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Alex_Sor

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Posts posted by Alex_Sor

  1. I wish you the best of luck on your journey.

    There are only two companies in the USA that make continuous columns. One of them has been making the same model (construction) for 100 years already :) Only different sizes :)

    I see that the alcohol and whiskey industry is very conservative. Everyone is satisfied with the "big shining tanks" of steel and copper. Nobody thinks that you can get three times the distillation rate from the same place in the room.

  2. 13 minutes ago, Silk City Distillers said:

    You’ll find that many here, and in the industry in general, are strongly against remote still control, because it enables reckless behaviors, that when go bad, impact all of us from a liability, regulatory, and scrutiny perspective.

    I completely agree!

    I have been in Automated Control and Embedded Systems for over 20 years, and I am a "very trained pessimist" when it comes to electronics and automation applications.

    In addition, all developers of "remote control" for some reason forget that Wi-FI does not have a guaranteed data delivery, and is very dependent on the level of external interference. (Especially from spark interference) And the Internet Protocol TCP/IP itself does not guarantee the delivery time of the data packet at all, does not guarantee the delivery of the data packet itself, does not guarantee the sequence of the network data packets.

    There are a lot of errors when transferring data, so no one in their right mind would make a real-time control system based on the Web that does not guarantee anything.

     

  3. Hi!

    I want to give my opinion if you are interested.

    1) for the US market, it is required to comply with the conditions of fire safety requirements, in particular, hot alcohol and electricity are very dangerous. This falls under the zoning: C1D2. Therefore, any electronics that do not have a UL listing requires special permission and inspections and examinations. Therefore, all electronics "not UL listing" can only be used by small manufactures "for themselves" and at their own peril and risk. Therefore, your electronics cannot be applied (and sold) to large alcohol factories.

    2) As my experience shows, and the experience of homemade forums in other countries, "smart electronics" is needed only by those who develop new moonshine stills and columns. A lot of data from the column allows you to better understand the processes inside. But the real work of the equipment requires very simple solutions, for example Danfoss valves that do not use electricity at all and evaporative type thermometers with remote sensors. You will not be able to control the column only from the phone screen 🙂 because anyway, some of the people must be on duty near your equipment during its operation. Heating alcohol is a dangerous process.

    All fashionable new technologies 🙂 are very expensive and not always useful. I am a conservative in this regard - many people on various forums have made similar "control from the phone" equipment, but none of them has received much sales. These themes come up periodically and die just as quickly.

    3) the process of distillation of alcohol takes place using "phase transitions". This is a natural stabilization process, very well studied and understood. You do not need to manage this process, it goes on as usual, and you just need to understand when it will start and when it can be completed. The operator of the column learns this in a couple of distillations and then does not require a lot of data about the temperature inside the column. The distillation process is quite simple and straight

  4. On 3/16/2021 at 12:14 PM, Oldguy said:

    Hi guys

    Anyone here have any experience running a small continuous column with packing underneath and plates on top? 

     

    It is pointless 🙂

    Packings (filling, backfilling) inside the column play the role of increasing the area and smoother distribution of the temperature difference over the height of the column.

    Main problems:

    1) The fill column cannot act as a stripping column because solids will clog all the passages.

    2) with a large diameter of the column, there is a big problem of uniform distribution of reflux over the diameter of the column and the vapor velocity upward along the diameter of the column.

    3) in the column "with filling" (nozzles are filled up) it is impossible to organize a lateral discharge of a part of impurities (alcohols and fusel oils). This creates dirty alcohol at the exit (lots of isoamylol alcohol impurities, etc.).

    Packing (filling, backfilling) of a certain height is equivalent to one theoretical plate. But in order to calculate this, you need to know which form of rings or special placeholders you are using. In real designs, either a plate column design or a "filled" design is used.

    Typically, filling is used on small diameter columns.

     

    P.S: I do not often leaf through this forum, so if you have similar questions, then write them to me in a personal message. The forum generates me an email notification if there is a message for me, and I will go to the forum.

    • Thumbs up 1
  5. The middle esters are formed at elevated (more than 40 ° C) temperatures and when acidic esters are heated.

    The middle esters are insoluble in water, but readily soluble in hydrocarbons and organic solvents. Under the action of water or an alkali solution, the middle esters can hydrolyze to form first alcohol and alkyl sulfuric acid, and then alcohol and sulfuric acid

    🙂

    Esters of wines and cognacs are mainly represented by esters - products of substitution of hydrogen atoms of OH groups in mineral or carboxylic acids by hydrocarbon radicals.

    They (esters) are involved in the formation of the aroma and taste of wines and cognacs. Certain high molecular weight esters are also involved in the formation of haze in beverages. Esters of lower and middle representatives of aliphatic acids and alcohols are colorless volatile liquids, often with a pleasant odor. Esters with the smallest number of carbon atoms are poorly soluble in water, but well in organic solvents. High molecular weight ethers are insoluble in water.

    Esters can undergo saponification (hydrolysis) to form the corresponding alcohol and acid. They are capable of transesterification (alcoholysis) in an acidic environment in the presence of a large amount of alcohol. When interacting with ammonia and its derivatives (ammonolysis reaction), they form amides.

    For example, with the action of ammonia on ethyl acetate, acetamide is formed, which gives the wine a "mouse" tone. The esters that make up the essential oils of raw materials for winemaking have little effect on the aroma of the resulting wines and cognacs, with the exception of methyl and ethyl esters of anthranilic acid, which have an odor that determines the aroma of Vitis labrusca grapes, as well as wines made from it.

