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.

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5 Notes on running experiments 5.1 Diagram of creating alcohol

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Rawalcohol

Distilleryyeastculture Alphaamylase

Antifoamingagent Water>5°dH PotatoesGlucoamylase Sulphuricacid

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.

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

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 0.5^mole/_litre.

•

Switch on system.

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•

Install the pH measuring probe and connect the supply line.

•

Call up the control menu for tank 1.

•

Make steam supply.

•

Enter the water supply quantity (~ 5...10 litre) on the PLC controller and fill in tank 1.

•

Enter the set temperature 90...95°C on the PLC control-ler. Steam will be routed through the water supply now.

•

Switch on the stirrer for tank 1.

•

Slowly open valve V23.

•

After reaching the set temperature in tank 1 , add ~10%

of the amount of crushed potatoes.

•

Add the enzyme alpha-amylase according to manufac-turer’s specifications.

•

Now, slowly add small portions of the potato mass until the fill level of tank 1 reaches the pH sensor.

•

After the potato mass and the enzymes have been com-pletely added, the temperature must be held at a con-stant temperature higher than 90°C for a minimum of 30 minutes.

•

Than cool the mash to a temperature of ~55...58°C (Set the temperature on the PLC controller). Cooling water flows through the outer jacket of tank 1.

•

pH value drop to 4.5...5.5 ( Enter the pH value on the PLC controller). The pump now feeds in the acid solu-tion to tank 1.

•

Add the enzyme gluco-amylase and the anti-foaming agent according to manufacturer’s specifications.

•

After this addition, the temperature must be held for a minimum of 30 minutes within a range from 55...58°C.

•

Cool the mash to a temperature of ~28...30°C.

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.

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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

V3 Closed V13 Closed V23 Closed

V4 Solenoid valve V14 Closed V24 Open

V5 Closed V15 Position 2 V25 Closed

V6 Closed V16 Position 1 V26 Safety valve

V7 Closed V17 Closed V28 Closed

V8 Open V18 Closed V31 Closed

V9 Closed V19 Closed V32 Closed

V10 Closed V20 Closed

•

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

•

Seal the fermentation tank hermetically against the at-mosphere.

–

Fill the fermentation lock with water.

–

Close the latches in the cover.

–

Check whether valve V21 is closed.

–

Set valve V15 so that the fermentation tank is enclosed from the atmosphere.

•

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.

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

V2 Closed V12 Closed V22 Closed

V3 Closed V13 Closed V23 Closed

V4 Closed V14 Closed V24 Closed

V5 Closed V15 Position 1 V25 Closed

V6 Closed V16 Position 1 V26 Safety valve

V7 Closed V17 Open / Closed V28 Closed

V8 Open V18 Closed V31 Closed

V9 Closed V19 Closed V32 Closed

V10 Closed V20 Open

Read the instructions by the manufacturer for an exact description of the distillation unit.

WARNING

The alcohol that is produced with this system is raw alcohol and is not suitable for consump-tion.

DANGER of poisoning!

•

Consuming raw alcohol, even in small doses, can lead to irreversible damage to health!

•

While operating the distillation, make sure that there is proper ventilation to prevent an accumulation of alcohol ingredients in the air.

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WARNING

Steam lines and parts of the distillation unit get very hot. Hot steam can escape at the pressure relief line.

DANGER of burning / scalding!

•

Tank 1 becomes very hot during the heating operation. Do not touch the jacket surface of the tank during operation .

•

Never operate the steam heating for tank 1 with-out a closed steam pressure-relief line.

•

Never operate the steam heating of tank 1 without the water supply in tank 1.

•

While operating the distillation unit, much of the equipment will get very hot. Do not touch the surface of the water bath, the distillation bubble and the column.

Trouble-free functionality of the cooling water system is absolutely necessary for proper distillation operation.

The distillation occurs as follows:

•

Close valve V17.

•

Fill the water bath to the mark with water.

•

Fill the condenser and the dephlegmator with wa-ter.

•

Set the thermostat for the cooling water flow ac-cording to the manufacturer’s instructions.

•

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

•

Switch on the stirrer for the distillation unit.

•

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.

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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"

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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.

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

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Fig. 6.1 Measurement value recording settings

11

12 13 14 15

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

6 6

–

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.

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Fig. 6.3 About GUNT Fig. 6.4 System Diagram

6.2.2 Menu point:File

–

New

(“Charts” only)

Creates a new data set.

–

Open

(“Charts” only)

Opens a saved data set and allows the data to be viewed in a “Measurement diagram” or measured values to be added.

–

Print (“Charts” only)

Prints out the time lapse graphs on the default printer.

–

Print window

(with “Charts”) Prints out a hardcopy on the stan-dard printer.

(with “System diagram”) Prints out the system dia-gram currently displayed on the standard printer.

6.2.3 Menu point:View

–

Clear graph (“Charts” only)

Clears the graph on the screen.

–

Play / pause (“Charts” only)

Starts / stops the advance of the display.

6.2.4 Menu point:Language

–

German

–

English

–

French

–

Spanish

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

Material: Stainless steel

Inspection glass: DN 50, DIN 28120 Temperature measurement probe PT 100

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

Mash volume approx. 40 litre

Heating capacity: 4500 W

Electrical supply: 3 x 400 V/ 50 Hz alternative 3 x 220 V/ 60 Hz Number of temperature sensors: 6

Column Diameter of column: 220 mm

Number of bubble caps 3

Number of inspection glasses 4 Inspection glass size DN 80

Stirrer: Speed: 135 rpm

Rating: 180 W

Electrical supply: 3 x 400 V/ 50 Hz alternative 3 x 220 V/ 60 Hz

Material: Still: Copper

Column, dephlegmator: Copper Condenser: Stainless steel Water bath: Stainless steel

Stirrer for mash and fermentation tanks

Geared motor: Max. speed (B1): 200 rpm

Max. speed (B2): 105 rpm

Transmission 13.2

Rating: 120 W

Electrical supply: 3 x 400 V/ 50 Hz alternative 3 x 220V /60 Hz

Cross-beam stirrer Æ x h 260 x 30 mm

Material: Stainless steel

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 “ 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

Control valve steam Nominal size: DN 15

Pressure stage: PN 40

K_vsvalue: 0.4

Characteristic curve: linear

Material: Stainless steel

Max. supply air pressure: 4 bar

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Control valve cooling water Nominal size: DN 20

Pressure stage: PN 16

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

Material: HDPE

7.2 Process schematic

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7.3 Items supplied

1 System complete in steel trolley on castors 1 pH-measuring probe

1 Ethyl alcohol container 1 Mash container, portable

1 Set of water hoses with sleeve material 1 Steam hose, stainless steel mesh-wound

1 Alpha amylase, 0,5 litre

1 Gluco amylase, 1 litre

1 Antifoaming agent, 1 litre

1 Distilling yeast, 500 gr

1 Software on CD

1 Data transmission cable 1 Instruction manual

7.4 Index

M

In document CE640E V0.3 Duplex (Page 51-78)