Batch distillation

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Batch distillation [1] refers to the use of distillation in batches, meaning that a mixture is distilled to separate it into its component fractions before the distillation still is again charged with more mixture and the process is repeated. This is in contrast with continuous distillation where the feedstock is added and the distillate drawn off without interruption. Batch distillation has always been an important part of the production of seasonal, or low capacity and high-purity chemicals. It is a very frequent separation process in the pharmaceutical industry.

Contents

Batch rectifier

Diagram of a Batch Rectifier BatchRectifier.png
Diagram of a Batch Rectifier

The simplest and most frequently used batch distillation configuration is the batch rectifier, including the alembic and pot still. The batch rectifier consists of a pot (or reboiler), rectifying column, a condenser, some means of splitting off a portion of the condensed vapour (distillate) as reflux, and one or more receivers.

The pot is filled with liquid mixture and heated. Vapour flows upwards in the rectifying column and condenses at the top. Usually, the entire condensate is initially returned to the column as reflux. This contacting of vapour and liquid considerably improves the separation. Generally, this step is named start-up. The first condensate is the head, and it contains undesirable components. The last condensate is the feints and it is also undesirable, although it adds flavor. In between is the heart and this forms the desired product.

The head and feints may be thrown out, refluxed, or added to the next batch of mash/juice, according to the practice of the distiller. After some time, a part of the overhead condensate is withdrawn continuously as distillate and it is accumulated in the receivers, and the other part is recycled into the column as reflux.

Owing to the differing vapour pressures of the distillate, there will be a change in the overhead distillation with time, as early on in the batch distillation, the distillate will contain a high concentration of the component with the higher relative volatility. As the supply of the material is limited and lighter components are removed, the relative fraction of heavier components will increase as the distillation progresses.

Batch stripper

Diagram of a Batch Stripper BatchStripper.png
Diagram of a Batch Stripper

The other simple batch distillation configuration is the batch stripper. The batch stripper consists of the same parts as the batch rectifier. However, in this case, the charge pot is located above the stripping column.

During operation (after charging the pot and starting up the system) the high boiling constituents are primarily separated from the charge mixture. The liquid in the pot is depleted in the high boiling constituents, and enriched in low boiling ones. The high boiling product is routed into the bottom product receivers. The residual low boiling product is withdrawn from the charge pot. This mode of batch distillation is very seldom applied in industrial processes.

Diagram of a Middle Vessel Column MiddleVesselColumn.png
Diagram of a Middle Vessel Column

Middle vessel column

A third feasible batch column configuration is the middle vessel column. The middle vessel column consists of both a rectifying and a stripping section and the charge pot is located at the middle of the column.

Feasibility studies

Generally, the feasibility studies of batch distillation are based on analyses of the following maps:

During the feasibility studies, the following basic simplifying assumptions are made:

Bernot et al. [2] used the batch distillation regions to determine the sequence of the fractions. According to Ewell and Welch, [3] a batch distillation region gives the same fractions upon rectification of any mixture lying within it. Bernot et al. [2] examined the still and distillate paths for the determination of the region boundaries under high number of stages and high reflux ratio, named maximal separation. Pham and Doherty in pioneering work [4] described the structure and properties of residue curve maps for ternary heterogeneous azeotropic mixtures. In their model, the possibility of the phase separation of the vapour condensed is not taken into consideration yet. The singular points of the residue curve maps determined by this method were used to assign batch distillation regions by Rodriguez-Donis et al. [5] [6] and Skouras et al. [7] [8] Modla et al. [9] pointed out that this method may give misleading results for the minimal amount of entrainer. Lang and Modla [10] extended the method of Pham and Doherty and suggested a new, general method for the calculation of residue curves and for the determination of batch distillation regions of heteroazeotropic distillation.

Lelkes et al. [11] published a feasibility method for the separation of minimum boiling point azeotropes by continuously entrainer feeding batch distillation. This method has been applied for the use of a light entrainer in the batch rectifier and stripper by Lang et al. (1999) [12] and it applied for maximum azeotropes by Lang et al. [13] Modla et al. [9] extended this method for batch heteroazeotropic distillation under continuous entrainer feeding.

See also

Related Research Articles

<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:

<span class="mw-page-title-main">Azeotrope</span> Mixture of two or more liquids whose proportions do not change when the mixture is distilled

An azeotrope or a constant heating point mixture is a mixture of two or more components in fluidic states whose proportions cannot be altered or changed by simple distillation. This happens because when an azeotrope is boiled, the vapour has the same proportions of constituents as the unboiled mixture. Azeotropic mixture behavior is important for fluid separation processes.

