CE640E V0.3 Duplex

Instruction Manual CE 640

Biotechnical Production of Ethanol

CAD_9 05/2013

BIOTECHNICAL PRODUCTION OF ETHANOL

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

CE 640

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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CE 640 4

BIOTECHNICAL PRODUCTION OF ETHANOL 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

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4.4 Fermenting the mash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40 4.5 Distillation of the mash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42

5

4.5.1

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

4.5.2

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

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

7

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

Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65 7.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65 7.2 Process schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69 7.3 Items supplied . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70 7.4 Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71 iii

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CE 640 1

Introduction Alcohol is an important base material for the chemical industry. It is mainly obtained from food-stuffs containing starch such as e.g. potatoes or cereal products.

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The experimental stand CE 640 Biotechnical Production of Ethanol makes it possible to trace and research the process of industrial alcohol production from the liquification and saccharification of the original materials to the conversion from sugar into alcohol on to the distillation of the alcohol. The experimental stand uses two stainless steel agitation vats for this. One is a cooking tank tempered with steam and cold water and one is a fermentation tank tempered with cold and hot water. Distilling the alcohol is done with a completely integrated 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 controls and rpm-regulated stirrers. Control and monitoring on the system is done on-site by an integrated PLC. Recording the measurement data and monitoring can also be supplemented with a connected PC. The experimental stand is used only for training students in the process-, bio- and food-stuffs technology and is not intended for industrial purposes.

1 Introduction

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BIOTECHNICAL PRODUCTION OF ETHANOL Learning Objectives / Experiments

–

2

Familiarization with the necessary individual steps and system components for production of ethanol:

•

gelatinisation by steam injection

•

liquefaction by use of alpha-amylase

•

saccharification by use of glucoamylase

•

fermentation: conversion of sugar into ethanol by yeast cultures under anaerobic conditions

•

distillation: separation of ethanol from the mash

1 Introduction

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CE 640 2

Unit description

2.1

General view

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1

2

3

4

5

15

14

13 11 12

10

Fig. 2.1

8

9

8

7

6

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

7

Mash container (B5)

Pressure regulator for cold water control valve

8

Diaphragm metering pumps (P1 & P4)

15

Pressure regulator for steam-pressure control valve

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4

Water

Process schematic CE 640

Warm Water

Fig. 2.2

Water

Process schematic

Water

2.2

Steam

BIOTECHNICAL PRODUCTION OF ETHANOL

Compressed Air

CE 640

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CE 640

Individual components

Measuring points

B1 B2 B3 B4 B5 B6 D1 P1 P2 P3 P4 R1 R2 R3 H1 V1 V2

V3 - V7 V8- V27 V26 V28-V32 T1 T2 T3 T4 T5 T6 T7 T8 T9 Q1 F1 PI1

Cooking tank (tank 1) Fermentation tank (tank 2) Acid solution container Ethyl alcohol container Mash container Caustic tank Distillation unit Diaphragm metering pump Compressed air feed pump B1 - B2 Compressed air feed pump B2 - D1 Diaphragm metering pump (caustic) Stirrer geared motor B1 Stirrer geared motor B2 Stirrer geared motor D1 Water bath heater Steam control valve Cooling water control valve

Solenoid valves Ball valves, hand actuated Steam pressure safety valve Ball valves, hand actuated Mash temperature B1 Mash temperature B2 Cooling water drain temperature B2 Distillation unit water bath temperature Mash temperature in distillation bubble Gas temperature after bubble cap 1 Gas temperature after bubble cap 2 Gas temperature after bubble cap 3 Gas temperature after dephlegmator pH value B1 Water flow to B1 Steam pressure indication

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

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BIOTECHNICAL PRODUCTION OF ETHANOL

2.3

Cooking tank for liquification / saccharification

Fig. 2.3

Mash tank

6

2 Unit description

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CE 640

2 4

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1

3

7

9

8

10 6 11 12

5

13 17 18

14

15

Fig. 2.4

16

19

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

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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 process 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 diaphragm 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 container. 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 Unit description

