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MICROENCAPSULATIO
N
Microencapsulation:

Definition: It is the process by which individual particles
  or droplets of solid or liquid material (the core) are
  surrounded or coated with a continuous film of
  polymeric material (the shell) to produce capsules in the
  micrometer to millimetre range, known as
  microcapsules.
Microencapsulation
(Cont.):
Morphology of Microcapsules:
The morphology of microcapsules depends mainly on the core
material and the deposition process of the shell.

1- Mononuclear      (core-shell) microcapsules contain the shell around
the core.

2- Polynuclear capsules have many cores enclosed within the shell.

3- Matrix encapsulation          in which the core material is distributed
homogeneously into the shell material.
- In addition to these three basic morphologies, microcapsules can
also be mononuclear with multiple shells, or they may form clusters of
microcapsules.
Morphology of Microcapsules (Cont.):
Microencapsulation
(Cont.):
Coating material properties:
•Stabilization of core material.
•Inert toward active ingredients.
•Controlled release under specific conditions.
•Film-forming, pliable, tasteless, stable.
•Non -hygroscopic, no high viscosity, economical.
•Soluble in an aqueous media or solvent, or melting.
•The coating can be flexible, brittle, hard, thin etc.
Microencapsulation
(Cont.):
Coating materials:

  Gums: Gum arabic, sodium alginate, carageenan.

  Carbohydrates:    Starch, dextran, sucrose

  Celluloses:   Carboxymethylcellulose, methycellulose.

  Lipids Bees wax, stearic acid, phospholipids.
  :
  Proteins: Gelatin, albumin.
Microencapsulation
(Cont.):
Benefits of Microencapsulation:
1- microorganism and enzyme immobilization.
- Enzymes have been encapsulated in cheeses to accelerate ripening
and flavor development.
The encapsulated enzymes are protected from low pH and high ionic
strength in the cheese.
• The encapsulation of microorganisms has been used to improve
stability     of     starter
cultures.
Benefits of Microencapsulation (Cont.):


2-Protection against UV, heat, oxidation, acids, bases (e.g.colorants
    and vitamins).
e.g. Vitamin       A     /    monosodium
      glutamate
appearance (white)
protection (water, T,
ligth)
3- Improved shelf life due to preventing degradative reactions
    (dehydration, oxidation).
4-Masking of taste or odours.
5- Improved processing, texture and less wastage of ingredients.
    - Control of hygroscopy
    - enhance flowability and dispersibility
    - dust free powder
    - enhance solubility
Benefits of Microencapsulation (Cont.):


6-Handling liquids as solids
7-There is a growing demand for nutritious foods for
   children which provides them with much needed
   vitamins and minerals during the growing age.
Microencapsulation could deliver the much needed
   ingredients in children friendly and tasty way.
8- Enhance visual aspect and marketing concept.
Benefits of Microencapsulation (Cont.):


9- Carbonless copy paper was the first marketable product to employ
   microcapsules . A coating of microencapsulated colorless ink is
   applied to the top sheet of paper, and a developer is applied to
   the subsequent sheet. When pressure is applied by writing, the
   capsules break and the ink reacts with the developer to produce
   the dark color of the copy.
Benefits of Microencapsulation (Cont.):


10-Today's textile industry makes use of microencapsulated materials
   to enhance the properties of finished goods.               One application
   increasingly utilized is the incorporation of microencapsulated
   phase change materials (PCMs).
 Phase change materials absorb and release heat in response to
   changes in environmental temperatures. When temperatures rise,
   the phase change material melts, absorbing excess heat, and feels
   cool. Conversely, as temperatures fall, the PCM releases heat as
   solidifies, and feels warm.
   it
This property of microencapsulated phase change materials can be
   harnessed to increase the comfort level for users of sports
   equipment, clothing, building materials, etc.
Benefits of Microencapsulation (Cont.):


