Purification of alcohol or metal from impurities. Industrial alcohol purification

Earlier in everyday life, water-alcohol solutions were purified from impurities by the following methods: 1) filtration; 2) freezing; 3) treatment with protein-containing substances. In the industrial alcohol and vodka, along with the last two, methods based on the following phenomena were used: 1) the preferential dissolution of impurities in certain substances, such as oils; 2) salting out.

Filtration. Filtration was carried out by passing a water-alcohol solution through certain filter materials, due to which fusel oil droplets and mechanical particles were partially separated from it. Filters were made from various materials, but preference was given to charcoal, felt, flannel, soldier's overcoat cloth, washed sand with particles of a certain size. Often these materials were used simultaneously.

Freezing. This method is based on the rule that the solubility of substances decreases with decreasing temperature, and this decrease in solubility is different for different substances. Here is how this method is described in: “Freezing was a purely Russian and very cheap ... technique. But it gave a wonderful effect. Thanks to Russian severe frosts, as well as the preservation of huge glaciers in summer, which practically held ice until autumn, freezing large batches of vodka was not possible difficult. Vodka was frozen in special small barrels that had an exposed bottom or a special plug, through which the alcohol that did not freeze in the cold was poured in. All the water contained in the vodka with fusel oil frozen to it in the form of a thin layer turned into an ice piece, which was easily thrown away ".

It should be noted that, in our opinion, since the proportion of water in the solution continuously decreases during freezing, and alcohol increases, and all impurities that are poorly soluble in water are readily soluble in ethyl alcohol, this purification method is ineffective. At the same time, there is no purification from impurities that have a high solubility in water. So, according to "... it turned out that with a content of 1-2% isoamyl alcohol, the ice is pure, and isoamyl alcohol remains entirely in the alcohol solution."

Processing with proteins. This method is based on the ability of ethyl alcohol to coagulate (coagulate) colloidal particles of proteins in water and form large flocculent aggregates from them. The resulting flakes capture the smallest solid particles and droplets of fusel oil present in the solution being cleaned and slowly settle. According to some data, proteins selectively absorb (adsorb) molecules of other impurity substances present in a water-alcohol solution. As follows from the literature, a single treatment of alcohol is not very effective. But repeated, although it leads to an increased loss of alcohol and a lengthening of the purification process, gives a product of very high quality. Milk, egg white, whole eggs, Karluk fish glue are used to purify alcohol. Cleaning is carried out as follows.

Take 1-2 (possibly more) egg whites or the same number of whole eggs per 1 gave a water-alcohol solution. First, they are beaten, then mixed with a small amount of water, added to the solution to be cleaned and mixed, since protein flakes are formed almost instantly. After that, the mixture is either left alone for several days until the flakes completely settle, after which the purified solution is separated from the flakes with impurity particles trapped by them by decanting, or filtered several hours after treatment.

Alcohol purification and sorting technologies using milk are given in. According to Wilke's recipe, "... about 3 liters of milk is consumed per 100 liters of alcohol, the effect of which is explained by the fact that the clot (protein flakes) formed when mixed with alcohol envelops particles of fusel oil and entrains them in the sediment. After mixing with milk, the alcohol was subjected to rectification and since in the old days distillation was carried out on a naked fire, straw was laid on the bottom of the cube in order to avoid burning the milk.Today, one can find in the recipes for the preparation of liqueurs indications for the use of milk, which is believed to give the product a lighter taste, liquid along At the end of the action, it is not distilled, but only decanted from the sediment.

According to "... Whole milk is considered unsuitable, because the fat contained in it can change the taste properties in an undesirable direction. Skinny milk is more suitable for all high-percentage alcohol liquids, especially for all kinds of vodkas. Use from 0.25 to 1 liter of milk per 100 liters First, a small amount of water is added to it and after thorough stirring with a whisk, this mixture is immediately added to the main mass of the liquid to be clarified.The protein then coagulates into flakes and after 1-2 days, and often after a shorter time, clarification is observed. When, after a long exposure, the product becomes crystal clear, it is drained from the sediment and only the cloudy part is subjected to special filtration. "

Here is how the modern technology of sorting cleaning with the help of powdered milk is described in the work: “Powdered skimmed milk is introduced into the sorting of Posolskaya vodka in the amount of 6.2 kg per 1000 dal.

Powdered milk is preliminarily poured with 20 dal of water, stirred and after 2-3 hours it is introduced into the water-alcohol mixture. After adding milk, the sorting is mixed and left alone for settling for 2-3 hours. Under the action of alcohol, milk protein coagulates, which ends with the precipitation of a flocculent substance. The flakes adsorb organic and coloring substances contained in the water-alcohol mixture on their surface, dragging them into the sediment. Thanks to this, vodka acquires a crystal luster and high taste.

Currently, in the industrial technology for the preparation of high-quality vodkas from the listed protein-containing substances, only skimmed milk powder according to GOST 10970-87 is used. This milk is produced from pasteurized skimmed cow's milk or its mixture with buttermilk by thickening and subsequent drying and must comply with the following physical and chemical parameters (in%): mass fraction of moisture - no more than 4.0; mass fraction of fat - no more than 1.5; mass fraction of protein - not less than 32.0; mass fraction of lactose - not less than 50.0. Purification of impurities with oils. The method is based on the experimentally established fact of the ability of fusel oil alcohols to be highly soluble in certain liquid hydrocarbons and edible fats, in particular in heavy and light petroleum oils, paraffins, poppy and olive oils, etc. Ethyl alcohol, if it is sufficiently diluted with water , does not dissolve in these substances. Due to the fact that impurities such as aldehydes also do not dissolve in hydrocarbons, before treating the water-alcohol solution with oil, the latter is treated with an alkali solution. In this case, the aldehydes are semi-imerized and become soluble in oil. Various oils can be used to extract fusel oils, but in industrial production, preference was initially given to liquid vegetable oils, later to petroleum oils, having a boiling point of about 240 ° C and a density of 0.85-0.88 g / ml (note that the characteristics close to to the above, it has oil, which, according to modern classification, is called solar oil). So, according to, to purify alcohol from fusel oil "... back in 1858, Breton (later Martinet) used poppy and olive oils, soaking flannel or pumice with them and filtering crude alcohol through filters prepared in this way, while it was assumed that fusel the oil is retained in the filter material.The filtered alcohol was then subjected to rectification, and in the distillate, according to the observations of I. Kozlov et al., no smell of fusel oil was noticed, but the smell of used fatty oil was noticed.To regenerate the latter, the filter material can be subjected to heating by means of superheated steam, moreover, fusel oil is distilled off, but part of the vegetable fat is also lost.

