1. FrymaKoruma 27. October 2003 Stefan Wienberg
Process Technology
FrymaKoruma
27. October 2003
Stefan Wienberg

2. 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

3. part 1 Presentation of ProTec
Introduction and Organisation
Strategy and Service
Infrastructure
R & D Activities

4. 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

5. 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

6. 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

7. 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

8. Fields of operation

9. Fields and applications
Trials, recommendations, machine´s start up
at customer´s production site worldwide
Batch production for customers ( kg)
Analytic for customers (Sympatec, Microscope)
Scale up and Validation batches
Developement of recipe and process

10. 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

11. 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:
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).

12. 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

13. 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

14. 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.

15. How does a emulsifier look like?
Lipophil area
(= hydrophob)
Hydrophil area
(= lipophob)
Emulsifier is solved in the outer phase

16. Working principle of emulsifier
water
water
oil
oil
W/O
O/W
Hydrophil head
Lipophil chain

17. 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 and 10 µm (up to 25 µm).

18. Process of emulsifying II
Only by applying a 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.
polydispers
monodispers

19. Process of emulsifying III

20. 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

21. 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 ,0%

23. 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 %

24. Imagination of Structure of Polyacrylic Acid

26. Grinding Process with MK 95 and MS 18
Recipe Percentage
Vaselinum album 88
Salicylic Acid 8
Benzoic Acid 4

27. Aspects of Grinding
Particle
Reactor
Energy
Transfer
Medium

28. Evaluation of grinding process

29. MK MS Discussion of both Technologies: Easy methode and equipement
Heat introduction
Particle distribution MK
More equipement
Less heat introduction
Better particle distribution MS

30. 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

31. Toothpaste