    Esters that affect the aroma of wines and cognacs are formed mainly as a result of alcoholic fermentation. They are mainly represented by ethyl esters of aliphatic acids with the number of carbon atoms from 1 to 12, as well as acetates of aliphatic alcohols from 1 to 12 (with an even number of carbon atoms) and cyclic (3-phenylethyl alcohol.

    The variety of esters of wines and cognacs is due to the large number of possible combinations between alcohols and acids. Their number is several dozen, and the concentration of ether is from fractions of a milligram to several milligrams per cubic decimeter (1 dm3 = 1 liter). Ethyl acetate is formed in the greatest amount. In wines there are also acid and medium esters of hydroxy acids and polybasic acids, such as , for example, lactic, succinic, malic, tartaric, etc. Their content in young wine is about 50mg/dm3, and after aging - up to 100-400mg/dm3.

    Acetates of furancarboxylic and terpenic acids have also been found. involving the use of yeast, you can achieve an increased content of some esters. egg wine materials in the presence of yeast forms 50-100mg/dm3 of ethyl esters of nylon, caprylic, capric and lauric acids, which determine the "soapy" tone characteristic of some types of cognac. The same esters, as well as ethyl linoleate, etc., are released from yeast during autolysis and are characteristic of champagne.

    Esters of higher fatty acids and alcohols with carbon atoms up to 32, as well as esters of glycerol and sterols, which are part of grape waxes, yeast lipids and oak wood, can participate in the formation of turbidity in wines and cognacs due to poor solubility in water alcoholic environment, especially when cooling. Gas-liquid chromatography and other methods are used to study the composition of ethers.

    🙂

  6. On 2/27/2021 at 5:54 PM, JustAndy said:

    Wine makers deploy copper (usually copper sulfate) with the same intent as copper in the still, to deal with reductive / sulfur aromas. However, I believe there can be an issue with elevated copper levels in the effluent. 

    My advice to you: if you want to work (preserve) grain and fruit aromas (esters) and tastes, then you need to apply vacuum distillation.

    No other distillation methods will give such capabilities and product purity from fusel oils and "stink".

    One of my friends lives in Georgia (Country on the Black Sea, not a state in the USA) he has a large harvest of tangerines every year. He makes tangerine mash, and then distills it. When I sold him my vacuum distillation controller and told him how to get flavors, he got amazing spirits :)

    In Georgia, distillers compete to make a purer alcohol :) they love wine and they are not interested in moonshine-whiskey :) (they explained to me that way).

  7. On 2/27/2021 at 3:17 AM, SlickFloss said:

    I appreciate the respect! And the lengthy answer! Where I’m from that term isn’t used pejoratively it’s just what a lot of us are

    Out of curiosity what type of odor were you originally trying to tie up? Im running a lot of this one high sulfur high lipid botanical macerate under vac and I’m looking for a little more aromatic clarity I’m wondering if this could be the answer

    To be honest :) I personally do not understand at all the desire of people to use copper for catalysts.

    Copper gives off a "bouquet" of medium ethers, I have seen this many times on chromatograms. As soon as copper is used, it does not matter - like plates, like an alambic, or like tubes of electric heaters inside the tank, so the parameters "average ethers" in the chromatogram will always be one and a half to two times higher. Higher compared to pure steel tank and heaters.

    The most difficult thing in all this is that each person is very sensitive to "average ethers" in his own way.

    To taste - I would argue a lot with someone who loves "tube copper shade" 🙂

    I love vodka :)

    This is a pure product that doesn't cause a hangover :) if you don't drink a lot. And all these variants of moonshine and tinctures - always contain whole "bunches" of impurities, moreover, of an uncontrolled composition (copper simply gives a set of impurities instead of sulfur and aldehydes instead of some of the alcohols).

    Therefore, if you have special requirements for taste, you need to experiment.

    In a vacuum, you need to understand that the higher the vacuum (closer to -99kPa), the more ethers are released into the final product without change. For example, the taste (and smell) of cereal mash (rye and wheat) will run well in the first third of the distillation if you are distilling under high vacuum.

    But if you have rotten grain, then the smell will not be very good ... Bad grain is best distilled into pure alcohol, and then used for tinctures.

  8. 2 hours ago, SlickFloss said:

    Sorry my redneck ass tryna keep up with your lab dwelling ass (that was meant as a compliment). Is that a copper liquid solution or is it a special type of solid that you steep in the kettle? Cheers

    A little information 🙂
    Colloidal copper.
    This is one of the main trace elements that are involved in the vital processes of the human body. It is one of the components of human blood and plays a very important role in the oxidation of vitamin C. Among non-ionic colloids, copper is today the strongest fungicide and disinfectant.
    This is the first :)

    Materials in an ultrafine state (dimensions of the order nanometers) have specific properties, which are due to the peculiarities of the formation of the structure and the presence of a large number of atoms located on the surface of the nanomaterial.
    Due to the uncompensation of the bonds of atoms located in the near-surface layers of nanosized particles, the symmetry of the distribution of forces acting on them is violated. This leads to an increase in the free energy of their surface in comparison with macro- and micro-sized materials and, as a consequence, to the intensification of adsorption processes, ion and atomic exchanges, etc.
    This is the main thing 🙂

    Colloidal solutions. What is it?
    Cold morning fog settling on the ground, a column of smoke over the fire, suspended particles in the water of rivers and lakes - we have seen all this many times. This is the "colloidal solution".
    We are constantly surrounded by dispersed systems.

    Applied to distillation :)
    Colloidal copper solution must be added to the distillation tank. For a tank in a 100-200 liters, only about 1 gram of colloidal copper is enough.
    Because of the huge total surface area of copper particles, they perform hundreds and thousands of times better than your copper trays inside copper columns.