In 1884, Bang and Ruffen published a method for purifying crude alcohol by treating it with petroleum hydrocarbons, which, not mixing with water or a weak alcoholic liquid, can extract higher alcohols, esters and other substances from the latter, forming fusel oil. According to initial assumptions, light hydrocarbons (petroleum ether) were used for this purpose, but then Bang and Ruffen preferred heavier ones, having a density of 0.81 to 0.82 ... Recently, petroleum oil with a specific gravity of 0.85 is taken - 0.88 g/ml."

According to, in industrial conditions, this technology was carried out as follows: "The purified alcohol, previously diluted with water to a strength of 25-30 °, enters the neutralization vat, where the appropriate amount of milk of lime is poured. The vat is equipped with a stirrer, the blades of which can be raised or lowered using a chain attached to the upper end of the vertical axis.Stirring is continued until the litmus paper, lowered into the vat, takes on a blue color, i.e., it does not show an alkaline reaction.The purpose of lime treatment is to neutralize free acids, as well as to decompose complex ethers and polymerization of aldehydes.At the end of the reaction, the stirrer is stopped and the liquid is allowed to clear, and when the lime settles to the bottom, the solution is lowered into the extraction apparatus, and the solution is washed with petroleum oil.A new portion is poured onto the lime mortar, the strength of which is far from being lost at once. water-alcohol solution, after which the mixer is again activated, etc. Only after many operations, the old lime, almost completely neutralized, is replaced by fresh lime milk, which, in turn, serves for a number of operations. The extraction apparatus, where the processed lime water-alcohol solution enters, consists of a conical vat ... A pipe for petroleum oil enters the lower part of the vat, perforated inside the extractor with thin holes upwards; there is a drain pipe hole under the cover and the level of the solution to be cleaned must be 15 cm lower than this hole, and the gap from this level to the drain hole is filled with petroleum oil, under which alcohol cannot evaporate.

The operation of the apparatus is as follows: after pouring in a water-alcohol solution and a protective layer of petroleum oil, the pump is set in motion and oil is injected through the lower pipe. Rising up, the streams of oil are saturated with fusel impurities and merge with the oil layer on the surface, and the latter, as it thickens from below, flows through the drain pipe into the cleaning vessels. In these vessels, petroleum oil leaves all the impurities it has extracted from the water-alcohol solution, and, leaving from there, in a state of original purity, it is again taken by the pump and injected into the extraction apparatus. Such a circulation of oil from the apparatus to the purifiers, and from there through the pump back to the apparatus, continues continuously until the water-alcohol solution is completely purified. After that, the pump is stopped and the liquid is allowed to settle, and all the oil floats up, carrying impurities with it. The water-alcohol solution purified in this way is sent for distillation. " According to D. I. Mendeleev, "... liquid oils, petroleum lubricating oils and other similar substances (for example, paraffin), almost not dissolving in alcohol, fusels are extracted from it oils ... and purify alcohol, which, after the second distillation (or during it), is purified by this method from most impurities. I personally experienced purification through shaking dilute alcohol with lubricating oils, combined with filtering through coal and distillation, gave alcohol of very high purity ... "According to the use of paraffin, it is more advisable, since the alcohol purified by it, in contrast to that purified by liquid petroleum oils, has no smell of oil.Usually, when cleaning, pieces of paraffin were loaded into the cube together with the distilled liquid in such an amount that after they melted (melting point - 55-60 ° C) a layer of liquid paraffin 1.5-2 cm thick formed on the surface of the distilled liquid The ethyl alcohol evaporating during the distillation passes through this layer, while the fusel oil alcohols dissolve and remain in it.

We have tested the purification of a water-alcohol solution using refined sunflower oil. Roasted seed oil is less suitable for this purpose due to its strong aroma. The water-alcohol solution with a strength of 28-30 ° was subjected to purification, obtained as a result of the distillation of the mature mash "to the end", that is, until the alcohol was completely separated. The liquid had an unpleasant fuselous odor and a cloudy appearance. 20 ml of oil was consumed per 1 liter of solution.

Purification was carried out as follows. After pouring 10-15 liters of the solution to be cleaned and the corresponding amount of oil into a 25-liter bottle, the container was vigorously shaken. within 40-60 s. This operation was repeated 2–3 times with 1–2 min intervals between shaking. Immediately after stopping shaking, the liquid begins to separate into two layers: the upper one, which is sunflower oil with substances dissolved in it, and the lower one, which is a water-alcohol solution with tiny oil droplets. The amount of the latter decreases over time, however, even after 20 hours, complete separation of the oil does not occur. 12 ^ after the end of shaking, the lower layer was drained using a siphon. Visually, this liquid has a cloudy color, a slight smell of sunflower and fusel oils. The upper layer remaining in the bottle has a pronounced smell of fusel oil, drowning out the smell of sunflower oil. The oil with the substances contained in it was poured into a metal

Capacity and subjected to regeneration by heating at 140-150°C for 20-30 min, until the smell of fusel oil completely disappeared. The regenerated oil was reused and the oil-treated hydroalcoholic solution was distilled. At the same time, the first and middle portions of the distillate had an extremely weak smell of fusel oil, which somewhat intensified as the distillation ended. However, even in the last fractions it was insignificant and the distillate was completely transparent.

In our opinion, incomplete cleaning is due to a number of reasons. First of all, this is due to the presence of fusel oil components in the solution, which have significant solubility in water and ethyl alcohol, due to which they are poorly absorbed by sunflower oil. In addition, a solution with a certain amount of tiny droplets of sunflower oil containing fusel oil components dissolved in it, which are also released during repeated distillation, is supplied for re-distillation. The smell of sunflower oil is completely eliminated, and the smell of fusel oil is even more weakened if, before re-distillation, the oil-treated solution is filtered through charcoal or bone charcoal.

The purification effect is enhanced if the water-alcohol solution to be purified is diluted with water to a strength of 20-25 ° or lower before mixing with sunflower oil and (or) the mixture with oil is kept for 3-4 days. However, much more effective in terms of reducing both the time and the degree of cleaning, re-cleaning the solution with fresh or regenerated oil, combined with filtering through coal.

