pro cess tec hnology frymakoruma 27. october 2003 stefan wienberg
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Process Technology
FrymaKoruma27. October 2003Stefan 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
IntroductionProTec in D-Neuenburg is the centre of competence within the FrymaKoruma
ProTec is combining the former tasks and demands ofProcess Technology Department of Fryma in CH-RheinfeldenandProTec 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
Continuous Improved
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 plant7 independent mills2 Coball mills2 deareator units2 scraper heat exchanger
R & D activities of ProTec
• 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
Summary of current R & D projects:
Fields of operation
224 Trials per year (2003) for our Customers
Chemistry24%
Food41%
Pharma / Healthcare
35%
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 millMZ colloid mill (also emulsifying)MK corundum stone mill MS Coball mill
Deareation VE dynamic systemsSE static systems
Heat exchange SWT/C scraper heat exchanger
Continuous plants MA
Vacuum processing unitsMaxxD, 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.
1.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).
The emulsions can be divided up into two groups:
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 resistantWater
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
oil
wateroil
W/O O/WHydrophil head
Lipophil chain
water
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 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
polydispers
Process of emulsifying III
Emulsions: Different ways of production
Hot/Hot ProcessBoth, 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 ProcessThe 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 CreamIsolan 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%
Scraper: 30rpm Agitator: 30rpm for the whole process
Heating of fat phase onto 75 °C,then feed in Main vessel, run homogenizer
600rpm and keep on temperaturePreparation of water phase
Feed water phase slightly in Main vesselVacuum 700mbar
Homogenizer 3000 rpm
Homogenization 3000 rpm; Vacuum 700mbar
Cooling downto 40 °CHomogenizer interval: Run 1500rpm 30s
Pause 150s
Feed additives + parfume,Temperature 40°C; Vacuum 700mbar
Homogenizer 3000 rpm
Preparation of additives, parfume
Homogenization 3000 rpm; 60sTemperature 40 °C; Vacuum 700mbar
Process Diagram Of W/O - Cream Production On Dinex
Deaeration;Temperature 40 °C; Vacuum 50 mbar
Discharge;Temperature 40 °C
Homogenizer 1000 rpm
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
Feed of water phaseVacuum 700mbar
Preparation of Carbopol Powder
Feed powder phase slightly in Main vesselTemperature 5..30°C; Vacuum 700mbar
Homogenizer on dispersation mode 3000 rpm
HomogenizationTemperature 5..30 °C; Vacuum 700mbar
Homogenizer on dispersation mode 3000 rpm30s
Feed additivesHomogenizer on dispersation mode 3000 rpm
Vacuum 700mbar
Preparation of additives
HomogenizationHomogenizer on dispersation mode 3000 rpm
Vacuum 700mbar
Process Diagram Of Carbopol Gel Production At Dinex
Feed NeutralisatorHomogenizer on pump mode 1500 rpm
Vacuum 700mbar
Preparation of Neutralisator (SodiumHydroxid or Triethanolamin)
HomogenizationHomogenizer on pump mode 1500 rpm
Vacuum 700mbar
DischargeHomogenizer on pump mode 1000 rpm
Recipe PercentageVaselinum album 88Salicylic Acid 8Benzoic Acid 4
Grinding Process with MK 95 and MS 18
Aspects of Grinding
•Particle•Reactor•Energy•Transfer •Medium
Evaluation of grinding process
Discussion of both Technologies:
Easy methode and equipementHeat introductionParticle distribution
MK
MSMore equipementLess heat introductionBetter particle distribution
Practical presentation:
Production of: MachineCarbopol gel Dinex 200W/O Emulsion (h/c-process) MaxxDToothpaste, opake Dinex 200
Grinding Process: MachineSalicylic and Benzoic Acid, MK 95 &dispersed in Vaselinum album MS 18
Raw materials Percentage
SIDENT 9 (SiO2) 14
SIDENT 22S (SiO2) 8
Sorbitol, 70% 47Water, demineralized 23,43Polyethylenglycol 400 3Sodium Laurylsulfate 1,2NaCMC (7MCF) 1,2Optamint # 757637 0,8Paraffinoil 0,5Titanium Dioxide 0,4Sodium Fluorid 0,22Methylparabene 0,15Saccharin Na 0,1Total 100
Toothpaste
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