ES2942082A2 - Separation of trichomes by the high efficiency wet method. Method and practical application (Machine-translation by Google Translate, not legally binding) - Google Patents

Abstract

This innovation is characterized by the use of the colligative properties of liquid solutions, which allow working with large amounts of plant material rich in trichomes, without contaminating it with the tissue content, enabling its cyclical use during the process and avoiding replacement, making it possible to reuse it many times. This strongly impacts the reduction of operating and environmental costs. There are also numerous technical-economic benefits in production processes. As for example in the production of cannabinoids, with the use of this technique drying is dispensed with, avoiding the high cost of the process and the high investments necessary to build the drying sheds. It also strongly influences the size and facilities needed for the extraction machines, since almost all the active principles of medicinal interest are found in the glandular trichomes of cannabis and the trichomes represent an almost insignificant volume compared to the extraction that is carried out from cannabis. dried flowers. They also reduce to zero the risk of contamination by mycotoxins that can be produced during the drying of the flowers. It preserves almost all of the volatile terpenes, of great medicinal interest, which are lost during drying. Among other advantages. This new procedure results in the construction of a very economical machine, capable of executing the process completely automatically and with a very high efficiency and low operating cost. (Machine-translation by Google Translate, not legally binding)

Description

DESCRIPTION

Separation of trichomes by the high efficiency wet method. Method and practical application

Technical sector

This invention relates to a method for refining plant material. More specifically, it refers to a method to separate glandular trichomes from the plant material that contains them, using chemical solutions designed not to be contaminated with the content of plant tissues during the operation and can be carried out continuously without having to renew them, increasing significantly the industrial efficiency of the procedure by not having to re-cool the new water and the trichomes are separated by filtration.

state of the art

In recent years, the use of medicinal products made from substances extracted from plants or parts of them has increased significantly. Some of them have specialized structures where substances of medicinal interest are produced, including glandular trichomes.

The subspecies of Cannabis sativa are the ones that have increased their importance the most in the treatment of many conditions (refractory epilepsy, neuropathic pain, spasticity and seizures caused by multiple sclerosis, malnutrition, nausea and vomiting induced by chemotherapy, glaucoma, among others). ), and numerous studies are underway with promising results in the treatment of more human and animal conditions. It is also used in phytotherapeutic treatments.

More than 95 percent of the cannabinoids produced by the plant (thc, cbd, cbg, among others) are found in the female flowers and nearby small leaves, in the almost microscopic, specialized capitate glandular trichomes, where they are synthesized together with the terpenes. Both compounds (phytocannabinoids and terpenes) have high medicinal interest individually and their use together produce the "entourage effect" or "entourage effect", which means that they synergize and have a better response with respect to the use of cannabinoids as It is a unique drug, which is why plant extracts are highly valued.

The most widely used technique in the world for the production of medicinal cannabis, involves drying the female flowers of cannabis plants, after their harvest, and then extracting their components used in the preparation of medicines. Due to the fact that post-harvest processing (drying and extraction) requires very onerous and complex structures and machinery, a technological model was designed that allows gradual production throughout the year, with the use of high-cost and sophisticated production structures. to satisfy the requirements of cannabis for its correct growth and productive development when the environmental conditions or the length of the day are not propitious in the different seasons. It is a way of achieving continuous production throughout the year, without incurring the obligation to make large investments in facilities and machinery for post-harvest processing. The drying technique for cannabis flowers must be carried out with strict control of humidity and temperature conditions (around 25 °C and 40-50% RH), in complete darkness and in a time that is around 10 to 25 days duration. If these parameters are not perfectly controlled, there is a great risk that fungi that produce highly dangerous mycotoxins and very low tolerance will develop in the results of the analysis.

Also during the drying process, the inevitable loss of a large amount of volatile terpenes occurs, some of great medicinal importance.

