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PIERALISI Deutschland GmbH

May 15, 2006

Biodiesel Workshop

Biodiesel
PIERALISI Group Knowledge Base

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

Why BIODIESEL
Resources
- limited resources of petroleum and natural gas,
- unequal distribution of this resources:
-- Petroleum 78% in OPEC area,
-- natural gas 32% Russia, 39% OPEC.

Price
- price for petrolum is constantly rising,
- price is influenced by many almost un-controlable factors.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

Why BIODIESEL (contd)


Environment
- fully renewable energy, does not entail CO2 emission,
- CO2 emission from transport sector expected
to keep rising worldwide,
biofuels are the only alternative.

Human health
- reduction of partiuculate matter emission
- Biodiesel particulate is much less cancerogenic

Security and Independence of supply


- transport sector almost 100% depending on oil

Rural development
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

Biodiesel Production
Today Europe is the biggest Producer of Biodiesel
(2004: > 2 mt), mainlyGermany, France and Italy.
Legislation in the EU (triggered by the Kyoto-Protocoll) is
boosting Biodiesel production (B5).
Big development in the US
(today ~ 1/10th of the EU production)
Biodiesel program in Brazil
Biodiesel is a way to acchieve development in many
countries: investment programs in Malaysia, India, Philipines
Thailand, Australia, Canada...
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

Biodiesel Production
Today Europe is the biggest Producer of Biodiesel ....

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

..... and biodiesel production capacity in the US will have to


double by 2010 to keep up with demand....

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

..... Demand and sales are predicted to increase a lot....

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

Conclutions
Biodiesel and biofuels are the only way to reduce emmisons
from the transport sector.
Biodiesel industry is well established in EU and will continue to
increase its production.
Biodiesel is becoming a worldwide reality.
Production capacity worldwide is expected to triple in the next
5 years.
So, there is definitely a market for PIERALISI to devellop

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

10

Vision 2010
Legislation: 5,75 % Market-share of biofules in 2010
In consequence:
100 new Biofuel plants will be needed only in the EU.
Approx. 40 new Biodiesel plants with a capacity of 100.000 t/y
and 60 new Bioethanol plants also with capacity of 100.000 t/y .
Investment will be approx. 3 bn Euro !
USA will act accordingly.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

11

Most probably this vehicle will never be powered by BIODIESEL

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

12

.....but this one IS already !

.....and its a FERRARI too !


PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

13

Biodiesel
Basics, Process, Sources, ....

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

14

Outline
Biodiesel whats that?
Biodiesel how its made
Biodiesel Process Steps
Biodiesel Process Variants
Biodiesel Influences from Triglyceride
Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

15

Outline
9 Biodiesel whats that?
Biodiesel how its made
Biodiesel Process Steps
Biodiesel Process Variants
Biodiesel Influences from Triglyceride
Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

16

Biodiesel whats that ?


Biodiesel is:
A result of the Transesterification of Triglycerides.
A mixture of Methylesters of different Fatty Acids (FA).
Produced via a viriaty of processes and processtechnologies.
Produced from a wide variety of natural triglyceride
sources.
A fuel which is able to partly substitute the mineral
diesel fuel.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

17

Biodiesel whats that ?


Biodiesel is defined as the mono-alkyl esters of
fatty acids derived from vegetable oils or animal
fats.
In simple terms, biodiesel is the product you get when a
vegetable oil or animal fat is chemically reacted with an
alcohol to produce a new compound that is known as a fatty
acid alkyl ester.
A catalyst such as sodium or potassium hydroxide is required.
Glycerol is produced as a by-product.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

18

Biodiesel whats that ?


Biodiesel Process Target
Amongst others, the main target of the process is
to drop the viscosity of the triglycerides
(oil/fat; example rapeseed oil 74 mm/s)

to the level of mineral diesel fuels


(2 - 7 mm/s at 20 C)

to make it suitable for the injection system of serial


diesel engines.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

19

Biodiesel whats that ?


The approximate proportions of the reaction are:
100 kg of oil + 10 kg of methanol
100 kg of biodiesel + 10 kg of glycerol

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

20

Biodiesel whats that ?

Biodiesel can be made from triglycedride sources like:


1. Vegetable oils such as soybean oil, corn oil, canola
(an edible variety of rapeseed) oil, cottonseed oil,
mustard oil, palm oil, etc.
2. Restaurant waste oils such as frying oils
3. Animal fats such as beef tallow or pork lard.
4. Trap grease (from restaurant grease traps), float
grease (from waste water treatment plants), etc.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

21

Outline
Biodiesel whats that?
9 Biodiesel how its made
made?
Biodiesel Process Steps
Biodiesel Process Variants
Biodiesel Influences from Triglyceride Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

22

Biodiesel Transesterification of Triglycerides


It is not necessary to be a chemist to understand where
biodiesel comes from and how it is used.

