethanol per 1 lb of hemp
18711	litres to cool from 25 to -20
16840	litres to heat and evaporate after ethanol loss
454	kwhr to Cool from 25 to -20
481	kwhr to heat to boiling point
3105	kwhr to evaporate
4040	kwhr total @ 100% Efficiency
75%	Efficiency
5387	kwhr Total
$           0.09	per kwhr
$          506.36	per day

 

Energy cost for CO2 Extraction at 1 ton per day including winterization
636	litres to cool from 25 to -20
636	litres to heat and evaporate after ethanol loss
15	kwhr to Cool from 25 to -20
18	kwhr to heat to boiling point
117	kwhr to evaporate
151	kwhr total @ 100% Efficiency
75%	Efficiency
201	kwhr Total
$           0.09	per kwhr
$        18.92	per day for winterization
43.20	Kwhr per day for CO2 extractors
$         3.88	Per day for CO2 extractors

In guidance published by the FDA in 2010,  plans for the reuse of solvents  must be accompanied by a  Declaration of the maximum number of times the solvent can be reused. 

 the FDA has recognized that contaminants buildup in the solvent over time as they are  recovered and reused  

As a consequence, the FDA guidelines recommend that the solvents be brought back to a suitable state before Reuse. A suitable reuse is defined by  the original specifications for the solvent that is being used.  

 In keeping with a risk-based approach to process validation, the key risk to address with solvent reuse is cross-contamination. Cross-contamination could happen when a  solvent dissolves a low level contaminant  from the biomass being extracted. As the solvent is removed, the contaminant can become magnified and concentrated in either the oil or the solvent during solvent recovery. Cross contamination then occurs when a contaminated solvent is used to extract a non contaminated batch.

Contaminants are typically identified during incoming inspection  but may show up  later during processing  as the oil becomes more refined. Hemp is typically sampled at receiving by quality assurance and a series of tests are conducted on the Hemp biomass in order to determine if the incoming material  is contaminated with pesticides, solvents, heavy metals or if it has significant microbial content. Contaminants that are identified in the quality inspection should be tested for build up in the extraction solvent during validation.

Other sources for contamination include carbon black or activated carbon that is typically used in ethanol extraction to remove chlorophyll from the ethanol. Combustion byproducts that are incorporated into the structure of carbon black can dissolve in the ethanol  and contaminate.

According to FDA guidelines, the number of times ethanol solvent can be reused must be validated according to a validation protocol. Once the method and process has been validated, the requirements for testing each reuse batch  may not be required depending on the risks identified during the validation study.

 As a general rule of thumb, a solvent may be reused successfully 20-50 times. Whatever your company’s current practice is, it is important to define the process, validate the process, establish specifications for reuse, and also set up a testing program to measure for contaminants. In all likelihood, a solvent changeover is probably in your future  and it’s cost should not be neglected in your overall operating cost model. It is easy to estimate the cost of solving change over as it is the same as the start-up cost:

Lbs processed per day	Daily requirement of  ethanol  (gallons)	Cost per gallon: $16-30/gal food grade $6-8/ gal denatured Calculated at $30/gal
500	500-1500	$15,000-45,000
1000	1000-3000	$30,000-90,000
2000	2000-6000	$60,000-180,000
10000	10000-30000	$300,000-900,000

 

 The solvent changeover cost on a 60 day change over cycle can then be estimated on a per year basis according to the following table:

Lbs processed per day	Change Over Frequency	Cost of Changeover	Max Annual Cost
500	60 days	$15,000-45,000	$270,000
1000	60 days	$30,000-90,000	$540,000
2000	60 days	$60,000-180,000	$1,080,000
10000	60 days	$300,000-900,000	$5,400,000

 

By extension, the solvent testing costs will also be important to address:

Lbs processed per day	Change Over Frequency	Cost of Testing (pesticides, solvents),  Unknowns testing can be 5-10k USD per unknown.	Max Annual Cost
500	60 days	$200-400	$2400
1000	60 days	$200-400	$2400
2000	60 days	$200-400	$2400
10000	60 days	$200-400	$2400

 

 It is important to insist that unknowns be flagged by your laboratory. 

Supercritical CO2 extraction is used in hemp processing in hemp extraction for extracting CBD oil from hemp biomass. You can also be used to extract any Botanical oil from any plant material.

The co2 extraction typically takes place above the supercritical pressure and temperature for CO2. Is 1,070 PSI and 31 degrees Celsius.

Under supercritical conditions, the CO2 behaves much like hexane in terms of its solubility selectivity.

Due to the risk of chemical contaminants that are found in 25 to 30% of  ethanol extracted oils, we recommend that CO2 oils be used for Vapor Products.

