The main methods of obtaining aromas. Practical distillation

Aromatic alcohol is a product obtained by distillation of infusions of a water-alcohol liquid with essential oil or fruit and berry raw materials. By appearance it is a colorless liquid with a strength of 75-80% vol. with thin pleasant aroma. Aromatic alcohol differs from the infusion by the absence of color and a more delicate aroma.

Aromatic alcohols are obtained by distillation of aromatic substances contained in one or more types of vegetable raw materials with a water-alcohol liquid, as well as chickpeas; distillation of alcoholized infusions, fruit drinks or juices.

In their composition, aromatic alcohols are solutions of aromatic substances of essential oils in a water-alcohol mixture.

On fig. 34 shows the hardware-technological scheme for the preparation of aromatic alcohols.

Aromatic alcohol from vegetable raw materials is obtained in the following way. Sorted vegetable raw materials after grinding are loaded into the cube of the distillation apparatus, poured with a water-alcohol mixture with a strength of 60% vol. for fresh raw materials and 50% vol. for dried and subjected to distillation.

Aromatic "alcohol from the infusion is obtained in the following way. The sorted raw materials after grinding are poured with a water-alcohol liquid of a certain strength and infused for 3-10 days with occasional stirring. After that, the infusion of the first drain is drained, which is used in the blend. Raw materials are loaded into a cube, filled with a water-alcohol liquid with a strength of 45% vol.

and subjected to distillation. The aromatic spirits obtained in this way are used for the preparation of Benedictine, Coffee, Chocolate liqueurs, Belovezhskaya bitters, etc.

Aromatic alcohols from fruit and berry raw materials are prepared from fortified juices or fruit drinks of the first plum. To do this, alcoholized juice or fruit drink is poured into a cube, its strength is adjusted with alcohol to 45% vol. and subjected to distillation.

Theoretical basis distillation. Essential oils contained in plant materials are complex mixtures of various organic compounds! They are highly volatile, but poorly soluble in water and weak water-alcohol solutions. When a mixture of essential oils with a water-alcohol solution is heated, as a result of high volatility and poor solubility, essential oils easily evaporate and concentrate in vapor.

The vapor pressure increases when the liquid is heated, and when the vapor pressure becomes equal to the ambient pressure, the liquid begins to boil. If the liquid consists of one substance, for example water, then upon further heating, the boiling point of the liquid remains constant until the entire liquid evaporates. If the liquid consists of several components, for example a mixture of various essential oils j? water-alcohol solution boiling at different temperatures, then, depending on their mutual solubility, when the composition of the distilled liquid changes, and it changes all the time during the distillation process, even at constant pressure, the boiling point can change. The composition of the resulting vapors also changes. The components of the mixture boiling at a lower temperature are more volatile and emit vapors with greater elasticity. Therefore, when distilling a mixture of liquids with different boiling points, the composition of the forming vapor differs from the composition of the distilled liquid great content low boiling component.

The distillation process is characterized by the coefficients of evaporation of the components of the distilled mixture. The evaporation coefficient /C is the ratio of the concentration of a given substance in the vapor phase at to its concentration in the liquid phase χ provided that the system under consideration is in an equilibrium state, i.e. K=y/x

The evaporation coefficients of individual substances differ from one another and vary depending on the alcohol content in the solution: the less alcohol, the more TO. The low-boiling component in the mixture has K>1, i.e., during evaporation, it concentrates in vapor; for the high-boiling component K

The evaporation coefficient of alcohol is always greater than 1 and increases with decreasing strength of the mixture (Table 6).

Since the content of essential oils in the distilled liquid is small, in the process of distillation aromatic alcohol they can be considered as an admixture. If we conditionally take the water-alcohol mixture as one component, then the degree of strengthening of the impurity during distillation is characterized by the evaporation coefficient of this impurity Kpr,- At a given concentration of alcohol Kpr = ~Control>/Xpr· The rectification coefficient K p is expressed by the ratio of the evaporation coefficient of the impurity K pr to the evaporation coefficient of alcohol K s: K-r \u003d Kpr\u003e / Ks · This coefficient shows how much faster or slower than alcohol a given impurity is concentrated ( essential oil) in pairs. If K p > 1, then the evaporation of the impurity is more intense than the evaporation of alcohol, i.e., its concentration in the distillate in relation to alcohol will be higher than in the cube, and such an impurity is the head one. In the case when K R<1, примесь концентри­руется в кубе и является концевой.

Thus, by evaporating a mixture of liquids boiling at different temperatures and then condensing the resulting vapors, it becomes possible to select individual fractions richer in the volatile component. This method, called simple distillation, is the basis for obtaining aromatic alcohols.

The recipe for liquor products provides for the selection of aromatic alcohol depending on the nature of various essential oils.

Distillation plant and distillation procedure. The installation (Fig. 35) consists of a copper distillation cube - alambika, a reinforcing (rectification) column; dephlegmator for partial condensation of water-alcohol vapors coming from the column and their partial return in the form of reflux through the column back to

a cube, a refrigerator for cooling and condensing water-alcohol vapors and cooling the resulting liquid, a control lamp for monitoring the speed of distillation, strength and transparency of aromatic alcohol, as well as for sampling and from two collections-mernikov with sight glasses and divisions on the scales .- One measuring cup is designed to receive aromatic alcohol, the other to collect the initial and terminal

Fractions, which, upon receipt of most aromatic alcohols, are production waste and are used to prepare denatured alcohol.