However, it is useful to review some of the fundamental


chemical principles that are behind biodiesel to give a
better understanding of the production process and the
properties of this green fuel.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

23

Biodiesel Transesterification of Triglycerides


All vegetable oils and animal fats consist primarily of triglyceride
molecules as shown below.
Extending away from this
backbone are the three long
A three carbon
fatty acid chains.
chain called
glycerol backbone
runs along the left
side of the molecule.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

24

Biodiesel Transesterification of Triglycerides


Note that this molecule contains the ester group three times. Thus, it
is called a triester.

Sometimes people refer to the reaction that converts oil or fat


(triglyceride) to methyl esters (biodiesel) as "esterification" as if the
reaction were converting something that is not an ester into an ester.
In reality, the reaction converts one type of ester into another type of
ester. This is why the reaction is corectly named Transesterification.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

25

Biodiesel Transesterification of Triglycerides


Transesterification is the process of reacting a triglyceride
molecule with an excess of alcohol in the presence of a
catalyst (KOH, NaOH, NaOCN3, etc.) to produce fatty esters
and glycerin. The chemical reaction with methanol is
schematically shown below.

Triglyceride + methanol

PIERALISI Deutschland GmbH


May 15, 2006

fatty esters + glycerol

Biodiesel Workshop

26

Outline
9 Biodiesel whats that?
9 Biodiesel how its made
9 Biodiesel Process Steps
Biodiesel Process Variants
Biodiesel Influences from Triglyceride
Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

27

Energea Demonstrastion and production facility


Zistersdorf, Austria

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

28

The Biodiesel Process an Overview


Important Note:
The process shown (and subsequently the all
process steps) is only one out of a variety of
different process variants utilised to produce
Biodiesel.
Discussing with the client, will result in an altered
process scheme meeting the individual needs and
reflecting the regional and political conditions.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

29

The Biodiesel Process an Overview

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

30

Biodiesel Transesterification of
Triglycerides
Crude Oil

Methanol

Transesterification

Catalyst

p-FA-ME
Methanol

Glycerine

The reaction is reversible !


As long as we have excess methanol present,
we are forcing the reaction to the methyl ester side !

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

31

Biodiesel Transesterification of
Triglycerides
Reaction rate
Extent of
Reaction

Time

Reaction: proceeding through time from


reactants to product
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

32

Biodiesel Transesterification of
Triglycerides
Transesterification reaction will proceed at
ambient temperture (21C), but needs 4 8 hours
to come to completion.
Reaction time shortend to 2 4 h at ~ 40 C and
1 2 hour at 60 C.
Higher temp. will further decrease reaction time
but requires pressure vessels due to methanol
boiling at 65 C.
High shear is also decreasing necessary reaction
time.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

33

The Biodiesel Process an Overview

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

34

The Biodiesel Process


Separation after Transesterification
After the Transesterification reaction has taken place, two major
products exist:
Glycerine and fatty acid methly ester (Biodiesel) both containing a
substantial amount of excess methanol that was used in the
reaction.
Using difference in specific gravity, the Glycerine phase and the
Biodiesel phase can be separated.
As an example this separation could be achieved in a fast
separation process with high efficiency using Pieralisi Vertical Disc
Separator.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

35

The Biodiesel Process

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Separation after Transesterification


p-FA-ME
Methanol

p-FA-ME
Methanol

Glycerine
(10%)
(Traces of
Solids)

Glycerine
Methanol

Solids

p-FA-ME, ME: ~ 880 kg/m

~ 50-70C

In case of ideal
reaction, no solids
will be present.

Glycerine, ME: ~ 1050 kg/m


p-FA-ME: partly esterified FA-methyl ester
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

36

The Biodiesel Process an Overview

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

37

The Biodiesel Process Washing

Once separated from the Glycerine, the Biodiesel is sometimes

purified by gently washing with warm water.


This step results in the removal of residual catalyst and soaps.
After the addition and the mixing with water, the two-phase mixture
can easily be separated by Pieralisi Vertical Disc Separator
Centrifuges.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

38

The Biodiesel Process Washing


ed
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Nitroge
Biodiesel
Methanol

Washing

Biodiesel

(Traces of
Solids)
Water,
3 6%,
acidified

Biodiesel
Water
(~ < 3500 ppm)
Methanol

Water
Methanol

Impurities:
Soaps
Triglycerides
Ions
Phosphates

Solids

Usually no
solids
present.

