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Manual Módulo Gunt CE640e - V0.4

The document is an instruction manual for a biotechnical ethanol production unit. It describes the various components of the unit, including a cooking tank for liquification and saccharification, a fermentation tank, and a distillation unit. It provides details on their functions and operating principles. The manual also covers safety considerations, the theoretical background of ethanol production processes, guidance on running experiments, and software for data acquisition.

Uploaded by

Mariana Soto
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
506 views

Manual Módulo Gunt CE640e - V0.4

The document is an instruction manual for a biotechnical ethanol production unit. It describes the various components of the unit, including a cooking tank for liquification and saccharification, a fermentation tank, and a distillation unit. It provides details on their functions and operating principles. The manual also covers safety considerations, the theoretical background of ethanol production processes, guidance on running experiments, and software for data acquisition.

Uploaded by

Mariana Soto
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 78

Instruction Manual

CE 640 Biotechnical Production


of Ethanol
CAD_9
05/2013

CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Instruction Manual

Please read and follow the safety regulations before the first installation!

Publication-no.: 918.000 00 D 640 03 (A) CAD_9

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

Table of Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

2 Unit description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2.1 General view . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3


2.2 Process schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.3 Cooking tank for liquification / saccharification . . . . . . . . . . . . . . . . . 6
2.4 Fermentation tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.5 Distillation unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.6 Control cabinet and control technology . . . . . . . . . . . . . . . . . . . . . . 15
2.7 PLC controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.8 Compressed air diaphragm pump (P2 & P3). . . . . . . . . . . . . . . . . . 23
2.9 Diaphragm metering pumps (P1 & P4) with
acid supply container (B3) and caustic supply container (B6) . . . . 24
2.10 Installation and commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.11 Cleaning the tanks and supply lines with steam . . . . . . . . . . . . . . . 26
2.12 Maintenance / care . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
2.13 Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

3 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

3.1 Intended Use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29


3.2 Structure of the Safety Instructions . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.3 Health hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
3.4 Hazards for unit and function. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

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4 Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

4.1 Basics of alcohol creation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37


4.2 Crushing the raw materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
4.3 Liquification / saccharification of the raw materials . . . . . . . . . . . . . 38
4.4 Fermenting the mash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
4.5 Distillation of the mash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

4.5.1 Basics of distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42


4.5.2 Construction of a distillation . . . . . . . . . . . . . . . . . . . . . . . . 45

5 Notes on running experiments . . . . . . . . . . . . . . . . . . . . . . . . 47

5.1 Diagram of creating alcohol. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47


5.2 Liquification and Saccharification . . . . . . . . . . . . . . . . . . . . . . . . . . 49
5.3 Fermentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
5.4 Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

6 Data acquisition software . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

6.1 Software installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59


6.1.1 System requirements:. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.1.2 Installation of software . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.2 Software operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.2.1 Menu point: Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
6.2.2 Menu point: File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.2.3 Menu point: View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.2.4 Menu point: Language . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64

7 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

7.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65


7.2 Process schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
7.3 Items supplied . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
7.4 Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

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1 Introduction

Alcohol is an important base material for the chem-


ical industry. It is mainly obtained from food-stuffs
containing starch such as e.g. potatoes or cereal
products.
The experimental stand CE 640 Biotechnical
Production of Ethanol makes it possible to trace
and research the process of industrial alcohol pro-
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

duction from the liquification and saccharification


of the original materials to the conversion from
sugar into alcohol on to the distillation of the alco-
hol.
The experimental stand uses two stainless steel
agitation vats for this. One is a cooking tank tem-
pered with steam and cold water and one is a fer-
mentation tank tempered with cold and hot water.
Distilling the alcohol is done with a completely inte-
grated distillation system.
Material transport through the system is done by
compressed air-driven conveyor pumps.
For optimal operating conditions, the cooking tank
and the fermentation tank have temperature con-
trols and rpm-regulated stirrers.
Control and monitoring on the system is done
on-site by an integrated PLC. Recording the mea-
surement data and monitoring can also be supple-
mented with a connected PC.
The experimental stand is used only for training
students in the process-, bio- and food-stuffs tech-
nology and is not intended for industrial purposes.

1 Introduction 1
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

Learning Objectives / Experiments


– Familiarization with the necessary individual
steps and system components for pro-
duction of ethanol:
• gelatinisation by steam injection
• liquefaction by use of alpha-amylase
• saccharification by use of gluco-
amylase
• fermentation: conversion of sugar into
ethanol by yeast cultures under an-
aerobic conditions
• distillation: separation of ethanol from
the mash

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2 Unit description

2.1 General view

1 2 3 4 5

15
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14

13
11
12

10 8 9 8 7 6

Fig. 2.1 General view

1 Steam pressure regulator valve (V1) 9 Mash pump (P3)


2 Cooking tank for liquification/ saccharification (B1) 10 Cold water control-valve (V2)
3 Fermentation tank (B2) 11 Flow meter (F1)
4 Distillation unit (D1) 12 Mash pump (P2)
5 Control cabinet 13 Steam shut-off valve (V23)
6 Ethyl alcohol container (B4) 14 Pressure regulator for cold water
7 Mash container (B5) control valve

8 Diaphragm metering pumps (P1 & P4) 15 Pressure regulator for steam-pressure
control valve

2 Unit description 3
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


2.2 Process schematic

Compressed Air

Warm Water
Steam
Water

Water

Water

Fig. 2.2 Process schematic CE 640

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

Individual components Measuring points


B1 Cooking tank (tank 1) V3 - V7 Solenoid valves
B2 Fermentation tank (tank 2) V8- V27 Ball valves, hand actuated
B3 Acid solution container V26 Steam pressure safety valve
B4 Ethyl alcohol container V28-V32 Ball valves, hand actuated
B5 Mash container T1 Mash temperature B1
B6 Caustic tank T2 Mash temperature B2
D1 Distillation unit T3 Cooling water drain temperature B2
P1 Diaphragm metering pump T4 Distillation unit water bath temperature
P2 Compressed air feed pump B1 - B2 T5 Mash temperature in distillation bubble
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

P3 Compressed air feed pump B2 - D1 T6 Gas temperature after bubble cap 1


P4 Diaphragm metering pump (caustic) T7 Gas temperature after bubble cap 2
R1 Stirrer geared motor B1 T8 Gas temperature after bubble cap 3
R2 Stirrer geared motor B2 T9 Gas temperature after dephlegmator
R3 Stirrer geared motor D1 Q1 pH value B1
H1 Water bath heater F1 Water flow to B1
V1 Steam control valve PI1 Steam pressure indication
V2 Cooling water control valve

The process diagram shows all components and


measuring points on the CE 640 as well as all
required pipe connections and supply lines. There
are several ball valves to be opened or closed for
the individual operating states.
More detailed information on setting the individual
ball valves during the individual operating states
can be found in chapter 5 of these instruction.