A distillation column designed to concentrate (strengthen) vapors of alcohol and essential oils has the shape of a cylindrical vessel with three mesh plates and drain glasses (pipe sections). The reflux condenser and cooler are made in the form of a vertical tube, through the annular space of which vapors move, and cooling water flows through the tubes.

Aromatic alcohol is obtained as follows. The distillation cube at 75% of its capacity is loaded with raw materials, tightly closed with a lid and connected to the reinforcing column with the help of pipes and couplings. Fresh raw materials are poured with a water-alcohol liquid with a strength of 60% by volume, and dried - with a liquid of fortress

50% vol. Alcoholic juices or fruit drinks are additionally strengthened in a cube up to 45% vol. When obtaining aromatic alcohol from raw materials, it is advisable to load the cube on the eve of the distillation in order to keep the raw materials in a water-alcohol solution for 10-12 hours. Then steam is fed into the cube shirt, slowly heating its contents. At a temperature of 75 ° C, water is let into the reflux condenser, and when the first drops of distillation appear in the lantern, water is also put into the refrigerator, continuing to heat the contents of the cube to a boil.

The vapors released from the cube enter the lower part of the column, pass through the holes of the mesh plates to the upper part and enter the dephlegmator. In the reflux condenser, vapors of predominantly water and other high-boiling components are condensed and returned in the form of reflux to the upper plate of the distillation column. Since the glasses protrude somewhat above the surface of the plates, a layer of phlegm is created on them, held by the vapor pressure from below. Excess phlegm from the upper plate flows in a glass to the middle plate, and from it in the same way to the lower one. As a result of triple contact of vapors with phlegm, they are enriched with low-boiling products, and phlegm is depleted and returned to the cube. The strengthening of the vapors in the dephlegmator is completed, from where they enter the refrigerator for condensation and cooling to a temperature

The resulting distillate drains n measuring cups through the control lamp. An alcohol meter and a thermometer are installed in the lantern to measure the strength of the distillate and its temperature. In addition, the lantern serves to control the speed of the flow (according to the size of the outflowing jet). The air vent serves to remove uncondensed gases and air into the atmosphere, which, gradually accumulating in the refrigerator, disrupt its normal operation.

The run is carried out at a certain speed, regulating it by supplying steam to the cube and water to the dephlegmator. Usually it does not exceed 6-7 dal / h. Aromatic alcohol is distilled at a temperature of 80-90 ° C (vapor pressure in the cube jacket is not more than 0.025 MPa), and at the end of the distillation the temperature is raised to 100 ° С (pressure in the jacket is not higher than 0.05 MPa). A helmet is installed in the center of the cube lid, where the vapor is separated from the liquid particles. The lid has a pressure gauge, a thermometer and a safety valve.

In order to prevent solid particles from burning, a wire basket is placed at a small height from the bottom of the cube.

With an increase in the amount of water supplied to the reflux condenser, the reflux ratio increases and, accordingly, the amount of distillate taken decreases, while the rate of distillation decreases. At the same time, the strength of the distillate increases, since more high-boiling products condense in the reflux condenser.

During the run, the head, middle and end Fractions are selected. The temperature of the water leaving the reflux condenser is maintained during the selection of the head fraction of aromatic alcohol at 50-70 °C, the end fraction is 70-80 °C. The average strength of most aromatic alcohols is 75-80% vol. Certain types of aromatic spirits, such as aromatic alcohols from cocoa and coffee, which are based on aromatic substances contained in the end of the shoulder straps, receive a lower strength.

The selection of the fraction (in % of the volume of the water-alcohol solution poured into the cube) is carried out depending on the type of aromatic alcohol: head - 0.1-2, medium - 50-70, end - 30-50.

The transition to the selection of each fraction is carried out according to the organoleptic evaluation of the sample from the control lamp.

The strength of aromatic alcohol is controlled by the readings of the alcohol meter in the control lamp: the decrease in strength from the beginning of the process to the end should be gradual. The distillation is stopped after the complete extraction of alcohol from the bottom liquid.

At the end of the run, the steam supply to the cube is stopped, the air cock on the cube lid is opened to release steam. When the temperature of the outgoing water is 20-25 °C, the supply of cold water to the dephlegmator is stopped, the distillation residue is drained and the cube is cooled to 50-60 °C. After that, the apparatus is unloaded, thoroughly washed with water, steamed and prepared for the next distillation. Collections of aromatic alcohol are washed with water until the foreign smell disappears in the wash water. The duration of the run is 5-7 hours.

The speed of distillation and the temperature regime at which the process takes place largely determine the quality of aromatic alcohol, therefore, compliance with the established distillation parameters is mandatory. The yield of aromatic alcohol and the content of essential oils in it depend on the properties of aromatic substances contained in the processed raw materials and the method of conducting the process.