Biodiesel ~ 880 kg/m


Water, ME: ~ 960 kg/m

~ > 40 C
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

39

ATEX
Water Content.... Part of Biodiesel specifications
Specification
Applies to

EUROPE

GERMANY

USA

EN 14214:2003

DIN V 51606

ASTM D6751

FAME

FAME

FAAE

g/cm

0.86-0.90

0.875-0.90

Viscosity 40C

mm/s

3.5-5.0

3.5-5.0

Distillation

% @ C

Flashpoint

120 min

110 min

CFPP

* country specific

summer 0 spr/aut -10 winter -20

Cloud point

Sulphur

mg/kg

CCR 100%

%mass

Carbon residue (10%dist.residue)

%mass

0.3 max

0.3 max

Sulphated ash

%mass

0.02 max

0.03 max

0.02 max

Oxid ash

%mass

Water

mg/kg

500 max

300 max

500 max

Total contamination

mg/kg

24 max

20 max

Cu corrosion max

3h/50C

Oxidation stability

hrs;110C

6 hours min
51 min

49 min

47 min

0.82-0.845

0.8 max

1.9-6.0

2.0-4.5

90%,360C

85%,350C - 95%,360C

130 min

55 min
* country specific

* report
10 max

10 max

15 max

0.05 max

0.05 max

0.1 max

1
N/A (25 g/m3)

0.5 max

0.5 max

Methanol

%mass

0.20 max

0.3 max

Ester content

%mass

96.5 min

Monoglyceride

%mass

0.8 max

0.8 max

Diglyceride

%mass

0.2 max

0.4 max

Triglyceride

%mass

0.2 max

0.4 max

Free glycerol

%mass

0.02 max

0.02 max

0.02 max

Total glycerol

%mass

0.25 max

0.25 max

0.24 max

120 max

115 max

Linolenic acid ME

%mass

12 max

C(x:4) & greater unsaturated esters

%mass

1 max

Phosphorus

mg/kg

10 max

Alkalinity

mg/kg

Gp I metals (Na,K)

mg/kg

5 max

GpII metals (Ca,Mg)

mg/kg

5 max

PAHs

%mass

Lubricity / wear

m at 60C

200 max
24 max

mgKOH /g

10 max

51 min

10 max

5 max

11 max
460 max
EUROPE

PIERALISI Deutschland GmbH


May 15, 2006

350 max
0.3 max

Acid value

Iodine value

EN 590:1999
Diesel

Density 15C

Cetane number

PETROLEUM DIESEL

GERMANY

Biodiesel Workshop

USA

DIESEL

40

The Biodiesel Process Washing


Water Content....
In the Biodiesel, different Water portions are present:
- free water,
- emulsified water,
- disolved water.

Biodiesel Specification: ASTM 6751-02, EN 14213 tells us:


< 500 ppm water in the final product.
Question of anlysing method !
US ASTM D 2709: only free water by centrifuging
Europe ISO 12937: total water by Karl-Fischer titration.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

41

The Biodiesel Process Washing


Water Content....
Since Europe leads the biodiesel market, EN 14213 will be the
specification to fulfill.
Water means total water
Test Method will be Karl-Fischer.
We always refer to total water !
Note:
There is an important difference between Biodiesel and mineral diesel:
- Biodiesel can host disolved water !

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

42

The Biodiesel Process an Overview

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

43

The Biodiesel Process Polishing

In some systems, the Biodiesel is distilled in an additional step to


remove small amounts of coloured bodies to produce a colourless
Biodiesel.
After the distillation, a final polishing may be required to minimise the
amount of residual particles to comply with the setted standard.
These very fine particles cannot be removed by gravity, the extremely
high g-force of more than 9.000 x earth gravity in PIERALISI
Vertical Disc Clarifier Centrifuges is necessary.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

44

The Biodiesel Process Polishing

Biodiesel

Biodiesel

Solids

In case of ideal process


conditions, only traces solids
will be present.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

45

The Biodiesel Process an Overview

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May 15, 2006

Biodiesel Workshop

46

The Biodiesel Process Neutralising /


Catalyst Removal / Salt Washing
Glycerine acidification and potassium sulphate washing process I
The glycerine by-product contains unused catalyst, fatty acid and soaps
that are neutralized with an acid. In some cases, the salt formed during
this phase is recovered for use as fertilizer. The salt and fatty acid can
be separated from the glycerine by Pieralisi 3-Phase Decanter
Centrifuges to achieve a highly dehumidified salt.
Glycerine acidification and potassium sulphate washing process II
The purity and dryness of the salt discharged in the potassium sulphate
washing process I is sometimes not good enough for further treatment
or selling to the buyer. In these cases, a washing of the solids with
methanol in a remixing tank with a subsequent second liquid solid
separation by a Pieralisi Decanter Centrifuge results in a white and
dry fertilizer that can either be packed or dried for final use.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

47

The Biodiesel Process Neutralising /


Catalyst Removal / Salt Washing
Glycerine
Methanol

FFA

FFA

Light phase:
-Fatty acid
-3 - 5%-v/v Glycerin
-< 0.5%-v/v salt

Methanol
Glycerine
Methanol
Salt

FFA
Sulphoric
Acid

Glycerine

Heavy phase:
-Glycerin with
-1% -v/v fatty acid
and < 1%-v/v salt

Methanol
Salt

Methanol

Feed:
-40 50% glycerin
-20 30% free fatty acid
-10 30% salt

~ 40-50C
PIERALISI Deutschland GmbH
May 15, 2006

Methanol
Impurities

Feed:
-75% methanol
-25% salt,
Biodiesel Workshop

pure Salt

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Outline
9 Biodiesel whats that?
9 Biodiesel how its made
Biodiesel Process Steps
9 Biodiesel Process Variants
Biodiesel Influences from Triglyceride
Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

49

The Biodiesel Process Reaction Types

The transesterification reaction can be handled in different ways:


Batch type reaction,
Continuously Stirred Tank Reactor (CSTR), single / multi-step,
Continuous Flow Pipe Reactor,
.
Lets have a look !

