Process Technology

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Process Technology

• FrymaKoruma
• 27. October 2003
• Stefan Wienberg

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Table of content

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

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part 1Presentation of ProTec

• Introduction and Organisation
• Strategy and Service
• Infrastructure
• R D Activities

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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
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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

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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
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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

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Fields of operation
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Fields and applications

• Trials, recommendations, machines start up
• at customers production site worldwide
• Batch production for customers (5..3000kg)
• Analytic for customers (Sympatec, Microscope)
• Scale up and Validation batches
• Developement of recipe and process

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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
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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
  alsomore complex emulsion systems are possible
  (W/O/W and O/W/O).

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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 --gt
• removable by water

oil drop
water phase
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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 --gt
• water resistant

Water
Oil
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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.
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How does a emulsifier look like?
Emulsifier is solved in the outer phase
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Working principle of emulsifier
water
water
oil
oil
W/O
O/W
Hydrophil head
Lipophil chain
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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).

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Process of emulsifying II
polydispers
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.
monodispers
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Process of emulsifying III
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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
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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
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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
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Imagination of Structure of Polyacrylic Acid
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Grinding Process with MK 95 and MS 18
Recipe Percentage Vaselinum album 88 Salicylic
Acid 8 Benzoic Acid 4
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Aspects of Grinding

• Particle
• Reactor
• Energy
• Transfer
• Medium

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Evaluation of grinding process
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Discussion of both Technologies
Easy methode and equipement Heat
introduction Particle distribution
MK
More equipement Less heat introduction Better
particle distribution
MS
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Practical presentation
Production of Machine Carbopol gel Dinex
200 W/O Emulsion (h/c-process) MaxxD Toothpaste,
opake Dinex 200 Grinding Process Machine Sal
icylic and Benzoic Acid, MK 95 dispersed in
Vaselinum album MS 18
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Toothpaste