Increasing the useful use of aromatic substances of raw materials is possible by distillation under vacuum. Vacuum distillation apparatuses differ little from conventional distillation apparatuses. They can be equipped with a column and a reflux condenser, but often work without them. The fundamental difference is that the entire apparatus is hermetically sealed. After the refrigerator, the air pipe is not installed. The lantern and collectors are also sealed. To create a vacuum, a dry air vacuum pump is installed in the apparatus, which pumps air out of a collection of aromatic alcohol. To capture water-alcohol vapors, the evacuated air is passed before the vacuum pump through a control refrigerator, in which the vapors condense. When rarefied, the distillation of aromatic alcohol is carried out at a temperature of 48-55 ° C. In this case, the yield of the head fraction increases by 10-30% and its organoleptic characteristics are significantly improved.

Features of obtaining aromatic alcohol from various types of raw materials. Aromatic substances of various types of raw materials are individual in their properties and have different volatility. When obtaining aromatic alcohols from vegetable raw materials, in some cases the most valuable aromatic substances are contained in the head shoulder straps and are quickly distilled off, in others, essential oils begin to be distilled in the middle and towards the end of the distillation.

It was established (E. T. Podlubnaya) that when aromatic alcohol is obtained from citrus peels, the main part of the essential oil passes into a distillate with head fractions and is quickly distilled off, therefore citrus distillate should be transferred to the end fraction much earlier than other aromatic alcohols, and the head the fraction is added to the aromatic alcohol. When obtaining aromatic cocoa alcohol, as noted above, the most pleasant and characteristic aroma appears at the end of the distillation, and, therefore, in this case, the tail fraction must be selected.

Aromatic spirits for tinctures Hunting, Coriander and Caraway retain their aroma throughout the entire distillation process, and the smell of individual components of the raw material appears gradually, without being released during the distillation process. Thus, in order to obtain a pronounced aroma of these substances, it is necessary to convert the head and middle fractions of these alcohols into aromatic alcohol, removing the terminal ones.

Nearly all aromatic alcohols end fractions have an unpleasant aroma and burning taste. Therefore, special attention should be paid to the timely transfer of distillation to the selection of the end fraction.

Some organic substances that make up essential oils are unstable and decompose at high temperatures, so their distillation should be carried out at the lowest possible temperature. The best way to lower the boiling point is achieved by distillation of aromatic substances under vacuum.

Alcoholic infusions are water-alcohol extracts from essential oil and non-aromatic raw materials. Infusions are prepared from individual types of raw materials or their mixtures according to the following scheme.(rice.)

Vegetable raw materials used for the preparation of infusions are weighed and sorted; when sorting, defective raw materials and impurities are removed. Sorted raw materials are crushed (dried herbs on a grass cutter, roots, nuts, seeds and other types of raw materials - on disc crushers). To obtain alcoholized infusions, crushed raw materials are poured with a solvent - a water-alcohol solution and infused with periodic stirring. When insisting, diffusion occurs - the extraction of aromatic and other components of the raw material.

Double infusion is carried out in wooden barrels or small vats (Fig.).

After the first infusion, the infusion of the first drain is drained, the raw material is poured with a fresh portion of the solvent and the infusion is continued with periodic stirring, after which the infusion of the second drain is obtained. The resulting infusions are used as semi-finished products, and the spent raw materials are fed to an evaporator to extract alcohol.

For infusion, a water-alcohol solution is used, the strength of which is on average 50-70% vol. for the first bay and 40-

60% vol. for the second.

The duration of infusion for each bay is 5-14 day The duration of infusion, the amount of water-alcohol solution and its strength for each type of product are indicated in the recipe. Stirring during infusion is carried out daily, pumping the solution with a pump from the bottom of the vessel to the top.

To speed up the infusion at some distilleries, an extractor-tincture is used, proposed by Ya.D. Fireturn. The extractor (Fig. 9.19) consists of a pressure tank 1 and an extractor 2, interconnected by a pipe 3 (with a valve 4, a three-way valve 5, an inspection lamp 6) and an air tube 7.

Extractor -

cylindrical stainless steel tank with a flat bottom and a spherical lid, 1/u high and 0.85 in diameter m. Inside it, at a height of 0.1 m a mesh bottom is installed, onto which crushed raw materials to be extracted are loaded through hatch 8. The hatch 9 serves for unloading of the fulfilled raw materials. The extractor is supplied with a water-meter glass tube with a scale.

The pressure tank has similar dimensions and devices, but differs in the absence of a false bottom. A three-way valve 11 is mounted on one of the fittings, which serves to collect alcohol and water in the quantities necessary to obtain a water-alcohol solution of a given strength. The volume of this solution is determined with

using a water measuring tube 12 with a scale. To mix the water-alcohol solution in the pressure tank, a centrifugal pump 13 is used, driven by an electric motor 14. The water-alcohol solution enters the pump through pipes 3 and 15 through three-way valves 5 and 16 and returns to the pump through pipe 17 with the three-way valve 18 open. tank. The same pump periodically mixes the infusion in the extractor by circulating it. During circulation, the infusion enters the pump through pipe 19 through valve 16 and through pipe 17 with open valve 18 is sent to the pressure tank, from which it returns to the extractor via pipe 3.