It is absolutely possible to make a solventless extract with CO2. Solventless extracts are typically made with subcritical CO2 extraction methods.

Hemp processing equipment can be scaled for 1 to 5 tons of extracted hemp per day. It’s generally not a fair comparison to compare the throughput on an instrument from two different companies. What is fair is to specify the throughput At the tonnage process per day and then look at the operating cost for that process. You can also look at the equipment and Facilities cost to accommodate that level of Production. after you have all of your costs accounted for including the hidden costs, then you can calculate the net present value for each investment.

Denatured ethanol is a mixture of denaturants and pure ethanol. Chemical companies add the denaturant to Pure ethanol so that they will not be consumed as a food.
Denatured recipes are published by the ttb that is administered by the National Bureau of Alcohol Tobacco and Firearms. There are many different recipes. one of the most common denaturants used in ethanol extraction is heptane. However there are other substances that may be used including acetone, isopropyl alcohol, methanol and other longer chain alcohols.
Is very limited data on the safety of heptane over the long term exposure. In fact the limit that the FDA has placed on the amount of heptane in a tincture for example was established in the 1990s on the basis of a single study published in 1981. That study the effect of heptane on Sprague dawley rats. That is why there are many disclaimers and the general guidance from the FDA is to limit the amount of solvent in any drug that is consumed.

No. Approximately 5 to 10% of the ethanol is left in the biomass and is counted as a solvent loss. These solvent losses add up to operating costs. This is especially true if organic ethanol is used or food grade ethanol is utilized as the extraction solvent.

Ethanol extraction typically destroys the terpenes when the ethanol is removed from the extract or is distilled from the winterized oil. Many ethanol extractors are seeking a way to preserve the terpene profile of the plant in the output oil. To this end people have tried techniques such as Steam distillation, CO2 stripping, and vacuum distillation.
Certainly, CO2 can be used to strip terpenes from Hemp biomass Prior to ethanol extraction. However, vacuum distillation is by far the most gentle and effective way to harvest the terpene profile prior to ethanol extraction.

CO2 extraction facilities have been scaled to do hundreds of tons per day of biomass extractions. These facilities are very safe compared to the equivalent extraction facilities that use Flammable solvents.
In Terms of extraction facilities for processing hemp, we have built facilities that will process 5 tons of hemp biomass per day in a safe, low cost, low energy, small footprint operation.

There are many inputs that need to be defined when creating a financial model comparing two different extraction methods. The first decision to be made is to decide what the financial metric will be used to make a decision on the superiority of one method over the other. 

In this case, we recommend the use of the Net Present Value as the way to model the return of each extraction technique because it accounts for the cash flow associated with the operation. Many ethanol extraction companies try to make the argument that ethanol extraction is lower cost because the equipment cost is less. However, the equipment cost will have very little impact on the overall profitability of the operation at the same throughput.

The best way to compare the two techniques is to fix the throughput so that an apples-to-apples comparison can be made. Comparisons such are payback time and return on investment can mislead someone into making a bad investment decision. 

So if we fix the throughput at one ton per day the cost of the hemp is equal between the techniques and operating cost variance is the only contributing factor.     

Here are the twelve key questions that need to be defined in order to do a comparison:

1. What is the direct labor to process?
2. What is the energy to process?
3. What are the solvent losses? 
4. What are the direct material startup costs including solvent startup costs?
5. What are the cannabinoid recovery rates?
6. How much solvent do I use, reuse, and when do I need to replace the solvent with fresh solvent?  and at what interval?
7. What is the insurance cost for each option?
8. What is the cost of hazardous waste disposal?
9. What is the cost of solvent removal?
10.  What is the cost of reuse of the solvent?
11.  What is the cost of HAP emissions?
12. What is the depreciation for each option including building costs for H2 vs F2 occupancy?

Once these questions are answered you will be able to build a pro forma income statement. 

Revenue

• Standard labor
• Standard materials
• Overhead

Gross margin

• SGA
• R&D

Net Margin

You can then hold SG&A and R&D constant for both techniques and account for the difference in depreciation to get to a net margin number.  

A cash flow statement can then be generated from net margin. One thing to note is that depreciation must be added back to net margin as it is a non-cash expense on the income statement.  

Cash flows are then added up for 5 consecutive periods (years) including the initial outlay of cash for startup working capital.  Those cash flows are then discounted at a discount rate (Weighted average cost of capital estimate at 13-17%).  

If you do this analysis, you will find that CO₂ extraction will absolutely crush ethanol extraction in terms of net present value.  

Yes.
In fact the operating cost for CO2 extraction is dramatically less than the operating costs associated with ethanol.