2 Unit description 5
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


2.3 Cooking tank for liquification / saccharification

Fig. 2.3 Mash tank

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

2
7 8 9
4
10
1 6
3
11
12
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

13
17

18

14 15 16 19
Fig. 2.4 Cooker tank / Mash tank

1 Shaft coupling 11 Supports


2 Geared motor 12 Water supply connection
3 Acid supply 13 Sealing plug
4 Cover flap 14 Drain valve
5 Overflow connection 15 Temperature sensor
6 Cover latch 16 Connection to feed-pump
7 Hand-hold for cover 17 Cooling water drain
8 Hinged cover 18 Cooling water feed
9 Inspection glass 19 Steam feed connection
10 pH measuring probe

2 Unit description 7
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

The mash or cooking tank is used for liquefying


and saccharifying the initial materials. This pro-
cess is known as mashing. The container uses an
stirrer for this, consisting of a geared motor and a
pitched blade stirrer on the shaft.
Heating the original materials is done with a direct
hot steam line into the cooking tank through a jet.
This enables an increase in liquid by around 15%.
To prevent the mash from running back into the
steam feed line, it is built into a non-return valve.
This valve can be removed from the interior of the
container with the jet as a complete unit.
The container is equipped with a double-jacket,
through which water can be pumped for cooling
the mash if required. Temperature monitoring is
done by a temperature sensor built into its floor.
The tank also has a pH value measuring probe for
regulating the pH value.
For the required lowering of the pH value during
the process, the tank has an acid inlet with a dia-
phragm metering pump. For the required lowering
of the pH value during the process, the tank has an
acid supply with a diaphragm metering pump.This
measuring probe is only installed when the system
is to be operated.
The cooking tank is designed as an open con-
tainer. That means that steam will escape through
the openings in the cover while cooking. To fill the
container with raw material such as grain, potatoes
or enzymes, the cover is made in two parts and
can be opened. It is secured by means of a
latch-pin.
The container, cover and all attachment parts are
made of stainless steel.

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


2.4 Fermentation tank
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Fig. 2.5 Fermentation tank

2 Unit description 9
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

3 4 9 10 11 12

5
2

6
1

7
17
16 8

19

13 14 15 18 19

Fig. 2.6 Fermentation tank (Tank 2)

1 Sealing plug 10 Fill opening


2 Clean-out opening 11 Supports
3 Coupling 12 Cooling water outlet
4 Geared motor 13 Cooling water control valve
5 Cover 14 Drain valve
6 Mash feed 15 Connection to feed-pump
7 Temperature sensor for mash 16 Temperature sensor for cooling water drain
8 Inspection glass 17 Cooling water inlet
9 Fermentation lock 18 Double jacket container
19 Shut-off valve for cooling water

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

The fermentation tank converts the sugar con-


tained in the mash into alcohol. This tank can be
sealed air tight and tempered with cold and hot wa-
ter using a water jacket. The cold or hot hot water
flows through a double jacket on the outside of the
tank. The fermentation tank is equipped with an
stirrer for optimal mash mixing. It consists of a
speed regulated geared motor and an stirrer with
two pitched blade stirrers. The temperature of the
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

mash is monitored with a temperature sensor.


To regulate the temperature more efficiently, an-
other temperature sensor is located on the cooling
water drain.
The cover of the container is equipped with a
latched clean-out opening and a fill opening. The
stirrer shaft is run into the container through a fer-
mentation lock (see Fig. 2.7).
1
2 1 Geared motor
3 2 Coupling
4 3 O-ring
8 4 Divider
5 5 Stirrer shaft
9 6 Sealing liquid area
6
7 Cover
8 Sealing liquid
7
9 Spacer post for geared motor
10 O-ring
10
Fig. 2.7 Fermentation lock, cut-out view The sealing liquid (normally water) in the fermenta-
tion lock completely closes the interior of the con-
tainer off from the atmosphere. The CO2 gener-
ated in the fermentation process pearls up as gas
bubbles through the sealing liquid and escapes
into the atmosphere without the air from outside
being able to enter the container.
In order to improve monitoring, the fermentation
lock is made of transparent plastic.

2 Unit description 11
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


All other components of the fermentation tank are
made of stainless steel, as is the cooking tank.

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


2.5 Distillation unit
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Fig. 2.8 Distillation unit

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

Fig. 2.9 Distillation unit, overview

The distillation unit is a modified boiler heater with


water bath (6). It contains bubble cap (1) tray col-
umn, dephlegmator (2) and condenser (4). T1 -
T10 indicate the positions of the individual temper-
ature sensors in the system. For a detailed de-
scription of the individual components and mea-
surement connections, please read the attached
operating instructions of the manufacturer.

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


2.6 Control cabinet and control technology

2
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Fig. 2.10 Control cabinet, overview

1 pH transducer
2 PLC controller (touch-screen)
3 Schematic diagram
4 EMERGENCY STOP button
5 Master switch
6 PC connection, USB

The control cabinet contains all required control


and regulating elements of the CE 640.
Control and regulation are carried out by the PLC
controller (PLC = programmable logic controller)
built into the side of the control cabinet. The con-
troller is menu guided. All entries and control in-
structions are entered via the touch screen. The
actual control of individual components such as
regulating valves, stirrer, pumps and heating con-

2 Unit description 15
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL


trol is handled with the PLC installed in the control
cabinet.
All of the temperatures that are recorded in the ex-
perimental stand are shown on the touch screen.
The pH values and the temperature from the pH
measuring probe are shown on a separate mea-
suring device.
The entire system can be switched on or off with
the main switch.
Actuating the EMERGENCY STOP button switches
the electrical power off for the entire system.
The measurement data can be recorded and
saved through an interface on the side of the con-
trol cabinet using the respective data acquisition
software.
The measurement data can be recorded and
saved via a USB interface to the bottom right of the
side of the control cabinet using the associated
data acquisition software.

16 2 Unit description
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2.7 PLC controller

The PLC controller is started automatically when


the experimental stand is switched on and shows
the start menu (Fig. 2.11).

On the Start menu, you will find an operating hour


meter and some touch fields.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Fig. 2.11 Start menu


The sub-menus are reached by touching the indi-
vidual touch fields on the screen.

The screen offers choices between the parameter


settings for temperature control circuits in:
• Mash (Cooking) tank (tank 1) with tem-
perature- und pH-value control
• Fermentation tank (tank 2) and
• Distillation with temperature control
The parameters for the control circuit must match
the respective installation location and the respec-
tive environmental conditions. For details in this
regard, please refer to current technical literature
on control technology.

To change the user language go to sub-menu Pa-


rameter (Fig. 2.12)
From here, the display language for the PLC con-
troller can be changed.
The system time, date and the brightness of the
screen can also be set.
If an error has occurred on the PLC, a list of the er-
Fig. 2.12 Parameter
rors that have occurred will be displayed.
Return brings you back to the previous start
menu.

2 Unit description 17
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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

1 3 2 From the start menu (Fig.2.11), the “Mash tank


B1” can be touched to change to the menu respon-
sible for the cooking tank.

This menu can be used to regulate the tempera-


ture T1 and to set the pH value in the container
(Fig. 2.13). In this instance (controlled operation)
the actual value is shown (1) and the set value of
the controller is displayed (2).
4 5 The pH value in the cooking tank is regulated by
adding acid and caustic using the diaphragm me-
Fig. 2.13 Mash tank
tering pumps.
To activate these controllers, the button " Manual "
(3) is to be switched to " Auto ".

On the display(4), the control valve set value can


be read for the temperature control for T1. If the set
value of the valves should be controlled manually,
the button (3) for temperature T1 must first be set
to “Manual”. This activates field (5) and the set
value can be defined between -100 % and +100 %.
-100% = Cooling water valve fully open
+100% = Heating steam valve fully open

The button "R1" can be used to switch the stirrer on


or off.

