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Distillation – from Bronze Age till today

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Stefan Schlosser at Slovak University of Technology in Bratislava
Stefan Schlosser
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Abstract and Figures

A short historical and pictorial excursion on distillation will be presented and new trends in development of distillation will be briefly discussed. The first distillation apparatus found in Mesopotamia (today´s Iraq) comes from the period 3500 BC. A part of distillation apparatus from Spišský Štvrtok (Slovakia) which dates back to 1500 BC (Bronze Age). It is supposed to be the oldest part of a distillation apparatus not only on territory of Slovakia but most likely in Europe. One of the first books on distillation written by J. French have been published in London in 1651. Industrial application other than ethanol distillation was distillation of tar and producing highly purified tar components such as anthracene, carbolic acid and benzene developed by Raschig in Germany who developed also the first modern random packing Raschig rings. Petroleum refineries were next wide application of distillation where this unit operation and related equipment were developed to today´s matured state. The first petroleum refinery Apollo in Bratislava was founded in 1895 and started operation in April 1896. During the first year of operation treated 23 560 ton of crude oil. A new refinery have been built in Bratislava with start up in 1957 and capacity of 120 000 ton per year. Present two distillation units have capacity 2 million ton/year each. New processes as extractive distillation and membrane distillation were developed and hybrid systems with distillation combined with membrane separations are under development may bring new impulse to distillation applications.
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Slovak Society of Chemical Engineering
Institute of Chemical and Environmental Engineering
Slovak University of Technology in Bratislava
PROCEEDINGS
38th International Conference of Slovak Society of Chemical Engineering
Hotel Hutník
Tatranské Matliare, Slovakia
May 23 – 27, 2011
Editor: J. Markoš
ISBN 978-80-227-3503-2
Schlosser, Š.: Distillation - from bronze age till today, Editor: Markoš, J., In Proceedings of the 38th
International Conference of Slovak Society of Chemical Engineering, Tatranské Matliare, Slovakia, 1–12,
2011.
Distillation – from Bronze Age till today
(extended abstract)
Štefan Schlosser
Institute of Chemical and Environmental Engineering, Slovak University of Technology,
Radlinského 9, 81237 Bratislava, Slovakia, stefan.schlosser@stuba.sk
Keywords: history, development, distillation, trends
Abstract
A short historical and pictorial excursion on distillation will be presented and new trends in
development of distillation will be briefly discussed. The first distillation apparatus found in
Mesopotamia (today´s Iraq) comes from the period 3500 BC. A part of distillation apparatus from
Spišský Štvrtok (Slovakia) which dates back to 1500 BC (Bronze Age). It is supposed to be the
oldest part of a distillation apparatus not only on territory of Slovakia but most likely in Europe.
One of the first books on distillation written by J. French have been published in London in 1651.
Industrial application other than ethanol distillation was distillation of tar and producing
highly purified tar components such as anthracene, carbolic acid and benzene developed by Raschig
in Germany who developed also the first modern random packing Raschig rings. Petroleum
refineries were next wide application of distillation where this unit operation and related equipment
were developed to today´s matured state. The first petroleum refinery Apollo in Bratislava was
founded in 1895 and started operation in April 1896. During the first year of operation treated 23
560 ton of crude oil. A new refinery have been built in Bratislava with start up in 1957 and capacity
of 120 000 ton per year. Present two distillation units have capacity 2 million ton/year each.
New processes as extractive distillation and membrane distillation were developed and
hybrid systems with distillation combined with membrane separations are under development may
bring new impulse to distillation applications.
Bronze Age
„Bronze Age – the first golden age of Europe“ was a campaign initiated and supported by
European Council started in 1994. In the Bronze age, which lasted in Europe about 2000 years,
were led bases of European civilisation and ethnic societies in today’s Slovak territory actively
participated in this process [1]. Rich discoveries of ceramic and metallic objects document high
level of development in our territory. These were presented in very successful exhibition “Golden
age in Carpathian mountains“ prepared by Archaeological Institute of Slovak Academy of Sciences
and installed in Fiorano Modenese in Italy in 2002 and further transferred to two other Italian cities
Legnano and Bondeno and in 2004 continued in three Slovak cities including Bratislava with
catalogue [1].
The first distillation apparatus have been found in Tepe Gaura in Mesopotamia (today´s
Iraq) comes from the period 3500 BC, Fig. 18 in book [2] shown in Fig. 1. A part of distillation
apparatus from Spišský Štvrtok (Slovakia) which dates back to 1500 BC is shown in Fig. 2a and its
reconstruction (upper part was not found) [3] is in Fig. 2b. It is supposed to be the oldest part of a
distillation apparatus not only on territory of Slovakia but most likely in Europe [3]. It is obvious
that both vessels are variants of the same type of still where function and efficiency had been
maintained despite size of vessel from Spišský Štvrtok is smaller with height of bottom part of 35
cm comparing to 48 cm for vessel from Tepe Gaura [3].