    Colloidal copper works in the tank itself already when the mixture (mash) is heated. And prevents the stench from evaporating from the tank.

    There are several simple ways to make fine copper particles. For example electrolytic.

    SlickFloss - don't consider yourself unworthy or stupid :) just because you don't know something. In the 21st century, Knowledge is available to everyone. Don't be afraid to ask :)
    You and I are the same - I, too, two years ago did not know about it (colloidal copper), simply because I did not ask myself the question "how to remove odors during vacuum distillation at temperatures below 70 Celsius." I was looking for a solution and I found it. A simple solution.

    I don't like the word "redneck". I believe that people who work in the field or on a farm deserve no less respect than those who launch rockets to the moon. 

  9. On 2/21/2021 at 6:59 PM, Southernhighlander said:

    I can build an all stainless still, by outward appearance, with my copper catalyzers inside that will result in spirits with no detectable sulfur taste.

    I will support Paul.

    The use of "catalysts" (special devices) inside the steel tank is the best price-quality option.

    From the point of view of Chemistry and Physics, in order for chemical reactions to occur with maximum efficiency, it is necessary to provide the largest possible contact surface of the substance-catalyst, and to provide a temperature higher than the "temperature of the beginning of catalytic reactions". That is why catalyst inserts must be in the path of alcohol-water vapor at temperatures above 70 Celsius. Copper does not work below 70 degrees Celsius.

    The surface area of classical copper (completely made of copper) distillers is inferior to catalyst inserts in terms of interaction area and has a very high cost.

    If we talk about a further increase in the efficiency of copper, and even at low temperatures, then we should work not with copper surfaces, but with "molecular" (colloidal) copper in solutions inside the tank. This makes it possible to increase the contact surface with the copper catalyst by a factor of hundreds and to work at temperatures below 70 Celsius (vacuum distillation).

    But this is a more complex technology.

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  10. On 2/18/2021 at 5:15 PM, Southernhighlander said:

    Pete B.

    I have never seen a continuous stripping still that did not need liquid condenser cooling,  How does that work?  

    I have seen a pot still condenser set up that had both an air cooled condenser and then a liquid cooled condenser.

    Maybe my friend Alexander has seen designs without liquid cooled condensers.  Alexander, if you see this post, let us know if any of the old industrial Soviet continuous still designs worked  without liquid cooled condensers and if so, were air cooled condensers used?

    My point is that if you do distillation (no matter what liquids or oils) you need to work with heaters or coolers. :)

    In any case, if you need to turn water (alcohol) steam into a liquid, you need to take away thermal energy from the steam and direct it somewhere. It can be cold water, it can be atmospheric air.

    But it should be remembered that water has the highest heat capacity, so water is very well suited for transferring heat energy. Your vehicles are water cooled. Why? because it allows for compact cooling devices. If you have a motorcycle :) you can estimate how much its cooling differs in efficiency from liquid cooling. Why a motorcycle needs large cooling fins on the cylinder.

    As for the USSR solutions for distillers, air cooling was not used due to the bulkiness and unpredictability of the weather. You cannot cool the cooler with air below 40 Celsius if you have a shade temperature of 40 Celsius in the summer. In the USSR, evaporators (not refrigerators with freon) were used for industrial installations.

    These are such large installations, where hot water from condensers was sprayed and fell into the tank, giving energy to the surrounding atmosphere. At the same time, part of the water evaporated, these water losses were inevitable.

    I think we need to use energy recovery in continuous columns and condensers. The input mixture (water and alcohol with yeast) is always at the ambient temperature (depending on the weather). The second positive point in this scheme is that heating the inlet mixture into the continuous column helps to increase the productivity of the stripping column. I have several schemes in which the alcohol vapor condenser was cooled by the inlet mixture from the fermentation tank.

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  11. Milking yeast is not a fantasy.

    Introduction.

    Classical fermentation (wort fermentation process) is a familiar process. Bacteria (yeast fungi) eat up sugar and release carbon dioxide and ethyl alcohol in the process. Everything is very good, but yeast eats sugar and defecates with alcohol at the same time 🙂 And then we boil the mixture together with the bacteria, kill them, and release alcohol and with it the by-products of the yeast's vital activity, including "heads", "tails" and various toxic substances.

    What if you don't kill the yeast? We don't kill a cow when we want milk? We don't kill bees when we want honey?

    This idea has occurred to people more than once, and it was even tested. The results were very interesting and positive. But how to take alcohol away from yeast without killing it? It's very simple - you need to create a vacuum! High vacuum so that the alcohol boils at 20-28 degrees Celsius, while the yeast does not die, and carbon dioxide and alcohol, as well as light (aromatic) impurities (heads, ethers) are removed from the mixture.

    Experiments have shown that the use of vacuuming fermenting wort leads to an increase in the degree of fermentation of sugars. Increase in the total degree of fermentation of sugars by an average of 10%. As a result of the removal of yeast metabolites from the mixture, the alcohol yield increases in terms of fermented sugars. Thus, under vacuum, the alcohol yield is 74% of the theoretical, while at atmospheric pressure it reaches only 50%.

    Alcohol quality problem.

    In recent years, the industrial production of edible ethyl alcohol has been characterized by a significant increase in the requirements for physicochemical and organic the leptic quality of alcohol. Much attention is paid to the modernization of rectification plants, which provide deep purification of alcohol from impurities formed during technological processes.