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

50

The Biodiesel Process Reaction Type


M

100 % complete
Extent of
Reaction

Stirred tank batch reactor

Progress

Time

Reaction proceeding with time


P

Recirculating reactor
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

51

The Biodiesel Process Reaction Type


Continuously Stirred Tank Reactor = CSTR
M

p-FA-ME
Methanol

Crude Oil

Methanol
Glycerine

Catalyst
100 % complete
Extent of
Reaction

Single operating point for CSTR


Time*
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

* Average hydraulic
residence time
52

The Biodiesel Process Reaction Type


To acheive a complete reaction requires two or more
stages.
M
Crude Oil

Methanol
p-FA-ME
Methanol

Methanol
Catalyst
Biodiesel
Methanol

100 % complete
Extent of
Reaction
Glycerine
Methanol
1st. Stage, 2nd Stage

PIERALISI Deutschland GmbH


May 15, 2006

Time* Biodiesel Workshop

Glycerine
Methanol
53

The Biodiesel Process Reaction Type


Reactants in
Catalyst
Products out

Crude Oil

Biodiesel
Methanol

Turbulent Flow
Methanol
100 % complete

Glycerine
Methanol

Extent of
Reaction

Time
Length

Reaction proceeds as the reactants move down the pipe.


PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

54

The Biodiesel Process Reaction Type


High Shear Multy Channel

Pumping the reactants trough


small (high shear) channels

High Pressure Inlet

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

55

The Biodiesel Process


Batch vs. Continuous Flow
Batch type reaction provides better flexibility to
adapt the process to different feedstocks.
Batch type reaction does not require a 24/7
operation.
Continuous reaction is better suited for high
volume separation-equipment (centrifuges).
Batch type reaction is the better solution for
smaller plants (capacity < 10-15.000 t/y).
Continuous reaction is the better solution for
larger plants (capacity > 15.000 t/y).
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

56

Outline
9 Biodiesel whats that?
9 Biodiesel how its made
Biodiesel Process Steps
Biodiesel Process Variants
9 Biodiesel Influences from Triglyceride
Source

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

57

Triglyceride Sources
Vegatable oils: soybean, canola, palm, etc.
Inedible oils: jatropha, etc.
Rendered animal fats: beef tallow, lard,
chicken fat
Recovered materials:
trap grease, soap-stock

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

58

Influences of Triglyceride source:


Most important differences:
Saturation Level, FFA Level, Water Content, Phosphatide
Level, Salt /solids level
High Saturation Level:

Winterization

High FFA Level:

Pre-esterification

High Water Content:

Flash-Drying

High Phosphatide Level:

Degumming

High Salt / Solids level:

Fat-Washing

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

59

Influences of high Saturation Level :


Potential risk of forming crystals in the
Biodiesel:
Out of specification.
Treatment: Winterization by cooling and crystall
separation.
( only in very few cases)

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

60

Influences of high FFA Level :


Free Fatty Acids potentially react with alkali
catalyst:
- Loss of catalyst,
- Formation of soap,
Resulting in increased water content.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

61

Dealing with high FFA level: Pre-esterification


The Pre-esterification also sometimes called
Neutralisation is often done via crude Glycerine /
Methanol.
Oil / FAT
Glycerine

Neutralisation

Crude oil
Methanol

Solids
Glycerine

Methanol
Catalyst

Crude Glycerine / Methanol / Catalyst


from Separation after transesterification.
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

Sent to separation.

62

Dealing with high FFA level: Pre-esterification


After Pre-esterification the mixture is separeted in e.g.
centrifuges.
Crude oil
Crude oil
Methanol

Sent to
transesterification

Solids
Glycerine

Glycerine
Methanol

Solids

Sent for further treatment to reach


higher Glycerine Quality
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

63

The Biodiesel Process an Overview

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May 15, 2006

Biodiesel Workshop

64

Influences of high Water Content :


Water potentially hydrolizes fats:
- Formation of FFA,
Resulting in increased water content and,
Formation of soap.
Treatment: Flach Drying

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

65

Influences of high Phosphatide Level:


High phosphatide level leads to high gum level
and disturbs the transesterification.
Gums potentially form gels at ambient
temperature.
Rising of viscosity,
Problems with separation after
transesterification (intermediate liquid phase).