The following is standard for switch fields


• Switch field is green : Element is switched on
• Switch field is red : Element is switched off

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

7 8 9
On button (7), the rpm of the stirrer can be set. The
rpm/speed can also be changed with the stirrer
running.
Using the buttons "V6 ", (8) und (9) , tank 1 can be
fed a defined volume of fresh water. Button (8) is
used for defining the volume in this case. Button
"V6 " is used for activating a solenoid valve, which
opens the fresh water supply. A flow meter is used
to determine the quantity of water flowing and this
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

is displayed with display (9). After achieving the


present volume, the solenoid valve closes auto-
Fig. 2.15 Mash tank matically.
Button "Pump P2 " is used for actuating a com-
pressed air-driven diaphragm pump, which feeds
the container contents from tank 1 to tank 2.
“Return ” brings you back to the previous menu.
The "Next " button (Fig.2.15) can be used for set-
ting the control parameters Kp, Tn and Tv for the
heating steam and cooling water control valve.
The button " Graph " can be used to show the
progress of the temperature and the pH value over
time.
The control valves for the temperature control of
tank 1 is a consistent pneumatic control valve,
which is regulated with an analogue signal.

Fig. 2.14 Mash tank parameter

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

The control menu of tank 2 is constructed the


same as the one for tank 1 (Fig. 2.13).
The difference is that tank 2 only has a tempera-
ture control for cooling.

The stirrer can be run either in temporal intervals or


continuously.
Following settings are possible:
Fig. 2.16 Fermentation
– stirrer speed in rpm
– on-time in min
– off-time in min

With Buttons "Pump P2 " and "Pump P2 " both of


the compressed air-driven diaphragm pumps are
operated.
• Pump 2 feeds the container content from
Fig. 2.18 Fermentation tank 1 to tank 2.
• Pump 3 feeds the container content from
tank 2 into the distillation unit.

The settings for control parameters Kp, Tn and Tv


for tank 2 is made the same as for tank 1
(Fig.2.14).

Tank 2 has a solenoid valve as actuator. There-


fore, a minimum switch-on duration can be set for
the solenoid valve in the menu with parameter
“minimum on period”. The precision of the
Fig. 2.17 Fermentation parameter
controller can be set with the “period” parameter.
The greater the value of “period” in relation to
“minimum on period”, the more precise the
controller can work.
The actuator solenoid valve is activated by binary
switching signals.

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

“Return” brings you back to the previous menu.

In the menu for distillation, the temperature T9 is


regulated as a command variable for the distillation
(Fig. 2.21). The function of the individual buttons
and displays are the same as for tanks 1 and 2.
An stirrer in the distillation bubble can be operated
from this page of the menu. The rpm of this stirrer
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

is not variable.

Fig. 2.21 Distillation


Pump 3 can be operated from here to fill the distil-
lation bubble with the container content of tank 2.
On a diagram with the positions of the various sen-
sors all measured temperatures of the distillation
unit are shown.

“Return” brings you back to the previous menu.


Fig. 2.20 Distillation, over temperature
The settings for control parameters Kp, Tn and Tv
for distillation are made the same as for tank 1
(Fig.2.14).
The distillation has a heater as an actuator. There-
fore, a minimum switch-on duration can be set for
the heater in the menu with parameter “minimum
on period”. The precision of the controller can be
set with the “period” parameter. The greater the
Fig. 2.19 Distillation Parameter
value of “period” in relation to “minimum on pe-
riod”, the more precise the controller can work.
The actuator heater is activated by binary switch-
ing signals.
The parameter “deviation for change over”
describes the relationship between command
variable control and disturbance variable control.
Normally this parameter is set to “0”
“Return” brings you back to the previous menu.

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CE 640 BIOTECHNICAL PRODUCTION OF ETHANOL

From the start menu (Fig. 2.11), the “Measure-


ment” button can be actuated to bring up an over-
view of all measurement data from the entire unit.

Fig. 2.23 Measurement

An numerical input field (Fig. 2.23) appears for


entering command variables or for changing
parameters or speeds (rpm).
Numbers are entered here without any delimiters
or separating characters of any kind and must be
confirmed with RET.
Example:

Fig. 2.22 Example for numerical input


To enter a temperature of 40.5°C, the numbers
405 must be entered and then the entry must be
confirmed with RET. The separation character is
inserted automatically and the value is accepted
as a new command variable.

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2.8 Compressed air diaphragm pump (P2 & P3)

To feed the container content from the cooking


tank (B1) into the fermentation tank (B2) and then
on to the distillation unit (D1), the CE 640 system is
equipped with two compressed air operated -
double diaphragm pumps. These pumps require a
compressed air supply to function. The maximum
air-pressure is set on a pressure regulator (1) on
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

the respective pump. The supply volume of the


pump is set with a control valve (2). Air lines can be
1 2 3 removed from the threaded connections (3).
The compressed air diaphragm pumps are
Fig. 2.24 Compressed air diaphragm designed for transferring liquids up to a viscosity of
pump P2 10,000 mPas. Solid material particles having a
diameter of up to <4 mm can be transferred in the
liquid with the pumps.
NOTICE! With solid particles having a diameter
greater than 4 mm, irreversible damage can occur
to the pump.

Fig. 2.25 The two metering pumps are


in the foreground and the
compressed air diaphragm
pump is in the centre in the

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2.9 Diaphragm metering pumps (P1 & P4) with acid supply container (B3)
and caustic supply container (B6)

The mash must be acidified to optimise the


saccharification process. Acid is added using the
diaphragm metering pump (P1), while caustic is
added using the diaphragm metering pump (P2).
Both pumps (Fig. 2.26 & Fig. 2.27) are operated
using the PLC controller. The acid solution from
the supply container (B3) and the caustic solution
from the supply container (B6) are conveyed into
the cooking tank through a hose connection.
The feed quantity can be set on the front of the
pump:
Fig. 2.26 Diaphragm metering pump (P1)
– Adjusting the pump stroke and
– Adjusting the stroke frequency
• The pump stroke is set with a rotary knob be-
tween 0 and 100%
• The stroke frequency is set with the small ro-
tary knob between 0 and 100%.
The pump cannot be started by hand (manually),
only by an external signal from the PLC.
Diaphragm metering pump

Fig. 2.27 Diaphragm metering pump (P4)

Fig. 2.28 Tank (B3 & B6)

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2.10 Installation and commissioning

The installation and commissioning of the device


demands a few prerequisites from the installation
location and the supply equipment:

– Setting up the test stand. The front and the


left and right hand sides of the test stand
must be readily accessible. The room in
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

which the test stand is set up must be ade-


quately ventilated.
– Connect the water supply to (4) cold water
and (5) hot water (Fig. 2.29)
1 2 3 4 5 6
– Attach drain lines to (1).

Fig. 2.29 Supply connections


– Attach steam supply to (2), technical special-
ist only.
– Attach steam pressure-relief line to (3), tech-
nical specialist only. The steam pressure-re-
lief line must end in a secure space or in the
open, outside.
– Connect the compressed air supply for the
system (6) (connection in the bottom right of
the left side).
– Attach the power supply (ensure that the cor-
rect voltage supply is used!).
– Check the fuse in the control cabinet before
switching the unit on.
– Screw the pH measuring probe into tank 1
1 3 2 4 5 6 and make electrical connections.
– Switch on the unit at the master switch.
Fig. 2.30 Supply connections

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2.11 Cleaning the tanks and supply lines with steam

In order to allow the tanks and pipes that come into


contact with the product to be cleaned with steam
before shutting down, additional steam lines and
valves (V28, V25, V32 and V31) have been in-
stalled.