38th International Conference of SSCHE
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Fig. 1. Reconstruction of a distillation apparatus from Tepe Gaura in Mesopotamia (today Iraq) [3].
(a) (b)
Fig. 2. A bottom part (boiler) of distillation apparatus from Spišský Štvrtok (Eastern Slovakia) [1] (a) and its
reconstruction (upper part (condenser) was not found) [3] (b).
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Late Antiquity
Zosimos of Panopolis was an Egyptian or Greek alchemist and Gnostic mystic from the end of the
3rd and beginning of the 4th century AD. (Wikipedia)
Fig. 3. Distillation apparatus of Zosimos, from Marcelin Berthelot, Collection des anciens alchimistes grecs (3 vol.,
Paris, 1887-1888).
Medieval time
The earliest distillation of Attar was mentioned in the Hindu Ayurvedic text Charaka
Samhita. The Harshacharita, written in 7th century A.D. in Northern India mentions use of fragrant
agar wood oil. (Wikipedia, history of perfume)
Fig. 4. Distillation apparatus using simple hand cooling for the receiver.
Arab scientists
The birth of the Arab physical sciences in the 7th and 8th centuries was one more expression
of the same breakthroughs that were happening in Arab mathematics, astronomy and geography,
driven partly by long-standing scientific traditions in the peoples who came into the Arabic
caliphate. Perhaps the Arab scientific field where the birth was most dramatic was in chemistry.
And the earliest and most powerful Arab practitioner of the new science of chemistry was Jabir Ibn
Hayyan, recruited by Caliph Harun Al Rashid to work in the early House of Wisdom in Baghdad.
Jabir Ibn Hayyan (Geber, 721-815) was a prominent Islamic alchemist, pharmacist,
philosopher, astronomer, and physicist [4]. He has also been referred to as "the father of Arab
chemistry" by Europeans. Jabir is mostly known for his contributions to chemistry. He emphasised
systematic experimentation, and did much to free alchemy from superstition and turn it into a
science. He is credited with the invention of many types of now-basic chemical laboratory
equipment, and with the discovery and description of many now-commonplace chemical substances
and processes - such as the hydrochloric and nitric acids, distillation, and crystalization that have
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become the foundation of today's chemistry and chemical engineering. Jabir is also credited with
the invention and development of several chemical instruments that are still used today, such as the
alembic, which made distillation easy, safe, and efficient. He noted that boiling wine released a
flammable vapor, thus paving the way to Al-Razi's discovery of ethanol.
Fig. 5. Alchemist Jabir helped lay the foundation of
modern chemistry.
Fig. 6. Early Arab distillation device (alembic), used by
early chemists like Jabir and Al Razi.
Fig. 7. Distillation in medieval time.
Fig. 8. Traditional Alembic Pot Still produced nowadays for home use http://www.essentialoil.com/alembic5.html .
Al-Razi (865-925) was the preeminent Pharmacist and physician of his time [5]. The discovery of
alcohol, first to produce acids such as sulfuric acid, writing up extensive notes on diseases such as
smallpox and chickenpox, a pioneer in ophthalmology, author of first book on pediatrics, making
leading contributions in inorganic and organic chemistry, also the author of several philosophical
works.
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Fig. 9. Chemist physician Al Razi at work in his laboratory
Fig. 10. Distillation in Al-Razi time.
Fig. 11. Circular furnace with fractional distillation apparatus (Abraham Elezar pseud., from A. Crusius Erfurt 1735).
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Al-Kindi (801-873, Baghdad, Iraq) [6]
He wrote in the 9th century a book on perfumes which he named ‘Book of the Chemistry of Perfume
and Distillations’. It contained more than hundred recipes for fragrant oils, salves, aromatic waters
and substitutes or imitations of costly drugs. The book also described one hundred and seven
methods and recipes for perfume-making, and even the perfume making equipment, like the
alembic, still bears its Arabic name.
Avicenna (Ibn Sīnā, 980- 1037, Persia, Afghanistan) [7]
Avicenna created an extensive corpus of works during what is commonly known as Islam's
Golden Age, in which the translations of Greco-Roman, Persian and Indian texts were studied
extensively. Greco-Roman (Mid- and Neo-Platonic, and Aristotelian) texts by the Kindi school
were commented, redacted and developed substantially by Islamic intellectuals, who also built upon
Persian and Indian mathematical systems, astronomy, algebra, trigonometry and medicine.