    A further increase in the physicochemical and organoleptic quality of alcohol can be achieved on the basis of technological solutions aimed at preventing or significantly reducing the formation of impurities during its production. As you know, under anaerobic conditions, the yeast cell Saccaromyces cerevisiae receives energy for reproduction and growth by converting glucose into ethyl alcohol. Besides actually plastic metabolism, part of this energy is spent in the so-called maintenance metabolism, associated, among other things, with the work of active transport systems against the gradient of the osmotic pressure of the environment. Since alcohol is the strongest factor in osmotic pressure, its accumulation during fermentation gradually leads to energy starvation of cells, cessation of growth and biosynthesis of alcohol, and their death. The process of suppression of vital activity and the death of yeast begins to manifest itself noticeably even when the alcohol content in the medium is 6-8% vol. and is accompanied by a number of metabolic changes and, accordingly, a sharp an increase in the amount of polluting metabolites. In this regard, when selecting industrial strains-producers of ethyl alcohol, one of the most important features is their osmotolerance. (i.e. the ability not to die at alcohol concentrations of 12-15%). Along with the impurities intensively formed by alcoholic yeast at the end of the fermentation period, impurities are also formed by the polluting microflora.

    For example, isopropanol is one of the impurities that are most difficult to separate by brago rectification, it is formed by clostridia that get into the wort with soil residues and grain weed. Increasing the level nya aseptic processes of fermentation and yeast generation also leads to a decrease in the content of impurities in alcohol and an increase in its organoleptic quality. The mash column, in which the mash is boiled under atmospheric pressure, is also a powerful generator of impurities. The content of some impurities in the brew distillate, for example, acetaldehyde, increases several times in relation to the original brew. New growths that were not contained in the brew are also added. The use of a vacuum in the distillation of the mash is known to significantly reduce the formation of impurities at this stage.

    When obtaining alcohol from grain, practically only starch, which makes up 52-54% of dry matter of grain, is used for the biosynthesis of alcohol. The rest is displayed with bard. The dry matter of stillage contains about 28% of crude protein, in which up to 40% of bypass proteins are especially valuable for cattle. Therefore, the grain stillage of distilleries is It is, in principle, a very valuable feed resource for animals.

    Studies have established that the course of fermentation in a vacuum is characterized by a number of distinctive features that make this technology very attractive, especially for the production of high-quality alcohol:

    1) Under vacuum conditions, alcohol is distilled directly in the fermentation tank at the fermentation temperature, and it is removed from the liquid phase immediately by to the extent of its formation. Thus, fermentation takes place at practically zero alcohol concentration in the brew.

    2) The rate of alcohol formation (hence, the productivity of the equipment) increases 2-3 times.

    3) The viability of the yeast and its activity is maintained at the original level, throughout the entire fermentation cycle.

    3) The yield of alcohol per ton of starch remains within the limits of not lower than the established norms. At the same time, the accumulation of yeast biomass increases in times.

    4) It becomes possible to increase the mixing module up to a 1:1 level.

    5) In the fermentation tank, when working with such hydromodules, there is practically no foreign microflora. There are no impurities typical for polluting microflora, for example isopropanol.

    6) At the exit from the fermentation tank, the concentration of alcoholic distillate is 35%, which makes it possible to send it directly to the epuration, excluding the beer column from the rectification unit.

    7) At the end of the fermentation cycle, due to the evaporation of water, the dry matter content in the liquid phase of the fermentation tank increases to 26-30%. This creamy, fluid-retaining liquid containing 32-36% crude protein is essentially a concentrated vinasse, ready for final drying.

     

    I will not bore you with details 🙂 I will give just one tablet, which contains data on the chemical analysis of various components during the "milking of bacteria" in comparison with conventional fermentation and classical distillation.

    (Control is classic fermentation)

    _tabl.thumb.jpg.ef417c5f41fda42a37ede5984ed914a7.jpg

     

  12. "Rectification" (from Latin "rectus" - direct and "facio" - do) is a process of separating double or multicomponent mixtures due to countercurrent mass transfer between vapor and liquid. Rectification - separation of liquid mixtures into practically pure components, differing in boiling points, through repeated evaporation of the liquid and condensation of vapors.

    This is the scientific definition of the term "rectification".

    From the point of view of this description, distillation in a pot (moonshine still) is not rectification, but is a simple separation of a mixture of different alcohols (ethyl and related fermentation results) from a water-alcohol mixture.

    Rectification, i.e. the separation of a mixture of alcohols into separate alcohols, and the separation of just ethyl alcohol separately from other components, is carried out (should be done) in distillation columns, in which it is precisely the separation of components along the height (different trays and withdrawal of different components from different trays from the column at the same time).

    Thus, the work of the "flute" on the moonshine tank is also not rectification.

  13. I  describe  (below) what simple equipment you need to buy in order to conduct tests and start moving into the topic of vacuum distillation.

    You need to provide:

    1)  tightness.  Not  all devices are equally gemetichny for excess and negative  pressure.  Tanks  that  withstand + 100kPa (+ 1 atm) may not
    withstand a vacuum of -50kPa. My first device, has a wall thickness of 1.5mm  stainless steel and a volume of 20 liters, the bottom and the top
    cover  are  flat,  because of this, under vacuum, I got the bottom and the cover 5mm inside the tank. The walls (cylinder) stood.

    2) strength. Chinese "stainless steel" of small thickness can collapse inside.  At  -50 kPa vacuum for every 1 cm2 will press 0.5 kilogram of
    pressure.  For  example,  a pressure of about 300 kilograms presses on the  lid of my pressure cooker, with a total of -50 kPa. It is 28cm in
    diameter!  I  ask  to  check  your  tanks - especially large size. And especially  "square"  - round section tanks hold vacuum better without
    deformations.   It  is  possible  to  apply  the  solution  to  create "frames"(shpangout's)   in   submarines,  which  will  strengthen  the
    strength of the tank without increasing its wall thickness. Frames are internal and external.

    it  is  not  necessary  to solder the frames to the tank inside - this will  complicate the cleaning - the frames can be performed as a power
    plug-in construction, which can be pulled out and washed separately.