This production technique, which includes the drying of flowers, greatly limits the possibility of carrying out crops without managing production parameters on a large scale (for example in the open sky), since being seasonal in nature, high volumes of flowers would be produced. in short periods of time, which would require having a large number of dryers to be able to process them, with the implication of making onerous investments to be used in that short period of time that the harvest lasts and with the aggravating circumstance of being very specialized structures They do not allow many options for use with other products.

"With the above-mentioned techniques for processing these oil-rich cultivars, it is common in the industry for daily cannabis extraction throughput to be as high as 100 lbs/day, assuming approximately 30 min/Ib for CO2 extraction. This may require an equipment investment of about $0.5 million, and may require a similar investment of $0.5 million or double $1.0 million for drying equipment to speed up drying and curing ". (Extracted and translated from the Backgroud of https://patents.justia.com/patent/9981203.)

The state of the art prior to this invention did not present many options to be able to carry out a complete, large-scale medicinal cannabis production process, avoiding the drying process or making it cheap to implement with recently harvested material.

History and simple methods of obtaining cannabis trichomes: https://www.florprohibida.com/blog/historia-hachis-al-agua/.

https://www.marihuanaonline.net/historia-del-hash-de-agua-helada-y-como-fabricarlo/.

There is a process of separation of trichomes in the wet method with the use of ice, snow or frost and cold water. This procedure and its practical apparatus is patented in 1998, in several countries by the same owner under the title "METHOD AND APPARATUS TO EXTRACT VEGETABLE RESINS" (EP1015118, CA2321815, AU1998063381, DK1015118, ES2262226, DE000069834261, PT1015 118, US6158591).

This method is used to obtain whole and split trichomes, taking advantage of the fact that cannabinoids and the vast majority of terpenes are insoluble in water and cannabis glandular trichomes become very brittle below 4°C. This procedure derives in a very simple device that carries out the process, materialized in an open container where the plant material and ice are placed, stirred with a mechanical tool and a time is waited where the decantation of the particles occurs, which, with a lower faucet are extracted together with the liquid and separated from it with the use of a filter.

https://patents.j ustia.com/patent/6158591

Other variants are currently offered on the market, such as the "ice-o-lator" kit, which allows the process to be carried out with a set of filters of different sizes, which, placed in a bucket, allow the separation of trichomes without the use of an apparatus. (https://www.cactusmartorell.com/blog-cannabico/how-to-extract-your-own-iceolator-hash/).

"Pollenseparator" invented by Elijah Pastarius. This method consists of an apparatus where the plant material is placed with ice and water, which is then filtered through several meshes to separate the trichomes. The commercial application of this patent is "Bubble Now XL".

https://patents.justia_com/patent/8640877

These methods are useful when working with very little volume of flowers, since the use of ice and the problem that the water is inevitably contaminated with the cellular content of the floral tissues makes it inapplicable on large scales, since It implies a great problem in the handling and the cost in the production of ice and cold water for the constant renewal that would demand to process a large quantity of flowers in short periods of time.

There is a Spanish patent "ES 2595090 B1" entitled "Procedure for obtaining plant extracts from glandular trichomes and use of said extracts for the treatment of diseases", invented by Funtane Vendrell José María, who performs separation of glandular trichomes with a rotating drum , but with previously dried flowers.

"Separation of cannabis trichomes using ice water", this method is similar to that of the aforementioned patent (METHOD AND APPARATUS TO EXTRACT VEGETABLE RESINS), but using only ice water. Its inventors are Krupal Pal, Thomas Adam Ulanovsky, IvanCasselman, and RyanDelmoranKo.

https://patents.justia.com/patent/10780442

The company Paralab markets a trichome extractor that uses ice water and is an identical model to the device mentioned in the invention.

https://paralab.es/productos/extractor-de-tricomas/.

"Glass trichome separation method" invented by Krupal Pal, Thomas Adam Ulanovsky and IvanCasselman, which involves grinding dried plant material, shaking cold, and then sieving to separate the trichomes. https://patents.justia.com/patent/11000856

"Method for collecting and separating cannabis" invented by William Stacy Page. A method that uses ultrasound to separate cannabis products, including trichomes. https://patents.justia.com/patent/10646881.