Extraction with Ethanol is a process that is typically run at low temperatures. First the ethanol is cooled to below -20oC before it is introduced to the hemp. Cooling the ethanol reduces the amount of extracted chlorophyll and waxes. If you account for the energy required to chill the ethanol down to those low temperatures and then also evaporate after use, the energy bill for extracting ethanol is approximately 3-6x the cost of extracting with CO2. However, the energy cost is really not the key driver in the overall operating costs.
Ethanol extraction requires a significant amount of ethanol to be used per pound of hemp. In fact, about 1 to 1.5 gallons of ethanol must be used per pound of dry hemp in order to extract. Hemp is a very absorbent biomass material and the ethanol must fully saturate the hemp plant before any extraction can take place. For this reason a large volume of ethanol is needed to extract cbd from hemp.
The key cost driver or ethanol extraction is recovery of that solvent from the biomass. Even though many ethanol extraction equipment companies provide centrifuges and or presses to eliminate the amount of ethanol left over in the biomass, The best equipment will provide only a 90 to 95% recovery of the ethanol. This 5 to 10% loss in ethanol is a huge cost driver for extracting ethanol.
For example, suppose you wanted to process 1000 lb of hemp. You would need 1000 gallons of ethanol to start out at a cost of $16-33 per gallon for food grade ethanol for a total cost of $16,000 to $33,000. If you recovered 90% of the ethanol the ethanol loss would be $1,600 – $3,300 per 1000 lbs. Furthermore if you process 1000 pounds per day, this would be your daily loss.
In contrast, you will lose the equivalent of about $70 per day for CO2 extractions for the exact same process.
Besides energy and solvent usage, there are many other hidden costs related to extraction with ethanol including solvent reuse costs, insurance cost, increased facilities cost, and testing costs.

Industrial Hemp extraction typically has a CBD content of 5 to 15% by weight. The THC content of the Industrial Hemp is required by law to be less than 0.3% by weight in the flower that is sold.

Yes, moisture content will affect weight yield. For example, if 10% of the hemp To be extracted was water, and that water was removed during CO2 extraction, the denominator would be larger in the yield calculation, thereby giving a smaller yield number. By extension, if the same hemp was extracted but had zero water in the hemp, the overall weight percent yield of the extract would be a greater percent of the weight.

One thing to note is that in ethanol extraction, water that is in the hemp will dissolve into the ethanol. If the ethanol is removed from the CBD oil with a falling film evaporator, some of the water will be Co evaporated with the ethanol, thereby increasing the amount of water in the ethanol for each extraction cycle. Some of the water will stay in the extract and is typically removed in a secondary stirred reactor before wiped film evaporator and distillation.

We Have taught hundreds of customers how to extract CBD oils from hemp and THC oils from cannabis. Our training package typically includes installation of the equipment, standard operating procedures, commissioning of the equipment in the facility, and training of operators on the procedures that are provided.

We also offer advanced training and quality management system implementation services for those companies who wish to achieve GMP certification.This training dresses all aspects of the quality management system, laboratory information management, batch record system, and Manufacturing execution.

There are basically four different employees that you need to have in order to run a hemp processing or hemp extraction facility. These are as follows:

1. assurance
2. Shift manager
3. Operators
4. Optionally analytical operators.

If your goal is to produce a quality product that complies with GMP requirements, you are going to need to have staff that can help you comply with those requirements.That typically means you need to have a quality assurance manager that is aware of the requirements And can Implement those requirements in your facility.

It is also necessary that you have a shift manager. This is someone who is organized and can schedule operators at each station and track the production output. This person will also ensure that operator training has occurred, ensure that yields are met, and also manage the workforce. They are also responsible for producing products that can form with the quality requirements of the end product.

Operators typically execute on the production plan by following standard operating procedures. They are typically trained on how to use the equipment and how to move materials in and out of the process. It is their job to record the data for the quality management system. The Operators typically will be successful if they are Hands-On and are able to follow instructions. It is also a big Advantage if the operator can conduct basic maintenance on the equipment. This requires someone who is Hands-On and has the physical strength to do simple maintenance tasks. This is important for the proper running in the efficiency of a hemp processing facility.

Last but not least, analytical operators or quality control technicians are important for providing yield and in-process testing to the manufacturing facility. They will work with quality assurance directly to ensure that incoming raw hemp biomass conforms to purchasing specifications and to Quality specifications. Quality control technicians are typically chemists and have a laboratory background.

Yes.
A pound of food grade ethanol when purchased in bulk is $4.71/lb at current price.
A pound of food grade CO2 when purchased in bulk is about $0.04/lb at current price.

There are many grades of CO2 including industrial and food grade and medical grade. We typically use food grade but medical grade is also highly desirable. the specifications for each of these grades are published by the Compressed Gas Association or by your gas supplier.