Cooking tank (B1)


The cooking tank can be cleaned with steam using
the valves (V23 and V1). Close the lid first and pro-
tect the pump (P2) from the steam by closing the
valve (V22).

Fermentation tank(B2)
The pipes between the cooking tank and the fer-
mentation tank can be cleaned with steam using
the valves (V28, V25 and V15). Once again, the
pump (P3) must be protected from the steam by
closing the valve (V21).
NOTICE!
The fermentation lock is made of plastic. Before
steam is fed into the fermentation tank, the fer-
mentation lock must be filled with water. The
steam must be metered in such a way as to ensure
that the fermentation lock is not damaged.

Distillation unit(D1)
The pipes between the fermentation tank and the
distillation unit can be cleaned with steam using
the valves (V28, V31, V32, V16 and V17).

NOTICE!
Cleaning with steam is not a replacement for
cleaning by flushing the system with water.

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2.12 Maintenance / care

Maintenance and care for the unit is required to


guarantee functionality and safety of the device.
After every completed segment of an experiment,
the parts used must be cleaned and rinsed thor-
oughly. This also applies for the tubes, hoses and
pumps, since otherwise encrustation or sedimen-
tation can occur in the components and tubing.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

This can disrupt the functionality of the system and


subsequent experiments.

NOTICE! The pH measuring probe is a sensitive


measuring instrument.
After the mash has undergone the saccharification
process, the sensor must be removed and cleaned
with water. The tip of the sensor must then be
packaged in the respective protective jacket and
the jacket must be filled with a buffer solution. The
sensor is never to be left dry for any length of time
(max. 2 h)!
The sensor can be damaged if stored in dry condi-
tions. This can cause faulty measurements or
complete failure of the sensor. More information
on working with the sensor can be found in the re-
spective user information.

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2.13 Shutdown

– When the system is to be shut down or any


length of time, all supply lines are to be dis-
connected and all liquids are to be drained
from the hoses and system components.
– The pH measuring probe is to be removed,
packaged and storage according to section
2.12.
– All parts of the system and hoses are to be
cleaned thoroughly and any encrustation
and solids are to be removed.
– Completely empty and rinse the container for
the acid solution.
– Rinse out the diaphragm metering pump with
lots of water to remove any residual acid from
the pump and the hose connections.
– Disconnect the system from the electrical
power supply.

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3 Safety

Before putting the device into operation, the


experiment instructions are to be read thor-
oughly and especially the safety notes
Prior to starting the experiments, all partici-
pants are to be briefed on the safety aspects
and the correct handling of the unit!
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3.1 Intended Use

The unit is to be used only for teaching purposes.

3.2 Structure of the Safety Instructions

The signal words DANGER, WARNING or CAU-


TION indicate the probability and potential severity
of injury.
An additional symbol indicates the nature of the
hazard or a required action.

Signal word Explanation

DANGER Indicates a situation which, if not avoided, will result in


death or serious injury.

WARNING Indicates a situation which, if not avoided, may result in


death or serious injury.

CAUTION Indicates a situation which, if not avoided, may result in


minor or moderately serious injury.

NOTICE Indicates a situation which may result in damage to


equipment, or provides instructions on operation of
the equipment.

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Symbol Explanation

Hazardous Electrical voltage

Risk of burns
hot surface

Toxic materials

Corrosive materials

Risk of entanglement
rotating parts

Hand injuries

Notice

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3.3 Health hazards

WARNING
Electrical connections are exposed when the
control unit is open.
Risk of electric shock.
• Disconnect from the mains supply before
opening.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

• Work should only be performed by qualified


electricians.
• Protect the control cabinet against water and
moisture.

WARNING
Hazardous electrical voltage
Risk of electric shock.
• Never operate the unit without a correctly in-
stalled earth wire.
• Non-compliance with this requirement
means that the operator and the unit are no
longer adequately protected.
• In case of danger, isolate the system from the
mains by using the EMERGENCY STOP
button or unplugging.

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WARNING
The alcohol that is produced with this system
is raw alcohol and is not suitable for consump-
tion.
DANGER of poisoning!
• Consuming raw alcohol, even in small doses,
can lead to irreversible damage to health!
• While operating the distillation, make sure
that there is proper ventilation to prevent an
accumulation of alcohol ingredients in the air.

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WARNING
Steam lines and parts of the distillation unit get
very hot. Hot steam can escape at the pressure
relief line.
DANGER of burning / scalding!
• Tank 1 becomes very hot during the heating
operation. Do not touch the jacket surface of
the tank during operation .
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• Never operate the steam heating for tank 1 with-


out a closed steam pressure-relief line.
• Never operate the steam heating of tank 1
without the water supply in tank 1.
• While operating the distillation unit, much of
the equipment will get very hot. Do not touch
the surface of the water bath, the distillation
bubble and the column.

Observe all safety notes for the distillation unit in


the attached operating instructions of the manu-
facturer. Non-adherence can lead to extensive
danger to health.

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WARNING
Handling acid and caustic carries a risk of
chemical burns.
DANGER of damage to health!
• The hazards and safety information de-
scribed in the safety data sheets must be fol-
lowed closely when handling the acid and
buffer solutions used in the experiments.

WARNING
Rotating parts.
RISK of injury!!
• Do not reach into the rotating coupling of the
stirrer in tank 1.
• Do not reach into the rotating coupling of the
stirrer in tank 2.
• Do not reach into the rotating stirrer of the
distillation bubble.

WARNING
Risk of crushing at hinged lid.
DANGER of injuries !
• When opening tank 1, always secure the
cover with the latch-pin.

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3.4 Hazards for unit and function

NOTICE!
– After completion of individual sections of the
experiment, always clean and rinse any sys-
tem parts and hoses/lines that have been
used, thoroughly.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

NOTICE!
– The pH measuring probe is never to be put into
storage dry. After using the measuring probe,
remove it, clean it and put in wet storage.
In addition, follow the instructions of the mea-
suring probe manufacturer.

NOTICE!
– After the experiment, do not leave any acidic
solution in the acid container and acid supply
container. After using acid, remove all acid
from the acid container, diaphragm metering
pump and hose connections and rinse out
with water.

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NOTICE!
– Before operating the distillation unit, be sure
to read all safety and operating notes in the
manufacturer’s instructions. Non-adherence
can lead to extensive damage to the device.

NOTICE!
– When operating the compressed air dia-
phragm pump, solid particles greater than >
4 mm are never to be fed through. The result is
otherwise, irreversible damage to the pump.

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4 Theory

4.1 Basics of alcohol creation

The foundation of alcohol creation is the alcoholic


fermentation through which glucose with the addi-
tion of yeast causes ethanol and carbon dioxide.
This happens according to the following formula:
C6H1206 -> 2 C2H5OH + 2 CO2
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

glucose + yeast -> ethanol + carbon dioxide


The yeast is used as a biological aid in creating al-
cohol, which starts the initial conversion of the glu-
cose into ethanol. Information on the precise prog-
ress during alcohol fermentation can be found in
popular literature on the subject.

To distil alcohol from high-starch content raw ma-


terials that normally have very low glucose or
sugar contents, the raw material must go through
various process steps in order to obtain a sufficient
amount of alcohol.