It is also effective to add caustic acid (NaOH) to the solution purified with sunflower oil, which is introduced into the still in the form of a solution immediately before distillation. Under the influence of soda during boiling, saponification of sunflower and fusel oils esters and neutralization of acids with the formation of non-volatile substances occurs. About 1.5 g of NaOH is enough for 1 liter of oil-treated water-alcohol solution. When using NaOH, filtering the oil-treated solution through charcoal can be omitted.

Salting out. The starting point for this purification method is the experimentally established facts of the limited solubility of many components of fusel oil in a water-alcohol solution and a decrease in their solubility when certain substances are added to this solution. Simplistically, we can assume that the water-alcohol solution obtained as a result of the first distillation is a system in which one part of the fusel oil molecules is evenly distributed between the molecules of water and ethyl alcohol (that is, it is in a dissolved state), and the second part is combined into the smallest droplets. These droplets have a density close to the density of a water-alcohol solution, and as a result, as well as small sizes

evenly distributed throughout its volume. It is clear that an increase in the density of the solution will lead to an increase in the lifting (buoyancy) force acting on these droplets, as a result of which they will float to the surface of the solution, from where they can be removed even mechanically. In practice, this increase in density is easy to implement by introducing into the solution substances that have significant solubility in water, but are insoluble in droplets of fusel oil. However, an increase in the density of the solution will not lead to its complete purification from all the components of fusel oil, since some of them still remain in it. Therefore, it is desirable that the substance introduced into the solution not only increase its density, but also simultaneously weaken the bond between water and ethyl alcohol molecules and fusel oil molecules, that is, reduce the fusel oil solubility in water and ethyl alcohol, as a result of which the fusel oil molecules should stand out from solution, unite into droplets and also emerge. The water-alcohol solution treated with such a substance will be freed from fusel oils, but it is not suitable for consumption due to the low concentration of ethyl alcohol in it and the high concentration of the solute. This disadvantage can be eliminated by distillation. But this purification method places new demands on the solute; it must be non-volatile, chemically inert to ethyl alcohol and the material of the containers used. The method of purification by distillation requires that this substance contribute to the reduction of the bond between water and ethanol molecules. The fulfillment of this requirement is especially important, since it leads to an increase in the coefficient of rectification of ethyl alcohol and provides the possibility of its additional purification during the distillation process. At the same time, a decrease in the bond between the molecules of ePhilo alcohol and water should not lead to the fact that Water and ethyl alcohol will separate and ethyl alcohol, together with fusel oil, will be on the surface of the water.

It would seem that common salt (NaCl) could be the most acceptable substances for the purification of a water-alcohol solution from poorly soluble components of fusel oil, due to its availability, low cost, relatively high solubility in water (36.0) and density (2.16 g / cm), 3 also calcium chloride (CaCl2) is an extremely hygroscopic substance, highly soluble in water (59.5 °, 159). However, due to top), that in comparison with the solubility in water, the solubility of NaCl in water-alcohol solutions is greatly reduced, for example, in a 30 ° aqueous-alcoholic solution it is only 14, table salt is of little use for these purposes. As for CaCl, using it, one can easily provide the necessary density of a water-alcohol solution, but this salt chemically interacts with ethyl alcohol, which is why it is also unsuitable for these purposes.

In the technology of industrial purification of alcohol, potash (potassium carbonate K2CO3) is most widely used. (Potash is a salt of white or, depending on the degree of purification, yellowish in color, very hygroscopic, density - 2.43 g / cm3, solubility in water: 112 g in cold and 156 ;:. solubility in 30 ° solution of about - 30. Note that in industry and in everyday life for a long time only ash from trees, grasses, cereal straw, sunflower stalks, from which it was extracted by dissolving in water, served as a raw material for producing potash for a long time. On average, 10 %, from grasses, straw and, especially from sunflower stalks, - about 30% of potash from the mass of ash.

Methods for purifying alcohol from fusel oil using potash are described in. Below we quote excerpts from both of these works, since the information given in them, complementing each other, makes it possible to form a more complete picture of the mechanism of this process.

The work states that "... if salt solutions of a certain concentration - potash, ammonium sulphate, magnesium sulphate - are added in a certain ratio to Crude alcohol, then it is observed that a dark liquid layer with an unpleasant odor settles over the liquid, which, when selected the proper concentration contains all the fusel oil, as well as the head products.Potash later turned out to be the best, because, already thanks to the neutralization of acids and the decomposing effect on aldehydes, it was always a valuable cleansing agent for raw alcohol. Purification by this method is carried out as follows: per unit volume of crude alcohol in 80 vol.% I take "about 4-5 volumes of potash solution, specific gravity 1.235 ^ 1.240 g / ml at 15 ° C, corresponding to a content of 295-302.5 g of salt per liter. Potash solution is heated in an iron cylinder * up to approximately 60 ° C and, with constant stirring, 80 vol.% alcohol is added to it until it stands out: yferhu layer equal to 1/30-1/60 of the total volume of liquid. For spirits of other strengths, the concentration of potash solution should be changed accordingly. Add crude alcohol with a pipe reaching almost to the bottom of the vat, mixing with a stirrer. When it is noticed that the upper layer has the proper thickness, then, by means of a special draining device, it is lowered into a separate vessel and proceed to the selection of the next layers. After the removal of the layers, distillation is started.

The same method is described in the following way: “The method ... is based on the isolation of fusel oil from alcohol by specific gravity. Purified alcohol is poured into a specially arranged vessel and a certain amount of potash or sulfate is added to it, in dry form or in the form of a concentrated solution * ammonium. After some time, the mixture will clearly separate into two layers, which can be accelerated by slightly heating the vessel. All impurities, i.e. esters and fusel oils with a small amount of alcohol, should pass into the upper layer. The thicker this layer, the more it entrains alcohol, and therefore, to reduce the loss, it is necessary to regulate the thickness of the upper layer by successive additions of water, heating or cooling.If the case is properly managed, in addition to the added salts, pure alcohol with an insignificant admixture of fusel oil (we will add water from ourselves) will remain in the lower layer.

