CE640E V0.3 Duplex

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CE 640

Biotechnical Production

of Ethanol

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All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Instruction Manual

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

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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

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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

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 All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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-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.

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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 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

7

Ethyl alcohol container (B4) Mash container (B5)

14 Pressure regulator for cold water control valve

8 Diaphragm metering pumps (P1 & P4) 15 Pressure regulator for steam-pressure control valve All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 2.1 General view

1 2 3 4 5 15 14 13 11 12 10 8 9 8 7 6

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2.2 Process schematic Compressed A ir Water Steam Warm Water Water Water

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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 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.

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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 All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 2.4 Cooker tank / Mash tank 7 8 6 14 15 16 19 4 3 5 17 18 13 10 2 1 9 11 12

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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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2.4 Fermentation tank All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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 Fig. 2.6 Fermentation tank (Tank 2)

3 4 9 10 11 12 13 14 15 18 19 2 1 17 19 6 7 8 5 16

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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 wawa-ter jacket. The cold or hot hot wawa-ter 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 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 Geared motor 2 Coupling 3 O-ring 4 Divider 5 Stirrer shaft 6 Sealing liquid area 7 Cover

8 Sealing liquid

9 Spacer post for geared motor 10 O-ring

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.

Fig. 2.7 Fermentation lock, cut-out view 1 2 3 4 5 6 7 8 9 10

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

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2.5 Distillation unit All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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The distillation unit is a modified boiler heater with water bath (6). It contains bubble cap (1) tray column, 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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2.6 Control cabinet and control technology

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-All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 2.10 Control cabinet, overview

1 2 3 4 5 6

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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.

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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.

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:

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Mash (Cooking) tank (tank 1) with tem-perature- und pH-value control

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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-rors that have occurred will be displayed.

Return brings you back to the previous start menu. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 2.11 Start menu

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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).

The pH value in the cooking tank is regulated by adding acid and caustic using the diaphragm me-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

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Switch field is red : Element is switched off

Fig. 2.13 Mash tank

1 3 2

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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 is displayed with display (9). After achieving the present volume, the solenoid valve closes auto-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 Fig. 2.15 Mash tank

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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:

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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.

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Pump 2 feeds the container content from

tank 1 to tank 2.

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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 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.

Fig. 2.16 Fermentation

Fig. 2.17 Fermentation parameter Fig. 2.18 Fermentation

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“Return” brings you back to the previous menu.

In the menu for distillation, the temperatureT9 is regulated as a command variable for the distillation (Fig. 2.19). 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 is not variable.

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.

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 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”

Fig. 2.19 Distillation Parameter Fig. 2.20 Distillation, over temperature Fig. 2.21 Distillation

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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.

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:

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.

Fig. 2.22 Example for numerical input Fig. 2.23 Measurement

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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 the respective pump. The supply volume of the pump is set with a control valve (2). Air lines can be removed from the threaded connections (3). The compressed air diaphragm pumps are designed for transferring liquids up to a viscosity of 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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 2.24 Compressed air diaphragm pump P2

1 2 3

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. 2.27 & Fig. 2.28) 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:

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Adjusting the pump stroke and

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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. 2.26 Diaphragm metering pump (P1)

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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:

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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 which the test stand is set up must be ade-quately ventilated.

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Connect the water supply to (4) cold water and (5) hot water (Fig. 2.29)

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Attach drain lines to (1).

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Attach steam supply to (2), technical special-ist only.

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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).

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Attach the power supply (ensure that the cor-rect voltage supply is used!).

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Check the fuse in the control cabinet before switching the unit on.

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Screw the pH measuring probe into tank 1

and make electrical connections.

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Switch on the unit at the master switch.

Fig. 2.29 Supply connections 1 2 3 4 5 6

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. 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

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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!

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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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.

•

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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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 .

•

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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

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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.

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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

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

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vis-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.

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 restinclud-ing time after liquification and after saccharification.

After the completion of the saccharification, the mash must be cooled before the next step in the process. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

–

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 rectificadistilla-tion 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

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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.

