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Pro cess Tec hnology. 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.
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ProcessTechnology 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 1Presentation 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 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 DeareationVE dynamic systems SE static systems Heat exchangeSWT/C scraper heat exchanger Continuous plantsMA 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: • 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).
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.
Hydrophil area (= lipophob) Lipophil area (= hydrophob) How does a emulsifier look like? 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 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
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 %
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
Discussion of both Technologies: Easy methode and equipement Heat introduction Particle distribution MK More equipement Less heat introduction Better particle distribution MS
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