The following proportion of materials gives the most favorable result: dissolve from 30 to 40 kg of potash or the corresponding amount of ammonium sulfate in 100 liters of water and add 40 liters of purified alcohol to this solution, the strength of which is assumed to be 80 vol.%. The temperature during the operation should be from 20 to 40 C. At this temperature, the mixture of liquids is clearly divided into two layers and the top layer can easily be increased or decreased at will by moderately heating or cooling the vessel, or by adding water or salt. You can do the opposite of the above, namely: first pour crude alcohol into the vessel, and therefore already add a solution of Salt, maintaining, however, the same proportions and temperature. The addition of salts in solid form, although possible, is less recommended. Having decanted the upper layer of the liquid, if necessary, a small amount of potash can be added to the lower layer or the liquid can be moderately heated, on the surface of which a new layer is formed containing the remains of fusel oil. By combining both decanters, first of all, ethyl alcohol is extracted, which has passed into this part of the liquid along with fusel oils, for which the decanter is treated according to the above method with a concentrated solution of potash or ammonium sulphate.

The final result is a very concentrated fusel essence, which can be utilized in the perfume industry, turning it into aromatic esters. The lower layers of the liquid, which are a mixture of salt solutions with ethyl alcohol, enter a simple distillation apparatus for distillation of alcohol, which is obtained in this case in its pure form. As for the salts remaining from distillation, they can be used for the following operations. In addition to potash and ammonium sulphate, many other salts can be used to purify alcohol according to the described method ... All these substances tend to release fusel impurities of alcohol into the upper layer. The order of the process and the temperature do not change. When alkaline materials are used, partly chemical purification also takes place, namely, the neutralization of the acids contained in the solution, but the main result is achieved here in any case mechanically.

10.12.2014

If an alcoholic drink has an unpleasant odor, contains fusel oils and various harmful impurities, it must be cleaned. Not everyone knows how to do this at home with the help of available means. Consider several traditional and unusual methods for cleaning alcohol or moonshine.

Elementary cleaning

The first way is very simple. To purify homemade alcohol, you need to have a hydrometer and clean water on hand, preferably from a spring. What are we doing? We dilute alcohol with water to a strength of 45 degrees. Scientists have proven that the amount of impurities in alcohol is directly related to its strength, therefore, the lower the degree, the purer the resulting alcohol.

Cleaning vodka with potassium permanganate

Successful cleaning of moonshine can be achieved using potassium permanganate (potassium permanganate). This method is probably known even to those who have never brewed moonshine, because. it does not require special financial investments and time costs. To begin with, you will need to get potassium permanganate (you can buy it at a pharmacy), pour it into moonshine at the rate of 2 g of potassium permanganate per 1 liter, stir well and leave to settle. It is better to clean in glass containers so that you can visually control the process. After 10-20 hours, you will find a precipitate at the bottom of the jar - these are harmful impurities. Now moonshine needs to be filtered. This can be done in various ways, for example, using cotton wool and a funnel. If you don't have a funnel, make one from a plastic bottle by cutting off the bottom. To make the cleaning process more efficient, close the jar of potassium permanganate with a lid and hold in a water bath for 10-15 minutes. Do not put in boiling water! The water temperature is about 60 degrees. This method also helps to get rid of the cloudiness of moonshine.

Cleaning alcohol with soda

Moonshine or vodka can be cleaned at home with the help of another quite affordable component - soda. The method is based on the chemical reaction of the interaction of acetic acid contained in alcohol and sodium bicarbonate (baking soda). We take soda at the rate of 10 g per 1 liter of moonshine. Soda must first be diluted with water in a ratio of 1: 1, pour the resulting mixture into a jar of moonshine, mix the contents well, then let it brew for 30-40 minutes and shake again. After that, put the jar in a dark place for the night. The next day, carefully drain the purified product without sediment and additionally filter through a layer of cotton wool or charcoal.

How to clean moonshine with egg white

Many experts in the manufacture of homemade alcohol advise to clean the product only with egg white. This method is completely new and is based on the property of protein to fold from interaction with alcohol. Everything is quite simple: we separate the protein of a fresh raw egg from the yolk, dilute it a little with water and beat, pour the mixture into a jar, mix and remove to settle for a day or two. Under the influence of alcohol, the protein coagulates and, turning into a white precipitate, captures the fuselage. For a 3-liter jar, 1 protein will be enough. Carefully drain the product so that the sediment remains in the jar, then carefully filter. Experts note that this method is applicable when the strength of moonshine is not lower than 50 degrees, otherwise the protein will not coagulate well. This method is used during the final cleaning, after all distillations, so that the final product does not “give away” with a boiled egg.

Purification of alcohol with black bread

You can also clean alcohol from fusel oils with black bread. This method was used by our grandfathers and great-grandfathers. It belongs to the final part of cleaning and is used after the previously listed methods. There is no easier method: take a piece of black bread, put it in a jar of vodka and after a few hours, when the harmful impurities are absorbed, remove it. The result is a clean product plus a subtle, spicy flavor.

Cleaning moonshine by freezing

This method helps to rid moonshine of turbidity and make it stronger. The bottom line is that the product is frozen. It is desirable that the temperature be very low, down to -29 degrees. Water and fusel oils freeze to the walls, and pure alcohol remains in the middle in the form of a liquid, which is what we drain from another container.

Classic charcoal cleaning

Ordinary activated charcoal, tablets of which are sold in any pharmacy, is a natural absorbent that can absorb harmful substances. These beneficial properties of coal have long been used by those who are engaged in the manufacture of alcohol at home. Charcoal must be ground to a powder before use. Take for cleaning 1 tablespoon with a hill of coal per 1 liter of moonshine. Crushed coal is added to moonshine, mixed, allowed to stand for several days, then the process is repeated. When re-filtering, do not forget to replace the old carbon with a new one!

Activated carbon can also be used in the manufacture of a multilayer filter for moonshine filtration. To do this, take a funnel, put a layer of cotton wool there, then a layer of gauze, a layer of coal and again a layer of gauze. In this case, the coal does not float, and the filtration occurs quickly and efficiently.

Purification of moonshine with silver

If someone advised you to clean moonshine with silver, in no case do it! It cannot be used either for filtering the mash or for the product after the run. Everything is simple here: silver ions do not allow bacteria and yeast to develop. Silver can only be used to purify water.

Now you are theoretically savvy and have learned the most effective ways to clean alcoholic beverages at home, and you have already outlined some for yourself, so go for it! Use unconventional methods and untested materials with caution. Let only the best drinks of your own production become the decoration of your festive table.