    External  frames  are  best  done  in the style of "steam-punk" 🙂 in combination  with copper and chrome (polished) it will be sold just to
    put as an element of the interior :)
    Here is a picture (to understand the essence) :
    klam0038-03.jpg
    ( no rivets needed :) )

    3)  A  simple diaphragm pump at 12 volt power. I have a few, I brought it  from  China  for  my  experiments - the price ranges from 10 to 15
    dollars, excluding delivery.
    I  have  four pumps now, different power and different pressure, up to -90kPa,  but  you  have enough for the experiments and -40 ...- 50kPa.
    for example:
    http://yanhuafaith.com/vacuum-pump-series/brush-vacuum-pump-series/z50series-148.html
    You can search for the same pumps in your USA, on eBay

    the pump that I indicated above - I put it right on the way out of the moonshine,  it pumps everything through it. Plastic does not smell, it
    can be used to store food. This pump is enough for you to conduct experiments.

    4) hoses with a thick wall. I use food 7mm internal and 2.5mm wall.
    http://www.symmer.ua/product.html?id=12
    "SYMMER Alco SAPE"  (plastic hose for alcohol)
    Hose material: translucent elastic PE
    Operating temperature: -10˚C + 60˚C
    Food
    Cadmium Free Cd, Barium Ba, Lead Pb
    Operating pressure / critical pressure: 10/25 bar
    This hose keeps pressure up to -90 kPa without deformation.
    This is an example, it is not necessary to buy a hose in this company :)

    You  can  use  a  normal silicone hose, but inside it, lay a spiral of stainless  wire  or  copper  wire  so  that  the hose does not wrinkle
    inside.

    5) manometer showing vacuum - for example, here:
    https://apollo-ireland.akamaized.net/v1/files/017el6xbowzq-UA/image;s=1000x700

    6)  to  assemble  a  simple  circuit:  a  power supply unit from a 12V computer,  a button or a toggle switch for on-off pump, hoses for tank and mash. :)

    well, through a tee - a pressure gauge on the pump suction, a pressure gauge  should  be  placed  higher  -  so  that  the moonshine from the moonshine outlet or the column would not get into it.

    7)  check  the vacuum - the pump will pump up for example -40kPa in an empty tank - we turn on the pump and wait until it pumps up the vacuum -40kPa  -  we  turn off the pump and wait - it should hold for about a minute, do not whistle anywhere.

    😎  fill  in  the  mash (mash), assemble the installation, stock up on paper with a pen (pencil) and camera 🙂
    we  start  to heat the mash - we heat up to 40 degrees (degassing) and at  the  same  time we thresh with a pump to -50 ... 55kPa. Find out a lot of interesting things about "carbonated drinks" :)

    9)  heat  the  braga  (mash)  up  to 51 .... 55 degrees, with the pump holding  -60...-70kPa, you can not warm it up first and then suck it
    out  -  explosive  boiling  is  possible  -  the  tank  will bounce :)
    Therefore  we heat and hold the vacuum. We supply cooling water to the cooler;  if  you  have a column, we also supply a little water. With a dephlegmator  it  will  be  difficult  -  you  will have to re-set the temperature in it for the vacuum. At this temperature methanol will go -  drops,  if  you have it, and other "aromatic".
    The output is small, with a tank of 20-25 liters (I have such a tank). I had up to 100 ml of “heads” of everything.

    10)  well,  how  have you reached 55 degrees - do not yawn and not run away  -  warm  up  to  57-61 degrees celsius and -60-70kPa. This is a very responsible place - a large output (just a stream) of alcohol of 96-98degrees  of  the  fortress  can go, if you have moonshine. So that the pump  does not choke, we also look at the outlet hoses so that they do not overflow. Time on-off pump, hands.

    11) if you do not go alcohol at 60 degrees of heat - gently warm up to 63...64,  maybe  you  have  a  great moonshine design or mash, but carefully  -  after  the  "start  pouring"  you may have to reduce the temperature from 63-64  to 55-57 degrees, you have to watch along the way, and  here  the  dances begin with a tambourine around the dephlegmator and its water cooling ... (I had many problems with the exact settings of  the process). So I would recommend if anyone has columns - use the column  in  the moonshine mode, in the first experiments not to suffer with a dephlegmator and its settings. The product and it will turn out cleaner  and  more pleasant than "according to the classics", you will see and feel yourself :)

    12)  well,  and  look after the process, do not forget to pump out the vacuum  with  the  pump (it will fall) and pump the product out of the hoses :) we  measure the density, make sure that the tank does not jump up to a boil,  and does not go "dregs" from splashing mash through your entire installation.

  14. Equipment   requirement:   1)  withstand  negative  pressure,  without
    “collapsing”.  2) it is necessary to resolve the issue with the output
    of  ready-made  moonshine  - there are two options - either the output
    tank  is  also  under  vacuum,  or  the  moonshine is pumped through a
    membrane pump, and then it is simply poured into a regular container.

    in  my  experiments, I simply connected a hose with thick walls to the
    outlet  of the column, and pumped air out of the equipment through it,
    and  in  the process, I pumped the moonshine with my pumps, pumped the
    pumps and pumped it into the bottle.

    I  used  Chinese-made diaphragm pumps made from plastic, which is food
    grade. Plastic is odorless and does not affect the taste.