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CE 640

Fermentation tank

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2.4

Fig. 2.5

Fermentation tank

2 Unit description

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CE 640

3

4

9

10

11

12

5 2

6

1

7

17 16

8

19

13

14 15

Fig. 2.6

Fermentation tank (Tank 2)

18

19

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

10

2 Unit description

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BIOTECHNICAL PRODUCTION OF ETHANOL

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CE 640

The fermentation tank converts the sugar contained in the mash into alcohol. This tank can be sealed air tight and tempered with cold and hot water 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 mash is monitored with a temperature sensor. To regulate the temperature more efficiently, another 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 fermentation lock (see Fig. 2.7). 1 2

1

Geared motor

3

2

Coupling

4

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

8 5 9 6 7

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 container off from the atmosphere. The CO2 generated 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.

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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

Distillation unit

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2.5

Fig. 2.8

Distillation unit

2 Unit description

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CE 640

Fig. 2.9

BIOTECHNICAL PRODUCTION OF ETHANOL

Distillation unit, overview

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 temperature sensors in the system. For a detailed description of the individual components and measurement connections, please read the attached operating instructions of the manufacturer.

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CE 640 2.6

Control cabinet and control technology 1

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2 3 4 5

6

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 controller is menu guided. All entries and control instructions are entered via the touch screen. The actual control of individual components such as regulating valves, stirrer, pumps and heating con2 Unit description

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BIOTECHNICAL PRODUCTION OF ETHANOL trol is handled with the PLC installed in the control cabinet. All of the temperatures that are recorded in the experimental stand are shown on the touch screen. The pH values and the temperature from the pH measuring probe are shown on a separate measuring 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 control 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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CE 640 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).

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On the Start menu, you will find an operating hour meter and some touch fields. Fig. 2.11

Start menu

The sub-menus are reached by touching the individual touch fields on the screen. The screen offers choices between the parameter settings for temperature control circuits in:

•

Mash (Cooking) tank (tank 1) with temperature- 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 respective 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 Parameter (Fig. 2.12) From here, the display language for the PLC controller can be changed. The system time, date and the brightness of the screen can also be set.

Fig. 2.12

Parameter

If an error has occurred on the PLC, a list of the errors that have occurred will be displayed.

Return brings you back to the previous start menu.

2 Unit description

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CE 640 1

BIOTECHNICAL PRODUCTION OF ETHANOL 3

From the start menu (Fig.2.11), the “Mash tank B1” can be touched to change to the menu responsible for the cooking tank.

2

This menu can be used to regulate the temperature 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 Fig. 2.13

5 Mash tank

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

18

•

Switch field is green :

Element is switched on

•

Switch field is red

Element is switched off

:

2 Unit description

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CE 640

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

7

Fig. 2.15

8

9

Mash tank

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 automatically. Button "Pump P2 " is used for actuating a compressed 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 setting 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

2 Unit description

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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 temperature control for cooling. The stirrer can be run either in temporal intervals or continuously.

Fig. 2.16

Fermentation

Following settings are possible:

–

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. Fig. 2.18

•

Pump 2 feeds the container content from tank 1 to tank 2.

•

Pump 3 feeds the container content from tank 2 into the distillation unit.

Fermentation

The settings for control parameters Kp, Tn and Tv for tank 2 is made the same as for tank 1 (Fig.2.14).

Fig. 2.17

Fermentation parameter

Tank 2 has a solenoid valve as actuator. Therefore, 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.

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CE 640

“Return” brings you back to the previous menu.

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In the menu for distillation, the temperature T9 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. Fig. 2.21

Distillation

Pump 3 can be operated from here to fill the distillation bubble with the container content of tank 2. On a diagram with the positions of the various sensors 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).