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  GRAIN VODKA WITH POTATOES Required: for 2 buckets of malt - 4-5 buckets of potatoes, water, 0.5 kg of yeast. Cooking method. Soak the malt in warm water and spread it in a thin layer. When it sprouts, dry it and grind it into flour, or grind it in a meat grinder or simply crush it. Boil the potatoes, pour them in the water in which they were boiled, put them in a basin and pour them on top ...

  
  
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  Another, small jar is also closed with a cork with two holes, but the second end of the connecting tube is inserted into one of them almost to the very bottom of the jar, and from the other it is diverted into a separate vessel (basin) filled with water, an independent tube, with the help of which the internal pressure in "refrigerator" will level out. A small jar is turned over and placed in the sink under a stream of cold water. Basin with a large jar ...

  
  
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  VODKA wormwood Required: for 1 bucket of vodka - 400 g of fresh wormwood leaves. Cooking method. Put the wormwood leaves in a bucket of vodka, stir, cover loosely with a lid and leave for 2 weeks. This vodka has a very pleasant aroma and promotes digestion. If you want to make a completely colorless mint vodka, add a few drops of peppermint oil to regular vodka. VODKA VANILLA Required: for…

  
  
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  Fermentation is a kind of process in which all the sugar contained in the original product is converted into a mixture of ethyl alcohol, carbon dioxide and water with various acids and fusel oils formed over time in their composition. In order for the waste raw materials to turn out to be “high-quality”, it is necessary to create certain conditions for this: timely monitor its constituent mass, mix it depending on the accuracy and settling time, ...

  
  

The invention relates to the alcohol industry, in particular to a method for purifying ethyl alcohol from impurities. The method consists in passing ethyl alcohol through a porous sorbent selected from the series: silicon oxide, aluminum oxide, synthetic zeolite and natural zeolite activated by air flow at 350-460 o C, followed by cooling in an inert gas atmosphere, an inert gas is passed through the obtained alcohol , then diluted with water and subjected to rectification to remove impurities of isopropyl alcohol. As a rule, a porous sorbent is subjected to regeneration in an inert gas flow at an elevated temperature, and nitrogen, argon, helium, carbon dioxide, or any mixture thereof is used as an inert gas. The method allows to obtain a high quality commercial product. 2 w.p. f-ly.