    If  you  want  to  conduct  your experience with a vacuum, you need to
    decide how to connect the hoses to the outlet and to the pump.

    your   first   experience   "manually",   according   to  my
    instructions.  After the experience, you yourself will decide what you
    need and what not. Good?

    ...  You  have  understood correctly that it will be good for Jin and
    Whiskey.
    In  2012,  the world became acquainted with gin Oxley, obtained by the
    “cold method”, as it was called, although it would be more accurate to
    say, vacuum distillation. The British brand Oxley pleased connoisseurs
    of  refined alcoholic beverages with a new classic dry gin based on 14
    herbal  ingredients,  including  juniper,  citrus and meadowsweet, the
    combination  of  which  creates  a fresh, bright and rich taste of the
    drink.

    The  gin  manufacturing process is based on a unique cold distillation
    technology:  the high temperature used in the traditional distillation
    process  can  have  a negative effect on the natural taste of alcohol,
    causing  the  loss of most of the delicate flavors. Oxley, the world's
    first  gin based on cold distillation, prevents the occurrence of such
    a  problem completely. Oxley produces only 240 bottles of original gin
    per day.

    ...

     

     

  15. 35 minutes ago, SteelB said:

    i wish i knew more about vaccum distilation, I am familiar with what your talking about i have never done it.

    Italian pamphlet-article on the vacuum distillation of grappa in comparison with taditsionny distillation.
    year 2009.

    Sorry,  it  is in Italian, I tried to translate their conclusions, and the   schemes   themselves   inside  the  document  are  in  principle
    understandable to any Engineer :)

    My translate:
    ...summary :

    Describes  an  innovative  distiller  operating in vacuum and a column
    without  plates,  and  the  profile  of volatile compounds of products
    obtained in different phases of the distillation process under various
    vacuum  conditions,  both during the second distillation of grappa and
    the   direct  production  of  various  types  of  brands  compared  to
    traditional  grappa  from  bain plants -marie acting in Italy. Results
    define  products  that  are  significantly  improved  or  have special
    features:

    strong  lowering  of  head  impurities,  such  as acetaldehyde and its
    acetal  and ethyl acetate; b) a reasonable reduction in the content of
    esters  (acetates of various alcohols and ethyl esters of fatty acids)
    belonging  to  the  classes of low, medium and high boiling, thus, the
    configuration  of  various  and  attenuated  fruit  notes; c) possible
    limited  reduction  of  methanol  and  maintaining a pattern of higher
    alcohols  and  other alcohols, also on C6; d) maintaining a good level
    of  monoterpenes  with possible profile changes and the implementation
    of  someone  very  typical (see Amarone). It should be emphasized that
    many  of  these  important  compositional  changes  cannot be obtained
    during  normal  operations  or  process  adaptations  to discontinuous
    systems, in particular, in bain-marie.

    System description

    The  plant described below and shown in figa and 1b, is a prototype of
    an innovative distillation system compared to traditional ones. It was
    the subject of extensive experimentation, begun with preliminary tests
    in  May  2003,  and  continued  with  others,  conducted mainly at the
    distillery  of the San Michele all'Adige Agricultural Institute. Being
    able  to  work  also as a vacuum evaporator, the plant can be used for
    distillation  and  concentration of substances of any type and nature,
    with   particular   emphasis   on   the   food,   cosmetic,  chemical,
    pharmaceutical and purification sectors.
    ..................

    _dist0.jpg

  16. On 9/22/2020 at 4:23 AM, SteelB said:

    I would prefer a natural flavor

    You need to consider applying vacuum distillation.
    You can use something like a "gin basket" in the path of alcohol vapor, but this path will result in "boiled cherries" instead of a pleasant smell because the temperature of the vapor will be high.

    I have a scientific article from Italy where the guys made an excellent grape drink (grappa) using vacuum distillation. The drink retained the aromas of grapes and received a strength of 35-55% of alcohol.

    I myself deal with vacuum distillation issues. Vaccum distillation preserves the subtle aromas of hop grain (if necessary) and grapes.
     
  17. Second interesting idea,
    maintain a constant boiling point of alcohol in the hollow column (we will rather focus on the upper point). We will try to predict the temperature change using the lower two sensors. Anything that has a lower temperature should condense directly back into the cube (reflux).

     

    kolonnads.JPG


    this is what we end up with: (this is a hydrometer with 94% alcohol content)
     

    94_2per_dist.jpg
    As practice has shown, the temperature in the reflux condenser cannot be the basis for controlling the distillation process. The problem is that it differs by 1 - 1.5C, depending on external conditions (room temperature, atmospheric pressure) and the type of distilled material (wine has some control boiling points, mash has others, mead has third, jam mash - fourth).

    An interesting feature was noticed. The temperature of the copper air cooler (column, where the fan is on the diagram) changes in an interesting and strictly defined way: the temperature at the end of the distillation (precisely at this point of the cooler = closer to the end of the first heat exchanger) behaves as follows: it slowly rises to somewhere around 67- 69C, and then drops sharply to 46-47C (within 10-11 minutes). And after this drop in temperature, the outgoing alcohol, as they say, “does not burn” (all the alcohols are already partially gone, there is nothing to burn).
    This temperature dip is explained, apparently, by the fact that the heat capacity of the boiling steam changes so that it is able to cool much earlier in the heat exchanger than the alcohol-containing steam. That is, there is more water in it and it condenses already at the first turns of the heat exchanger.