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. It is used to refine crude oil.

<span class="mw-page-title-main">Fractionating column</span> Equipment to separate liquids by distillation

A fractionating column or fractional column is equipment used in the distillation of liquid mixtures to separate the mixture into its component parts, or fractions, based on their differences in volatility. Fractionating columns are used in small-scale laboratory distillations as well as large-scale industrial distillations.

<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">Pot still</span> Distillation apparatus for flavored liquors

A pot still is a type of distillation apparatus or still used to distill liquors such as whisky or brandy. In modern (post-1850s) practice, they are not used to produce rectified spirit, because they do not separate congeners from ethanol as effectively as other distillation methods. Pot stills operate on a batch distillation basis. Traditionally constructed from copper, pot stills are made in a range of shapes and sizes depending on the quantity and style of spirit desired.

<span class="mw-page-title-main">Column still</span> Apparatus used to distill liquid mixtures consisting of two columns

A column still, also called a continuous still, patent still or Coffey still is a variety of still consisting of two columns. Column stills can produce rectified spirit.

<span class="mw-page-title-main">Azeotropic distillation</span> Any of a range of techniques used to break an azeotrope in distillation

In chemistry, azeotropic distillation is any of a range of techniques used to break an azeotrope in distillation. In chemical engineering, azeotropic distillation usually refers to the specific technique of adding another component to generate a new, lower-boiling azeotrope that is heterogeneous, such as the example below with the addition of benzene to water and ethanol.

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

Extractive distillation is defined as distillation in the presence of a miscible, high-boiling, relatively non-volatile component, the solvent, that forms no azeotrope with the other components in the mixture. The method is used for mixtures having a low value of relative volatility, nearing unity. Such mixtures cannot be separated by simple distillation, because the volatility of the two components in the mixture is nearly the same, causing them to evaporate at nearly the same temperature at a similar rate, making normal distillation impractical.

Reactive distillation is a process where the chemical reactor is also the still. Separation of the product from the reaction mixture does not need a separate distillation step which saves energy and materials. This technique can be useful for equilibrium-limited reactions such as esterification and ester hydrolysis reactions. Conversion can be increased beyond what is expected by the equilibrium due to the continuous removal of reaction products from the reactive zone. This approach can also reduce capital and investment costs.

<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.

The Marcusson apparatus, Dean-Stark apparatus, Dean–Stark receiver, distilling trap, or Dean–Stark Head is a piece of laboratory glassware used in synthetic chemistry to collect water from a reactor. It is used in combination with a reflux condenser and a distillation flask for the separation of water from liquids. This may be a continuous removal of the water that is produced during a chemical reaction performed at reflux temperature, such as in esterification reactions. The original setup by Julius Marcusson was refined by the American chemists Ernest Woodward Dean (1888–1959) and David Dewey Stark (1893–1979) in 1920 for determination of the water content in petroleum.

A zeotropicmixture, or non-azeotropic mixture, is a mixture with liquid components that have different boiling points. For example, nitrogen, methane, ethane, propane, and isobutane constitute a zeotropic mixture. Individual substances within the mixture do not evaporate or condense at the same temperature as one substance. In other words, the mixture has a temperature glide, as the phase change occurs in a temperature range of about four to seven degrees Celsius, rather than at a constant temperature. On temperature-composition graphs, this temperature glide can be seen as the temperature difference between the bubble point and dew point. For zeotropic mixtures, the temperatures on the bubble (boiling) curve are between the individual component's boiling temperatures. When a zeotropic mixture is boiled or condensed, the composition of the liquid and the vapor changes according to the mixtures's temperature-composition diagram.

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

A heteroazeotrope is an azeotrope where the vapour phase coexists with two liquid phases. Sketch of a T-x/y equilibrium curve of a typical heteroazeotropic mixture

The McCabe–Thiele method is a technique that is commonly employed in the field of chemical engineering to model the separation of two substances by a distillation column. It uses the fact that the composition at each theoretical tray is completely determined by the mole fraction of one of the two components. This method is based on the assumptions that the distillation column is isobaric - i.e the pressure remains constant - and that the flow rates of liquid and vapor do not change throughout the column. The assumption of constant molar overflow requires that:

This page contains tables of azeotrope data for various binary and ternary mixtures of solvents. The data include the composition of a mixture by weight, the boiling point (b.p.) of a component, the boiling point of a mixture, and the specific gravity of the mixture. Boiling points are reported at a pressure of 760 mm Hg unless otherwise stated. Where the mixture separates into layers, values are shown for upper (U) and lower (L) layers.