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

66

Dealing with high Phosphatide Level: Degumming


There are many different degumming processes on the
market.
Crude oil
Crude oil

Phosphatides
Water

Degumming

Acid / Lye

Gums
Water
Solids

Two step Degummimg with Acid


(1) and Lye (2) dosing.

Sent to separation.

Note: Degumming is part of the oil refining process.


Pieralisi only offers Sparators for low capacities !
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

67

Dealing with high Phosphatide Level: Degumming


After initial Degumming the mixture is separated in e.g.
centrifuges.
Gums
Water

Crude oil

Sent to
washing step.

Crude oil

Gums
Water
Solids

Gums
Water

Solids

Waste

Gums (heavy phase) needs special outlet (big C.P.) !


PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

68

Dealing with high Phosphatide Level: Washing


Purifing the oil by washing with water.
Gums
Water
Crude oil

Crude oil

Washing
Gums
Water

Water

Sent to separation.

Washing with water.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

69

Dealing with high Phosphatide Level: Washing


After washing the mixture is again separated in e.g.
centrifuges.
Crude oil
Gums
Water

Crude oil

Gums
Water

Sent to
transesterification

Waste

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

70

Influences of high Salt and Solids Level :


Potential risk of disturbing the
transesterification
Inefficient reaction, formation of side-products.
Treatment: oil washing ( only for used edible oils)

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

71

Dealing with high Salt and Solids Level in used edible


oils / fats : Washing
Washed fat
Crude fat

Water
~ 0,5 %-v/v

Static Mixer

Water
Salts
Solids

Salts
Water
~ 2 6%-v/v

Heavy phase:
Wastec

Solids

~ 95- 98C

PIERALISI Deutschland GmbH


May 15, 2006

Light phase:
sent to
transesterification

Solids: Waste

Biodiesel Workshop

72

The Biodiesel Process an Overview

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

73

Biodiesel
PIERALISI Separation Equipment

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

74

PIERALISI Machines for the BIODIESEL


Processes
3-Phase Separation: How does it work?
Decanter The Work Horse of our Separation
Equipment
Vertical Separator The Race Horse of our
Separation Equipment
Typical Decanter Flow Chart for Ex-proof Installations
Typical Flow Charts for Separators
Operation Modes of Gastight Machines
Capacity Overview
References
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

75

3-Phase Separation:
How does it work?
Light Phase

Light Phase Weir

Sedimentation
Tank with 1 x g
or rotating Bowl with
high g-Force
PIERALISI Deutschland GmbH
May 15, 2006

3-Phase
Mixture
Interface

Inlet Barrier
Heavy Phase

Biodiesel Workshop

Sediment

76

Decanter The Work Horse of our Separation


Equipment for:
High solid concentration in feed
Separation of coarse solid particles
Operation with lower g-forces < 2500 x g
Good dewatering perfomance
Forced solid discharge by screw conveyor

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

77

3-Phase Decanter

Conventional
Design

New
Design CP-A

Heavy Phase out

Light Phase out

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

78

Decanter The New Generation in Operation

Adjusting device for


trimming the paring
radius of the heavy
liquid of CP-A

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

79

3-Phase Decanter:
Where it is mainly used:

OIL / FAT
HIGH FFA

BIODIESEL DRYING

TRANSESTERIFICATION 2

TRANSESTERIFICATION 1

CATALYST

SEPARATION

FURTHER
TREATMENT
FOR HIGHER
GLYCERIN
QUALITY

POLISHING
ACID

GLYCERIN / FATTY ACID / POTASSIUM SULPHATE SEPARATION

FATTY ACID
RECYCLING

GLYCERIN

SEPARATION
GLYCERIN
ACIDIFICATION

WASHING

POTASSIUM SULPHATE /
METHANOL SEPARATION

THERMAL DRYING
OF CLEAN FERTILIZER
POTASSIUM SULPHATE

POTASSIUMSULPHATE
WASHING

FURTHER TREATMENT FOR HIGHER GLYCERIN QUALITY


OR PRE-ESTERIFICATION (RE-NEUTRALISATION, THERMAL
PURIFICATION BY EVAPORATION)

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

80

Remember the working Principle of 3-Phase


Separation:
Whats different for Vertical Disc Separators?
Light Phase
Interface

Light Phase Weir

3-Phase
Mixture

Sheets or
Discs
Sedimentation
Tank with 1 x g
or rotating Bowl with
high g-Force
PIERALISI Deutschland GmbH
May 15, 2006

Inlet Barrier
Heavy Phase

Biodiesel Workshop

Sediment

81

Vertical Separator The Race Horse of our


Separation Equipment for:
Low solid concentration in feed
Separation of fine solid particles
Operation with high g-forces > 6000 x g
Good separation perfomance
Increased separation efficiency due to disc
stack