From RAOULT’s law:

pA= P0AxAand pB= p0BxB

( in this case x_A+ x_B= 1 and p_A+ p_B = p )

and with DALTON’s law : pA= yAp and pB= yBp

( in this case y_A+ y_B= 1 and p_A+ p_B= 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 x_A.

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:

y x x A A A = + -a a 1 ( 1) All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 4.1 Pressure diagram benzene / toluene

Fig. 4.2 Boiling diagram / equilibrium diagram benzene / toluene

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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.

a = y x

y x

A A

B B

For an ideal two part mixture by using RAOULT’s Law and DALTON’ Law it produces:

a =p p A B 0 0

The greater the amount ofa , 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.

Further information on these mixtures and the quantitative determination of equilibrium condi-tions can be found in technical literature.

Fig. 4.3 Boiling diagram / equilibrium diagram for real mixtures

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4.5.2 Construction of a distillation

Each distillation device is basically constructed ac-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 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 high boiling point on the isolation column fixtures. Columns with filling materials or with bottoms can be used as isolating columns. Another possibility is 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 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 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.

Fig. 4.4 Distillation apparatus 4

1

2

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5 Notes on running experiments 5.1 Diagram of creating alcohol

All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013 Condensation Cooling Saccharification Cooling Fermentation _Evaporation Cooling Condensation Distillation Raw a lcohol Dis tiller y y eas t c ultur e Alpha amylase Antifoaming agent Water > 5°dH Potatoes Gl uco a m y la se Sulphuric acid

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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 / saccharification. The designations of the valves can be seen in process image (see 2.2 or 7.2).

Valve Setting/ function Valve Setting/ function Valve Setting/ 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

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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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.

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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 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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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. Valve Setting/ function Valve Setting/ function Valve Setting/ function

V1 Closed V11 omitted V21 Closed

V2 Closed V12 Open V22 Closed

V4 Solenoid valve V14 Closed V24 Open

V6 Closed V16 Position 1 V26 Safety valve

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-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. Valve Setting/ function Valve Setting/ function Valve Setting/ function

V1 Closed V11 omitted V21 Open

V6 Closed V16 Position 1 V26 Safety valve

V7 Closed V17 Open / Closed V28 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.

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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 switchheat-ing 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 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. All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

•

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" All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

–

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:

–

Start

–

File

–

View

–

Language All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

Fig. 6.1 Measurement value recording settings

11

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6.2.1 Menu point:Start

–

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-ton (3). These settings are made in another win-dow that appears with the following options:

–

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.

Fig. 6.2 Time elapsed 5 4 1 2 3 7

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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.

–

EXIT

Exits the program.

Fig. 6.3 About GUNT Fig. 6.4 System Diagram

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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

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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 alternative 3 x 220 V/ 60 Hz Compressed air requirements: 1,5 ... 6 bar

Steam requirements: Q 15 kg/h

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

Mash tank Capacity: 60 litre

Æ x h 341 x 675 mm

Material: Stainless steel

Inspection glass: DN 50, DIN 28120

Temperature measurement probe PT 100

Fermentation tank Capacity: 48 litre

Æ x h 341 x 675 mm

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 Æ x h 260 x 30 mm

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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 7 m

Max. particle size 4 mm

Max. air consumption: 12 m³/h

Connections: Intake side 3/8 “

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 6 m

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

K_vsvalue: 0.4

Characteristic curve: linear

Max. supply air pressure: 4 bar

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Control valve cooling water Nominal size: DN 20

Pressure stage: PN 16

K_vsvalue: 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

K_vvalue 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

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7.2 Process schematic All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

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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

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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 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 All R ights R eserved G .U.N.T. G erätebau GmbH, B arsbüttel, Germany 05/2013

CE640E V0.3 Duplex

CE 640

Biotechnical Production

of Ethanol

Instruction Manual

Table of Contents

1

Introduction . . . 1

2

Unit description . . . 3

3

Safety . . . 29

4

Theory . . . 37

5

Notes on running experiments . . . 47

6

Data acquisition software . . . 59

7

Appendix . . . 65

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