In chemistry, the chemical process of steam distillation was first described by Avicenna. The
technique was used to produce alcohol and essential oils; the latter was fundamental to
aromatherapy. He also invented the cooling coil, which condenses the aromatic vapours. This was a
breakthrough in distillation technology and he made use of it in his steam distillation process, to
produce essential oils. He first experimented with the rose. Until his discovery, liquid perfumes
were mixtures of oil and crushed herbs, or petals which made a strong blend. Rose water was more
delicate, and immediately became popular. Both of the raw ingredients and distillation technology
significantly influenced western perfumery and scientific developments, particularly chemistry. As
a chemist, Avicenna was one of the first to write refutations on alchemy, after al-Kindi.
One of the first books on distillation “The art of distillation“ written by J. French have been
published in London in 1651 [8].
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e Matliare, Slovakia Kl-Tu-1, 256.pdf
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Fig. 12. Figures of distillation apparatus from J. French book [8].
19
th
and 20
th
century
In preindustrial era until the 19
th
century, renewable raw materials were the major source of
energy and material use. During the Industrial Revolution, the use of coal increased sharply and
coal quickly becomes a key raw material in the chemical industry and energy production.
Industrial application other than ethanol distillation was distillation of tar and producing
highly purified tar components such as anthracene, carbolic acid and benzene developed by Raschig
in Germany who developed also the first modern random packing Raschig rings, Fig. 14. In the 20
th
Fig. 13. Fritz Raschig
Fig. 14. Ceramic Raschig rings
38th International Conference of SSCHE
May 23–27, 2011, Tatransk´
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century, there has been a changeover in fossil fuel sources from coal to crude oil and natural gas
due to lower prices, simpler logistics and the versatility in usage of oil and gas. Petroleum refineries
and petrochemical plants were typical with wide application of distillation where this unit operation
and related equipment were developed to today´s matured state.
The first petroleum refinery Apollo in Bratislava was founded in 1895 and started operation
in April 1896 [9]. During the first year of operation treated 23 560 ton of crude oil. Refinery was
renamed to Slovnaft in 1949. A new refinery have been built in Bratislava with start up in 1957 and
capacity of 120 000 ton per year. Present two distillation units have capacity 2 million ton/year
each.
Fig. 15. Atmospheric-vacuum distillation of crude
oil in Apollo.
Fig. 16. Apollo distillation after American
bombardment in June 1944.
Fig. 17. Atmospheric-vacuum distillation 3 of crude
oil in Slonaft with capacity of 1.3 mil ton/year
after intensification.
Fig. 18. Atmospheric-vacuum distillation of crude
oil in Slonaft with capacity of 2 mil ton/year.
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e Matliare, Slovakia Kl-Tu-1, 256.pdf
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Desalination of sea water
Scarcity of drinking water in large territories requires its production from available sources
like brackish water or sea water. One possibility is to use distillation and multi-stage flash
distillation (MSF) was developed which scheme is shown in Fig. 19. Like all evaporative processes,
MSF can produce high-quality fresh water with very low salt concentrations (10 ppm or less), from
salt concentrations as high as 60,000 to 70,000 ppm total dissolved solids, nearly twice the salinity
of seawater. In MSF, evaporation or “flashing” occurs from the bulk liquid. This minimizes scale
and is a major reason MSF has been popular for several decades. Generally, only a small percentage
of feed water is converted to water vapour in one stage, depending on the pressure maintained in
each stage. MSF plants may contain between 4 and 40 stages, but most typically are in the range of
18 to 25. Multi-stage flash plants are typically built in sizes from 10,000 m
3
/day to over 35,000
m
3
/day, with several units grouped together. MSF accounts for the greatest installed thermal
distillation capacity [10-11]. As of early 2005, the largest MSF plant in operation was in Shoaiba in
Saudi Arabi [12]. This plant desalinates seawater for municipal purposes with a total capacity
455,000 m
3
/day, see Fig. 20.
Fig. 19. Simple scheme of multi-stage flash distillation process [11].
Fig. 20. Multi-stage flash distillation (MSF) desalination plant in Shoaiba currently as the largest in the world [12].
21th century
Historical milestones of distillation development are summarised in Table 1. In connection with
the limited availability and increasing price of crude oil and natural gas, the question now arises
how to face this situation and what raw material base will develop in the future? Biomass as a
renewable raw material could be answer [13-14]. There is a historical line of dominant resources
used from local renewable resources to coal, coal gas and tar industries to crude oil and natural gas
in petroleum refineries and petrochemical industry and recently switch to biomass in biorefineries
and other renewable resources is of increased importance.