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

82

3-Phase Vertical Separator with manual Discharge


Product in

Non rotating In- and


Outlet Group
Light Phase out

Heavy Phase out

Rotating Bowl
Sediment

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

83

S 300 BD 33
3-Phase Vertical Separator with manual Discharge
How it looks like
One of the most
succesful Biodiesel
machines in the last
three years

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

84

3-Phase Vertical Separator with Manual Discharge:


Where it is mainly used:

OIL / FAT
HIGH FFA

BIODIESEL DRYING

TRANSESTERIFICATION 2

TRANSESTERIFICATION 1

CATALYST

SEPARATION

FURTHER
TREATMENT
FOR HIGHER
GLYCERIN
QUALITY

POLISHING
ACID

GLYCERIN / FATTY ACID / POTASSIUM SULPHATE SEPARATION

FATTY ACID
RECYCLING

GLYCERIN

SEPARATION
GLYCERIN
ACIDIFICATION

WASHING

POTASSIUM SULPHATE /
METHANOL SEPARATION

THERMAL DRYING
OF CLEAN FERTILIZER
POTASSIUM SULPHATE

POTASSIUMSULPHATE
WASHING

FURTHER TREATMENT FOR HIGHER GLYCERIN QUALITY


OR PRE-ESTERIFICATION (RE-NEUTRALISATION, THERMAL
PURIFICATION BY EVAPORATION)

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

85

Manual Discharge
of Solids

PIERALISI Deutschland GmbH


May 15, 2006

Automatic Discharge
of Solids

Biodiesel Workshop

86

3-Phase Vertical Separator with automatic Discharge


Discharge

Production
Product in

Light Phase out


Heavy Phase out

Sediment
Discharge
Operating
Water in
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

87

FPC 12 BD 32
3-Phase Vertical Separator with automatic
Discharge
How it looks like
In operation
since 2003

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

88

3-Phase Vertical Separator with automatic Discharge:


Where it is mainly used:

OIL / FAT
HIGH FFA

BIODIESEL DRYING

TRANSESTERIFICATION 2

TRANSESTERIFICATION 1

CATALYST

SEPARATION

FURTHER
TREATMENT
FOR HIGHER
GLYCERIN
QUALITY

POLISHING
ACID

GLYCERIN / FATTY ACID / POTASSIUM SULPHATE SEPARATION

FATTY ACID
RECYCLING

GLYCERIN

SEPARATION
GLYCERIN
ACIDIFICATION

WASHING

POTASSIUM SULPHATE /
METHANOL SEPARATION

THERMAL DRYING
OF CLEAN FERTILIZER
POTASSIUM SULPHATE

POTASSIUMSULPHATE
WASHING

FURTHER TREATMENT FOR HIGHER GLYCERIN QUALITY


OR PRE-ESTERIFICATION (RE-NEUTRALISATION, THERMAL
PURIFICATION BY EVAPORATION)

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

89

Whats left? The two Clarification Jobs:


Final polishing,

CATALYST

OIL / FAT
HIGH FFA

vertical clarifier

B IO D IE S E L D RY IN G

T R A N S E S T E R IF IC AT IO N 2

T R A N S E S T E R IF IC AT IO N 1

typically by
with manual
discharge.
Pre-drying of

SEPARATION

FURTHER
TREATMENT
FOR HIGHER
GLYCERIN
QUALITY

POLISHING
ACID

GLYCERIN / FATTY ACID / POTASSIUM SULPHATE SEPARATION

FATTY ACID
RECYCLING

GLYCERIN

SEPARATION
GLYCERIN
ACIDIFICATION

POTASSIUMSULPHATE
WASHING

WASHING

sulphate after

POTASSIUM SULPHATE /
METHANOL SEPARATION

washing typically
THERMAL DRYING
OF CLEAN FERTILIZER
POTASSIUM SULPHATE

FURTHER TREATMENT FOR HIGHER GLYCERIN QUALITY


OR PRE-ESTERIFICATION (RE-NEUTRALISATION, THERMAL
PURIFICATION BY EVAPORATION)

PIERALISI Deutschland GmbH


May 15, 2006

potassium

Biodiesel Workshop

by regular
gastight
decanter.
90

Typical Decanter Flow Chart for Ex-proof Installations


Sperrgas fr ZulaufrohrDichtung/
Inert blanketing
feed pipe sealing

314.1

PV 220.4

315.1

317.1

224

Inert gas,
max. 6 bar

Sperrgas fr Wellendichtung
hintere Nabe/
Inert gas blanketing
small hub sealing
Sperrgas fr Wellendichtung
vordere Nabe/
Inert gas blanketing
big hub sealing