11- Pesticides     are encapsulated to be released over
  time, allowing farmers to apply the pesticides less
  amounts than requiring very highly concentrated and
  toxic initial applications followed by repeated
  applications to combat the loss of efficacy due to
  leaching, evaporation, and degradation.
Benefits of Microencapsulation
(Cont.):

12- Ingredients in foods are encapsulated for several
  reasons.
   Most flavorings are volatile; therefore encapsulation of
  these components extends the shelf-life of these
  products.
   Some ingredients are encapsulated to mask taste,
  such as nutrients added to fortify a product without
  compromising the product’s intended taste.
   Alternatively, flavors are sometimes encapsulated to
  last longer, as in chewing gum.
Benefits of Microencapsulation
(Cont.):

13- Controlled and targetted release of active ingredients.
   Many varieties of both oral and injected pharmaceutical
   formulations are microencapsulated to release over longer periods
   of time or at certain locations in the body.
   Aspirin, for example, can cause peptic ulcers and bleeding if doses
   are introduced all at once. Therefore aspirin tablets are often
   produced by compressing quantities of microcapsules that will
   gradually release the aspirin through their shells, decreasing risk of
   stomach damage.

14- Microencapsulation allows mixing of incompatible compounds.
Microencapsulation
   Technologies
Microencapsulation processes with their
           relative particle size ranges.

     Physico - Chemical             Physico - mechanical
         Processes                       Processes
  Coacervation (2 – 1200 um)       Spray-drying (5 – 5000 um)
Polymer-polymer incompatibility     Fluidized- bed technology
        (0.5 – 1000 um)                   (20 – 1500 um)
      Solvent evaporation          Pan coating (600 – 5000 um)
        (0.5 – 1000 um)
 Encapsulation by supercritical    Spinning disc (5 – 1500 um)
               fluid


                                           Co-extrusion
Encapsulation by Polyelectrolyte         (250 – 2500 um)
   multilayer (0.02 – 20 um)
Microencapsulation processes with their
     relative particle size ranges (cont.).

     Physico-Chemical                    Chemical Processes
     Processes (cont.)
    Hydrogel microsphere Interfacial polymerization
                                               (0.5 – 1000 um)


Phase Inversion   (0.5 — 5.0 um)           In situ polymerization
                                              (0.5 – 1100 um)


    Hot Melt (1 — 1000 um)
Microencapsulation Techniques
(Cont.):

I. Physico-Chemical Processes:
1- Coacervation:
- Two methods for coacervation are available, namely
   simple and complex processes.

-In simple coacervation , a desolvation agent is added for
   phase separation.

- Whereas complex coacervation     involves complexation
   between two oppositely charged polymers.
1-                 Coacervation
(Cont.):

Complex coacervation:
1- First the core material (usually an oil) is dispersed into
   a polymer solution (e.g., a cationic aqueous polymer,
   gelatin).
2- The second polymer (anionic, water soluble, gum
   arabic) solution is then added to the prepared
   dispersion.
3- Deposition of the shell material onto the core particles
   occurs when the two polymers form a complex.
4-This process is triggered by the addition of salt or by
   changing the pH, temperature or by dilution of the
   medium.
1-               Coacervation
 (Cont.):
5- Finally, the prepared microcapsules are stabilized by
   crosslinking (with formaldehyde), desolvation or
   thermal treatment.
   Complex coacervation is used
to produce microcapsules containing
fragrant oils, liquid crystals, flavors,
dyes or inks as the core material.
Microencapsulation Techniques
(Cont.):

2- Polymer-polymer incompatibility:
 - Also called phase separation.
1- This method utilizes two polymers that are soluble in
   a common solvent, yet do not mix with one another
   in the solution.