    The design of the refrigerator can be as follows:

    fixed 4 fans with a diameter of 140 mm from a computer at 12 volts. Heat exchangers cope with the task easily, there are no stagnant zones in them, they are straight-through. Toward the end of the first heat exchanger, a temperature sensor was attached, which controls the switching on of the refrigerator fans with a setpoint of 30C.

     

    rnyem3d8yph07oab9yu5ftfvgqw.jpeg

    As a result, a control algorithm for the apparatus was formed:
    1. We heat the distillation cube (about an hour - one and a half - depending on the external temperature of the environment and the volume of the apparatus, in the experiments a tank of 20-25 liters was used). We are not doing anything. We are waiting for the "heads" to appear. We are waiting for the electronic thermostat (in fact, a unique digital signal) to trigger, which is set to 30C. It was noticed that after turning on the thermostat, it does not turn off until the very end of the distillation process (if the outside air temperature is above zero). The actuation of the thermostat and the switching on of the column fans exactly coincides with the beginning of the "heads" outflow. We start the timer for 5 minutes (this time is always enough to drive off 200 ml of heads). After 5 minutes, we can begin to take away ethyl alcohol ("strong body"). We are waiting for 30 minutes. During this time, about 1 liter comes out (with a usual filling of a cube of 20 liters) of a strong "product" (60 percent ethyl alcohol).

    2. We pass to the selection of "weak body" (low concentration of alcohol, "tails"). We distil for 1 hour (distillation of the "weak body" takes about 1 hour while the "alcohol is burning" - this is still somewhere around 1.5-2 liters). And during this hour we do nothing, but only fix the maximum temperature of the temperature sensor.
    In general, the temperature on the column fan at this point can float within 53-69C, but not by 20C. At 20C, the temperature changes only at the end of the distillation and abruptly. For example, you recorded the maximum temperature on a column with a fan, let it be 69C. After driving off the "strong body", we begin to control the deviation from this temperature maximum. If another maximum is caught, fix it (write it down). And again we are waiting for a deviation from the maximum at 20-22C. As soon as the temperature drops below the level (for example, 69-21 = 48C), we switch to the “tails” distillation mode.

    3. In the “tails” selection mode, simply set the timer, for example, for 1-1.5 hours and get as much as possible. During this time, all residues of alcohol will be distilled off anyway. After 1.5 hours, you can turn on some kind of alarm about the end of the process, and after - all equipment can be cooled down and turned off.

     

    Real experiment:
    Distilled 18 liters. Sugar mash.

    0:00 - Start heating the distillation cube.
    1:00 - Boil violently. The reflux condenser (column with fan) is warming up.
    1:02 - Thermostat has tripped. The fans spun. The setting is 30 degrees for on, 28 for off. Heads began to flow.
    1:06 - 250 ml. "Heads" drove away. 57-60C - steady-state temperature at the control point of the column with the fan.
    1:30 - 1 liter of 60% alcohol solution distilled.
    1:58 - 2.5 liters distilled off (1 liter of "strong body" and 1.5 liters of remnants of the "weak body"). The temperature slowly crept up.
    2:03 - Temperature at the set point of the refrigerator 69.7C.
    2:10 - The temperature slowly crept down.
    2:16 - 66.3C.
    2:24 - 58.3C.
    2:28 - 55.0C.
    2:29 - 54.0C.
    2:30 - 52.2C.
    2:31 - 51.0C.
    2:32 - 48.0C.
    2:33 - 46.0C.
    2:35 - 46.2C - the end of the "weak body" distillation.
    2:39 - 46.6C.
    3:27 - 45.0C - the end of the "tails" stripping.
    -end-
     
    Experiment two:
    The next time the distillation went the same way, only the temperature was shifted a little higher - it was warm in the room. But the 20C difference persisted. During the distillation process, two temperature jumps are observed - at the beginning to 63C and at the end to 69C with a drop between the peaks to 53C (one peak for methanol, the second for ethanol?). But in the end - all the same a failure, as I said, but sharp and at 20C from the maximum.


    In general, in the course of experiments, I concluded that The key to controlling the distillation process is not the temperature in the distillation cube or dephlegmator, but the temperature at the desired point of the dephlegmator (only in a column with a fan, see the diagram-figure). The algorithm would be perfect if it were not for the low temperatures in the room. If the distillation takes place in the open air (if the distillation is going somewhere in the garage) around 0С, the algorithm "breaks down". The temperature at the thermostat temperature sensor drops below the on-off thresholds.

    It was noticed that even with different brews, at different outside air temperatures, the time for distillation really differs, but this difference in the duration of the process consists only in the heating time of the tank with the contents and can go from 1 to 1.5 hours. The rest of the time of the distillation process practically does not change (with the same filling of the tank).

    Thanks for your attention.

    8wamdm9upzpqkoruhmtjzt6rtke.jpeg

    u5dyg6zfowrhszvs2uf9eo_kd28.jpeg

    97j0ga2fe0fif8nhnf87ww-nyng.jpeg

  18. Automation for any moonshine still with a steamer
    (I do not know how exactly the word for a can or a hollow cylinder at the outlet of the moonshine is translated into English, see the figure and diagrams).

    Many people have questions about how you can make the work of a moonshine still fully automatic without using expensive solutions. (for example using Arduino).
    I am collecting simple and unusual solutions that have been posted on the Internet by individual craftsmen in the past years.

     
     

    gr.jpg

    shema_apparat_.JPG

    I propose a simple experiment that can show you what happens to temperature changes in a "classic" moonshine still. The experiment was carried out on a small cube (10-25 liters), but the temperature values are very characteristic and you can rely on them in your experiments.

    Main idea:
    It is possible to track the beginning of the process and, in automatic mode, smoothly enter the working state of the moonshine still using three temperatures: the vapor at the top of the tank, the temperature in front of the can and after it.

