Chapter 1

History of Distillation

Norbert Kockmann     Laboratory of Equipment Design, Department of Biochemical and Chemical Engineering, TU Dortmund University, Dortmund, Germany

Abstract

Distillation is one of the oldest and most commonly used separation and purification methods (besides crystallization) and probably one of the most thoroughly investigated and understood. This chapter traces its historical development from the first applications more than 5000 years ago in Mesopotamia to the medieval period, the nineteenth-century industrial developments, and contemporary applications. In view of the multitude of information on distillation in the literature, the emphasis here is on the major applications and equipment leading to the current mature technology. Processes and materials together with scientific knowledge are mirrored in the development of distillation. Current developments encompass deeper knowledge of heat and mass transfer as well as the integration of various process functions.

Keywords

Alcohol distillation; Coal tar refining; Cryogenic air separation; Innovation; Innovation cycle; Integrated process steps; Mass production; Petroleum distillation; Process intensification; Structured packing; Tray development

Chapter Outline

1.1 Introduction?1

1.2 From neolithic times to alexandria (3500 BC–AD 700)?2

1.3 The alembic, the arabs, and albertus magnus (AD 700–1450)?6

1.4 Printed books and the rise of science (1450–1650)?8

1.5 From laboratory to industry (1650–1800)?14

1.6 Scientific impact and industrialization (1800–1900)?17

1.7 Engineering science (1900–1950)?22

1.8 Improvements and integration (1950–1990)?30

1.9 What will be the next innovation cycle (1990–2020 and beyond)??34

1.10 Summary?36

References?37

1.1. Introduction

The history of technical developments must also include social, cultural, and political perspectives. To reconstruct history from the current point of view means that we have to rely on arguable data and information. Findings on which we want to build a certain argumentation need an imaginative interpretation. The result is often not a factual, engineering-like argument presented with precision and reliability. Distillation is a well-defined separation unit consisting of the partial evaporation of a liquid mixture and successive condensation, with a composition that differs from that of evaporation. The word distillation derives from the Latin verb destillare, meaning to drop down or to trickle down. Distillation had a broader meaning in ancient and medieval times because nearly all purification and separation operations were subsumed under the term distillation, such as filtration, crystallization, extraction, sublimation, or mechanical pressing of oil. This becomes evident because in earlier times there was no clear understanding of heat or the consistency of materials. Here, no further treatment will be presented on the history of alchemy, since chemistry and alchemy were not fully distinguishable until the modern age. The equipment used for distillation flourished in Alexandria during the Roman Empire, and the apparatus did not change much until the sixteenth century. With the increased knowledge made possible by the invention of printing and with the larger demand for distilled products such as concentrated alcoholic or mineral acids, various stills thrived and were placed partly into industrial production. French scientists, English industrialists, and German craftsmen brought the equipment to the lab and fostered its industrial application. The modern era with its development of high-tech information has made possible a much wider picture and large-scale global development. Wherever possible, we rely on the primary literature. To get a wider picture, however, it is also necessary to consult the secondary literature. Robert Forbes (1943) [1] gives an extensive illustration of the history of the art of distillation until 1840 and the death of Cellier-Blumenthal, one of the most gifted designers of distillation columns. Ludwig Deibele [2] presents an intensive treatment of the development of distillation until the end of the nineteenth century, with only a short look into the twentieth century. In 1935, A.J.V. Underwood wrote a little book on the historical development of distillation plants [3]. However, developments over the last 100 years are nearly completely missing and will be described in this contribution. In earlier times, developments have been presented in journal review articles and conference contributions. Hence, we have found descriptions in encyclopedias quite helpful (Ullmann's [4]) or handbooks (Perry's [5]). The text follows the historical timeline, though not always rigidly so. Often product or equipment lines give a better understanding of innovative developments. Special emphasis is placed on the innovation process and its main drivers and motivations. Two hundred years ago, Jean-Baptiste Cellier-Blumenthal invented the first continuously working distillation column in France and patented it in 1813. With this hallmark of distillation, we will celebrate this new chapter in the historical development of distillation.

1.2. From neolithic times to alexandria (3500 BC–AD 700)

The first civilizations started in Mesopotamia, Egypt, Syria, and China and spread from there. We cannot directly conclude from ancient texts what the ancient civilizations knew about the processing of foods or pharmaceutical products such as ointments, balsam, tinctures, or creams. Often priests and temple servants used distillation devices and kept their recipes secret. Hermann Schelenz [6] maintained that distillation was invented by the Persians, who used this process to produce rose water, rose oil, and other perfumes. He further stated that distillation was derived from dry distillation of wood for turpentine and wood tar. Together with Edmund von Lippmann [7], Schelenz found that the Egyptian Ebers papyrus (1550 BC) on medical issues already described the distillation of essential oils from herbs.
FIGURE 1.1 Extraction pot with evaporating liquid, condensing vapor, and extraction material in the chamfer of the pot [8]. The lid is sealed against the pot to avoid vapor and condensate losses. Around 3500 BC the Sumerians were the first to apply evaporation and condensation of a liquid to refine a substance for extracting essential oils from herbs [8]; see Figure 1.1. Many of the pots and stills shown on the right side of the figure were found in excavations undertaken 250 km north of Baghdad in Iraq [9]. The liquid in the still evaporates by gentle heating from below and condenses at the colder cap. Droplets run down to be collected in the ring, where organic material such as leaves and herbs are extracted by the liquid. The typical dimensions of the earthenware pot are approximately 50 cm in diameter and 25–50 cm in height [9]. From fermented substances, alcohol may also rise and condense to help extract the ingredients, which were often essential oils or fragrances. This distillation under reflux and extraction is still employed today with the lab apparatus called the Soxhlet extractor. Forbes discusses the early appearance of distillation. Because of his narrow definition of distillation, he concludes that the Alexandrian chemists were the first to develop and apply distillation to refine essential oils, rose water, wood turpentine, and other substances. Asphalt was found naturally and distilled to more viscous tar for ship- or house-building. Hence, both light and heavier fractions were the first products of ancient distillation processes. Chinese distillation activities from ancient times have also been reported [10]. Early types of pots similar to those seen in Figure 1.1 were also found in China around 2000 BC. Kettles were found dating from 1000 BC, which indicate distillation operations. Joseph Needham [10] illustrates the development of the distillation apparatus in a genealogical tree (see Figure 1.2). The first primitive stills were earthenware pots heated from below with a lid (1), through which the vapor could condense. Further developments led to the device shown in Figure 1.1 with the internal collection of the lighter fraction (Figure 1.2a,b). Besides distillation, these rims could also serve as water sealants for anaerobic fermentation of foodstuffs, such as cabbage to produce sauerkraut. Two mayor drawbacks of the early stills can be observed with this design: The condensate is collected in the warm part of the still and the internal volume is limited, which may lead to unwanted reflux of the condensate back to the still. This is now the view of the modern engineer, who has a trained view of technical drawbacks. We should not forget the limits of knowledge at that time and must not judge based on our current views. It was quite difficult to remove the entire product from the gutter. An outlet tube was added (2b) to increase the capacity and performance, probably during the Hellenic era. Similar devices have been found in excavations of medieval apothecaries in...