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 24% Pharma / Healthcare 35%

Food 41%

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

Our machines our business

Grinding:
ML perforated disc mill MZ colloid mill (also emulsifying) MK corundum stone mill MS Coball mill VE dynamic systems SE static systems SWT/C scraper heat exchanger

Deareation
Heat exchange

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

Water

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

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 (= lipophob)

Lipophil area (= hydrophob)

Emulsifier is solved in the outer phase

Working principle of emulsifier

water

water

oil

oil

W/O
Hydrophil head Lipophil chain

O/W

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 m (up to 25 m).

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

Process ofDer emulsifying III Emulgierproze

k bi ein lis e ie ru ng

Koaleszens

Tropfenaufbruch
St a

St a

bi li

si

er un g

Keine 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 Tegosoft, fluid Tegosoft HP Beewax Castoroil, hydrog. Glycerine Mg SO4 7H2O Water demineralised 3,00 % 9,50 % 9,50 % 0,60 % 0,40 % 3,00 % 0,60 % 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 Carbopol f.e. 940NF or 980NF Sodium hydroxide (18%) 97,75 % 1,50 % 0,75 %

Imagination of Structure of Polyacrylic Acid

Grinding Process with MK 95 and MS 18

Recipe Vaselinum album Salicylic Acid Benzoic Acid Percentage 88 8 4

Aspects of Grinding

Particle Reactor Energy Transfer Medium

Evaluation of grinding process

Discussion of both Technologies:

MK
MS

Easy methode and equipement Heat introduction Particle distribution

More equipement Less heat introduction Better particle distribution

Practical presentation:
Production of: Carbopol gel W/O Emulsion (h/c-process) Toothpaste, opake Machine Dinex 200 MaxxD Dinex 200

Grinding Process: Machine Salicylic and Benzoic Acid, MK 95 & dispersed in Vaselinum album MS 18

Toothpaste
Raw materials SIDENT 9 (SiO2) SIDENT 22S (SiO2) Sorbitol, 70% Water, demineralized Polyethylenglycol 400 Sodium Laurylsulfate NaCMC (7MCF) Optamint # 757637 Paraffinoil Titanium Dioxide Sodium Fluorid Methylparabene Saccharin Na Total Percentage 14 8 47 23,43 3 1,2 1,2 0,8 0,5 0,4 0,22 0,15 0,1 100