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Transformation of raw material platform to biomass will not be quick and simple. It requires
concerted cooperation of several scientific disciplines as agriculture, forestry, biology,
biotechnology, chemistry, chemical engineering, environmental sciences, but also industrialists,
strong economical and political impulse, etc. Renewable raw materials will be increasingly used in
the future. New processes have to be developed to transform biomass to fuels, energy and chemicals
in economically competitive way. This will be a challenge also for distillation especially in hybrid
systems.
Table 1. Milestones of distillation development.
Date
Process/equipment
Scientist
Reference
3500 BC
Ceramic distillation apparatus from
Tepe Gaura in Mesopotamia (today´s
Iraq)
[2-3]
1500 BC
Ceramic distillation apparatus from
Spišský Štvrtok (Slovakia)
[1, 3]
801-873
Book of the Chemistry of Perfume and
Distillations
Al-Kindi
[6]
721-815
Developed alembic distillation
apparatus, identified flammable vapours
when distilling wine.
Jābir ibn
Hayyān [4]
865-925
He is known to have perfected methods
of distillation and extraction, which
have led to his discovery of sulfuric acid
and alcohol.
Al-Razi
[5]
980- 1037
Steam distillation was first described.
He invented the cooling coil to
condense vapours from distillation
Avicenna
(Ibn Sīnā)
[7]
1651
One of the first books on distillation was
published
French, J.,
[8]
End of
19
th
century
Industrial distillation of tar
http://www.raschig.de/Co
mpany-en
End of
19
th
century
First modern random packing for
distillation columns
Raschig
http://www.raschig.de/Co
mpany-en
Beginning of
20
th
century
Development of several stage
evaporators in sugar industry
20
th
century
Development of distillation for
petroleum refineries and petrochemical
plants. Bubble-cap trays and packed
columns were mostly used initially.
50-ties
Valve trays and structured packings
instead of random packings were
introduced.
60-ties
High capacity multi-stage flash
distillation (MSF) and multiple-effect
distillation (MED) equipment have been
developed sea water desalination
[10-11]
80-ties
High capacity and highly efficient trays
have been developed
21
th
century
Hybrid distillation and membrane
separation processes are under
development for bioethanol dewatering
[15-18]
21
th
century
Membrane distillation process is under
development.
[19-22]
38th International Conference of SSCHE
May 23–27, 2011, Tatransk´
e Matliare, Slovakia Kl-Tu-1, 256.pdf
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New developments in distillation
Modern civilisation faces several challenges among them shortage of water in many areas,
shortage of fossil raw materials with need to switch fuel and chemical industry to renewable
resources and environmental aspects of our civilisation connected with changes of climate.
Membrane distillation
Membrane based distillation has potential to improve economy of sea water desalination.
Recent research results gives impulse for further development [19-23].
Extractive distillation of ethanol.
For fuel applications, ethanol essentially free of water has to be produced. Considering the low
concentration achieved during fermentation, a huge separation effort has to be expected. In addition,
an azeotrope is formed in this system, which cannot be further separated by simple distillation.
Entrainers, which are fed in counter-current into the separation column, are hence chosen to interact
selectively with the high-boiling component, in this case water, thus reducing its activity and
increasing the relative volatility of ethanol. A high capacity is also important to keep the column
diameter to a minimum. Entrainers enhance the separation factor, and the ionic liquid
[C2mim][BF4] is more efficient than ethanediol if similar concentrations are used. The use of an
ionic liquid entrainer reduces thus the number of plates and/or the recirculation ratio, leading to
overall reduced separation costs [24]. Ionic liquids may provide higher energy efficiency than other
methods.
Hybrid systems with distillation
Hybrid systems with distillation and vapour permeation shows promising results in
decreasing energy demand for bioethanol dewatering for fuel applications [15-18, 25]
Acknowledgement: Support of the Slovak grant agency VEGA No. 1-1184-11 is acknowledged
References
[1] Furmánek, V., Golden age in Karpatian mountains. Ceramics and metal of bronz age in
Slovakia (2300 - 800 BC) (in Slovak). 2004, Archeological Institute of Slovak Academy of
Sciences Nitra.
[2] Levey, M., Chemistry and chemical technology in ancient Mesopotamia, New York, 1959
[3] Ryšánek, J. and Václavů, V., Distillation equipment from Spišský Štvrtok (in Czech),
Archeologické rozhledy, 41 (1989) 196.
[4] Jābir ibn Hayyān. Wikipedia http://en.wikipedia.org/wiki/J%C4%81bir_ibn_Hayy%C4%81n
[5] Muhammad ibn Zakariya al-Razi. Wikipedia
http://en.wikipedia.org/wiki/Muhammad_ibn_Zakariya_al-Razi
[6] Al-Kindi (Alkindus). Wikipedia http://en.wikipedia.org/wiki/Al-Kindi
[7] Avicenna (Ibn Sīnā). Wikipedia http://en.wikipedia.org/wiki/Avicenna
[8] French, J., The art of distillation, Richard Cotes, 1651
[9] Kudlička, E. and Valo, P., Slovnaft 100, Redakcia mesačníka Slovakia, Bratislava, 1995 (?)