By switching the three-way valve 18, the finished infusion is pumped into enameled containers or bottles for storage.

The extraction unit works as follows. In the pressure tank, a water-alcohol solution is prepared, which is lowered into the extractor onto the pre-loaded raw material. After 45-50 minutes of infusion, the first circulation is carried out for 15-20 min, insist again 45-50 min, circulate infusion 15-20 min, and so 6-7 times during the first eight hours. Then 16 h infuse the solution without stirring. From the beginning of the next day, circulation is resumed, alternating with infusion 7-8 times. More frequent or continuous circulation is not recommended as the infusion may become cloudy.

It is known to use in distilleries for infusions of an extraction plant, in which the extraction of raw materials is carried out by frequently mixing it with a solvent with periodic breaks at certain intervals.

to equalize the concentration of soluble substances in the resulting infusion and for settling.

The extraction plant (Fig. 9.20) consists of mixers 1, extractors 2, collectors for infusion 3, pump 4, designed to pump the solvent for mixing, and ceramic filters 5. The extractor is a hermetically sealed vessel, inside which is placed a mesh basket for crushed raw materials.

After loading, the crushed raw materials are poured with a water-alcohol solution and infused for two hours. Then the infusion from the extractor is poured into the collector and is pumped from it back to the extractor by a pump. Draining and pumping fluid continues 10-20 min. Then the raw material is again subjected to infusion for 40-50 min. Every 40-50 min within 8 hours this operation is repeated.

Thus, the solvent is mixed with the extracted raw material 6 times, after which the raw material is infused with the solvent for 16 hours without stirring. The next day, the process of extracting raw materials begins with draining the infused liquid from the extractor and mixing it by pumping it with a pump for 10-20 min. Every 40-50 min this operation is repeated. During the shift, 7-8 mixings are carried out. By the end of the shift, a sample of the alcoholized infusion is taken and, if it meets the requirements of the recipe, the infusion is drained. The process of extracting raw materials is continued until an infusion is obtained that meets the requirements of the recipe in quality.

The second filling of raw materials with a water-alcohol solvent and the extraction process are carried out, as in the first filling, for 30 or 60 hours, after which the quality is checked and used as an infusion of the second drain.

The following is the composition of raw materials (kg) when preparing a water-alcohol infusion on several of its types for the preparation of 1000 gave drinks:

Preparation of aromatic spirits. Aromatic alcohol is a product of the distillation of volatile substances with water-alcohol vapors, essential oils and other aromatic substances contained in essential oil or fruit and berry raw materials. Aromatic alcohols are obtained by distillation. To obtain aromatic alcohols, liquids are used that are partially soluble one in the other (essential oils and a water-alcohol solution), or liquids that are insoluble one in the other (essential oils and water). During the distillation of such liquids, an equilibrium is established between the composition of the liquid phase and the vapor phase. The state of such a system is determined by composition, pressure and temperature.

The relationship between these parameters can be established using the phase rule, according to which the number of phases plus the number of degrees of freedom in an equilibrium system is equal to the number of components plus two:

where F is the number of phases; S is the number of degrees of freedom, i.e. the number of parameters that can be arbitrarily set to fix the equilibrium system, K is the number of components

In the case of distillation of a mixture of liquids that are insoluble in one another, the number of phases in the system is three (two immiscible liquids and steam), the number of components is two

The number of degrees of freedom is 2+2-3=1 This means that of all the parameters that determine the state of the system, you can arbitrarily choose only one, causing them to value the rest.

Figure 9.21 Scheme for the preparation of aromatic alcohol

Aromatic alcohols are produced in a still distillation apparatus, which consists of a still, a distillation column,

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a reflux condenser, a refrigerator, a control lamp for monitoring the distillation rate, the quality of alcohol and for sampling, two measuring tanks (collections).

Aromatic alcohols are obtained according to the method of V.K. Fertman from dry essential oil raw materials or from fresh citrus fruit peels without prior infusion. Raw materials are sorted, crushed, loaded into a cube, filled with a water-alcohol solution with a strength of 60% vol. for fresh and 50% vol. -for dried and distilled. Upon receipt of aromatic alcohol from fresh citrus fruit peels, preserved with a solution of table salt, they are freed from the preservative, crushed, loaded into a cube, poured with a water-alcohol solution with a strength of 60% vol. and overtaken.

Regardless of the method of obtaining aromatic alcohol in the process of distillation, fractions are selected: initial, aromatic alcohol, terminal. The volume of selected fractions (depending on the volume of water-alcohol liquid loaded into the cube) is (in%): initial - 0.1-0.2; medium - 50-70; end -30-50.

The initial fraction is an alcohol solution of terpenes; in appearance it is a turbid liquid with a sharp unpleasant

smell, its strength is 80-90%.

Fraction of aromatic alcohol in appearance - a transparent liquid with a pleasant smell, corresponds to the natural aroma of the feedstock; the main component of this fraction is oxygen-containing derivatives of terpenes, which is the most valuable part of the essential oil. The strength of the aromatic alcohol fraction is 60-80%. The end fraction contains sesquiterpenes and other substances with an unpleasant odor. The distillation is completed at zero reading of the alcohol content in the lantern. The initial and final fractions are used for the production of denatured alcohol.