"Methods and Compositions of Cannabis Extracts" invented by Steven Rosenblat, Jeffrey Tucker, and Steve De Angelo. This patent refers to the use of extracts made from separated trichomes of cannabis flowers with cold water. https://patents.justia.com/patent/20110256245.

"Filter and apparatus for cannabis plant" invented by Mitchell Leffel. It consists of a device that cuts the cannabis plant and separates the parts, including the trichomes by vibration and a series of filters.

https://patents.justia.com/patent/20170001200

"Method and apparatus for obtaining trichomes from cannabis plants" invented by Michael Robert Himes and others. This method consists of freezing the plant material with a cryogenic liquid or gas, which is then impacted by the frozen material and by means of vibration and mesh filters, the trichomes are separated.

https://lp.espacenet.com/publicationDetails/originalDocument?FT=D&date=20200130&DB=&locale=eslP&CC=US&NR=2020030397Al&KC=Al&ND=4.

"Sieving table for flowers, stems, leaves, pollen and plant trichomes" invented by Ivan Carlos Alvarez Martínez. It consists of a table resting on legs with sieves of different sizes to separate the plant material that is placed in the first sieve.

https://lp.espacenet.com/publicationDetails/biblio?11=8&ND=38,adjacent=true&locale=es_LP& FT=D&date=20181114&CC=ES&NR=1220376U&KC=U

"Vegetable resin separation and extraction method" invented by David Cilia. This method consists of shaking in water or dry sieving a mixture of trichomes and plant debris that are separated in saline solutions by flotation of trichomes and settling of plant debris.

https://patentscope.wipo.int/search/en/detail.jsf?docId=US242515495&_cid=P22-KVA680-54808-3

"Rotary (trichome) separation apparatus and process" invented by James Watts et al. This invention comprises a rotating drum where the plant material is placed, which is pulverized with the injection of an inert freezing liquid. https://patentscope.wipo.int/search/en/detail.jsf?docId=US239434966&tab=PCTDESCRIPTION

"Apparatus and method for separating plant trichomes using double vortex turbulence" invented by Didier Camilleri et al. This method consists of separating the trichomes from a plant mixture using the force of double eddies generated by an apparatus and then by filtering.

https://patentscope.wipa.int/search/enidetail.jsf?docId=US327112549&tab=PCTDESCRIPTION&_cid=P22-KVA7UZ-71141-11

"Glandular trichome purification process" invented by Mark Rose. It consists of spraying frozen-dried plant material at -20 °C, rich in glandular trichomes, which is then sieved.

https://patentscope.wipo.int/search/enidetail.jsf?docId=US210001782&_cid=P22-KVA7UZ-71141-11

"Trichhome Isolation System and Method" invented by lan Atkinson et al. This method consists of the separation of trichomes using solutions with chelating agents that attack the cells of the trichomes' feet, freeing them from the plant tissue.

https://patentscope.wipo.int/search/en/detail.jsf?docld=W02020248071&_cid=P11-ZVC5W5-38335-4

"Method and device for separating hemp trichomes" invented by Gerald Mexmain. The patent consists of the separation of trichomes from freshly harvested hemp by placing it in a rotating drum with dry ice to lower its temperature.

HTTPS://PATENTSCOPE.WIPOINT/SEARCH/EN/DETAILISF?DOCID=EP322922436&_CID=P21-KW12XX-72705-3

All the methods cited in the State of the Art prior to this invention are inapplicable for large scales considering the inputs and techniques used in each of them.

Description of the invention

In the state of the art prior to this invention, the inconvenience of separating the glandular trichomes of plants or part of them that have them, without previously drying them, cannot be solved with an apparatus or machine that is efficient and low-cost on large scales. , since with the use of the devices and tools that apply the technique that uses cold water alone or with ice and/or frost, they represent a great expense of energy and water consumption by having to renew it continuously in the process, due to the fact that this is inevitably contaminated with the contents of plant tissues and in the event that ice is used, it is destroyed during the process. All of this has a strong impact on the amount of energy needed to replenish ice and cold water to run a large-scale process.

