Short-path distillation

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Short-path vacuum distillation apparatus with vertical condenser (cold finger), to minimize the distillation path; 1: Still pot with stirrer bar/anti-bumping granules 2: Cold finger - bent to direct condensate 3: Cooling water out 4: cooling water in 5: Vacuum/gas inlet 6: Distillate flask/distillate. Short path distillation apparatus.svg
Short-path vacuum distillation apparatus with vertical condenser (cold finger), to minimize the distillation path; 1: Still pot with stirrer bar/anti-bumping granules 2: Cold finger – bent to direct condensate 3: Cooling water out 4: cooling water in 5: Vacuum/gas inlet 6: Distillate flask/distillate.

Short-path distillation is a distillation technique that involves the distillate traveling a short distance, often only a few centimeters, and is normally done at reduced pressure. [1] [2] Short-path distillation systems often have a variety of names depending on the manufacturer of the system and what compounds are being distilled within them. A classic example would be a distillation involving the distillate traveling from one glass bulb to another, without the need for a condenser separating the two chambers. This technique is often used for compounds which are unstable at high temperatures or to purify small amounts of compound. The advantage is that the heating temperature can be considerably lower at reduced pressure than the boiling point of the liquid at standard pressure, and the distillate only has to travel a short distance before condensing. A short path ensures that little compound is lost on the sides of the apparatus. The Kugelrohr is a kind of a short path distillation apparatus which can contain multiple chambers to collect distillate fractions. To increase the evaporation rate without increasing temperature there are several modern techniques that increase the surface area of the liquid such as thin film, wiped film or 'wiper' film, and rolled film all of which involve mechanically spreading a film of the liquid over a large surface. [3]

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<span class="mw-page-title-main">Distillation</span> Method of separating mixtures

Distillation, or classical distillation, is the process of separating the components or substances from a liquid mixture by using selective boiling and condensation, usually inside an apparatus known as a still. Dry distillation is the heating of solid materials to produce gaseous products ; this may involve chemical changes such as destructive distillation or cracking. Distillation may result in essentially complete separation, or it may be a partial separation that increases the concentration of selected components; in either case, the process exploits differences in the relative volatility of the mixture's components. In industrial applications, distillation is a unit operation of practically universal importance, but is a physical separation process, not a chemical reaction. An installation used for distillation, especially of distilled beverages, is a distillery. Distillation includes the following applications:

Fractional distillation is the separation of a mixture into its component parts, or fractions. Chemical compounds are separated by heating them to a temperature at which one or more fractions of the mixture will vaporize. It uses distillation to fractionate. Generally the component parts have boiling points that differ by less than 25 °C (45 °F) from each other under a pressure of one atmosphere. If the difference in boiling points is greater than 25 °C, a simple distillation is typically used.

<span class="mw-page-title-main">Still</span> Apparatus used to distill liquid mixtures

A still is an apparatus used to distill liquid mixtures by heating to selectively boil and then cooling to condense the vapor. A still uses the same concepts as a basic distillation apparatus, but on a much larger scale. Stills have been used to produce perfume and medicine, water for injection (WFI) for pharmaceutical use, generally to separate and purify different chemicals, and to produce distilled beverages containing ethanol.

<span class="mw-page-title-main">Vacuum distillation</span> Low-pressure and low-temperature distillation method

Vacuum distillation or Distillation under reduced pressure is a type of distillation performed under reduced pressure, which allows the purification of compounds not readily distilled at ambient pressures or simply to save time or energy. This technique separates compounds based on differences in their boiling points. This technique is used when the boiling point of the desired compound is difficult to achieve or will cause the compound to decompose. Reduced pressures decrease the boiling point of compounds. The reduction in boiling point can be calculated using a temperature-pressure nomograph using the Clausius–Clapeyron relation.

<span class="mw-page-title-main">Rotary evaporator</span> Device used in chemical laboratories

A rotary evaporator (rotavap) is a device used in chemical laboratories for the efficient and gentle removal of solvents from samples by evaporation. When referenced in the chemistry research literature, description of the use of this technique and equipment may include the phrase "rotary evaporator", though use is often rather signaled by other language.

Degassing, also known as degasification, is the removal of dissolved gases from liquids, especially water or aqueous solutions. There are numerous methods for removing gases from liquids.

<span class="mw-page-title-main">Volatility (chemistry)</span> Tendency of a substance to vaporize

In chemistry, volatility is a material quality which describes how readily a substance vaporizes. At a given temperature and pressure, a substance with high volatility is more likely to exist as a vapour, while a substance with low volatility is more likely to be a liquid or solid. Volatility can also describe the tendency of a vapor to condense into a liquid or solid; less volatile substances will more readily condense from a vapor than highly volatile ones. Differences in volatility can be observed by comparing how fast substances within a group evaporate when exposed to the atmosphere. A highly volatile substance such as rubbing alcohol will quickly evaporate, while a substance with low volatility such as vegetable oil will remain condensed. In general, solids are much less volatile than liquids, but there are some exceptions. Solids that sublimate such as dry ice or iodine can vaporize at a similar rate as some liquids under standard conditions.

<span class="mw-page-title-main">Continuous distillation</span> Form of distillation

Continuous distillation, a form of distillation, is an ongoing separation in which a mixture is continuously fed into the process and separated fractions are removed continuously as output streams. Distillation is the separation or partial separation of a liquid feed mixture into components or fractions by selective boiling and condensation. The process produces at least two output fractions. These fractions include at least one volatile distillate fraction, which has boiled and been separately captured as a vapor condensed to a liquid, and practically always a bottoms fraction, which is the least volatile residue that has not been separately captured as a condensed vapor.