The transition from one fraction to another is carried out according to the organoleptic evaluation of the sample from the control lamp.

Well, we have already done a great job - we got mash from malt wort, containing 6-9% alcohol. Now we are faced with the task of "squeezing out" this very alcohol in its pure form. We have to make two distillations using moonshine equipment: after the first we will get raw alcohol (low wine, low wine, sam) with a strength of about 30%, after the second - whiskey distillate with a strength of about 75%, which, after dilution to 55-60%, will go in a barrel for maturation (your barrel should already be soaked with water for 3-4 weeks and ready for soaking with an alcohol solution). Below, a more or less detailed description of the process of both primary and repeated / fractional distillation will be presented - obtaining whiskey distillate at home; I will try without water to touch on the features of processing on various equipment, as well as answer frequently asked questions. Go.

I will deviate from the usual practice and will not load the dictionary of terms from the very beginning. We'll figure it out along the way.

So, we need to carry out 2 distillations. Distillatio - dripping from the cooled surface of the condensate vapor formed after the evaporation of the liquid. The palm, according to a number of sources, belongs to the alchemists (Greek, Arabic). You and I are lucky, because over two millennia people have improved both the process and equipment to the maximum. The equipment, it must be said, is not complicated: a container into which liquid is poured and heated (cube), steam pipes and condenser-refrigerator (coil). At the very beginning, in the section , I briefly outlined the situation with the choice of moonshine. I repeat, the simplest devices were initially used for the production of whiskey / pitrik. Therefore, choosing just a well-made cube that suits your volume, and a simple distiller that matches the performance of the cube and the heat source, in any case, you will close the issue of obtaining distillate by 99%. Yes, there are a lot of nuances and details: there are cubes that are heated on an open fire, there are cubes with heating elements, there are cubes with bubblers, there are steam boilers; there are cubes with standardized connectors (for example, HD3, HD4), there are homemade ones; there are steel distillers, there are copper ones, there are brass ones, etc.; there are devices with dry steamers, there are straight lines, there are with reinforcing fittings ... Don't worry. Over time, while maintaining interest in the process, you will gradually reveal most of the subtleties for yourself. But to begin with, all this is superfluous. We bought the simplest cube, the simplest (preferably copper) distiller, the drawer (preferably copper) for strengthening and that's enough - it's time to do business, and not be in doubt or argue with theorists. Practice is the best criterion of truth.

Question #1. Why is a copper distiller better? Answer: copper does an excellent job of neutralizing odors that accompany moonshine brewing (it's a matter of sulfur compounds, but we won't delve into chemistry), it has the necessary
thermal and catalytic properties. To put it simply, the process of obtaining whiskey distillates using a copper distiller is more pleasant, both in terms of aromatics and in terms of the taste of the resulting product. Many moonshiners, in order to save money, buy stainless steel distillers, inserting a copper wire washcloth into the ascending part. Could be so. It is possible from without a copper muddle. Don't worry about it - distill with what you have.

Question number 2. What type of bottom liquid heating is better? Answer: the one that you have and know how to use. Naturally, the authentic version - the cube is located on an open fire (burning peat, firewood, gas). But in the 21st century, you can use heating elements (the main thing is to filter the wort and mash well - burning is the most undesirable side effect on such equipment), and a steam generator, and PVC ... Do not bother yourself - distill on what you have.

What equipment do I have? I started with the simplest moonshine still with a 20l cube made of stainless steel and straight-through
fittings from the same stainless steel. At the moment (taking into account the need to continuously fill 150 liters of total barrel capacity with noble distillates) for the preparation of wort, mash and sam, we have UPVC-50 (complete with a helmet and a simple distiller) for the preparation of wort, mash and sam (complete with a helmet and a simple distiller), and for fractional distillation - a cube Luxstahl 25l with copper distiller (plus a copper drawer for reinforcement; heat source is an induction hob).

Let's get back to practical issues. So let's do the first distillation. Pour the mash into the cube by 2/3 of the volume: when heated, the mash will foam a lot and, if you don’t keep track or take preventive measures, then it will spray (getting into the selection along with ethyl alcohol vapor of the mash itself, and this, as you might guess, is bad) do not pass. We place the cube on a heat source (gas stove, induction hob, etc.) or turn on the heating element. Visually and / or with a thermometer we control the temperature cubic liquid. Periodically, if the design of the cube allows, the mash can be actively mixed, removing the resulting foam. If earlier, incl. at the stage of setting the mash, you used sofaxil (an effective and, in principle, harmless in terms of harm to the taste of whiskey and health in general, defoamer), then you can not be afraid of this problem. Upon reaching t = 65-70 ° C, we attach a hermetically distiller, supply water to the coil. After the temperature exceeds 80 ° C, the selection will begin - first drip, then drip-jet, jet. We pour out the first 50 ml and, having adjusted the heat supply to a selection rate close to the maximum (the criterion is the absence of splash entrainment), we squeeze out all the alcohol from the mash to dryness. That is, until reaching t=100°C in the bottom liquid; well, or at least up to 99 ° C, if you feel sorry for water, gas / electricity. As a result, you should get raw alcohol with an average strength of 25-35 vol. % (depending on equipment).