The invention relates to the alcohol industry, in particular to the development of methods for purifying ethyl alcohol to obtain a high quality commercial product. Ethyl alcohol is an important product in the production of alcoholic beverages. For food purposes, it is usually obtained by the distillation of fermented sugar-containing material such as beet molasses, sugar cane molasses or starchy substances such as potatoes and various types of cereals: rye, wheat, barley, rice, maize. The result is raw alcohol containing significant impurities of fusel oils. The most important by-products of alcoholic fermentation are acetaldehyde, acetal, glycerol, succinic acid and the so-called fusel oil, which is a mixture of butyl and amyl alcohols and their higher homologues. Succinic acid and fusel oils are not formed from sugar, but as a result of a special fermentation process of amino acids, which are obtained from the proteins of the nutrient substrate. The most common methods for purifying ethanol from impurities are azeotropic, extractive, salt distillation and membrane purification methods [V.I. Zverev. Obtaining high-purity ethanol. Journal. Appl. Chemistry, 1997, v. 70, no. 7, pp. 1154-1158]. Most of the research on ethanol purification concerns the removal of a certain group of impurities, in particular methanol, aldehydes, fusel oils, etc. To remove these impurities, ethanol distillation at atmospheric pressure is most often used. As a result, a rectified alcohol with a significantly reduced amount of impurities is obtained. There are the following types of rectified alcohol: 1st grade, highest purification, extra, luxury, which are subject to GOST 5962-67. Alcohol must be transparent, colorless, without foreign inclusions, have a taste and smell characteristic of each of its types, produced from the appropriate raw materials, without any taste or smell of foreign substances. For the manufacture of vodka, a water-alcohol mixture is used, composed of ethyl alcohol of a certain degree of purification and purified water, with the addition of various ingredients in order to refine the smell and increase the range of taste qualities. In the manufacture of vodka, alcohols of various grades are used, including low-quality ones. Currently, in the process of ethanol purification, the goal is to use a simpler and cheaper method while maintaining high quality for the target product. The most common cleaning agent for fusel oil has always been fresh charcoal. The latter acts mainly chemically, oxidizing alcohols with the help of oxygen concentrated in its pores; alcohols are thus converted into acids (also aldehydes) which form esters. Some of these ethers are retained by the charcoal, while some remain in the purified alcohol, so that filtration through charcoal, while refining the taste and smell of the alcohol, does not actually remove the fusel oils. The patent [US 2946687, 1960] describes the use of modified and partially activated carbon from heavy woods. Water-alcohol mixture for purification is subjected to treatment with activated carbon. However, the goal of purification is not achieved, since the oxygen contained in the pores of activated carbon oxidizes methanol, propyl, butyl and amyl alcohols (fusel oil) to harmful aldehydes and esters that remain in the finished product. Despite the reduction of various impurities present in the water-alcohol mixture, bottled vodka may have a cloudy sediment with this process. The source of this sediment is the used activated carbon containing polyvalent calcium and magnesium cations. A known method of purification of ethyl alcohol by pre-treatment of concentrated ethyl alcohol with sodium borohydride, passing it through activated carbon and separating the purified alcohol by distillation [RF Patent 2046787, C 07 C 31/08, 27.10.95]. The use of this method increases the efficiency of the use of activated carbon, reduces the loss of the target product and makes it possible to obtain high purity ethyl alcohol suitable for optical measurements. A known method of purification of water-ethanol mixture on activated carbon using ultra-low temperatures from -45 to -22 o C in the first stage of processing and from -22 to 5 o C in the second stage in order to minimize the content of unpleasant tasting substances in vodka due to the formation so-called clathrate compounds. It is assumed that clathrate compounds formed during the mixing of ethanol with water at high temperatures also capture unpleasant-tasting compounds such as acetals and hemiacetals. Once captured in the clathrate cavity, these unwanted compounds are no longer removed or are poorly removed by activated carbon [RF Patent 2107679, C 07 C 31/08, 27.03.98]. Closest to the claimed is a method using activated carbon as an adsorbent [US Patent 5370891, C 12 C 3/08, 1990]. According to this method, the purification process is carried out by passing a water-alcohol mixture through three layers of activated carbon at 5-20 o C. The disadvantage of this method is the low purification efficiency and the high cost of the process, since high selectivity for the target product is achieved by using low-quality alcohol grades containing significant amounts of isopropyl alcohol, which causes a harsh taste in terms of organoleptic indicators, as raw materials. In addition, the regeneration of activated carbon in such quantities becomes economically unprofitable. All known methods do not completely eliminate the specific taste of vodka, and therefore even high-quality vodka is recommended to be consumed very chilled. In the patent GB 2127011, 04/04/1984, a method for isolating ethyl alcohol from a mixture of it with organic substances, including higher branched alcohols, branched or cyclic alkanes, aromatic hydrocarbons or ethers, is described by passing the mixture through molecular sieves. The mixture to be separated contains up to 20 wt.% ethyl alcohol. This means that all of the listed compounds are larger than the molecule of ethyl alcohol in size. This is the principle of mixture separation. The ethanol molecules are retained by the molecular sieve, while the larger molecules pass through the column and are collected in the receiver. The ethyl alcohol is then extracted from the molecular sieve by displacing the alcohol vapor with an inert gas when heated. This method cannot be applied in the food or medical industry, since the product extracted from the molecular sieve by displacement with an inert gas when heated will be contaminated with impurities and must be subjected to a complex additional purification procedure. Foreign matter may also appear as a result of catalytic transformations of chemical compounds that occur at elevated temperatures when the molecular sieve is heated during the extraction of ethyl alcohol. The invention solves the problem of developing a method for purifying ethyl alcohol, characterized by high quality indicators of a commercial product. The problem is solved by the following method of purification of ethyl alcohol. A sorbent with a specific surface area of ​​at least 150 m 2 /g, selected from the following series: silicon oxide, aluminum oxide, synthetic zeolite, natural mineral, is loaded into the reaction column, the sorbent is activated with an air flow for 2-3 hours at 420-460 o C, cooled to room temperature temperature in the flow of an inert carrier gas (nitrogen, argon, helium or CO 2). A mixture of ethyl alcohol with fusel oils is passed through a column with a sorbent in an inert gas atmosphere. After separation of the initial fraction of alcohol, enriched with a part of impurity substances (methyl alcohol, acetaldehyde, ethyl acetate), a fraction of pure ethyl alcohol is collected until the other part of impurities (butyl and amyl alcohols) appears at the outlet of the adsorber. Control over the absence of impurities in the collected liquid is carried out chromatographically. Ethyl alcohol is collected in a container through which an inert gas is bubbled to displace traces of dissolved oxygen. The other part of the impurities (butyl and amyl alcohols and ethers) remaining on the sorbent is removed from the sorbent by displacing them with an inert gas when heated. The sorbent in the adsorption column is subjected to regeneration by heating in an inert gas flow at elevated temperatures. The purified part of the alcohol is separated, diluted with water and rectified to remove isopropyl alcohol. The alcohols of fusel oils isolated during regeneration can be used as flavorings in the confectionery industry. The resulting rectified alcohol has a high degree of purification and can be used for medical purposes, as well as for the preparation of top quality vodkas. The difference of the proposed method from the method described in the patent GB 2127011 is the use of a fundamentally different method for the extraction of ethyl alcohol, based on the different ability of substances to be retained by a solid porous sorbent when a stream of liquid substances is passed through the sorbent. The essence of the invention is illustrated by the following examples. Example 1 33.32 g of Al 2 (SO 4 ) 3 9H 2 O are dissolved in 150 ml of water and added with stirring to a solution of 8.0 g of SiO 2 powder in 40.2 ml of 17.4 M NaOH solution. The resulting gel is subjected to crystallization at a temperature of 180 o C for 3 days. The precipitate formed is filtered off, washed with distilled water, dried at 120 o C. The resulting powder with a molar ratio of SiO 2 /Al 2 O 3 = 2.3 and a specific surface area of ​​150 m 2 /g is tabletted and loaded into an adsorption column. Then activate the air flow at a temperature of 350 o With 2 hours. Cooled in a stream of inert nitrogen gas. Raw alcohol with an impurity content of fusel oils of 5 wt.%, supplied with a space velocity of 1.0 h -1 , is passed through the sorbent at room temperature. After separation of the initial fraction of alcohol, enriched with a part of impurity substances (methyl alcohol, acetaldehyde, ethyl acetate), a fraction of pure ethyl alcohol is collected until the other part of impurities (butyl and amyl alcohols) appears at the outlet of the adsorber. Control over the absence of impurities in the collected liquid is carried out chromatographically. Ethyl alcohol is collected in a container through which nitrogen is bubbled. The sorbent in the adsorption column is subjected to regeneration by heating in a stream of nitrogen at a temperature of 200 o C. After separating the purified part of the alcohol, it is diluted with water in a ratio of 1:1 and subjected to rectification. The resulting rectified alcohol meets the requirements of GOST 5964-82. The output of the pure fraction is 45 wt.% of the missed volume of raw alcohol. Example 2. Synthetic zeolite NaA with a molar ratio of SiO 2 /Al 2 O 3 = 2.0 and a specific surface of 150 m 2 /g is used as a sorbent. The process conditions are as in example 1, but argon is used as an inert gas. The output of the pure fraction 35 wt.% from the missed volume of raw alcohol containing 10 wt.% impurities. Example 3 A synthetic zeolite of the pentasil type with a molar ratio of SiO 2 /Al 2 O 3 = 42.0 and a specific surface area of ​​500 m 2 /g is used as an adsorbent. The process conditions are as in example 1, but helium is used as an inert gas. The output of the pure fraction 65% of the missed volume of raw alcohol containing 5 wt.% impurities. Example 4. -Al 2 O 3 with a specific surface area of ​​180 m 2 /g is used as an adsorbent. The process conditions are as in example 1, but CO 2 is used as an inert gas. The output of the pure fraction is 15% of the missed volume of raw alcohol containing 10 wt.% impurities. Example 5 SiO 2 with a specific surface area of ​​200 m 2 /g is used as an adsorbent. The conditions for the process as in example 1. The output of a pure fraction of 55% of the missed volume of raw alcohol containing 7 wt.% impurities. Example 6 A natural mineral, clinoptilolite, with a specific surface area of ​​150 m 2 /g, is used as an adsorbent. Process conditions as in example 1, but as an inert gas using a mixture containing 50 vol.% nitrogen and 50 vol. %CO2. The output of the pure fraction 25% of the missed volume of raw alcohol containing 20 wt.% impurities. As can be seen from the examples, the proposed method allows to obtain a commercial product (ethyl alcohol) with high quality indicators, with a high yield.

