Cannabis Fun Club in Russia
Scientific works on marijuana
[03/31/2005] Extraction and purification of oils contained in marijuana and hashish

Step 1 : preparing marijuana or hashish for extraction.

If the raw material is to be plant material, the seeds should first be removed. Then the leaves and flowers should be crumbled, and the stems should be chopped with scissors. The marijuana is thoroughly dried. The plant material, spread out on a baking sheet, is placed in an oven preheated to 120C and turned off for 15 minutes. The procedure is repeated until the leaves and flowers easily crumble into dust if rubbed with your palms. This procedure prevents the raw material from burning.

Hashish can be heated in the oven or in a frying pan on low heat for a few minutes until it begins to smoke slightly. After this, the hashish will crumble easily in your fingers or a mortar. Crushed hashish spoils quickly in the air, so do not crumble it in advance.

Step 2 : raw material grinding

There are several reasons why you should grind your raw material as finely as possible. The broken cell walls allow the oil to be extracted (separated) more completely, and grinding also reduces the overall volume of material we are working with, allowing us to use a smaller extraction apparatus, as well as a smaller amount of solvent.

plant material

the seeds are separated

the leaves are dried for 15 minutes at 120C the stems are dried

dried leaves dry stems crushed into dust with a coffee grinder or mixer crushed with scissors

well dried stems and leaves + SOLVENT

boil for 3-4 hours under reflux

soxhletize

solvent containing cannabinoids and other substances meal

the solvent is distilled off

cannabis oil containing some solvent and water is heated in an oil bath

Cannabis oil freed from water and solvent

Place the marijuana in a coffee grinder or blender and grind it. Using a blender on low speed allows the material to be ground to mix evenly. If necessary, you can stir the contents of the blender with a stick after turning it off. The stems are easier to grind by hand and then mix with the crushed leaves and flowers.

Reflux boiling .

The desired oil is separated from the rest of the plant material by boiling it in a solvent. This oil (containing THC and its homologous compounds, chlorophyll, and terpenes, the substances that impart odor) dissolves in the solvent (usually alcohol), while the other plant substances are not soluble in alcohol. These substances are then removed by filtering the mixture of solvent containing oils and plant material. The solvent is removed by distillation. Since boiling the solvent is quite a dangerous process (these substances are highly flammable), special methods must be used to safely carry out the above operation.

The reflux boiling apparatus consists of the following elements.

1. A small pot, preferably stainless steel, that will hold the ground cannabis and solvent. The above materials should fill the pot no more than 2/3 full.

2. A large saucepan with a domed lid that is at least 5% wider and 2 times taller than the small saucepan. Both saucepans should have a flat bottom.

3. A large bowl for boiling water, at least twice as wide as the large saucepan.

4. Electric stove with two hotplates.

5. several meters of rope

6. Large thick polyethylene garbage bags. 3mm thick is best.

7. a rubber band 2.5 cm wide that can be wrapped around a large pan.

Assembly . A large basin is placed on the stove. A large saucepan is placed in it, and so that its bottom does not directly touch the bottom of the basin, a rope twisted into rings is placed between them. A small stainless steel saucepan with prepared plant material in it is placed inside the large saucepan. The lid of the large saucepan is closed upside down, that is, its handle will be inside. A piece of a garbage bag (its bottom) is put on top of this structure so that the upper half of the saucepan with the lid is covered with this bag. Then the bag is pressed to the saucepan with a tourniquet. All the air is blown out of the bag, before tying it up, it is necessary that the bag fits tightly to the saucepan. As much ice as possible is placed on top of the inverted lid of the saucepan, covered with a bag.

The basin at the base of the structure is filled with water and heated to 100C but no more. As the heat from the boiling water in the basin is transferred to the inner pot, the solvent also boils. Solvent vapors rise inside the pot, touch the lid of the large pot, on which there is ice. From cooling, these vapors condense on the lid of the pot and drip down. The pressure that increased during the boiling of the solvent drops. With such boiling, the probability of ignition of the solvent vapors or the release of toxic vapors into the air is completely excluded.

The reason that prompts us to use two pans instead of one large one is the need for the cooling surface to be larger than the area from which evaporation occurs.

The plastic bag over the lid is used for several reasons. First, the reactor is completely isolated from the outside atmosphere, which helps prevent leaks and fires. However, using a solid material as an insulator could lead to a critical increase in pressure. In this case, the bag will begin to swell, and the ice lying on its surface will fall into a basin of boiling water, cooling the reactor and reducing the pressure, which, as is known, is directly proportional to the temperature.

There are several solvents that can be used to extract cannabis oil. Their properties, advantages and disadvantages will be listed below.

1. Methyl alcohol , methanol (boils at 64C) is a solvent often used for our purposes, and when used correctly, it gives good results. Methanol can be bought in many pharmacies, and is sold in large quantities by companies distributing chemical reagents. Methanol vapors are toxic and explosive. Any trace amounts of solvent in oil will harm the health of the user. Methanol evaporates completely at 88C and does not capture a large number of foreign water-soluble substances. Methods for removing traces of solvent will be described below.