Question #3. Is it necessary to carry out the selection of heads and tails at the first distillation? Answer: The direct answer is no. But taking into account a very attractive prospect, to select a significant part of isoamylol with the first ml (the well-known "stinker"; coefficient
rectification of this during the distillation of low-alcohol solutions is quite large, respectively, it “flies away” among the first), I personally pour out the first 50 ml (the loss is small). At the same time, I have an “excuse” in front of the Old Believers who reject this initiative - the first distillation is carried out by my colleague and I on a steam-water boiler, which ensures relatively uniform heating and boiling of the mash. In other cases, especially when using an open fire, it is impossible to achieve an even boil, and, accordingly, the whole physics of the process becomes no longer so obvious. Forget about the tails at the first chase, we have fractional distillation ahead of us - everything will happen there.

By the way, at this stage you can roughly estimate the yield of alcohol from raw materials in relation to your conditions and equipment. For example, you mashed 15 kg of malt and got 10 liters of 30% raw alcohol as a result. The math is simple: 10*30/100= 3 liters of AC (absolute alcohol); 3000 ml AS / 15 kg malt = 200 ml/kg. This is normal for the first time, taking into account the losses at all stages. With experience, you can get close to values ​​​​of 300-340 ml / kg. Let me remind you, we are talking about barley malt!

Raw alcohol is not suitable for ingestion or bunkering in a barrel for maturation - there are too many unnecessary (tasteless, harmful) fractions in it. In order to “separate” these fractions, we will carry out repeated distillation (the so-called fractional distillation).

Question number 4. What strength should be raw alcohol for the second distillation? Answer: 25-30 vol.% If, after the first distillation, you got a higher spirituality, then it is highly desirable to dilute it to the indicated values. For what? If you exaggerate as much as possible, then when distilling a solution of alcohol, 25-30 vol. %, the most “correct” separation of fractions occurs (there will be a desire to understand everything in detail - the same rectification coefficient, coupled with chemistry and physics, will help you).

To carry out fractional distillation, we pour raw alcohol into the cube, mount a strengthening drawer, a copper distiller, turn on the heat. If the equipment allows, then we install a thermometer in the upper part of the fittings - in the process we will focus on the vapor temperature. From time to time we touch the tsarga with our hand - as soon as it starts to heat up noticeably, we connect the water to the coil and reduce the intensity of the heat supply to medium values. Next, we compare our actions with the readings of the thermometer and the speed / volume of distillate draining. After the readings of 78-80 ° C slip on the thermometer, the first drops will begin to fall into the receiving container. At this moment, it is necessary to try to adjust the power of the heating device so that during the selection of the head fraction, the rate of obtaining distillate is exactly “drop by drop”. This will make it possible to separate volatile, low-boiling components from the “body” quite well (they are defined by smell as colorful-acetone). The volume of heads must be calculated in advance (according to the formula Vheads = Vraw × 0.05) and selected completely without regrets (we do it for ourselves). That is, if you have 10 liters of raw alcohol 30%, then the first fraction should be 0.5 liters (500 ml); we select it, as I already mentioned, slowly, and upon cutting off, we either use it on the farm for technical purposes, or, having accumulated a sufficient amount, we send it for rectification.

That's it, the heads were cut off, it's time to take the most valuable thing - the body or the heart of the epaulette. It is this fraction that, after dilution, will go to the barrel for maturation. We substitute a new receiving container (I usually use a glass 2-3l jar), a little
we increase the heating power, achieving drip-jet selection of distillate (about 30 ml/min). The volume of the body may differ depending on the strengthening ability of your equipment, on average 20-30% of the volume of raw alcohol poured into the cube. To determine the moment of transition to the selection of tailings, we will focus on the fortress "in the stream". When the vapor temperature reaches 91°C (see diagram alcohol steam in " "), i
I personally begin to collect the distillate in a 100 ml volumetric flask and determine the alcohol content with an ASP-3 hydrometer of 40-70% until reaching 60% strength. We combine instrumental control with organoleptic, or rather olfactory, examination - we timely detect the appearance of fusel notes besides a pronounced bready smell (inherent in “near-tailed” portions, which it is desirable to keep in the body to give a full taste to the future of whiskey). That's it, we change the receiving tank and consider the selection of the main part of the shoulder strap for us to be completed.

This could be the end of the description of the distillation process - obtaining whiskey distillate at home. But I suspect you still have a couple of questions.

Question number 5. What should be the rate of distillate production? Answer: the slower the extraction on simple equipment, the purer the resulting distillate; but everything has its reasonable limits: drip-jet, moderate jet selection is what you need.

Question number 6. How much time to plan for fractional distillation? Answer: in relation to my experience, it will take about 4-6 hours to distill 15-18 liters of 30% raw alcohol into 4-5 liters of whiskey distillate, of which 1-1.5 hours to heat the cube, 1.5-2 hours to drip selection of heads, 2-3 hours for the selection of the body and half an hour-hour for the selection of tails.