[10] Cooley, H., Gleick, P.H., and Wolff, G., Desalination with a grain salt. A California
Perspective. 2006. p. 100 + 28.
http://www.pacinst.org/reports/desalination/desalination_report.pdf
[11] Fritzmann, C., Lowenberg, J., Wintgens, T., and Melin, T., State-of-the-art of reverse osmosis
desalination, Desalination, 216 (2007) 1.
[12] Shoaiba Desalination Plant, Saudi Arabi. http://www.water-technology.net/projects/shuaiba/
38th International Conference of SSCHE
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e Matliare, Slovakia Kl-Tu-1, 256.pdf
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[13] Clark, J.H. and Deswarte, F.E.I., (Eds.), Introduction to chemicals from biomass, J. Wiley,
Vol. 184 p., 2008
[14] Demirbas, A., Biorefineries For Biomass Upgrading Facilities, Springer, 2010
[15] Vane, L.M. and Alvarez, F.R., Membrane-assisted vapor stripping: energy efficient hybrid
distillation-vapor permeation process for alcohol-water separation, Journal Of Chemical
Technology And Biotechnology, 83 (2008) 1275.
[16] Huang, Y., Baker, R.W., and Vane, L.M., Low-Energy Distillation-Membrane Separation
Process, Industrial & Engineering Chemistry Research, 49 (2010) 3760.
[17] Vane, L.M., Alvarez, F.R., Huang, Y., and Baker, R.W., Experimental validation of hybrid
distillation-vapor permeation process for energy efficient ethanol-water separation, Journal Of
Chemical Technology And Biotechnology, 85 (2010) 502.
[18] Cote, P., Noel, G., and Moore, S., The Chatham demonstration: From design to operation of a
20 m(3)/d membrane-based ethanol dewatering system, Desalination, 250 (2010) 1060.
[19] Hanemaaijer, J.H., van Medevoort, J., Jansen, A.E., Dotremont, C., van Sonsbeek, E., Yuan,
T., and De Ryck, L., Memstill membrane distillation - a future desalination technology,
Desalination, 199 (2006) 175.
[20] Nagaraj, N., Patil, B.S., and Biradar, P.M., Osmotic Membrane Distillation - A Brief Review,
International Journal of Food Engineering, 2 (2006.
[21] Criscuoli, A., Carnevale, M.C., and Drioli, E., Evaluation of energy requirements in membrane
distillation, Chemical Engineering and Processing, 47 (2008) 1098.
[22] Yang, X., Wang, R., Shi, L., Fane, A.G., and Debowski, M., Performance improvement of
PVDF hollow fiber-based membrane distillation process, Journal Of Membrane Science, 369
(2011) 437.
[23] Curcio, E. and Drioli, E., Membrane Distillation and Related Operations—A Review,
Separation and Purification Reviews, 34 (2005) 35.
[24] Jork, C., Seiler, M., Beste, Y.A., and Arlt, W., Influence of ionic liquids on the phase behavior
of aqueous azeotropic systems, Journal of Chemical and Engineering Data, 49 (2004) 852.
[25] Baker, R.W., Wijmans, J.G., and Huang, Y., Permeability, permeance and selectivity: A
preferred way of reporting pervaporation performance data, Journal Of Membrane Science,
348 (2010) 346.
38th International Conference of SSCHE
May 23–27, 2011, Tatransk´
e Matliare, Slovakia Kl-Tu-1, 256.pdf
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  • Jul 2021
In the present paper, an intensive analysis of simulation of conventional distillation and extractive distillation to separate a mixture of toluene and heptane (toluene-heptane azeotrope) has been performed. A literature review has been performed for both conventional and extractive distillation and also the advancements and new techniques developed to increase the efficiency of both processes. Aspen Hysys was used as the simulator of choice for simulating both conventional distillation and extractive distillation, whereas Aspen Plus was used to compute the VLE data for interaction of the three compounds with each other. Comparison of the energy consumed by both the processes to achieve the same separation efficiency was done. Cost analysis was performed by using aspen cost analyzer. Cost efficiency was used as the criteria to determine the best process. Extractive distillation was determined to be costing less than1⁄3 times the price of conventional distillation process. Hence extractive distillation is clearly the more economical process.
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... Owing to its low volatility the presence of entrainer in the mixture causes a rise in the volatility of non-polar components present in the mixture. The basic information about the separation process is given in (Schlosser 2014). The extractive distillation process is much more attractive than conventional distillation from the standpoint of both energy consumption and capital investment(J. ...