The process of alcohol creation is divided into five


steps:
• Crushing the raw materials
• Condensation
• Saccharification
• Fermentation
• Distillation
Each of these steps requires different process
conditions to achieve optimal yields of alcohol.

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4.2 Crushing the raw materials

The target of crushing is pulping the starch con-


tained in the raw materials. During this process,
ensure that the starch is not destroyed during the
crushing. Pulping is normally done with ham-
mer-mills or monopumps.

Crushing the raw materials is not a component of


the CE 640 experiment stand. Information on the
topic of crushing can be read in popular literature
on the subject.

4.3 Liquification / saccharification of the raw materials

The liquification / saccharification of the raw mate-


rials, so-called mashing, has the purpose of con-
verting the starch contained in the raw materials
into glucose.
For the liquification and saccharification, special
enzymes must be added to the raw mash that are
essential for the conversion from starch into glu-
cose. The advantage of enzymes, in comparison
to other catalysers, is their chemo-selectivity.
Therefore, perfectly suitable enzymes for the re-
spective pairing of substrate/product are available.
The liquification is done while adding an enzyme (
in this case, alpha-amylase) at a temperature of
90- 95°C.
Liquefying the raw mash is necessary since the
heating causes the enclosed starch to cluster into
long chains of molecules. This can make stirring
and feeding the mash mechanically impossible.
The enzyme alpha-amylase breaks the long
chains of starch molecules into short molecule
chains. This leads to a clear reduction in the vis-

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cosity of the mash and therefore to a higher flow


capability and better feeding capabilities.
To achieve optimal enzyme activity, the ambient
conditions must be adapted to the respective type
of enzyme. For alpha-amylase, that means an am-
bient temperature of 90- 95°C and a pH value of
> 6.5.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

After the mash has been liquefied and the starch is


in short molecule chains, the starch must be con-
verted into glucose. This procedure is the saccha-
rification. This requires adding another enzyme to
the mash. Prior to this however, the ambient condi-
tions must be changed again to achieve an optimal
enzyme activity and therefore a high percentage of
glucose in the mash. For the enzyme gluco-amy-
lase, the mash must be cooled to 55- 60°C and the
pH value must be lowered to 4.5 - 5.5.
The entire procedure of liquification and saccharifi-
cation of the mash takes about 2 to 3 hours includ-
ing the half hour resting time after liquification and
after saccharification.
After the completion of the saccharification, the
mash must be cooled before the next step in the
process.

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4.4 Fermenting the mash

The fermentation converts the glucose in the mash


into alcohol. Yeast must be added to the mash for
this. The yeast coverts the glucose into ethanol
and carbon dioxide.
Yeast is a living micro-organism that belongs to the
fungus group. Unlike enzymes from the previous
process steps, yeast has the ability to reproduce.
The scope of reproduction depends on the appli-
cable ambient conditions. Yeast is very sensitive
to temperature, as are all organisms.
Temperature range 28 ... 32°C :
Optimal, the conversion from glucose
into alcohol achieves a maximum.
Temperatures below 12°C :
Yeast initiates activity.
Temperatures above 40°C :
Yeast dies.
Besides alcohol and carbon dioxide, heat is gener-
ated during the fermentation process, which slowly
heats the mash. Therefore, the temperature must
be monitored and the fermentation tank must be
cooled in some cases.
To achieve a good mixture between the mash and
the yeast during the fermentation process, an stir-
rer slowly mixes the mash. This mixing can carry
on continuously at low rpm or at high rpm in
intervals.
The fermentation of the mash must be done in a
closed container that does not allow any contact
with the atmosphere. Otherwise, there is a danger
of a bacteria contamination that could result in
turning the alcohol fermentation into a vinegar
fermentation.

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During the fermentation process, carbon dioxide is


produced, which escapes into the atmosphere
through a fermentation lock. This can be recog-
nized by the gas bubbles escaping in the sealing
liquid of the fermentation lock.
The duration of the fermentation depends on dif-
ferent factors:
– Temperature
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– Type of yeast
– Intensity of the mixing
Normally, a fermentation experiment takes be-
tween approx. 68 - 72h. That makes regular moni-
toring of the processes necessary.
The following must be checked regularly:
– Fermentation lock
– Fermentation temperature:
– Foam build-up and fill level in the fer-
mentation tank
During the fermentation, carbon dioxide foam
builds up on the surface of the mash. This is not
permitted to escape through the fermentation lock.
The height of the foam layer must be checked reg-
ularly through the inspection-glass therefore. The
build-up of this foam layer is a sign of active fer-
mentation in the mash.

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4.5 Distillation of the mash

After completed fermentation, the distillation is the


last step in creating alcohol. The distillation of alco-
hol from the mash is done with the help of a water
bath distillery. This system works in the same way
as large industrial systems.

4.5.1 Basics of distillation

Distillation and rectification are two important ther-


mal separation procedures. This can obtain one or
more of the volatile components from a volatile
mixture with several volatile components with a
high degree of purity. This separation process
functions by means of the basic operations of
evaporation and condensation. The difference be-
tween distillation / rectification and the separation
process of evaporation is that in evaporation only
one of the components is volatile. In distillation /
rectification the vapour phase has a different com-
position to the liquid phase. This fact is the basis
for distillation and rectification.
The difference between rectification and distilla-
tion is that in rectification the vapours emanating
from the recovered condensate are partially re-
turned to the column and made to perform materi-
als transfer with the rising vapours on or at suitable
column fitments.
In distillation the rising vapours are immediately
condensed in a condenser and drawn off without a
return line.
The concentrations in the vapour phase (y) and the
liquid phase (x) can be calculated for the ideal case
using RAOULT’s Law and DALTON’s Law, if the
vapour pressure curves of the respective compo-
nents are known. Normally however the molecular
proportions of the two phases at equilibrium are

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determined experimentally. The calculation of the


molecular proportions should for instance result in
an ideal two part mixture benzene (A) / toluene (B).
An ideal two part mixture has been achieved when
the partial vapour pressure curves are linear and
the molecules of the components behave exactly
as the pure components on their own.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

From RAOULT’s law:

Fig. 4.1 Pressure diagram pA = P0A xA and pB = p0B xB


benzene / toluene
( in this case xA + xB = 1 and pA + pB = p )

and with DALTON’s law :

pA = yA p and pB = yB p
( in this case yA + yB = 1 and pA + pB = p )

the pressure diagram shown in figure 4.1 can be


created. The pressure diagram shows that the two
part mixture of benzene / toluene behaves ideally
based on the two straight line partial pressure
curves ( 1 + 2 ). Curve 3 shows the total vapour
pressure by molecular proportion xA.
Diagram 4.2 shows the typical course of the boiling
and condensation lines in the boiling diagram for
benzene / toluene at a pressure of p = 1.01 x105
Pa. From the boiling diagram, as shown in the dia-
gram, an equilibrium diagram can be created.
The quantitative determination of the equilibrium
condition is determined as follows:
Fig. 4.2 Boiling diagram / equilibrium
diagram benzene / toluene a xA
yA =
1+ x A ( a - 1)

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For this, a is defined as relative volatility. This is


the relation between the molecular proportions at
equilibrium of the vapour phase and of the liquid
phase.

yA xA
a=
yB xB
For an ideal two part mixture by using RAOULT’s
Law and DALTON’ Law it produces:

p0A
a=
p 0B
The greater the amount of a , the further the equi-
librium trend is from the diagonals and the easier
the distilling separation.
In diagram 4.3 for instance boiling diagrams and
equilibrium diagrams for non-ideal two part mix-
tures are shown.

