How Artisan Distillation Works

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How Artisan Distillation Works

• Kris Arvid Berglund
• University Distinguished Professor
• of Forestry and Chemical Engineering
• Michigan State University
• East Lansing, MI 48824 USA
• and
• Professor of Biochemical
• Chemical Process Engineering
• Luleå University of Technology
• SE-971 87 Luleå SWEDEN

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MSU/ LTU ARTISAN DISTILLING PROGRAM

• Established to promote the establishment and
  expansion of artisan distillers
• Activities include education, service, and
  research
• Designed as a dedicated program for distilled
  spirits

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FACILITIES

• Michigan Brewing Company-houses program,
  alternating premises license
• A150l Christian Carl still equipped with a three
  tray side column and a packed column is for high
  rectification work. (120l to be added at LTU)
• A 450l Christian Carl still for stripping and
  botanicals
• An 800l, 38-tray Christian Carl still (on line in
  March 2009)
• A 10l Christian Carl still for experimental work
• Comprehensive analytical instrumentation GC,
  HPLC, Anton Paar DMA 5000 densitometer

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EDUCATIONAL ACTIVITIES

• Workshops- two day
• MSU, Webberville, MI
• WSU, Mt. Vernon, WA
• Cornell University, Geneva, NY
• Coursework at MSU, CHE 491
• Book entitled, Artisan Distilling on CD-ROM,
  internet download (free) at www.artisandistilling.
  org

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RESEARCH ACTVITIES

• Develop quality indicators- congener monitoring
  and control
• Control of regulated compounds
• Yeast screening for congeners
• Activated carbon finishing

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Some definitions

• The agency that licenses at the Federal level is
  Alcohol and Tobacco Tax and Trade Bureau, the
  Department of Treasury (TTB), not the Bureau of
  Alcohol, Tobacco and Firearms, the Department of
  Homeland Security (BATF).
• All spirits are defined in the Code of Federal
  Regulations-27 CFR Part 5.21
• Make sure anything you wish to make is defined!

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Recognized classes of spirits

• Class 1 neutral spirits or alcohol.
• Class 2 whisky.
• Class 3 gin.
• Class 4 brandy.
• Class 5 blended applejack.
• Class 6 rum.
• Class 7 tequila.
• Class 8 cordials and liqueurs.
• Class 9 flavored brandy, flavored gin, flavored
  rum, flavored vodka, and flavored whisky.
• Class 10 imitations.
• Class 11 geographical designations.
• Class 12 products without geographical
  designations but distinctive of a particular
  place.

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DISTILLATION- MOTIVATION

• Concentrate aromas, flavors, and alcohol
• Several operational parameters possible
• Remove the negative compounds

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DISTILLATION

• A process involving an equilibrium between two
  phases - liquid and vapor.
• For a pure compound, a sharp boiling point
  usually exists.
• For a mixture, however, a phase equilibrium
  exists over a range of temperatures.

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UNIQUE VLE OF ETHANOL-WATER SOLUTIONS

• For ideal mixtures, the mvc is always at a higher
  concentration in the vapor phase than the lvc
• The boiling point of the mixture should be a
  continuously increasing value as the
  concentration of the lvc is increased
• This is not the case for ethanol-water
• The boiling point has a minimum value for a
  mixture
• This is called a minimum boiling azeotrope

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vapor
DEW CURVE
mixture
BUBBLE CURVE
liquid
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AZEOTROPE
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INCREASING TEMP.
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COMPARISONOF UNITS- MOLE, WEIGHT, AND VOLUME
FRACTIONS
VOLUME
MOLE
WEIGHT
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TYPES OF DISTILLATION

• Simple batch- no rectification
• Alambic- some rectification
• Column- active rectification

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BATCH DISTILLATION

• Use cuts
• Heads- remove acetaldehyde, methanol
• Hearts- product rich in aromas and flavors
• Tails- fusel oils, dilute

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RECTIFICATION- EQUILIBRIUM CONTACT

• Rectification is the result of equilibrium
  contact between two phases
• The liquid and vapor leaving the contact are in
  equilibrium
• Rectification, also called enrichment, results in
  a higher concentration than would occur in a
  single equilibrium contact

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SIMPLE BATCH (RAYLEIGH) DISTILLATION
                                                  
                                                  
                                                  
                                      
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1
2
20
vapor
2
mixture
1
liquid
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DIRECT FIRED STILL (ALAMBIC)
Some vapor condenses to liquid and returns to the
pot
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Classic cognac distillation
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INDIRECT STEAM HEATING (ALAMBIC)
Some vapor condenses to liquid and returns to the
pot
Steam
Figure courtesy of Christian Carl Ing. GmbH
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INDIRECT HEATING WITH RECTIFICATION
INCREASING TEMPERATURE DOWN THE COLUMN, HIGHEST
TEMPERATURE IS IN THE POT
Figure courtesy of Christian Carl Ing. GmbH
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RECTIFICATION COLUMNS

Figure courtesy of Christian Carl Ing. GmbH
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SIEVE TRAY
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BUBBLE CAP TRAY
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BATCH COLUMN STILL
Partial condensor
D, xD
L
Reflux ratio
Boiler
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The number of trays needed for a specific
separation is determined by stepping off..
5
4
3
2
1
xDIST
XFEED
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vapor
mixture
1
2
3
4
5
liquid
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If the reflux ratio is constant, the product
concentration will decrease during the batch
3
3
2
2
1
1
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Since the concentration in the pot decrease
during a bath, in order to keep the product
concentration high, the reflux must be increased
3
3
2
2
1
1
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REFLUX IS INCREASED BY INCREASING COOLING WATER
FLOWRATE TO PARTIAL CONDENSER
T
TEMPERATURE SENSOR
WATER TO CONDENSER
Figure courtesy of Christian Carl Ing. GmbH
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FLAVOR COMPOUNDS (CONGENERS) IN DISTILLED SPIRITS
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TYPICAL COMPOUNDS BY GC
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TYPICAL GC RESULTS
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ETHANOL RESULTS FROM PLUM DISTILLATION
HEADS
HEARTS
TAILS
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CONGENER CONCENTRATIONS IN PLUM DISTILLATES
HEADS
HEARTS
TAILS
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CONTACT

• Prof. Kris Arvid Berglund
• Email berglund_at_msu.edu
• Email kris.berglund_at_ltu.se
• www.artisandistilling.org

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ACKNOWLEDGEMENTS

• Christian Carl Ing. GmbH
• Project GREEEN, State of Michigan
• Michigan State University
• Luleå University of Technology