Comparative And Economic Analysis of Conventional and Extractive Distillation to Separate a Mixture of Heptane -Toluene Using Aspen Hysys
Article
  • Jul 2021
In the present paper, an intensive analysis of simulation of conventional distillation and extractive distillation to separate a mixture of toluene and heptane (toluene-heptane azeotrope) has been performed. A literature review has been performed for both conventional and extractive distillation and also the advancements and new techniques developed to increase the efficiency of both processes. Aspen Hysys was used as the simulator of choice for simulating both conventional distillation and extractive distillation, whereas Aspen Plus was used to compute the VLE data for interaction of the three compounds with each other. Comparison of the energy consumed by both the processes to achieve the same separation efficiency was done. Cost analysis was performed by using aspen cost analyzer. Cost efficiency was used as the criteria to determine the best process. Extractive distillation was determined to be costing less than 1/3 times the price of conventional distillation process. Hence extractive distillation is clearly the more economical process.
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... The use of essential oils dates back to Ancient Egypt where they extracted by steeping plant parts into animal fats and vegetable oils [13]. Around 1000 AD, a turning point for botanical extraction came when Avicenna from Arabia invented the steam distillation method which is now the industry standard for extracting most essential oils [14]. Beginning in 1347, the Yersinia pestis outbreak known as "The Great Plague" became widespread and was responsible for killing one-third of the European population [15]. ...
Antimicrobial activity of the volatile substances from essential oils
Article
Full-text available
  • Apr 2021
Background Essential oils are volatile and lipophilic liquid extracts made from plants as secondary metabolites that can be obtained by distillation. To date, several studies have investigated the direct antimicrobial activity of liquid essential oils. However, this study investigated the antimicrobial properties of the volatile substances present in various essential oils. Methods A modified zone of inhibition protocol was developed using agar petri dishes with a center glass vial to allow evaporation and aerosolization of the potential active constituents from essential oils. In total, nineteen essential oils were tested against five Gram positive bacterial species, five Gram negative bacterial species and one fungi. Results This study found potent antimicrobial activity from the volatile constituents of several essential oils. Rosemary, tea tree, and cassia volatiles were found to be the best broad-spectrum antibacterial agents, whereas clove volatiles had almost no antimicrobial activity. Conclusions These results support the anecdotal historical evidence of the antimicrobial activity of the volatile constituents essential oils. Modern medical implications for this work may be related to the use of aromatic essential oils for respiratory or dermatological infections.
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... Desde la antigüedad nos hemos interesado por extraer y trasladar el sabor desde unos productos a otros. Los primeros aparatos de destilación que conocemos datan desde hace más de 5.000 años y provienen de Mesopotamia, en el actual Irak (1). También en el actual Irak se inventó la destilación del alcohol, por el químico Al-Kindi en el siglo IX (2). ...
Migración de sabores: Técnicas clásicas y modernas (Flavor migration: Classical and modern techniques)
Conference Paper
Full-text available
  • Oct 2019
Revisión de tcnicas de extracción y migración de sabor con énfasis en la infusión rápida por cavitación con óxido nitroso.
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... Frankincense essential oil was also known in Arabia where it became the most significant trade commodity creating enormous wealth for the country. It is believed that it was Arabs who discovered the process of steam distillation and passed this knowledge to Europeans (Schlosser, 2011). ...
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Steam Distillation: Principle and Applications for the Extraction of Essential Oils from Plants
Chapter
  • Aug 2023
Around 80% of the populace depends on herbal medicines to meet their well-being needs. Subsequently, therapeutic and aromatic plants are significant in light of the fact that the items obtained from plants are utilized to make herbal medicines. The essential oils are used in aromatherapy, a form of an alternative therapy for supporting well-being or health of people. The essential oils exist in the oily form and have a characteristic essence, scent, or aroma of the plant from which it is extracted and the reason the name “essential” is added before its title. The available literature shows that usage of essential oils began more than 2500 years in the Middle East countries. The conventional method of segregating unpredictable mixtures as essential oils is distillation. The boiling point of these oils is usually high, which evaporate near boiling point of water. This forms the basis of using water or steam for distillation methods and was most commonly used method for extraction of essential oils from herbal plants. During this process, the fragments of parts of plants containing volatile oil are exposed to the steam or boiling water, releasing fragrance with oils through evaporation. The volatile compounds are diffused into the vapors of water and transported to the condenser and finally collected in the receiver where they are segregated from the aqueous layer. If dry distillation is attempted, the organic components may tend to decompose. There are many additional advantages of steam distillation method, e.g., the method generates organic solvent-free products; the technology is reliable and involves inexpensive equipment. Nowadays, the advancement in distillation methods improves the yield and quality of essential oils with faster extraction kinetics at lower cost. Microwave-assisted methods and solvent-based extraction methods are also included in this chapter.