VENT

Druckberwachung Gehuse
Pressure supervision of casing

P 220.3

314.1
316.1
FLC 224.1

Inertgassplung
ber Zulaufrohr /
Inert gas pre-purging
via feed pipe

FIS 220.2

318.1

FLC 220.1

ZST 710

ZST 709
ST 701

TT 704
CV 318.1a

PRODUCT IN

PV 224.2

ST 702

Local control board


start
stop inerted
stop not inerted
stand by
production
alarm reset
lamp test

DECANTER FP 600 2 RS

220

PRODUCT IN

pre-purging
stop inerted
stop not inerted
stand by
production
common alarm

start
stand still inerted
stand still not inerted

emergency stop

Control board with


PLC

TT 711

SAFE AREA

FLC 221.1

FLC 222.1

FLC 223.1
LS 223.2

M 223.3

LIGHT LIQUID PHASE

DRAIN
HEAVY LIQUID PHASE

M 705

SOLIDS

TT 706

Nitrogene

221

222

223

VENT

Screw conveyor

Lieferumfang Pieralisi
Pieralisi scope of supply:

LS 222.4

LS 221.4

LS 222.3

LS 221.3

LS 222.2

LS 221.2

221.1
P 221.6

V 222.5

CV 221.6

Espey MultiChamber-Seal

V 221.5

222.1
P 222.6

PIERALISI Deutschland GmbH


May 15, 2006

CV 222.6

Biodiesel Workshop

91

Inertgassplung
ber Zulaufrohr /
Inert gas pre-purging
via feed pipe

ZONE 1

Druckberwachung
Gehuse
Pressure supervision
of casing

Local control board


Control board with
PLC

start
stop inerted
stop not inerted
stand by
production
alarm reset
lamp test

pre-purging
stop inerted
stop not inerted
stand by
production
common alarm
start
stand still inerted
stand still not inerted

316.1

Inertgas-Beschleierung /
Inertgas blanketing

314.1

Inertgassplung
Getriebe /
Inert gas pre-purging
to gearbox

315.1

emergency stop

SAFE AREA

Typical Flow Chart for Separator


with Manual Solid Discharge
for Ex-proof Installations
PIERALISI Deutschland GmbH
May 15, 2006

Biodiesel Workshop

92

221.2

FIS 221.4

PRODUKT EIN/
PRODUCT IN
V 221.3

V 220.5

V 220.3

220.2

PV 220.4

P 220.6

CV 221.7

PCV 221.5

Siphon/
Syphon
1300 mm

Inert gas,
max. 6 bar
PV 221.6

G 221.2

316

221.1

220.1

FLC 316.1

314

FLC 221.1

FLC 220.1

V 320.2

G 220.2

SPLANSCHLUSS F R
M AN. SPLUNG /
M AN. FLUSHING
CO NNEC TION

SCHWERE PHASE
EIN (WASSER)
HEAVY PHASE IN
(WATER)
320

FLC 318.1

315

PV 320.1

Druckberwachung Gehuse
Pressure supervision of casing

FLC 314.1

Inertgas-Beschleierung /
Inertgas blanketing

FLC 315.1

Inertgassplung Getriebe /
Inert gas pre-purging to gearbox

221

220

ZONE 1

SV 220.5a

Control board with


PLC

SV 320.1a
S 114.7

PCV.114.6

222

114.2
STEUERWASSER
EIN/
OPERATING
WATER IN

Inertgassplung
ber Zulaufrohr /
Inert gas pre-purging
via feed pipe

SV 221.6a
PCV 221.5

FLC222.1

SV 114.1a
PV 114.1

114.1

FLC 114.3

114
G 222.3

OLT 114.5 P 114.4

Local control board


pre-purging
stop inerted
stop not inerted
stand by
production
discharge
common alarm

start
stand still inerted
stand still not inerted

FLC 310.1

FLC 223.1

FLC 401.1

emergency stop

DN 25

PV 223.6

DN 50

V 412.1
LS 222.6

Lieferumfang Pieralisi
Pieralisi scope of supply:

SAFE AREA

start
stop inerted
stop not inerted
stand by
production
manual discharge
alarm reset
lamp test

222.1

310

223

410

LS 223.2

LS 223.3

Enlftung/
Vent

STEUERLUFT/
COMPRESSED AIR
V 222.2

V 114.2

SCHLAMM AUSTRAG/
SLUDGE OUT LET

TT 901

Zwischenbehlter,
ca. 300 - 400 l/
Intermediat tank

LS 222.5

WASSER ZUM
WASSERSCHLOSS/
WATER FOR SEAL
POT UNIT

Typical Flow Chart for Separator


with Automatic Solid Discharge

LS 222.4

222.2
V 222.10

P 222.8
V 222.7

PV 223.4

223.2

CV 222.9

SCHWERE PHASE +
STEUERWASSER/
HEAVY PHASE +
OPERATING WATER

In Ex-proof Installations

Zum Feststoffsammelbehlter

P 223.5

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

93

Type Size Process Version Execusion

The PIERALISI Vertical


Separators

200

BD

300

BD

300

BD

300

BD

FPC

12

BD

FPC

18

BD

Design

A Summary:

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

94

Operation Modes of gastight Machines


STAND STILL
INERTED

STAND STILL
NON-INERTED

PRE-PURGING

START

POWER ON
*1)

STOP INERTED

STAND BY

STOP NONINERTED

PRODUCTION
*2)

From all Operation


Modes

EMERGENCY STOP
*2)

Via pre-defined
Alarms

*1)

During regular Operation*:


Transition between 2 Operation Modes by manual command
Transition between 2 Operation Modes by automatic action
Transition between 2 Operation Modes by alarm action
*Certain malfunctions / alarms automatically lead to transition
actions which during regular operation can be chosen manually.