Question #7. Is it possible to soak a new barrel with raw alcohol, and then send it for fractional distillation? Answer: definitely yes! A new barrel after soaking with water (with a change every 2-3 days) for 3-4 weeks is very possible
continue soaking with 30% raw alcohol obtained after distillation of the mash. After a couple of months, raw alcohol will pick up, as it may seem, an “excessive” smell and taste - do not be afraid, after the second distillation you will get an excellent whiskey distillate from it (clear and fragrant)!

You see, there is nothing super complicated and difficult. The main desire, some free time and... and we are already one step away from achieving our goal - to cook whiskey with our own hands!

It remains to dilute the resulting distillate and send it to a prepared barrel for maturation. Let's take a look at everything in the next article!

link to forum thread http://forum.homedistiller.ru/index.php?topic=59750.180

Introductory notes from the author of the thread on the HomeDistiller forum:

"The theme was created for those distillers who want to get, so to speak, classic distillates, and not under-rectified, super distillates, headless distillates that can be diluted with water and immediately drunk, namely the classics, i.e. distillates that require long aging in oak barrels to end up with a harmonious distillate with a full range of flavors and aromas."

"... the drinks obtained are not intended to be consumed 0.5 per person, as they say, as a headache in the morning will be guaranteed. The drinks are intended to be enjoyed in small quantities."

The pleasure of distillates is not measured in liters

interpretation of the material. Alphabet Vinokur

Sixty-eight pages on the forum have been reduced to the minimum possible, while maintaining the fundamental principles of the author of the material. This is my interpretation. I highly recommend you check out the source. At least from 1 to about 40 pages. Unfortunately further, in 95% of cases it goes off-top.

So, the MAIN PURPOSE of fractional distillation is, using the basic principles of industrially produced drinks, to obtain a high-quality distillate on household equipment.

​

Routing fragrant sam

from fruits, berries and cereals (in terms of grain, in my private opinion,

optimal - ).

Requirements for mash and raw alcohol to obtain high-quality distillate

1. From the must / mash, ideally you need to get wine / mash, with a strength in the range of 7-10%

2. After the first distillation of the mash into raw alcohol, it is highly desirable to obtain SS with a strength of 25-30%. Ideal - 30%.

It is allowed to obtain SS with a strength slightly more than 30% with further addition of water to dilute the SS to 30%, but at the same time the volume of added water should not exceed 10%.

Subject to paragraph 1 and paragraph 2, we obtain SS with all the impurities necessary for the formation of a fragrant bouquet of the future distillate and with the lowest content of unnecessary ones.

PS - where and how does the "byaka" go?

Studies (See Skurikhin's book "The Chemistry of Cognac and Brandy") showed that when distilling wine with a strength of 7% -10% and then raw alcohol 25% -30%, the rectification coefficients of fusel oils, aldehydes, esters and acetals are more than one, those. most of the bad impurities come out with the head fraction.

equipment requirements

Also, studies have shown that the rectification coefficients of impurities depend on the reflux index of the apparatus. Knowing the reflux rates of classic distillation apparatus, you can set up your household distiller to work in the desired selection mode. Those. "program" your machine to produce fruit or grain distillates, much like industrial distillery equipment. It is known that the reflux index for the "double-run Charente steam apparatus" is 0.057. It must be adhered to on your device during the haul.

Setting up home equipment
We perform the following actions:

​

1. First, the calculation. For this we use a calculator.

Enter in the calculator

1) the strength (in percent) of the raw alcohol poured into the cube from 25% to 30%. I remind you that ideally 30%

2) k - the required reflux index, in our case 0.057

We get

3) % - the initial strength of the distillate, which must be adhered to in order to get a "distillate like in a distillery".

​

PS - if you know exactly the strength of the mash, then through a similar calculation, you can determine the initial strength when distilling wine / mash in the SS.

2. Machine setup

option 1.

According to the strength of the selected distillate, we need a strength of 81.97%

option 2 is preferred.

Possible with a thermometer in front of the refrigerator.

It is important for us to know the dependence of the alcohol content in vapor on temperature. For example, we need to get a reflux index of 0.057 on the apparatus, using the reflux calculator, we find that the initial distillate should come out with a strength of 81.97%, then we find this strength on the graph vertically and at the intersection of the curve horizontally we get a steam temperature of 84.25C. We install it by adjusting the heating and / or the power of the dephlegmator.

For both options, the tuning is carried out not by the first drops, but after the apparatus enters the haul (selection of heads) in a thin, thin stream.

Fractional distillation

After adjusting the distiller for strength or steam temperature in front of the refrigerator, we distill 30% SS, broken down into fractions.

Important! After setting, we don’t adjust anything else until the end of the haul. We only change the container.

According to the methodology, five fractions are selected. Each fraction is indicated as a percentage of the filled volume of the SS. The sixth fraction, tails, is selected at will.

Fractions:
1 - 5% head
2 - 10% first body
3 - 20% body
4 - 5% fragrant body
5 - 2.5% heavy body
6 - tails, how many will remain

Important! Fractions are selected according to the above-specified volumes,

to switch from the 3rd fraction to the 4th when the strength of the outgoing distillate reaches 60%, regardless of the preliminary calculation.