Molecular distillation is a type of short-path vacuum distillation, characterized by an extremely low vacuum pressure, 0.01 torr or below, which is performed using a molecular still. It is a process of separation, purification and concentration of natural products, complex and thermally sensitive molecules for example vitamins and polyunsaturated fatty acids. This process is characterized by short term exposure of the distillate liquid to high temperatures in high vacuum in the distillation column and a small distance between the evaporator and the condenser around 2 cm. In molecular distillation, fluids are in the free molecular flow regime, i.e. the mean free path of molecules is comparable to the size of the equipment. The gaseous phase no longer exerts significant pressure on the substance to be evaporated, and consequently, rate of evaporation no longer depends on pressure. The motion of molecules is in the line of sight, because they do not form a continuous gas anymore. Thus, a short path between the hot surface and the cold surface is necessary, typically by suspending a hot plate covered with a film of feed next to a cold plate with a line of sight in between.

<span class="mw-page-title-main">Fragrance extraction</span> Separation process of aromatic compounds from raw materials

Fragrance extraction refers to the separation process of aromatic compounds from raw materials, using methods such as distillation, solvent extraction, expression, sieving, or enfleurage. The results of the extracts are either essential oils, absolutes, concretes, or butters, depending on the amount of waxes in the extracted product.

<span class="mw-page-title-main">Kugelrohr</span>

A Kugelrohr is a short-path vacuum distillation apparatus typically used to distill relatively small amounts of compounds with high boiling points under greatly reduced pressure.

<span class="mw-page-title-main">Evaporator</span> Machine transforming a liquid into a gas

An evaporator is a type of heat exchanger device that facilitates evaporation by utilizing conductive and convective heat transfer to provide the necessary thermal energy for phase transition from liquid to vapor. Within evaporators, a circulating liquid is exposed to an atmospheric or reduced pressure environment, causing it to boil at a lower temperature compared to normal atmospheric boiling.

<span class="mw-page-title-main">Sublimatory</span>

A sublimatory or sublimation apparatus is equipment, commonly laboratory glassware, for purification of compounds by selective sublimation. In principle, the operation resembles purification by distillation, except that the products do not pass through a liquid phase.

<span class="mw-page-title-main">Condenser (laboratory)</span> Laboratory apparatus used to condense vapors

In chemistry, a condenser is laboratory apparatus used to condense vapors – that is, turn them into liquids – by cooling them down.

Multiple-effect distillation or multi-effect distillation (MED) is a distillation process often used for sea water desalination. It consists of multiple stages or "effects". In each stage the feed water is heated by steam in tubes, usually by spraying saline water onto them. Some of the water evaporates, and this steam flows into the tubes of the next stage (effect), heating and evaporating more water. Each stage essentially reuses the energy from the previous stage, with successively lower temperatures and pressures after each one. There are different configurations, such as forward-feed, backward-feed, etc. Additionally, between stages this steam uses some heat to preheat incoming saline water.

<span class="mw-page-title-main">Reflux</span> Condensation of vapors and their return to where they originated

Reflux is a technique involving the condensation of vapors and the return of this condensate to the system from which it originated. It is used in industrial and laboratory distillations. It is also used in chemistry to supply energy to reactions over a long period of time.

Membrane distillation (MD) is a thermally driven separation process in which separation is driven by phase change. A hydrophobic membrane presents a barrier for the liquid phase, allowing the vapour phase to pass through the membrane's pores. The driving force of the process is a partial vapour pressure difference commonly triggered by a temperature difference.

A separation process is a method that converts a mixture or a solution of chemical substances into two or more distinct product mixtures, a scientific process of separating two or more substance in order to obtain purity. At least one product mixture from the separation is enriched in one or more of the source mixture's constituents. In some cases, a separation may fully divide the mixture into pure constituents. Separations exploit differences in chemical properties or physical properties between the constituents of a mixture.

A rising film or vertical long tube evaporator is a type of evaporator that is essentially a vertical shell and tube heat exchanger. The liquid being evaporated is fed from the bottom into long tubes and heated with steam condensing on the outside of the tube from the shell side. This is to produce steam and vapour within the tube bringing the liquid inside to a boil. The vapour produced then presses the liquid against the walls of the tubes and causes the ascending force of this liquid. As more vapour is formed, the centre of the tube will have a higher velocity which forces the remaining liquid against the tube wall forming a thin film which moves upwards. This phenomenon of the rising film gives the evaporator its name.

The low-temperature distillation (LTD) technology is the first implementation of the direct spray distillation (DSD) process. The first large-scale units are now in operation for desalination. The process was first developed by scientists at the University of Applied Sciences in Switzerland, focusing on low-temperature distillation in vacuum conditions, from 2000 to 2005.

References

  1. Harwood, L.M.; Moody, C.J. (1989). Experimental Organic Chemistry: Principles and Practice (Illustrated Edition). Hoboken: Wiley-Blackwell. p. 150.
  2. Hickman, K. C. D. (2002-05-01). "High-vacuum Short-path Distillation-A Review". Chemical Reviews. 34 (1): 51–106. doi:10.1021/cr60107a002.
  3. "Wiped Film Evaporators & Thin Film Distillation Guide". Lab Society - Buy Lab Equipment Online. 2021-01-05. Retrieved 2021-06-30.