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

95

Examples of Capacities of PIERALISI Centrifuges


for various Applications in Biodiesel Processes
Process

Machine

S 200
S 300

Pre-Esterification Transesterification

Washing

Polishing

Neutralising / Catalyst Removal /


Salt Washing
Methanol/PotasGlycerin/fatty
Separation of Final Polishing
Separation of
Separation of
acid/Potassium- siumsulphate
Biodiesel and of Biodiesel
Triglycerides and Biodiesel and
sulphate separa- separation after
Water after
Glycerin after
Glycerin after
tion for Glycerin washing
Pre-Esterification Transesterification Washing
recovery line
[m3/h]
[m3/h]
[m3/h]
[m3/h]
[m3/h]
[m3/h]
Centrifugal Disc Separators with manual discharge of solids
2-4
3-5
5-8
6 - 12
11 - 15
14 - 20
Centrifugal Disc Separators with automatic discharge of solids

FPC 6
FPC 12
FPC 18

1,5 - 2,5
3-5
7 - 10

2 - 3*
5 - 7*
10 - 14*

3 - 4*
6 - 9*
12 - 16*
Centrifugal Decanters

3-5
8 - 12
15 - 20

Baby 2
FP 600 RS/M
FP 600 2 RS/M
Jumbo 2
Jumbo 3
Jumbo 4
Mammoth 2
Mammoth 3

0,5 - 0,8
1,5 2,5**
2 3**
5 8**
6 10**
10 14**

- 0,5
-2
-2
-4
-6
-6
-9
-9

Remarks:
The capacities in the particular processes may deviate from the figures mentioned in this table!
* Due to absence of solids usually no automatic solid discharge machines are used for this process step
** Capacities achievable with special new design CP-A with adjustable liquid-liquid interface

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

96

References
Biodiesel Reference List (Abstract)

May 2006

Machine

Engineering company (our customer)

Final customer

Decanter Sharples P 3400 3-Phase


Decanter PIERALISI FP 600 2 RS/M 3-Phase
Separator FPC 12 Purifier
Separator FPC 18 Purifier
Separator FPC 18 Purifier
Separator FPC 6 Purifier
Separator FPC 12 Purifier
Separator FPC 12 Purifier
Separator FPC 18 Purifier
Separator S 300 Purifier
Separator FPC 18 Purifier
Separator S 300 Purifier
4 x Separator S 300 Purifier
2 x Separator S 300 Purifier
Separator S 300 Clarifier
Separator S 300 Clarifier
Separator S 300 Clarifier
Separator S 200 Clarifier
Decanter PIERALISI Jumbo 3 3-Phase CP-A
Separator S 300 Purifier
Decanter PIERALISI FP 600 2 RS 3-Phase CP-A
2 x Separator S 300 Purifier
S 300 Purifier
2 x Separator S 300 Purifier

Energea, Austria
Petrotec, Germany
ENA Biodiesel, Austria
Agrar-Technik, Germany
Agrar-Technik, Germany
Petrotec, Germany
Petrotec, Germany
Petrotec, Germany
Energea, Austria
Energea, Austria
Energea, Austria
Energea, Austria
Energea, Austria
Agrar Technik
Agrar Technik
Campa Diesel
Agrar Technik
Agrar Technik
Petrotec
GHP
PTI, Austria
Solvent Dwory
Euroservice
GHP

Energea, Austria
Petrotec, Germany
Elbe l Prignitz, Germany
Biodiesel Kyritz, Kyritz, Germany
Bionet, Spain
Petrotec, Germany
Petrotec, Germany
Petrotec, Germany
Arfuel, Australia I
Arfuel, Australia I
Arfuel, Australia II
Arfuel, Australia II
Biodiesel plant Teeside, UK
Biodiesel plant Brunsbttel, Germany
Biodiesel plant Brunsbttel, Germany
Campa Diesel, Germany
Emmtec Service, Netherlands
Inter-Tram KFT, Hungary
Petrotec, Germany
GHP, Oranienburg, Germany
Biodiesel Zistersdorf
Solvent Dwory, Poland
Euro Service, Poland
GHP, Oranienburg, Germany

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

97

PIERALISI Deutschland GmbH


May 15, 2006

Biodiesel Workshop

98