Process Technology

FrymaKoruma
27. October 2003
Stefan Wienberg
Table of content

• part 1:
Introduction Process Technology Center ProTec
Fields of operation
• part 2:
Emulsions: General information and trial
• part 3:
Gel: General information and trial
• part 4:
Grinding: Aspects and trial
part 1

Presentation of ProTec

•Introduction and Organisation

•Strategy and Service
•Infrastructure
•R & D Activities
 Introduction
ProTec in D-Neuenburg is the centre of competence
within the FrymaKoruma

ProTec is combining the former tasks and demands of

Process Technology Department of Fryma in CH-Rheinfelden
and
ProTec of Koruma GmbH in D-Germany

Our main objective is the wet process technology.

ProTec is the core of all process technology demands within

FrymaKoruma
 Strategy and Service

• Organisation and conducting customer trials in our process laboratory

• Recommendation on new applications, recipes and optimisation of
production methods
• Developing projects in cooperation with customers
• Production and formulation of new specimens
• Coordination of seminars, work shops and instruction of existing and new
customers
• Cooperation with Universities and associations (Hochschulen, DGK)
• Technical publications
• Documentation of process technology
• Cooperation with service department and feed back of field know how
• Process guarantee and test inspection
 Infrastructure
• 200 m2 for trails on FrymaKoruma test units
• 3 independent meeting rooms
• 2 rooms for measurement and analytical tests
• Steam generator, chilled and hot water generators
• Test equipment (under control, supervision and application
by ProTec:
10 process units (for batch size from 7 L up to 160 L)
1 continuous processing plant
7 independent mills
2 Coball mills
2 deareator units
2 scraper heat exchanger

Continuous Improved
 R & D activities of ProTec

Summary of current R & D projects:

• Cooperation with the technical University of Detmold
(pharmaceutical emulsions)
• Cooperation with the workgroup Galenik of the DGK
• Determination of power density, throughput, power
consumption and noise emission of new machines
• Testing of new machines, developed by FrymaKoruma
• Testing of various grinding beats for CoBall-Mills
• Investigations to mill into the sub micron domain
Fields of operation

224 Trials per year (2003) for our

Customers
Chemistry
Pharma /
24%
Healthcare
35%

Food
41%
Fields and applications

•Trials, recommendations, machine´s start up

at customer´s production site worldwide
•Batch production for customers (5..3000kg)
•Analytic for customers (Sympatec, Microscope)
•Scale up and Validation batches
•Developement of recipe and process
Our machines our business
Grinding: ML perforated disc mill
MZ colloid mill (also emulsifying)
MK corundum stone mill
MS Coball mill
Deareation VE dynamic systems
SE static systems
Heat exchange SWT/C scraper heat exchanger
Continuous plants MA
Vacuum processing units
MaxxD, Dinex, Frymix, DisHo, VME, DT
What is a Emulsion?

A emulsion is a meta stable disperse system of

two liquids, which are not soluble in each other.
The emulsions can be divided up into two groups:
1.Oil in water (O/W) emulsions and
2. Water in Oil (W/O) emulsions.
Beside these two mayor groups of emulsions also
more complex emulsion systems are possible
(W/O/W and O/W/O).
O/W emulsion

By dispersion of oil into water the oil

drops are the inner, dispersed phase.
Water is the outer, continuous phase.
Cosmetic / pharma applications -->
removable by water
oil drop

water phase
W/O Emulsion

By dispersion of water into oil the

water drops are the inner, dispersed
phase. Oil is the outer, continuous
phase.
Cosmetic / pharma applications -->
water resistant
Water

Oil
 How can the emulsion be stabilized?
Reduction of the surface tension is the key to avoid the
coagulation of the emulsion.
Substances which reduce the surface tension are called surfactants.
The number of surfactants (emulsifiers) is enormous and
they are divided up into several groups according to their
properties.