How to clean vodka and food alcohol from impurities at home.

You can also clean vodka and alcohol at home. But we’ll warn you right away: this will not save you from deadly methyl alcohol. And from harmful impurities - easily. Additional purification will improve the quality of vodka and prevent hangovers (if you drink in reasonable quantities).

Part 1. Vodka from the store

You bought a bottle in a store and suddenly doubted its proper cleaning. You can insure yourself by cleaning the vodka yourself. Home cleaning may well remove foreign impurities in the product. There are several ways to clean vodka. They can be used either singly or in combination.

Filtration

This is the simplest: take a paper towel, roll it up with a funnel, put a piece of cotton wool on the bottom, you can add more activated or plain charcoal, put another paper funnel on top. And slowly, in a thin stream, pour vodka through this structure.

You can use a good water filter to filter vodka.

Instead of paper towels, it is convenient to use paper coffee filters.

You can take activated charcoal, you can buy charcoal tablets in a specialized store for cleaning moonshine, or you can pull out a cooled coal from the barbecue in the country. It is better not to take purchased coals for barbecue - they give an unpleasant smell to the product.

Infusion

You can add the same coal to vodka and insist on it for several days. Tightly closed containers with vodka should be shaken twice a day. After infusion, it is better to filter the vodka, as described above.

Milk and proteins

Ancient folk way. Add milk or egg white to vodka. Shake. Protein or milk will curdle, bind impurities and fusel oils and precipitate. And you filter the vodka, and drain the sediment.

Potassium permanganate

In vodka you need to add 2-3 grams of potassium permanganate. Insist during the night. There should be sediment at the bottom. Then we filter the vodka, leaving a sediment in the bottle.

Freeze

Vodka is poured into a bag and placed in the freezer. In our freezers, vodka does not freeze, its freezing temperature is below 20 degrees. But impurities turn into small pieces of ice. They must be filtered first through a fine sieve, then through a paper filter.

Part 2. Alcohol

The days of Royal alcohol are long gone. And you can’t buy food alcohol in stores now. But sometimes they still get it. In different ways and for different purposes, but ethyl or medical alcohol gets to consumers. Rare extreme people drink it pure. Usually alcohol is diluted to a strength of vodka - 40 degrees. This must be done carefully. And the resulting product must be cleaned. Since when diluting even pure alcohol with pure water, impurities are still released.

Step 1. Distinguish from methyl (technical)

It is very important. In general, it is better not to buy alcohol in a dubious place. Although if the official sale is prohibited, then all places are dubious. Sometimes alcohol is bought at distilleries, this is a fairly reliable place. However, if drinking alcohol comes into contact with you:

Smell. Bad alcohol will smell like acetone. But just do not bring your nose close to alcohol - you will burn your mucous membrane. It is necessary to bring the container with alcohol to the side of the nose, no closer than 15 centimeters, and wave the alcohol vapors at yourself with your hand. This is how professional tasters evaluate aromas, it is safe. Methanol itself does not differ from ethyl alcohol, but its impurities differ.

Set it on fire. Ethyl alcohol burns with a blue flame, technical alcohol with a green one.

Heat up the copper wire. When hot copper wire gets into the alcohol, a sharp unpleasant odor can be released - this means you have methyl alcohol. Edible alcohol will not react to this.

Step 2. Find good water

Not boiled and not distilled. It is best to take bottled water and filter it additionally. Or spring - and also filter. Mineral water with added salts is not suitable.

Step 3. Glucose

You can buy it at a pharmacy or cook it yourself. 1 kg of sugar must be diluted in a liter of water and put on fire. Boil, constantly removing the white foam. When the foam stops forming, the syrup is ready.

Step 4. Quantity calculation

Approximate proportion: 2 parts alcohol to 3 parts water. That is, for 100 ml of alcohol, you need to take about 150 ml of water. On the Internet, you can easily find a calculation table, according to which you will understand how much water is needed for a certain strength of alcohol and for a certain strength of the drink in the end. The above proportion is for 96% alcohol and approximately 40% vodka.

Step 5Connect

Pour the required amount of water into a container, add a spoonful of glucose and stir. Then pour alcohol into the water.

Important! It is necessary to pour alcohol into water, and not vice versa. In the latter case, you will get a whitish liquid, undrinkable.

After you have introduced alcohol, mix the resulting liquid. Keep in mind that its volume may be less than the combined volume of water and alcohol. Part of the liquid volume is lost during the reaction.

Step 6. Purification and filtration

It is necessary to add coal to alcohol, you can even have a few activated tablets. Leave for 2-3 hours, then filter through a dense cloth or through cotton wool. Additionally, you can use any method of cleaning vodka from those outlined in the first part of the article.

Step 7: Exposure

Pour the diluted vodka into bottles and let stand for 2 days. Sometimes it is recommended to defend a week.

To eliminate the specific smell and improve the taste of vodka, additional home cleaning and aromatization is used, adding a variety of fruits, berries, herbs, and various spices to it.
So how are we going to clean it up?

To clean vodka on the floor of a liter bottle, add 5 tablets of Karbolen (activated carbon) bought at the pharmacy, slightly crushed into small pieces with a knife handle (but not crushed into powder).
Then the bottle is closed and actively shaken for 2-3 minutes, while the vodka turns black. After 10 minutes, shaking is repeated. After half an hour, the bottle can be shaken again.
After that, the bottle is left completely alone in the dark for 2-3 days.
At the end of settling, a dense black layer of activated carbon is deposited at the bottom of the bottle, and above it is the purest vodka, which is very carefully drained from the sediment with a siphon.
Do not try to filter the vodka to speed up the process - the filter will instantly become clogged with coal and the filtration will stop.
It is necessary to patiently wait until the coal itself completely precipitates.
The loss of vodka in this case is about 5%, which remain at the bottom in a black coal sediment. The more Karbolen is put in, the greater the loss of vodka will be.
Purified in this way, vodka is superior in purity and taste to any of the most expensive ones.