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Osmotic Membrane Distillation - A Brief Review
Article
  • Jan 2006
  • INT J FOOD ENG
In recent years, osmotic membrane distillation is gaining importance as an attractive/complementary athermal membrane process. Osmotic membrane distillation is having potential to concentrate the biomolecules/liquids to a very high level under mild operating condition, without product damage. Further, this process can be employed as a pre-concentration step to reduce water load significantly on subsequent processing steps. The present review exclusively deals with process features, theoretical aspects involving water transport mechanism, influence of various process conditions on transmembrane flux along with recent application of osmotic membrane distillation process. Also, suggestions for future work and possible process integration of osmotic membrane distillation with other processes are also discussed.
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Membrane Distillation and Related Operations—A Review
Article
  • Jan 2005
Membrane contactors represent an emerging technology in which the membrane is used as a tool for inter phase mass transfer operations: the membrane does not act as a selective barrier, but the separation is based on the phase equilibrium. In principle, all traditional stripping, scrubbing, absorption, evaporation, distillation, crystallization, emulsification, liquid‐liquid extraction, and mass transfer catalysis processes can be carried out according to this configuration. This review, specifically addressed to membrane distillation (MD), osmotic distillation (OD), and membrane crystallization (MCr), illustrates the fundamental concepts related to heat and mass transport phenomena through microporous membranes, appropriate membrane properties, and module design criteria. The most significant applications of these novel membrane operations, concerning pure/fresh water production, wastewater treatment, concentration of agro food solutions, and concentration/crystallization of organic and biological solutions, are also presented and discussed.
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Permeability, permeance and selectivity: A preferred way of reporting pervaporation performance data
Article
  • Feb 2010
  • J MEMBRANE SCI
A majority of the papers on pervaporation published in the Journal of Membrane Science (JMS) report results as raw data; that is, as fluxes (Ji) and separation factors (βij). These values are not only a function of the intrinsic properties of the membranes used, but also depend on the operating conditions of the experiments (feed concentration, permeate pressure, feed temperature): change the operating conditions and all the numbers change. This makes comparison of pervaporation data sets obtained under different operating conditions difficult. Furthermore, these values can lead to confusion in understanding the real trend of membrane intrinsic properties as operating conditions change. In this paper, the benefits of reporting the results in a normalized form, that is, as permeabilities (Pi), permeances (Pi/ℓ) and selectivities (αij) are described. Data from our laboratory and from two recent papers are used to illustrate these benefits.
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Influence of Ionic Liquids on the Phase Behavior of Aqueous Azeotropic Systems
Article
  • Jun 2004
The use of ionic liquids (ILs) in chemistry and electrochemistry has been studied for some decades. Only recently, researchers have focused on the suitability of ILs as selective solvents in the field of separation technology. ILs represent suitable entrainers and extraction solvents for the separation of azeotropic mixtures by means of extractive distillation and solvent extraction. In this work, ternary vapor−liquid and liquid−liquid equilibria of the azeotropic mixtures ethanol + water and THF + water containing different kinds of commercially available ILs are presented. The four ionic liquids used are derived from butyl-methylimidazolium tetrafluoroborate [BMIM]+ [BF4]- by systematic variation of the cation or the anion. The influence of the IL structure on the relative volatility of the low boiling component in extractive distillation and on the selectivity in solvent extraction processes is discussed in this work.
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Low-Energy Distillation-Membrane Separation Process
Article
  • Mar 2010
A low-energy separation process combining distillation and membrane vapor permeation is introduced as an alternative to conventional distillation. The process can be applied to any liquid mixture for which appropriate selective membranes are available. However, in this paper, the discussion is limited to water/organic solvent mixtures using membranes that preferentially permeate water. Such membranes are available. The process is illustrated with two mixtures: ethanol (light component)/water (heavy component) and acetic acid (heavy component)/water (light component) mixtures. In both cases, the combination process reduces the energy consumption of the separation to half that of simple distillation.