2. Isopropyl alcohol . Isopropanol. There are several advantages in favor of using this solvent. It is cheap, easy to get (abroad, though) and also much less toxic and explosive than methanol. Unfortunately, due to the fact that it often contains up to 30% water, a large number of unnecessary substances are extracted that contaminate the oil. The amount of oil obtained is 2 times more than when using methanol, and the quality is 2 times lower. In addition, such oil will have a more disgusting taste and can burn the throat. However, if you later do a second extraction with a more selective solvent, this disadvantage disappears. Due to the impurity of water, isopropanol boils at much higher temperatures, which complicates evaporation in a water bath. To evaporate isopropanol, it is recommended to use an oil bath (which allows you to maintain a higher temperature in the reactor)

3. Ethanol , ethyl alcohol (boils at 78.5C) This is a very convenient solvent. Its extracting qualities are not much different from methanol, but it is not as toxic. It is difficult to get (just not in Russia ) Next comes advice on obtaining alcohol from liqueur, and an explanation of why you should not drink industrial alcohol. I will skip this, for obvious reasons - I)

4. Petroleum ether (boils at 30-60C) Petroleum ether is a mild solvent, and much more selective than any of the above. Oil extracted with petroleum ether is twice as strong as oil extracted with alcohol. Plant material can be extracted directly with ether, but because of its flammability, it is recommended to first separate the oil from the plant material with some alcohol, and then re-extract with ether. This will require much less of the dangerous solvent. Petroleum ether is usually only available in chemical supply stores.

Step 4 : Soxhletization.

After boiling, it is necessary to separate the remains of the solvent containing oil, which is still in the boiled plant meal. This can be achieved by squeezing the meal and rinsing with clean solvent. A colander is placed on a small saucepan, the inner side of which is wrapped with a coffee filter (or silk - ed.). All the contents of the small saucepan are dumped into the colander. The solvent containing oil begins to drip into the saucepan through the holes in the colander, freed from plant particles. When all the liquid has flowed down, the same structure is assembled as the one used for boiling, but a colander is added to it over the small saucepan.

The mixture of solvent and oil in a small saucepan begins to boil and alcohol vapor rises up, condensing on the lid. At this temperature, the oil does not evaporate, but remains inside the pan. Drops of pure condensed solvent drip from the ice-cooled lid into a colander, washing its contents repeatedly. The oil remaining on the meal gradually ends up in the saucepan. When all the oil has been extracted, drops of solvent (dripping from the bottom of the colander) placed on the glass and evaporating do not leave a colored stain on the glass. The soxhlet apparatus should not be disassembled until the contents have cooled. To do this, fill a basin with ice water or ice cubes.

Step 5 : solvent removal

To drive off the solvent, the soxhleted cake is thrown away and a bowl or frying pan is put in its place (inside the colander). The apparatus is reassembled and put into a water bath. The mixture of oil and solvent boils, the vapors rise and condense on the lid cooled with ice. From there, the condensed drops of pure solvent flow into the bowl. The oil does not evaporate and remains in a small saucepan. The collected solvent, being almost pure, can be reused next time. After removing the solvent, boiling continues without a lid, to eliminate traces of water and solvent from the oil. It makes sense to add a small amount of water to the oil and evaporate it in an oil bath. When the water evaporates, there will be no traces of solvent in the oil, since the boiling points of all alcohols are lower than that of water. The resulting oil can be eaten or smoked.

Step 6 : Cleaning

The oil produced by the above method is of fairly good quality, but still contains substances that give the oil taste, smell and color. Sometimes these substances are left in the oil because they can improve the aromatic properties of the oil. However, their removal significantly improves the psychoactivity of the oil, but accordingly reduces the yield.

The oil obtained as a result of extraction is dissolved in a five-fold amount of alcohol by weight. The mixture is poured into a bottle with a rubber stopper, containing an equivalent volume of water. All solvents used should be cold. Petroleum ether is poured into the bottle in a volume equal to the volume of water. The bottle is closed with a stopper and the bottle is turned upside down, and then quickly returned to its original position. After the mixture has flowed from the walls of the bottle, the stopper is removed to reduce the pressure inside. Shaking the bottle is repeated several times and each time the pressure is relieved, then the bottle is left to settle for half an hour. After 30 minutes, the mixture in the bottle should separate into 3 layers - the bottom layer will contain water, alcohol and foreign impurities of oil, insoluble in petroleum ether. A thin layer in the middle is formed by an emulsion of waxes in ether and air bubbles. The top layer is purified cannabis oil dissolved in petroleum ether. A pre-prepared cork with two holes is inserted into the bottle, into which two glass tubes are inserted. One piece of the tube should stick out of the cork by a couple of centimeters at the top and bottom. A short piece of hose is put on its upper end, into which air will then need to be passed (blown). The other tube should be of such a length that when the cork is inserted, the lower hole of the tube is 1 cm from the bottom of the upper layer (oil/ether) in the bottle. A hose is put on its upper part, which goes into another bottle or jar. After assembly, you need to start blowing out the bottle.

Since the glass tube is slightly missing from the bottom of the oil/ether layer, the part that cannot be blown out immediately will be removed later. The blown ether/oil solution is left behind. The same amount of pure petroleum ether is poured into the bottle as for the first time. The process is repeated until the ether layer is clean after shaking the contents of the bottle). This will mean that the oil is completely separated from the water/alcohol layer

The combined extracts are placed in the apparatus in the same configuration as it was last used (with a colander and a solvent collector bowl). The apparatus is placed on a water bath and slowly heated to 60C. The ether evaporates and can be stored for future use. The oil continues to be heated in the bath for some time to evaporate the remaining solvent. The resulting purified oil is much stronger than that obtained as a result of alcohol extraction.

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