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