Beside O/W or W/O emulsifier surfactants are also used as

anti foaming agent, wetting agent, dispersing agent and
solubilisator.
How does a emulsifier look like?

Hydrophil area Lipophil area

(= lipophob) (= hydrophob)

Emulsifier is solved in the outer phase

Working principle of emulsifier

water

water
oil

oil

W/O O/W
Hydrophil head

Lipophil chain
 Properties supplied by the emulsifier

• Reduction of the surface energy

• Generation of steric and electrostatic inhibitions
(inhibition of coalescence of the drops)
• Inner phase is dispersed under high shear force to
achieve a homogeny monodispers mixture of the drops.
• The drop size of emulsions is typical in a range between
1 and 10 µm (up to 25 µm).
 Process of emulsifying II

Only by applying a polydispers

considerable amounts of
energy a monodispers
distribution of the inner
phase is possible.
This energy is supplied
from our strong rotor /
stator systems in the
processing units. monodispers
Process ofDer
emulsifying III
Emulgierprozeß

ng
Koaleszens

lis e
ru
bi ein
ie
a k
St
Tropfenaufbruch

St
a bi
lisi
er Keine
un
g Koaleszenz

Emulgator Stabilisator Disperse Phase Kontinuierliche Phase

Emulsions:
Different ways of production
Hot/Hot Process
Both, fat- and water-phase are heat up separately to a certain temp. (70 – 85
°C). The hot oil phase and the hot water phase were combined under vacuum
at the high temperature and emulsified. Emulsification is done by the rotor
stator system. Subsequently the product is cooled down.

Hot/Cold Process
The fat phase is heat up to a temp. (app. 10 °C above the highest melting
point of the ingredients). The hot fat phase and the cold water phase were
combined under vacuum and emulsified at the mixing temperature.
Subsequently the product is cooled down.
Advantage: shorter cooling times, saving of energy
Recipe W/O creme, example

Basic Formulation: W/O Cream

Isolan PDI 3,00 %
Tegosoft, fluid 9,50 %
Tegosoft HP 9,50 %
Beewax 0,60 %
Castoroil, hydrog. 0,40 %
Glycerine 3,00 %
Mg SO4 7H2O 0,60 %
Water demineralised 73,4 %
TOTAL 100,0%
Production of a Carbopol gel
Carbopol: Anhydrous, very hygroscopic
polyacrylic acid. Used as thickening agent in
a lot of different formulations. Carbopol can
build clear, high viscose gels.
Available in pharma grade.
Recipe:
Water, demineralised 97,75 %
Carbopol f.e. 940NF or 980NF 1,50 %
Sodium hydroxide (18%) 0,75 %
Imagination of Structure of Polyacrylic Acid
Grinding Process with MK 95 and MS 18

Recipe Percentage
Vaselinum album 88
Salicylic Acid 8
Benzoic Acid 4
Aspects of Grinding

•Particle
•Reactor
•Energy
•Transfer
•Medium
Evaluation of grinding process
Discussion of both Technologies:
Easy methode and equipement
MK Heat introduction
Particle distribution

More equipement
MS Less heat introduction
Better particle distribution
 Practical presentation:

Production of: Machine

Carbopol gel Dinex 200
W/O Emulsion (h/c-process) MaxxD
Toothpaste, opake Dinex 200

Grinding Process: Machine

Salicylic and Benzoic Acid, MK 95 &
dispersed in Vaselinum album MS 18
 Toothpaste
Raw materials Percentage
SIDENT 9 (SiO2) 14
SIDENT 22S (SiO2) 8
Sorbitol, 70% 47
Water, demineralized 23,43
Polyethylenglycol 400 3
Sodium Laurylsulfate 1,2
NaCMC (7MCF) 1,2
Optamint # 757637 0,8
Paraffinoil 0,5
Titanium Dioxide 0,4
Sodium Fluorid 0,22
Methylparabene 0,15
Saccharin Na 0,1
Total 100