Fig. 2.19

Distillation Parameter

The distillation has a heater as an actuator. Therefore, 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 period”, the more precise the controller can work. The actuator heater is activated by binary switching 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.

2 Unit description

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BIOTECHNICAL PRODUCTION OF ETHANOL

From the start menu (Fig. 2.11), the “Measurement” button can be actuated to bring up an overview 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

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.

2 Unit description

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CE 640

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

2.8

1

Compressed air diaphragm pump (P2 & P3)

2

Fig. 2.24

3

Compressed air diaphragm pump P2

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 are never to be fed through. The result is otherwise, irreversible damage to the pump.

3 Safety

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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 addition of yeast causes ethanol and carbon dioxide. This happens according to the following formula:

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

C6H1206 glucose + yeast

->

2 C2H5OH

+

->

ethanol

+

2 CO2 carbon dioxide

The yeast is used as a biological aid in creating alcohol, which starts the initial conversion of the glucose into ethanol. Information on the precise progress during alcohol fermentation can be found in popular literature on the subject. To distil alcohol from high-starch content raw materials 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.

4 Theory

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CE 640 4.2

BIOTECHNICAL PRODUCTION OF ETHANOL Crushing the raw materials The target of crushing is pulping the starch contained in the raw materials. During this process, ensure that the starch is not destroyed during the crushing. Pulping is normally done with hammer-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 materials, so-called mashing, has the purpose of converting 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 glucose. The advantage of enzymes, in comparison to other catalysers, is their chemo-selectivity. Therefore, perfectly suitable enzymes for the respective 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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BIOTECHNICAL PRODUCTION OF ETHANOL cosity of the mash and therefore to a higher flow capability and better feeding capabilities.

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

To achieve optimal enzyme activity, the ambient conditions must be adapted to the respective type of enzyme. For alpha-amylase, that means an ambient 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 converted into glucose. This procedure is the saccharification. This requires adding another enzyme to the mash. Prior to this however, the ambient conditions must be changed again to achieve an optimal enzyme activity and therefore a high percentage of glucose in the mash. For the enzyme gluco-amylase, 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 saccharification of the mash takes about 2 to 3 hours including 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.

4 Theory

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CE 640 4.4

BIOTECHNICAL PRODUCTION OF ETHANOL 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 applicable 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 generated 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 stirrer 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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BIOTECHNICAL PRODUCTION OF ETHANOL During the fermentation process, carbon dioxide is produced, which escapes into the atmosphere through a fermentation lock. This can be recognized by the gas bubbles escaping in the sealing liquid of the fermentation lock.

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

The duration of the fermentation depends on different factors:

–

Temperature

–

Type of yeast

–

Intensity of the mixing

Normally, a fermentation experiment takes between approx. 68 - 72h. That makes regular monitoring of the processes necessary. The following must be checked regularly:

–

Fermentation lock

–

Fermentation temperature:

–

Foam build-up and fill level in the fermentation 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 regularly through the inspection-glass therefore. The build-up of this foam layer is a sign of active fermentation in the mash.

4 Theory

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CE 640 4.5

BIOTECHNICAL PRODUCTION OF ETHANOL Distillation of the mash After completed fermentation, the distillation is the last step in creating alcohol. The distillation of alcohol 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 thermal 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 between 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 composition to the liquid phase. This fact is the basis for distillation and rectification. The difference between rectification and distillation is that in rectification the vapours emanating from the recovered condensate are partially returned to the column and made to perform materials 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 components 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. From RAOULT’s law: Fig. 4.1

Pressure diagram benzene / toluene

pA = P0A xA and pB = p0B xB ( 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 diagram, an equilibrium diagram can be created. The quantitative determination of the equilibrium condition is determined as follows: Fig. 4.2

4 Theory

Boiling diagram / equilibrium diagram benzene / toluene

yA =

a xA 1+ x A ( a - 1)

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BIOTECHNICAL PRODUCTION OF ETHANOL 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=

yA yB

xA xB

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

p0A p 0B

The greater the amount of a , the further the equilibrium 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 mixtures are shown. Fig. 4.3

44

Boiling diagram / equilibrium diagram for real mixtures

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

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BIOTECHNICAL PRODUCTION OF ETHANOL Construction of a distillation 4

Each distillation device is basically constructed according to Fig. 4.4 .