The same occurs with the aforementioned methods that require prior drying of plant material, cryogenic agents, chelating agents, etc., which require very high-cost inputs and operations.

This invention is based on the separation of glandular trichomes by the wet method using chemical solutions, mainly liquids, made with any solute/s and solvent/s or combinations, which have the condition that all the chemical components of the glandular trichomes are insoluble. totally or partially in said solutions (or the majority, provided that the main components are totally or partially insoluble).

Pure substances can also be used that have those same physical-chemical properties required by the solutions for the separation of trichomes.

This invention takes advantage of the colligative properties of the solutions used in the process, such as cryoscopic decrease and osmotic pressure variation, boilliscopic increase and vapor pressure decrease.

https://es.wikipedia.org/wiki/Propiedad_coligativa.

One of the advantages of this invention is being able to work at the most suitable trichome separation temperature point for each plant species or part of it, in the state of humidity, phenology, chemical content, variety, type of agronomic management, time elapsed. from the harvest, among others, that appear at the time of carrying out the trichome separation procedure. It is important to emphasize that many of the plant species with glandular trichomes of interest considerably increase the capacity and speed of detachment of glandular trichomes with temperatures below zero degrees, including cannabis.

There is also the convenience of being able to work at different temperatures, taking into account the physical-chemical properties of compounds that are of interest to extract them, as well as others that are not desirable to be released from plant tissue, constituting an act of purification itself.

With the characteristic that some solutions can remain liquid at temperatures below 0°C, we can carry out this procedure in a range between 140°C and -70°C, as appropriate.

Another advantage of this invention is that it makes it possible to prepare a suitable solution for each plant sample that is presented, to work at the most suitable temperature point and to have the same osmotic pressure as the plant sample, when dealing with fresh material. This means carrying out the process in an isotonic environment where the plant material has a zero net flow of solvent from the solution, allowing the integrity of the tissues to be maintained intact during the process, thus preventing the substances contained in the plant tissues from being leached, contaminating the solution and this can be continuously reused, meaning great savings in energy and water, making its application possible to process large volumes of plant material with a small fraction of water than those used by the methods mentioned in the prior state of the art.

https://fciencias.ugnes/imagesistories/documentos/semanaCiencia2011/guionBiologiaCelular.p df

(Observation of osmotic phenomena in cells: plasmolysis and turgor)

This is because the cold water used in these processes is drinkable with a very low salt content. Added to that the added ice that melts, composed of pure water, contributes to increase the dilution of the cold water used. This represents a highly hypotonic environment for the plant tissue where, due to the osmotic effect, the entry of a large amount of water and quickly into the plant tissues occurs, contributing to the destruction of cells and tissues due to the pressure exerted in said entry of water. solvent (water), worsening in tissues damaged during production or harvest, degree of tenderness, degree of hydration, etc.

In the case of using frozen plant material in the trichome separation procedure with ice and cold water, the contamination of the water by leaching is aggravated, since during the slow freezing of the tissues the cells dehydrate and macrocrystals are formed that produce mechanical damage. The concentration of solutes in the tissues also increases considerably due to the formation of ice, since the water in the tissues changes phase to ice in its pure state, leaving a concentrated solution without freezing, generating a very marked increase in osmotic pressure. Then, when using cold water with or without ice, which, having a higher temperature (above 0°C), thaws the plant tissues and leaching occurs more markedly than when fresh tissues are used, due to the destruction of plant tissues that caused the formation of ice.

https://proain.com/blogs/notas-tecnicas/efecto-de-las-heladas-en-la-agricultura

("Effect of frost on agriculture")

When previously frozen plant parts are used, this procedure consists of using chemical solutions whose concentration allows them to remain liquid at temperatures lower than those at which the flowers freeze, preventing them from thawing and the tissue contents from entering the solution. In this case, the osmotic pressure generated by the high concentration of the solution does not matter, since the interior of the tissues is frozen, so no solvent enters that can leach its content.