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Experimental validation of hybrid distillation‐vapor permeation process for energy efficient ethanol–water separation
Article
BACKGROUND: The energy demand of distillation-based systems for ethanol recovery and dehydration can be significant, particularly for dilute solutions. An alternative separation process integrating vapor stripping with a vapor compression step and a vapor permeation membrane separation step, termed membrane assisted vapor stripping (MAVS), has been proposed. The hydrophilic membrane separates the ethanol–water vapor into water-rich permeate and ethanol-enriched retentate vapor streams from which latent and sensible heat can be recovered. The objective of this work was to demonstrate experimentally the performance of a MAVS system and to compare the observed performance with chemical process simulation results using a 5 wt% ethanol aqueous feed stream as the benchmark. RESULTS: Performance of the steam stripping column alone was consistent with chemical process simulations of a stripping tower with six stages of vapor liquid equilibria (VLE). The overhead vapor from the stripper contained about 40 wt% ethanol and required 6.0 MJ of fuel-equivalent energy per kg of ethanol recovered in the concentrate. Introduction of the vapor compressor and membrane separation unit and recovery of heat from both membrane permeate and retentate streams resulted in a retentate ethanol concentrate containing ca 80 wt% ethanol, but requiring only 2.2 MJ fuel kg−1 ethanol, significantly less than steam stripping alone. CONCLUSION: Performance of the experimental unit with a 5 wt% ethanol feed liquid corroborated chemical process simulation predictions for the energy requirement of the MAVS system, demonstrating a 63% reduction in the fuel-equivalent energy requirement for MAVS compared with conventional steam stripping or distillation. Published 2009 by John Wiley & Sons, Ltd.
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Membrane-assisted vapor stripping: Energy efficient hybrid distillation - Vapor permeation process for alcohol - Water separation
Article
BACKGROUND: Energy efficient alternatives to distillation for alcohol recovery from dilute solution are needed to improve biofuel sustainability. A process integrating steam stripping with a vapor compression step and a vapor permeation membrane separation step is proposed. The objective of this work is to estimate the energy and process costs required to make a fuel grade ethanol (0.5 wt% water) from 1 and 5 wt% ethanol aqueous streams using the proposed process. RESULTS: Using process simulation and spreadsheeting software, the proposed membrane-assisted vapor stripping process was estimated to require as little as 8.9 MJ of fuel-equivalent energy per kg of fuel grade ethanol recovered from a 1 wt% ethanol feed stream, 2.5 MJ kg−1 for a 5 wt% ethanol solution. This represents an energy saving of at least 43% relative to standard distillation producing azeotropic ethanol (6 wt% water). Process costs were also found to be lower than for distillation at the 3.0 × 106 kg-ethanol year−1 scale modeled. CONCLUSION: In this hybrid system, the stripping column provides high ethanol recoveries and low effluent concentrations while the vapor compression-membrane component enables the efficient recovery of latent and sensible heat from both the retentate and permeate streams from the membrane system. Published in 2008 by John Wiley & Sons, Ltd.
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Performance improvement of PVDF hollow fiber-based membrane distillation process
Article
  • Mar 2011
  • J MEMBRANE SCI
The performance of membrane distillation depends on both membrane and module characteristics. This paper describes strategies to improve the performance of hollow fiber membrane modules used in direct contact membrane distillation (DCMD).Three different types of hydrophobic polyvinylidene fluoride (PVDF) hollow fiber membrane (unmodified, plasma modified and chemically modified) were used in this study of direct contact membrane distillation (DCMD). Compared to the unmodified PVDF hollow fiber membrane, both modified membranes showed greater hydrophobicity and mechanical strength, smaller maximum pore sizes and narrower pore size distributions, leading to more sustainable fluxes and higher water quality (distillate conductiviy < 1 μs cm−1) over a one month test using synthetic seawater (3.5 wt% sodium chloride solutions). Comparing the plasma and chemical modification the latter has marginally better performance and provides potentially more homogeneous modification.MD modules based on shell and tube configuration were tested to identify the effects of shell and lumen side flow rates, fiber length and packing density. The MD flux increased to an asymptotic value when shell-side Ref was larger than 2500, while the permeate/lumen side reached an asymptotic value at much lower Rep (>300). By comparing the performance of small and larger modules, it was found that it is important to utilize a higher shell-side Re in the operation to maintain a better mixing near the membrane surface in a larger module. Single fiber tests in combination with heat transfer analysis, verified that a critical fiber length existed that is the required length to assure sufficient driving force along the fiber to maintain adequate MD performance. In addition, for multi-fiber modules the overall MD coefficient decreased with increasing packing density, possibly due to flow maldistribution. This study shows that more hydrophobic membranes with a small maximum pore size and higher liquid entry pressure are attainable and favorable for MD applications. In order to enhance MD performance various factors need to be considered to optimize fluid dynamics and module configurations, such as fiber length, packing density and the effect of module diameter and flow rates.Research highlights▶ Both plasma and chemically modified PVDF membranes showed improved properties. ▶ These modified PVDF membranes performed more stably in MD process. ▶ A critical fiber length existed to assure adequate MD performance. ▶ Higher shell-side Re is preferred to improve mixing condition in larger MD modules. ▶ The overall MD coefficient decreased with increasing packing density.
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