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

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.

1

2

3

Fig. 4.4

4 Theory

Distillation apparatus

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.

45

Gluco amylase

5 Notes on running experiments

Potatoes

Condensation

Water > 5°dH

Alpha amylase

Sulphuric acid

Cooling

Condensation

Raw alcohol

Notes on running experiments

5.1 Diagram of creating alcohol

Evaporation

Fermentation

5

Distillation

Cooling

Saccharification

Cooling

CE 640

Antifoaming agent

Distillery yeast culture

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

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BIOTECHNICAL PRODUCTION OF ETHANOL The diagram shows the principle of the process with the respective conditions that must be attained for the respective process steps. This diagram 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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BIOTECHNICAL PRODUCTION OF ETHANOL Liquification and Saccharification

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

The liquification of potatoes begins outside of the experimental stand. The potatoes must be crushed into a mash. The amount of potatoes depends on the desired fill level of the system. A reference 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

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.

5 Notes on running experiments

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BIOTECHNICAL PRODUCTION OF ETHANOL •

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 controller. 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 manufacturer’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 completely added, the temperature must be held at a constant 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 solution 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 fermentation tank must be open. The three-way valve V15 before 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 content (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 residual mash. End all functions on tank 1 after the saccharification is complete.

5 Notes on running experiments

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CE 640 5.3

BIOTECHNICAL PRODUCTION OF ETHANOL 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

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

52

•

After pumping over, the distilling yeast must be added to the mash. The metering is to be done according to manufacturer’s specifications.

•

Seal the fermentation tank hermetically against the atmosphere.

–

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.

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

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 interior 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 fermentation 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 necessary

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 increases slightly and then drops continuously after ~12 h.

•

5 Notes on running experiments

After a mixing time of ~5h the stirrer should only be operated in intervals. Interval operation supports the escape of carbon dioxide from mash. The durations for the intervals 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 determining the alcohol content with an alcohol meter and the residual 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 distillation unit. Open the filling opening in the cover of the fermentation tank.

•

Afterwards, pump P3 can be switched on from the PLC controller and the mash can be pumped into the distillation 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 degrading of the residual mash.

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CE 640 5.4

BIOTECHNICAL PRODUCTION OF ETHANOL Distillation

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

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

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 consumption. DANGER of poisoning!

5 Notes on running experiments

•

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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BIOTECHNICAL PRODUCTION OF ETHANOL 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 without 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:

56

• • •

Close valve V17.

•

Set the thermostat for the cooling water flow according to the manufacturer’s instructions.

•

Set the gas temperature T9 for control to 78...79°C.

•

Switch on the stirrer for the distillation unit.

Fill the water bath to the mark with water. Fill the condenser and the dephlegmator with water.

5 Notes on running experiments

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CE 640

5 Notes on running experiments

•

While heating, monitor the temperature and the water pressure in the water bath continuously. After achieving the temperature set for T9, the heating is controlled by switching the heater. The condensing 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 temperature at the same time.

•

After separating all alcohol, switch the distillation unit off according to the manufacturer’s instructions.

•

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 manufacturer. 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:

6.1.2

•

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

Installation of software The following are needed for the installation:

–

A fully operational PC with USB port (for minimum 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"

•

6 Data acquisition software

Right-click on "USB FAST SERIAL ADAPTER"

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–

•

Update the driver software

•

Search the computer for driver software

•

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. (Assuming 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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CE 640 6.2

Software operation After starting the program for the first time, the language must be selected once.