You must first make sure that the entire tissue is frozen, and it is advisable to do it quickly to avoid the formation of macro-crystals and deposits of supersaturated solution, since when you do it slowly, the pure water molecules displace the solute molecules outside the crystal during the phase change, gradually increasing the concentration of the surrounding solution, with the consequent increasing cryoscopic decrease, making it remain in a liquid state even at very low temperatures. These lagoons of concentrated solutions in the liquid state inside the tissues, generated during slow freezing, present a high osmotic pressure, being able to absorb solvent from the system, generating the escape of compounds into the solution.

For this, the plant tissue is quickly frozen at a temperature below the freezing point that it presents at the time of the trichome separation and it is placed in a concentrated solution that has at least the same temperature that it was decided to freeze the tissue. vegetable. This "working temperature" will be determined by the hydration state of the plant tissue, the time necessary to separate the desired amount of trichomes, that is, the desired yield, and the characteristics of the system.

The loss of working temperature, that is, the solution tends to heat up, is due to the intrinsic characteristics of the system and the environment where it is located. In cool sheds and with the hydraulic circuit of the machine very well insulated, the solution has insignificant cold losses, achieving very high energy efficiency that greatly influences the reduction of the cost of the procedure.

The speed of loading and unloading the plant material from the main container also greatly influences the loss of cold.

https://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-75182006000500009

(Chilean magazine Nutr., Vol. 33, no. 3, December 2006, "Rehydration of dehydrated foods").

Example of embodiment of the invention

From flower samples from a batch of 2000 kilos of recently harvested cannabis inflorescences, leaves and part of stems rich in glandular trichomes, its freezing point is determined to be -0.9 °C and. The batch of flowers is placed in a quick-freezing chamber as the separation process progresses, seeking that every 100 kilos that are introduced into the machine are at -1.5°C.

Then proceed to prepare 1000 liters of an aqueous solution of sodium chloride at 3.5% w/w (which has a freezing point below -2.2°C) and cool it to -1.5 °C in a container designed for that purpose.

Once the saline solution and the flowers reached -1.5°C, 100 kilos of flowers are placed at the bottom of the main container and the screened lid is placed to prevent the passage of plant material to the top of the container. This screened lid is designed to allow small particles to pass through, including the released trichomes. The machine is designed to introduce the solution from the bottom of the container and extract it from the top, or vice versa, depending on whether or not the trichomes float in the solution created for the process. In this case, it was determined that the trichomes float, therefore, the plant material is placed below the sieved lid and the liquid is introduced at the bottom and the outlet is at the top.

After introducing the vegetable parts into the container and placing the screened lid, the container is hermetically covered and the equipment is turned on.

The saline solution begins to be pumped into the system from its special container into the main container, through ducts and holes that produce a gentle agitation of the frozen plant mass, in order to release the trichomes, without causing unnecessary ruptures of the plant tissue. The solution and the vegetable mass are at the same temperature, preventing the thawing of the tissues and the release of their contents into the solution, achieving that it remains totally clean throughout the process and can be used for many cycles without having to renew it.

The machine is programmed so that the system has a recirculating flow rate of around 150 liters/minute, this implies that the 1000 liters of solution will pass through the vegetable mass 4.5 times in 30 minutes.

The solution leaves the main container, in this case from the upper part, dragging with it the released trichomes and goes through a series of sand and/or gravel filters, of different granulometry, located in series from largest to smallest, to retain particles of different calibers. in a range determined by the granulometry of the filter material. Each filter point has several equal filters (in this example 3) in parallel that allow, once saturated with trichomes, to be able to extract them without cutting the process. The filter that is saturated with trichomes automatically closes its entry, diverting the flow through the filter of the same size located next to it in parallel. The filters designed allow the extraction of the trichomes through the upper part of it, with a backwash system with the same solution of the system. The extracted trichomes are dried and stored in a freezer at -5°C or less to continue with the subsequent purification process.