More efficient and more affordable than other methods is filtration, in which vodka passes through filters made of adsorbing substances; activated carbon is most often used in their role.
You can also strain the vodka through a vessel with charcoal or place the charcoal directly into the vodka at the rate of 50 g of charcoal per 1 liter of vodka. Leave the charcoal for 3 weeks, remembering to shake the container in which the cleaning is taking place daily. After 3 weeks, filter the liquid. Now you can see for yourself by tasting that vodka has become cleaner. It is better to use coal left over from burning birch firewood.

You can pass vodka through household filters for purification such as "Spring", "Barrier", etc.

An old Russian method for cleaning homemade vodka:
it is necessary to pour a little milk or egg white into the made vodka. These products bind fusel oils and together with them form a sediment at the bottom. Carefully pour the vodka into a clean vessel and distill again. After that, put freshly baked rye bread in it. The product obtained as a result of all these operations is practically pure alcohol, devoid of any impurities.

According to the same principle, vodka can be purified with potassium permanganate. Pour 2-3 g of potassium permanganate powder into a 3-liter jar and wait until a precipitate forms. Next, carefully pour the purified vodka into another bowl, avoiding sediment getting into it.

Freeze cleaning.
Place the bottle in the freezer of the refrigerator, defrost after a while and carefully pour into a clean dish, and try not to get ice from the walls of the bottle into the purified drink. The mechanism of the proposed method is not complicated: the water in the vodka freezes, creating an ice crust on the inner surface of the bottle and absorbing harmful impurities, including fusel oils. Try defrosted vodka, and you yourself will feel that its taste, and hence the quality, has improved significantly.

Flavoring vodka
To eliminate the specific smell and improve the taste of vodka, aromatization is used by adding a variety of fruits, berries, herbs, and various spices to it. They are also added to the finished purified vodka, which is infused for a certain time to obtain the desired effect.
Initially, hops were used to flavor vodka and moonshine. Even in small quantities, it can almost completely destroy the fusel smell and taste.
Bee honey, which is also an effective aromatic additive, is distinguished by similar qualities.
Many medicinal herbs can be used for aromatization. Such vodka, in addition to a pleasant smell, also acquires medicinal properties.
If the plant infused in the same vodka is changed from time to time to a fresh one, then a concentrated infusion will be obtained, which can then be used to improve the taste and smell of vodka, simply by adding it in a small amount.
It is most practical to infuse the flavor with vodka in a glass bowl. If you need urgent flavoring (for example, for the arrival of guests), it is best to put the bottles in a pot of water on wooden blocks and boil for an hour. After cooling in cold water.
When making homemade vodka, the flavoring agent can also be added to the sourdough. Herbs, lemon and orange skins are very appropriate here. However, the aroma is barely noticeable. To enhance it, it is better to first insist on the flavor of your choice the water used to obtain the mash (or prepare a decoction), and only then dilute the sourdough in this water.

Here are some recipes for vodka and moonshine with improved taste and smell.

orange vodka
Ingredients: refined sugar, water - 1 l, vodka - 2 l, peels from 4-5 oranges.
Preparation: boil the syrup from refined sugar and water. Mix with vodka. Pour into the bottle and throw in the same orange peels. Put in a place protected from light for 3-4 days. Then filter and bottle.
Varenukha
Ingredients: dried fruits (pears, apples, cherries, plums, figs), vodka, horns, honey, pepper pods to taste.
Preparation: Rinse dried fruits and horns, fill with vodka, add honey and pepper to taste. Cover the dish with a piece of bread and spread with unleavened dough. Put for 12 hours in a very warm place (in the village - on a hot stove). Drink hot. Fruit can also be eaten.
grape vodka
Ingredients: grape juice - 1 l, sugar - 1 kg, tea - 1 tbsp. l., bay leaf - 5 pcs., black peppercorns - 5 pcs., vanillin - 0.5 tsp., vodka - 1 l.
Preparation: add the listed ingredients to the vodka. Insist 5-6 days, stirring regularly. Strain. These flavors perfectly eliminate moonshine smell.
cherry vodka
Ingredients: vodka, cherry fruits.
Preparation: fill the bottle 3/4 with ripe cherries (half of them should be pitted), fill with vodka and put in the cellar for 1.5 months. After the above time, drain the vodka and squeeze the cherries through the canvas. Let them rest. After a day, mix the juice with vodka, bottle it, seal it. It is recommended to try in a year.
Usually women prefer drinks that are weaker and sweeter than classic moonshine. Especially for them, we will give several recipes for drinks with a pleasant, mild taste.
strawberry vodka
Ingredients: strawberries or strawberries - 3 kg, sugar - 1.5 kg, vodka - 1 bottle.
Preparation: Grind strawberries or strawberries with sugar, add vodka.
"Cognac"
Ingredients: strong moonshine - 3 l, sugar and high quality tea - 1 tbsp each, bay leaf - 3 pcs., black peppercorns - 5 pcs., clove buds - 3-5 pcs., A few orange or lemon peels.
Preparation: mix all the ingredients thoroughly and let the vodka brew for 10 days.
Robin
Ingredients: raspberries, vodka, sugar syrup to taste.
Preparation: fill the bottle 3/4 with ripe raspberries. Fill with vodka and keep two days in the shade. Drain, discard the raspberries, put them in 1/2 bottles of fresh ones and again fill them with the same vodka for two days. Drain, strain. Dilute sugar syrup and add to taste.
Absinthe
Ingredients: vodka, leaves and flowers of field wormwood.
Preparation: dry the upper leaves and flowers of the field wormwood in the shade, then immerse in vodka so that they take up a quarter of the container. Vodka can be consumed in 1-2 weeks.
Caraway vodka
Ingredients: cumin - 350-400 g, water - 1 l, sugar to taste.
Preparation: distill water with cumin through a distillation apparatus. The resulting caraway water can be stored in the refrigerator or in the cellar for several months. When you need cumin vodka, sweeten the water quite a bit, pour it into vodka to taste - and the drink is ready.
colored vodka
Vodka can be given a very beautiful color without the use of any artificial dyes.
For her to buy:
- blue color - insist it on cornflowers;
- green - on mint;
- red - on blueberries;
- purple - on sunflower seeds;
- yellow - on saffron.