Fig. 4.3 Boiling diagram / equilibrium Further information on these mixtures and the
diagram for real mixtures quantitative determination of equilibrium condi-
tions can be found in technical literature.

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4.5.2 Construction of a distillation

Each distillation device is basically constructed ac-


4
cording to Fig. 4.4 .
The batch evaporates in the distillation bubble (2).
In this instance, a sufficiently large evaporation
chamber must exist. The constant heating of the
batch mixture can be achieved by e.g. an stirrer in
the distillation bubble. The heating (3) of the batch
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mixture can be done directly or indirectly through a


water bath with sensitive batch materials.
The isolation column (1) separates the parts of the
gas mixture with a low boiling point from those with
a high boiling point by condensation of those with a
1
high boiling point on the isolation column fixtures.
Columns with filling materials or with bottoms can
be used as isolating columns. Another possibility is
2 the dephlegmator. This is constructed as a water
container, through which the gas is routed in tubes.
The water temperature of this container must be
slightly higher than the initial temperature of the
3 cooling water from the condenser.
The isolating column of the CE 640 is a bubble cap
tray column with 3 layers in combination with a
water-filled dephlegmator.
The last components of a distillation apparatus is
Fig. 4.4 Distillation apparatus the condenser(4), in which the gas parts that have
a low boiling point are condensed and escape the
condenser and the distillation process as liquid.

4 Theory 45
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5.1
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CE 640

Distillery yeast culture

Antifoaming agent

Gluco amylase
Sulphuric acid

5 Notes on running experiments


Alpha amylase
Water > 5°dH
Potatoes
Diagram of creating alcohol

Condensation Cooling Saccharification Cooling Fermentation


Notes on running experiments

Raw alcohol Condensation Cooling Evaporation


BIOTECHNICAL PRODUCTION OF ETHANOL

Distillation

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The diagram shows the principle of the process


with the respective conditions that must be at-
tained for the respective process steps. This dia-
gram applies for the procedure used in creating
raw alcohol from potatoes.
The steps liquification > cooling > saccharification
> cooling are performed in tank 1.
The fermentation is performed in the fermentation
tank.
Evaporating > cooling > condensing is all done in
the distillation unit.

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5.2 Liquification and Saccharification

The liquification of potatoes begins outside of the


experimental stand. The potatoes must be
crushed into a mash. The amount of potatoes de-
pends on the desired fill level of the system. A ref-
erence value for the CE 640 is ~10...15 kg.
The hand valves are to be positioned according to
the following table for the liquification /
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

saccharification. The designations of the valves


can be seen in process image (see 2.2 or 7.2).

Setting/ Setting/ Setting/


Valve Valve Valve
function function function
V1 Control valve V11 omitted V21 Closed
V2 Control valve V12 Closed V22 Closed
V3 Closed V13 Closed V23 Open
V4 Closed V14 Closed V24 Closed
V5 Closed V15 Position 1 V25 Closed
V6 Solenoid valve V16 Position 1 V26 Safety valve
V7 Solenoid valve V17 Closed V28 Closed
V8 Open V18 Closed V31 Closed

V9 Open V19 Closed V32 Closed


V10 Closed V20 Closed

NOTICE! Before the experiment, the overflow


hoses must be connected to all overflow points of
the system.

The liquification process is as follows:


• Set valves according to the previous table.
• Close valve V23.
• Fill the acid supply container with sulphuric acid solution
of concentration 0.5mole/litre .
• Switch on system.

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• Install the pH measuring probe and connect the supply


line.
• Call up the control menu for tank 1.
• Make steam supply.
• Enter the water supply quantity (~ 5...10 litre) on the
PLC controller and fill in tank 1.
• Enter the set temperature 90...95°C on the PLC control-
ler. Steam will be routed through the water supply now.
• Switch on the stirrer for tank 1.
• Slowly open valve V23.
• After reaching the set temperature in tank 1 , add ~10%
of the amount of crushed potatoes.
• Add the enzyme alpha-amylase according to manufac-
turer’s specifications.
• Now, slowly add small portions of the potato mass until
the fill level of tank 1 reaches the pH sensor.
• After the potato mass and the enzymes have been com-
pletely added, the temperature must be held at a con-
stant temperature higher than 90°C for a minimum of
30 minutes.
• Than cool the mash to a temperature of ~55...58°C (Set
the temperature on the PLC controller). Cooling water
flows through the outer jacket of tank 1.
• pH value drop to 4.5...5.5 ( Enter the pH value on the
PLC controller). The pump now feeds in the acid solu-
tion to tank 1.
• Add the enzyme gluco-amylase and the anti-foaming
agent according to manufacturer’s specifications.
• After this addition, the temperature must be held for a
minimum of 30 minutes within a range from 55...58°C.
• Cool the mash to a temperature of ~28...30°C.

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After cooling the mash, the liquification and saccharification


processes are complete. The mash can now be fed into the
fermentation tank with pump P2. To do this, close V13 and
V21.

In order to equalize the pressure, the filling opening of the fer-


mentation tank must be open. The three-way valve V15 be-
fore the pump must be set so that the mash feeds into the
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

overflow. This is required to ensure that only saccharified


mash is pumped into the fermentation tank and not the con-
tent (clearance volume) in the pipe. After ~5...10 seconds
V15 is set so that the mash is pumped into the fermentation
tank.

Tank 1 must be cleaned as soon as possible after pumping


the mash out to prevent any biological degrading of the resid-
ual mash.
End all functions on tank 1 after the saccharification is com-
plete.

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5.3 Fermentation

After pumping from the cooking tank into the fermentation


tank, the fermentation portion of the experiment is begun.
The portion takes up the most time. The duration of this phase
normally takes several days. First, all required supplies must
be made ready for this long period. The hand valves are to be
set according to the following table for the fermentation
process.

Setting/ Setting/ Setting/


Valve Valve Valve
function function function
V1 Closed V11 omitted V21 Closed
V2 Closed V12 Open V22 Closed
V3 Closed V13 Closed V23 Closed
V4 Solenoid valve V14 Closed V24 Open
V5 Closed V15 Position 2 V25 Closed
V6 Closed V16 Position 1 V26 Safety valve
V7 Closed V17 Closed V28 Closed
V8 Open V18 Closed V31 Closed
V9 Closed V19 Closed V32 Closed
V10 Closed V20 Closed

• After pumping over, the distilling yeast must be added to


the mash. The metering is to be done according to man-
ufacturer’s specifications.
• Seal the fermentation tank hermetically against the at-
mosphere.
– Fill the fermentation lock with water.
– Close the latches in the cover.
– Check whether valve V21 is closed.
– Set valve V15 so that the fermentation tank is
enclosed from the atmosphere.

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• Then switch on the stirrer of the fermentation tank to


achieve a good mixture.

NOTICE! The stirrer is not to be operated continually


during fermentation since the foam build-up would be
too great.

During fermentation, carbon dioxide builds up in the in-


All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

terior of the fermentation tank. This escapes through


the fermentation lock on the head of the fermentation
tank (can be recognized by gas bubbles in the fermenta-
tion lock). The development of gas bubbles only begins
after a few hours of the fermentation process, however.
• During the fermentation process, perform the following
checks regularly:
– Temperature in the fermentation tank
– Fill level in the fermentation tank
– Fill level in the fermentation lock - refill if nec-
essary
The temperature can be set and monitored on the PLC
controller.
The temperature in the fermentation tank is regulated by
feeding cold and hot water into the double jacket around
the fermentation tank.