Salt-effect distillation is a method of extractive distillation in which a salt is dissolved in the mixture of liquids to be distilled. The salt acts as a separating agent by raising the relative volatility of the mixture and by breaking any azeotropes that may otherwise form.

<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.

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

A residue curve describes the change in the composition of the liquid phase of a chemical mixture during continuous evaporation at the condition of vapor–liquid equilibrium. Multiple residue curves for a single system are called residue curves map.

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

Dmitri Petrovich Konovalov was a Russian-Soviet physical chemist who worked on gas-liquid phases of solutions in equilibrium and came up with several rules that were also independently worked on by J. Willard Gibbs and the rules are often called Gibbs-Konovalov rules. They provide the basis for distillation and separation of components that form azeotropes.

References

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  3. Ewell, R. H.; Welch, L. M. (1945). "Rectification in Ternary Systems Containing Binary Azeotropes". Industrial & Engineering Chemistry. American Chemical Society (ACS). 37 (12): 1224–1231. doi:10.1021/ie50432a027. ISSN   0019-7866.
  4. Pham, Hoanh N.; Doherty, Michael F. (1990). "Design and synthesis of heterogeneous azeotropic distillations—II. Residue curve maps". Chemical Engineering Science. Elsevier BV. 45 (7): 1837–1843. doi:10.1016/0009-2509(90)87059-2. ISSN   0009-2509.
  5. Rodríguez Donis, Ivonne; Gerbaud, Vincent; Joulia, Xavier (2002). "Feasibility of heterogeneous batch distillation processes". AIChE Journal. Wiley. 48 (6): 1168–1178. doi:10.1002/aic.690480605. ISSN   0001-1541.
  6. Donis, Ivonne Rodríguez; Esquijarosa, Jhoany Acosta; Gerbaud, Vincent; Joulia, Xavier (2003). "Heterogeneous batch-extractive distillation of minimum boiling azeotropic mixtures". AIChE Journal. Wiley. 49 (12): 3074–3083. doi:10.1002/aic.690491209. ISSN   0001-1541. S2CID   96403367.
  7. Skouras, S.; Kiva, V.; Skogestad, S. (2005). "Feasible separations and entrainer selection rules for heteroazeotropic batch distillation". Chemical Engineering Science. Elsevier BV. 60 (11): 2895–2909. doi:10.1016/j.ces.2004.11.056. ISSN   0009-2509.
  8. Skouras, S.; Skogestad, S.; Kiva, V. (2005). "Analysis and control of heteroazeotropic batch distillation". AIChE Journal. Wiley. 51 (4): 1144–1157. doi:10.1002/aic.10376. ISSN   0001-1541.
  9. 1 2 Modla, G.; Lang, P.; Kotai, B.; Molnar, K. (2003). "Batch heteroazeotropic rectification of a low α mixture under continuous entrainer feeding". AIChE Journal. Wiley. 49 (10): 2533–2552. doi:10.1002/aic.690491009. ISSN   0001-1541.
  10. Lang, P.; Modla, G. (2006). "Generalised method for the determination of heterogeneous batch distillation regions". Chemical Engineering Science. Elsevier BV. 61 (13): 4262–4270. doi:10.1016/j.ces.2006.02.004. ISSN   0009-2509.
  11. Lelkes, Z.; Lang, P.; Moszkowicz, P.; Benadda, B.; Otterbein, M. (1998). "Batch extractive distillation: the process and the operational policies". Chemical Engineering Science. Elsevier BV. 53 (7): 1331–1348. doi:10.1016/s0009-2509(97)00420-x. ISSN   0009-2509.
  12. Lang, P.; Lelkes, Z.; Otterbein, M.; Benadda, B.; Modla, G. (1999). "Feasibility studies for batch extractive distillation with a light entrainer". Computers & Chemical Engineering. Elsevier BV. 23: S93–S96. doi:10.1016/s0098-1354(99)80024-6. ISSN   0098-1354.
  13. Lang, P.; Modla, G.; Benadda, B.; Lelkes, Z. (2000). "Homoazeotropic distillation of maximum azeotropes in a batch rectifier with continuous entrainer feeding I. Feasibility studies". Computers & Chemical Engineering. Elsevier BV. 24 (2–7): 1665–1671. doi:10.1016/s0098-1354(00)00448-8. ISSN   0098-1354.

Further reading