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

The program has three tasks:

–

Clear representation of the current measured 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: 11

12 Fig. 6.1

13

14

–

Start

–

File

–

View

–

Language

15

Measurement value recording settings

6 Data acquisition software

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Menu point: Start

6.2.1 5

4

1

2

3

6 Fig. 6.2

–

7

6 Time elapsed

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 automatic plotting can be made after pressing the button (3). These settings are made in another window that appears with the following options:

–

Time interval (11)

–

Number of measured values (12)

–

Selection switch (13) Position left: Measuring points are attached 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 characteristics, 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

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

Shows information about GUNT. Fig. 6.4

System Diagram

–

EXIT

Exits the program.

Fig. 6.3

About GUNT

6 Data acquisition software

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BIOTECHNICAL PRODUCTION OF ETHANOL 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 standard printer. (with “System diagram”) Prints out the system diagram 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

64

Menu point: Language

–

German

–

English

–

French

–

Spanish

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CE 640 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

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

alternative

3 x 220 V/ 60 Hz

Compressed air requirements: 1,5 ... 6 bar 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

Material:

Stainless steel

Inspection glass:

Fermentation tank

341 x 675 mm DN 50, DIN 28120

Temperature measurement probe

PT 100

Capacity:

48 litre Æxh

Material: Inspection glass:

341 x 675 mm Stainless steel DN 50, DIN 28120

Temperature measurement probe

7 Appendix

PT 100

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BIOTECHNICAL PRODUCTION OF ETHANOL 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: Column

Diameter of column:

3

Number of inspection glasses

4 DN 80

Speed:

135 rpm

Rating:

180 W

Electrical supply: alternative Material:

220 mm

Number of bubble caps Inspection glass size Stirrer:

6

3 x 400 V/ 50 Hz 3 x 220 V/ 60 Hz

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: alternative Cross-beam stirrer

Æxh Material:

66

3 x 400 V/ 50 Hz 3 x 220V /60 Hz 260 x 30 mm Stainless steel

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CE 640

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

Connections:

Material:

12 m³/h

Intake side

3/8 “

Delivery Side

3/8 “

Air intake

1/8 “

Diaphragm:

EPDM

Sphere:

EPDM

Housing: Diaphragm metering pump

L x W x H:

PP 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: Materials

50...60 Hz

Metering head:

PP

Valves:

PP

Seals:

EPDM

Balls: Control valve steam

ceramic

Nominal size:

DN 15

Pressure stage:

PN 40

Kvs value:

0.4

Characteristic curve: Material:

linear Stainless steel

Max. supply air pressure:

7 Appendix

4 bar

67

05/2013

CE 640

BIOTECHNICAL PRODUCTION OF ETHANOL Control valve cooling water

Nominal size:

Pressure stage: Kvs value: Characteristic curve: Material: Nominal signal range

Solenoid valve

Nominal size: Pressure Range: Kv value Connection: Connection voltage:

Ethyl alcohol container Capacity: Material:

Mash container

L x W x H: Capacity: Material:

68

DN 20 PN 16 4.0 linear Cast iron 0,4...2,0 bar

DN 4 0...6 bar 0.5 G3/8 “ 24 VDC

10 litre PE

600 x 400 x 165 mm 30 litre HDPE

7 Appendix

05/2013

BIOTECHNICAL PRODUCTION OF ETHANOL

CE 640

Process schematic

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

7.2

7 Appendix

69

05/2013

CE 640 7.3

70

BIOTECHNICAL PRODUCTION OF ETHANOL 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,

1

Software on CD

1

Data transmission cable

1

Instruction manual

500 gr

7 Appendix

05/2013

BIOTECHNICAL PRODUCTION OF ETHANOL

CE 640 7.4

Index A Alpha- Amylase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38, 50 B Boiler heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 Bubble cap tray column . . . . . . . . . . . . . . . . . . . . . . . 14, 45 Buffer solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

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

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

7 Appendix

71

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BIOTECHNICAL PRODUCTION OF ETHANOL

CE 640 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