    An error of 0.5 degrees of temperature sensors is enough, for software processing of data from sensors this is more than enough.
    The sensors are simply pressed against the pipe and thermally insulated with silicone. Since we are not interested in the exact temperature of the steam at these points, but only in its difference, I think this approach is appropriate.

    So, the most interesting thing is the schedule for reaching the operating state during the test distillation, the purpose of which was to obtain temperature values in manual mode.


     

    graffik_3dallas.JPG

    The graph shows the passage of steam from the distillation cube to the refrigerator, depending on the temperatures indicated above. It can be seen here that after 54 degrees at the entrance to the steam can, you need to be very careful and gradually reduce the power for a smoother exit to the operating mode.
    We will be guided not by the value of the temperature, but by the difference in the readings of these two sensors, but it is still necessary to be tied to the readings of the sensor at the entrance to the steam chamber, say: the temperature is more than 50 and the difference is 24 degrees => we reduce the power.
    The temperature difference allows you to ignore the atmospheric pressure.

    The end of the exit of the "tails" will be in the region of 70-71 degrees, (see the graph), while this will be the same temperature of the sensor before and after the dry jar (the first can after the steam exits the tank).
    The temperature in the tank at the end of the distillation can be 90-90.75 degrees Celsius, or, if you need all the "tails", then 95-97 degrees.

    The author of this solution (experiment) recommended focusing on the following temperatures at the top of the tank:
    68C - depending on the tank capacity, up to 30 minutes (acetone, methanol) leaves the tank.
    79-80C - the main distillation process is underway.
    above 80C - alcohol residues and tails come out.

    Thanks for your attention.

  19. On 11/15/2018 at 10:32 PM, PeteB said:

    The problem I have experienced with centrifugal pumps is if there is still some CO2 in the beer they cavitate especially if trying to push to a reasonable height ie. with back pressure. The flow control valve and column height would cause back pressure. Also any solids in the feed could obstruct the control valve. The centrifugal would be fine if no residual CO2 or solids.

    I think the rubber type impeller pump which is a positive displacement type would be far less likely to have problems, Jo Dehner suggested the same.

    1) the presence of CO2 in the inlet mixture is not a problem, it is good for distillation (stripping of the column). This increases productivity. You need to use an agitator in the tank that mixes the mixture before it enters the pump. It is generally useful to quickly stir the mixture in the tank in front of the pump, and add an antifoam agent to the tank, at the rate of 50 ml per 100 liters. An antifoam agent based on silicon, it is inert and does not affect taste and smell, but it will remove foam. Foam is the biggest problem with fast distillation.

    2) if there is a lot of CO2, you can install a simple device that will remove excess CO2 in front of the column enters. This device is more than 50 years old :) I can give a picture and a description of its operation. But I repeat: CO2 in the inlet mixture is useful and increases the productivity of the column.

    3) accurate feeding of the inlet mixture is very important for the stable operation of the column. The use of impellers (pumps for pumping the mixture) has the main problem: these pumps allow the mixture to "slip" past the pump impeller, that is, the pump cannot keep the same pressure in the system under different loads. There must be no valves in the circuit from the pump to the entry into the column! You can consider displacement pumps, but they can become clogged with mixture.
    An excellent solution for very accurate feeding of the inlet mixture with grains and impurities is the peristatic pump. There are a lot of peristatic pumps of different capacities, pump controllers allow very precise dosing of the mixture supply. The peristaltic pump is not afraid of impurities (grains) in the mixture flow.
     
  20. On 11/9/2019 at 8:56 PM, Dehner Distillery said:

    I build continuous stills.

    www.redbootstills.com

    It is very good that there are people who make continuous columns in the USA!
    My respect!

    But ... I looked at your continuous apparatus - why do you need 35 plates if you do not select different fractions in your column? it is very inefficient. You have a very tall column.
    For stripping columns 6-16 trays are sufficient, depending on the quality of the inlet mixture.
    I am designing stripping and fine columns.
     
  21. Here is the picture with the graphs that I promised.
    The horizontal axis is the liquid capacity (load) that the trays can provide.
    The vertical axis is the steam velocity.
    The closed loop of each tray type indicates the acceptable range of use for that tray type.
    As you can see, the bubble cap tray has a very small range of stable operation, and even then at very low vapor and liquid velocities.

    kpd.jpg

    and here are more options for different plates :)

     

     

    tarl.jpg

  22. 29 minutes ago, Beerideas said:

    I've read a fair bit on perforated trays vs bubble caps and I can't work out a straight answer.  Which is preferable and why?

    There are many more options for valves and spacers.
    Check out the picture here:
    http://adiforums.com/topic/11751-anyone-running-continous-stills-really-suprised-at-the-lack-of-them/?do=findComment&comment=69699

    Each of the options (according to the picture) has its own advantages and disadvantages.
    Each of the options can be applied.
    Each option has its own allowable range of steam velocities inside the column.

    If I have time, I can write a page of text with a more detailed explanation of what and how, with pictures.
     
     
  23. 19 minutes ago, Oldguy said:

    I was planning to use a thin film evaporator to strip the grain out, im hoping that as this is a small distillation itself it will also up the alcohol content of the feed.

    from my last post, plate type (5) is suitable for processing dirty mixture with grains. The hole diameter must be at least 8mm.
    A thin layer - I'm not sure what will be effective.

    in the alcohol industry, nobody filters the grains separately. Grains also contain alcohol.

    it is easier to process the mixture completely, without filtration. The stripping column must be able to work with dirty mixtures, I designed such samples.

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