NOTICE! During fermentation, the temperature in-


creases slightly and then drops continuously after
~12 h.

• After a mixing time of ~5h the stirrer should only be oper-


ated in intervals. Interval operation supports the escape
of carbon dioxide from mash. The durations for the inter-
vals can only be determined from trying it yourself.

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• If the fill level in the fermentation tank is too high and fluid
is forced out the fermentation lock, some mash will have
to be drained out through valve V13.

During the fermentation process, mash samples can be taken


and tested for alcohol and residual sugar content. This is done
by separating the liquid from the floating particles and deter-
mining the alcohol content with an alcohol meter and the re-
sidual sugar content with a saccharimeter.
• The fermentation process is completed after a period of
~68...72 h. No more gas bubbles should be escaping
through the fermentation lock then.
• The mash must then be fed into the distillation unit. This
is done by opening valves V21 and V17 and setting the
three-way valve V16 so that the feed is to the distilla-
tion unit. Open the filling opening in the cover of the fer-
mentation tank.
• Afterwards, pump P3 can be switched on from the PLC
controller and the mash can be pumped into the distilla-
tion unit.
• After pumping is complete, close valve V17.

The fermentation tank must be cleaned as soon as possible


after pumping the mash out to prevent any biological degrad-
ing of the residual mash.

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5.4 Distillation

The last process step is the distillation of the alcohol


from the mash. The valves must be set as follows for the
distillation process.

Setting/ Setting/ Setting/


Valve Valve Valve
function function function
V1 Closed V11 omitted V21 Open
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

V2 Closed V12 Closed V22 Closed


V3 Closed V13 Closed V23 Closed
V4 Closed V14 Closed V24 Closed
V5 Closed V15 Position 1 V25 Closed
V6 Closed V16 Position 1 V26 Safety valve
V7 Closed V17 Open / Closed V28 Closed
V8 Open V18 Closed V31 Closed
V9 Closed V19 Closed V32 Closed
V10 Closed V20 Open

Read the instructions by the manufacturer for an


exact description of the distillation unit.

WARNING
The alcohol that is produced with this system
is raw alcohol and is not suitable for consump-
tion.
DANGER of poisoning!
• Consuming raw alcohol, even in small doses,
can lead to irreversible damage to health!
• While operating the distillation, make sure
that there is proper ventilation to prevent an
accumulation of alcohol ingredients in the air.

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WARNING
Steam lines and parts of the distillation unit get
very hot. Hot steam can escape at the pressure
relief line.
DANGER of burning / scalding!
• Tank 1 becomes very hot during the heating
operation. Do not touch the jacket surface of
the tank during operation .
• Never operate the steam heating for tank 1 with-
out a closed steam pressure-relief line.
• Never operate the steam heating of tank 1
without the water supply in tank 1.
• While operating the distillation unit, much of
the equipment will get very hot. Do not touch
the surface of the water bath, the distillation
bubble and the column.

Trouble-free functionality of the cooling water system is


absolutely necessary for proper distillation operation.
The distillation occurs as follows:
• Close valve V17.
• Fill the water bath to the mark with water.
• Fill the condenser and the dephlegmator with wa-
ter.
• Set the thermostat for the cooling water flow ac-
cording to the manufacturer’s instructions.
• Set the gas temperature T9 for control to
78...79°C.
• Switch on the stirrer for the distillation unit.

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• While heating, monitor the temperature and the


water pressure in the water bath continuously. Af-
ter achieving the temperature set for T9, the heat-
ing is controlled by switching the heater. The con-
densing alcohol flows into the alcohol supply and
then into the ethanol container (B4) from there.
• During the distillation procedure, slowly increase
the value for temperature T9 to 90...95°C and set
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

the cooling water thermostat to a higher tempera-


ture at the same time.
• After separating all alcohol, switch the distillation
unit off according to the manufacturer’s instruc-
tions.
• After the distillation unit has cooled to ~30...40°C ,
the residual mash can be drained through valve
V19 and can be disposed of. Clean the distillation
unit according to the instructions of the manufac-
turer. All liquids are to be drained and the system
dried.

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6 Data acquisition software

6.1 Software installation

6.1.1 System requirements:

• PC with Pentium IV, 1 GHz


• Minimum 1024 MB RAM
• Minimum 11GB of available hard disk space
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

• 1 CD-ROM drive
• USB-port
• Graphics resolution min. 1024 x 768 Pixel,
True Color
• Operating system:
Windows XP / Windows Vista/ Windows 7

6.1.2 Installation of software

The following are needed for the installation:


– A fully operational PC with USB port (for mini-
mum requirements see chapter 6.1.1).
– G.U.N.T. CD-ROM
All components necessary to install and run
the program are contained on the CD-ROM
supplied by G.U.N.T.

Hardware driver installation


Without Internet
– Set up USB connection to PC
– Call up the Device Manager
Manually install the driver for "USB FAST
SERIAL ADAPTER"
• Right-click on "USB FAST SERIAL
ADAPTER"

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• Update the driver software


• Search the computer for driver soft-
ware
• Insert the CD-ROM in the drive (e.g.
drive D)
• Install the driver from D:\USB-COM-M
– Restart the PC

Installation with Internet connection (Windows 7)


– BWhen prompted to install new device driver
software, download the driver from the
Internet. (The "Automatically install Windows
update" option may need to be activated.))
– Install the driver from the Internet.
– Restart the PC

Installing the CE 640 software


– Insert the CD-ROM in the drive (e.g. drive D)
– Open EXPLORER under WINDOWS and
select the CD-ROM.
– Open the subdirectory \installer\.
– Run Setup.exe in D:\installer\setup.exe. (As-
suming D is the CD-ROM drive.)
– Follow the instructions in the dialog box.
The computer must be restarted after completing
the installation.

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6.2 Software operation

After starting the program for the first time, the lan-
guage must be selected once.

The program has three tasks:


– Clear representation of the current mea-
sured values in the system diagram
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

– Plotting of measured values (x,t)


– Graphical display of values

Program structure
The menu items are context-specific, i.e. not all
menu items are always enabled. The menu bar
contains 5 options with the following sub-items:
11 – Start
– File
– View
– Language

12 13 14 15

Fig. 6.1 Measurement value recording


settings

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6.2.1 Menu point: Start

5 4 1 2 3 7 – Charts
This view shows the measured values plotted in
graphical form. The plot button (1) can be used to
manually add the current measured value to the
measured value list once a file has been defined.
The green field lights up for short period when the
measurement value is read in. The second button
(2) can be used to automatically plot measured
values in the specified interval. Settings for auto-
matic plotting can be made after pressing the but-
6 6 ton (3). These settings are made in another win-
dow that appears with the following options:
Fig. 6.2 Time elapsed
– Time interval (11)
– Number of measured values (12)
– Selection switch (13)
Position left: Measuring points are at-
tached on existing data records.
Position right: Data record is written in
the existing file.
– Memory location & file name (14)
– Comment for data record (15)

The button (4) can be used to stop and restart the


advance. Click with the left mouse button in the
field (7) for background (7) and (5) for characteris-
tics, colours and characteristics can be changed.
Scaling for the graphs is done by clicking with the
left mouse key on the start or end value (6) of the
scale.