After going through the filtering system, the solution goes through other points where, depending on the degree and type of contaminants that the plant mass can bring from the cultivation site, decontamination processes are carried out to maintain the useful life of the saline solution for as long as possible. possible. These treatments can include the sequestration of used agrochemical molecules, elimination of microorganisms, dust particles, among others.

Then the solution returns to the special container for the solution, where the programmed temperature is automatically maintained (In this example it is -1.5°C), with a cooling system that has a serpentine inside the container, where liquid nitrogen circulates. . The machine has several temperature control points in the main container, conduction pipes, filters and solution container.

The machine is insulated on its entire exposed surface and is located in a room that has a controlled room temperature (18 °C).

The process is repeated continuously until over 95% of the trichomes of the batch mentioned in this example can be separated.

In this example, it was possible to extract 1.20 kilos of pure glandular trichomes from the 100 kilos of fresh flowers. In 30 minutes of operation.

Then, through a discharge opening located in the lower part of the main container, the plant material is quickly discharged without glandular trichomes. Previously, the saline solution was drained from the main container into the solution container and a few seconds were waited for the plant mass to drain excess liquid, before extracting it.

Another cycle is immediately restarted with a new load of 100 kilos of vegetable mass frozen at -1.5°C, with the same previous solution.

Claims (18)

1. A trichome separation process characterized by the use of the colligative properties of chemical solutions made with any solute, solvent, or combinations of several of these, where the substance(s) of interest present in the trichomes are totally or partially insoluble that They fulfill the function of separating the trichomes from the plant parts and drag them so that they can be separated by filtration. 2. The process of claim 1 characterized by the use of pure substances, where the substance or substances of interest present in the trichomes are totally or partially insoluble. 3. The process cited in claim 1, characterized by the use of any plant part of any species and/or variety that contains glandular trichomes. 4. The process of claim 1, characterized by the use of gravel and/or sand filters of homogeneous granulometry in such a way that they retain particles of size in an assigned range. 5. The filter of claim 4 characterized by the entry of the flow located below the upper end, in the shape of a chamber that tapers towards the upper end and ends in a valve, through which the trichomes are extracted by backwashing. The filter outlet is at the bottom, below the filtering unit made up of gravel and/or sand of homogeneous granulometry. 6. The filter of claim 4 characterized by a trichome extraction system activated by backwashing, which uses the same liquid that is being used, entering from the bottom and activated by a valve. 7. The process of claim 3 characterized by the use of plant material that has a temperature between 0°C and 140°C. 8. The process of claim 3 characterized by the use of plant material that has a temperature between 0°C and (-70°C). 9. The process of claim 7 characterized by the use of chemical solutions that have the same temperature and osmotic pressure of the plant parts. This temperature is the one where the separation of trichomes from the vegetable matter to be processed is best carried out. 10. The process of claim 8 characterized by the use of chemical solutions that still remain liquid at temperatures equal to or lower than that at which the vegetable mass freezes completely. (It is recommended that the chemical solutions to be used be frozen at a lower temperature than the freezing point of the plant tissues present at the time the process is carried out). 11. A machine characterized by executing the trichome separation procedures as cited in claims 1,2, 3, 4, 5, 6, 7, 8 and/or 9. 12. The machine mentioned in claim 11, characterized by carrying out the procedure continuously and cyclically, with the reuse of the same liquid used in the trichome separation process. 13. The machine mentioned in claim 11, characterized by the incorporation of treatment processes for the elimination of solid, chemical and microbiological contaminants from the chemical solution or pure substance used in the trichome separation process. 14. The machine mentioned in claim 11, characterized by using any method of regulating the temperature of the liquid used in the trichome separation process. 15. The machine mentioned in claim 11, characterized by using any filtering system to separate the glandular trichomes. 16. The machine mentioned in claim 11, characterized by using a hydraulic agitation system for the vegetable material. 17. The machine mentioned in claim 11, characterized by using one or more agitation systems for the vegetable material. 18. The machine mentioned in claim 11 characterized by one or multiple input and output options for the liquid used in the trichome separation process to the place where the plant material is located.