Separation of the resulting fractions into "light" and "heavy" drinks

Basic division proportions:

Heads - not used

The first body 30% goes to a light drink, 70% to a heavy drink
The main body is 60% for a light drink, 40% for a heavy drink.
Aromatic body 40% goes to a light drink, 60% to a heavy one
Heavy body 10% goes to light drink, 90% to heavy

Tails - not used

Light can be drunk after dilution and "rest" in the glass.

Heavy - in a barrel. Minimum for 6 months.

Fractional distillation is only partly a craft, but to a greater extent already an art. The prescribed algorithm is the basic postulates. The quality of the final distillate depends on the qualifications of the process manager, i.e. from you, as from VINOKUR. GOOD LUCK!!!

Cognac is a noble drink that is quite difficult to make at home. based on the use of ordinary ethyl alcohol as a raw material, make it possible to obtain only a crude fake. Only by making a real one you can enjoy a fragrant bouquet without fear for the quality of the consumed alcoholic beverage.

What is cognac distillate?

Cognac distillate is made from white wines of certain varieties with the obligatory observance of all the rules of distillation and aging. Only with strict observance of all production conditions will cognac acquire its characteristic color, bouquet and taste.

Consider the stages of the distillate manufacturing process:

1. Preparation of wine materials, including the cultivation and harvesting of grape varieties with a minimum sugar content.
2. Obtaining grape juice and preparing must from it.
3. Fermentation
4. Primary and secondary distillation of the resulting wine with the separation of the middle fraction.

The efforts spent on production will pay off, because the cost of 1 liter of self-made cognac distillate is significantly lower than the price of cognac in the store. The result of the correct passage of all stages will be homemade cognac, which is nice to drink yourself or treat friends.

Cognac distillate or cognac spirit - which is better?

Nothing is better, they are different names for the same product. According to the latest national standard (GOST), cognac distillate was introduced instead of the cognac spirit that existed in the legislation until 2012.

At the same time, it should be noted that the description of the technology for the production of cognac spirit is identical to the standard for the production of cognac distillate.

Failure to comply with the requirements for production technology increases the amount of harmful substances, including fusel oil, which is included in cognac distillate, the hazard class of which is defined as the third.

Grape varieties for the production of cognac distillate

Cognac distillate can only be obtained from certain varieties of sour grapes. Their distinguishing feature is their low sugar content. In France, Folle Blanche, Colombard and Ugni Blanc are used for this purpose, which are distinguished by particularly intense and persistent aromas.

So which grape variety to choose for making your cognac? These should be fruits of white, less often pink varieties with clear juice without nutmeg aftertaste. Grown everywhere in the south of Russia, Isabella is not suitable as a wine material for the production of cognac due to the low yield of the product.

The Institute of Winemaking and Viticulture recognized as the most suitable varieties:

• Grushevsky white;
• Kunlean;
• Bianca;
• Swim;
• Aligote;
• Scarlet Tersky.

These grape varieties at the stage of technical maturity have the necessary sugar content and acidity, as well as thermal stability and high juice content, which is necessary for the production of must by the drip method.

Preparation of wine materials for cognac distillate

Sort the harvested grapes, removing spoiled fruits. It is impossible to wash the grapes because of the yeast cultures on the skin that are necessary for fermentation. To obtain juice, crush the grapes along with the seeds.

Pour the resulting juice together with the pulp into an enameled vat and sprinkle with a little sugar if the berries are slightly underripe. Within two weeks, natural yeast forms on the surface and the fermentation process starts. If fermentation is not too active, add wine yeast. Seal the container tightly and place in a warm place. Remember to stir once a day.

After 1-2 weeks, measure the strength of the young wine with an alcoholometer. If it shows 11-12%, drain it by straining the pulp through cheesecloth. Long-term aging of the wine is not recommended due to the possibility of a Madeira flavor.

Primary distillation

Cognac distillate is produced from young white wine by double distillation. Pass the wine material obtained as a result of fermentation through a distiller to produce raw alcohol. It is also very important at the stage of the first distillation to be able to correctly separate the middle fraction from the head and tail.

The result of the primary distillation will be raw distillate with a strength of 25-30% and stillage.

It is permissible to leave the middle fraction together with the tail for re-distillation. In this case, before the process of re-distillation, it is necessary to lower the strength of the raw alcohol by diluting it with pure water.

Secondary distillation

Improving the quality of the product is achieved through repeated distillation, during which it is also necessary to separate the fractions and cut off the central one from them.

The head fraction has a sharp unpleasant odor and has a strength of about 80-85%. About 3% of raw alcohol and up to half an hour of working time are spent on its production.

The central fraction, which is the desired cognac spirit, is cut off as the pungent odor weakens. The cut-off is also made based on the strength of the product: the start of selection is at 78%, the end at 58%, in order to avoid unpleasant tail tones in the distillate.

As the strength of the produced product decreases from 50% and below, the stage of cut-off of the tail fraction is suitable. The third fraction has a significant volume and often takes from 40 to 50 percent of the total raw alcohol. The tail can be left for further distillation.

The result of the secondary distillation and separation of the middle fraction will be a high-quality cognac distillate - a colorless transparent liquid with a taste of ethyl alcohol and a pronounced wine aroma, suitable for further aging.