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– System diagram
This view shows the current measured values in a
clear process diagram. The measurement values
are temperature and pH value in tank 1

– About GUNT
Shows information about GUNT.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Fig. 6.4 System Diagram


– EXIT
Exits the program.

Fig. 6.3 About GUNT

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6.2.2 Menu point: File

– New
(“Charts” only)
Creates a new data set.
– Open
(“Charts” only)
Opens a saved data set and allows the data to be
viewed in a “Measurement diagram” or measured
values to be added.
– Print
(“Charts” only)
Prints out the time lapse graphs on the default
printer.
– Print window
(with “Charts”) Prints out a hardcopy on the stan-
dard printer.
(with “System diagram”) Prints out the system dia-
gram currently displayed on the standard printer.

6.2.3 Menu point: View

– Clear graph
(“Charts” only)
Clears the graph on the screen.
– Play / pause
(“Charts” only)
Starts / stops the advance of the display.

6.2.4 Menu point: Language

– German
– English
– French
– Spanish

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7 Appendix

7.1 Technical data

Apparatus Complete L x W x H: 3400 x 1200 x 2000 mm


Weight: approx. 500 kg
Electrical supply: 3 x 400 V/ 50 Hz
Alternatives optional, see type plate
Compressed air requirements: 1,5 ... 6 bar
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Steam requirements: Q 15 kg/h


pmin 3 bar
Cooling water requirements: min. 400 litre/h
via fresh water connection

Mash tank Capacity: 60 litre


Æxh 341 x 675 mm
Material: Stainless steel
Inspection glass: DN 50, DIN 28120
Temperature measurement probe PT 100

Fermentation tank Capacity: 48 litre


Æxh 341 x 675 mm
Material: Stainless steel
Inspection glass: DN 50, DIN 28120
Temperature measurement probe PT 100

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Water bath distillery L x W x H: 950 x 600 x 1700 mm


Mash volume approx. 40 litre
Heating capacity: 4500 W

Electrical supply: 3 x 400 V/ 50 Hz


alternative 3 x 220 V/ 60 Hz
Number of temperature sensors: 6
Column Diameter of column: 220 mm
Number of bubble caps 3
Number of inspection glasses 4
Inspection glass size DN 80
Stirrer: Speed: 135 rpm
Rating: 180 W
Electrical supply: 3 x 400 V/ 50 Hz
alternative 3 x 220 V/ 60 Hz
Material: Still: Copper
Column, dephlegmator: Copper
Condenser: Stainless steel
Water bath: Stainless steel

Stirrer for mash and fermentation tanks


Geared motor: Max. speed (B1): 200 rpm
Max. speed (B2): 105 rpm
Transmission 13.2
Rating: 120 W
Electrical supply: 3 x 400 V/ 50 Hz
alternative 3 x 220V /60 Hz
Cross-beam stirrer Æxh 260 x 30 mm
Material: Stainless steel

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Diaphragm feed pump L x W x H: 190 x 140 x 200 mm


Max. head 72 m
Max. capacity 27 litre/min
Max. suction lift wet 7m
Max. particle size 4 mm
Max. air consumption: 12 m³/h
Connections: Intake side 3/8 “
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Delivery Side 3/8 “


Air intake 1/8 “
Material: Diaphragm: EPDM
Sphere: EPDM
Housing: PP

Diaphragm metering pump L x W x H: 262 x 102 x 186 mm


Max. operating pressure: 16 bar
Max. capacity 2.1 litre/h
Max. suction lift wet 6m
Connection: 6 x 4 mm
Connection voltage: 100...230 VAC
Connection frequency: 50...60 Hz
Materials Metering head: PP
Valves: PP
Seals: EPDM
Balls: ceramic

Control valve steam Nominal size: DN 15


Pressure stage: PN 40
Kvs value: 0.4
Characteristic curve: linear
Material: Stainless steel
Max. supply air pressure: 4 bar

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Control valve cooling water Nominal size: DN 20


Pressure stage: PN 16
Kvs value: 4.0
Characteristic curve: linear
Material: Cast iron
Nominal signal range 0,4...2,0 bar

Solenoid valve Nominal size: DN 4


Pressure Range: 0...6 bar
Kv value 0.5
Connection: G3/8 “
Connection voltage: 24 VDC

Ethyl alcohol container Capacity: 10 litre


Material: PE

Mash container L x W x H: 600 x 400 x 165 mm


Capacity: 30 litre
Material: HDPE

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7.2 Process schematic


All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

7 Appendix 69
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7.3 Items supplied

1 System complete in steel trolley on castors


1 pH-measuring probe
1 Ethyl alcohol container
1 Mash container, portable
1 Set of water hoses with sleeve material
1 Steam hose, stainless steel mesh-wound
1 Alpha amylase, 0,5 litre
1 Gluco amylase, 1 litre
1 Antifoaming agent, 1 litre
1 Distilling yeast, 500 gr
1 Software on CD
1 Data transmission cable
1 Instruction manual

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7.4 Index

A
Alpha- Amylase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38, 50
B
Boiler heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Bubble cap tray column . . . . . . . . . . . . . . . . . . . . . . . 14, 45
Buffer solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
C
Carbon dioxide . . . . . . . . . . . . . . . . . . . . . . . . . . 37, 40 - 41
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 05/2013

Chemo- Selectivity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Compressed air diaphragm pump . . . . . . . . . . . . . . . . . . 23
Condenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 45, 56
Control cabinet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Control valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Cooking tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Crushing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
D
Damage to health . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Data acquisition software. . . . . . . . . . . . . . . . . . . . . . . . . 16
Dephlegmator . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 45, 56
Diaphragm metering pump . . . . . . . . . . . . . . . . . 24, 28, 35
Diaphragm pump . . . . . . . . . . . . . . . . . . . . . . . . . 19, 23, 36
Distillation . . . . . . . . . . . . . . . . . . . . . 17, 21, 32, 42, 45, 55
Distillation unit . . . . . . . . . . . . . . . . . . . . . 13, 20, 36, 48, 54
E
Enzymes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8, 38
Ethanol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
F
Fermentation . . . . . . . . . . . . . . . . . . . . . . . . 37, 40 - 41, 48
Fermentation lock . . . . . . . . . . . . . . . . . . . . . . . . 11, 41, 53
Fermentation tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9, 11
Flow meter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Fresh water supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
G
Gluco- Amylase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Gluco-Amylase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
Glucose . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37 - 38
I
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Installation of software . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
L
Liquification. . . . . . . . . . . . . . . . . . . . . . . . . . . 1, 38 - 39, 49

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M
Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Maintenance unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Mash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Mash tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Mashing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8, 38
P
PLC controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17, 53
Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Pitched blade agitator . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Pitched blade agitators . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Poisoning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32, 55
Process diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
R
Raw alcohol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32, 55
S
Saccharification . . . . . . . . . . . . . . . . . . . . . . . 1, 38 - 39, 49
Saccharimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
Safety notes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Sealing liquid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
Software operation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
Starch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Stirrer . . . . . . . . . . . . . . . . 8, 11, 18, 20 - 21, 40, 50, 53, 56
System diagram. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
System time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
T
Temperature control . . . . . . . . . . . . . . . . . . . . . . . . . 17 - 19
W
Water bath distillery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
Y
Yeast . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37, 40
P
pH measuring probe . . . . . . . . . . . . . . . . 16, 25, 28, 35, 50
pH reduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
pH value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

72 7 Appendix

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