2- The polymers form two separate phases, one rich in
   the polymer intended to form the capsule walls, the
   other rich in the incompatible polymer meant to
   induce the separation of the two phases. The second
   polymer is not intended to be part of the finished
   microcapsule wall.
Microencapsulation Techniques
(Cont.):

3- Solvent Evaporation:
 - It is the most extensively used method of microencapsulation.
1-Prepare an aqueous solution of the drug (may contain a viscosity
    building or stabilizing agent)
2- Then added to an organic phase consisting of the polymer
    solution in solvents like dichloromethane or chloroform with
    vigorous stirring to form the primary water in oil emulsion.
3- This emulsion is then added to a large volume of water containing
    an emulsifier like PVA or PVP to form the multiple
    (w/o/w).
    emulsion
4- The double emulsion is then subjected to stirring until most of the
    organic solvent evaporates, leaving solid microspheres.
5- The microspheres can then be washed and dried.
Microencapsulation Techniques
(Cont.):

4- Polymer Encapsulation by Rapid Expansion of
   Supercritical Fluids:
- Supercritical fluids are highly compressed gasses that
   possess several properties of both liquids and gases.
- The most widely used being supercritical CO2 and
   nitrous oxide (N2O).
- A small change in temperature or pressure causes a
   large change in the density of supercritical fluids   .
Polymer Encapsulation by Rapid
     Expansion of Supercritical Fluids
     (Cont.):

Steps
:
1-Supercritical fluid containing the active ingredient and the shell
   material are maintained at high pressure and then released at
   atmospheric pressure through a small nozzle.

2-The sudden drop in pressure causes desolvation of the shell
   material, which is then deposited around the active ingredient
   (core) and forms a coating layer.

-Different core materials such as pesticides, pigments, vitamins,
   flavors, and dyes are encapsulated using this method.
-A wide variety of shell materials e.g. paraffin wax and polyethylene
   glycol are used for encapsulating core substances.
-The disadvantage of this process is that both the active ingredient
   and the shell material must be very soluble in supercritical fluids.
Microencapsulation by rapid expansion of
          supercritical solutions
Microencapsulation
                Techniques (Cont.):
 5- Hydrogel microspheres:
1- Microspheres made of gel-type polymers, such as alginate, are
produced by dissolving the polymer in an aqueous solution
2-Then, suspending the active ingredient in the mixture
3- Extruding through a precision device, producing micro droplets
4- Then fall into a hardening bath that is slowly stirred. The hardening
bath usually contain calcium chloride solution.

Advantage: The method involves an           all -aqueous     system and avoids
residual solvents in microspheres.

The particle size of microspheres can be controlled by:
A- using various size extruders or     B- by varying the polymer solution flow
rates.
Hydrogel
microspheres
Microencapsulation Techniques
    (Cont.):

II Physical Processes:
1- Spray-Drying & spray-congealing :
-    Microencapsulation by spray-drying is a low-cost commercial
     process which is mostly used for the encapsulation of fragrances,
     oils and flavors.
Steps
:
1- Core particles are dispersed in a polymer solution and sprayed into
     a hot chamber.

2- The shell material solidifies onto the core particles as the solvent
   evaporates.

- The microcapsules obtained are of polynuclear or matrix type.
micro-encapsulation by spray-drying.
Spray drying
Microencapsulation Techniques
(Cont.):

Spray-congealing:
- This technique can be accomplished with spray
   drying equipment when the protective coating is
   applied as a melt.
1- the core material is dispersed in a coating material
   melt.
2- Coating solidification (and microencapsulation) is
   accomplished by spraying the hot mixture into a cool
   air stream.
- e.g. microencapsulation of vitamins with digestable
   waxes for taste masking.
Microencapsulation Techniques
(Cont.):

2- Fluidized-Bed Technology:
- Different types of fluid-bed coaters include top spray, bottom
    spray, and tangential spray.
- used for encapsulating solid or liquids absorbed into porous
    particles.
Steps
:
1-Solid particles to be encapsulated are suspended on a jet of air
   and then covered by a spray of liquid coating material.

2- The rapid evaporation of the solvent helps in the formation of an
   outer layer on the particles.

3- This process is continued until the desired thickness and weight
   is obtained.
Schematics of a fluid-bed coater.
         (a) Top spray;
       (b) bottom spray;
      (c) tangential spray
Fluid-bed coater
Microencapsulation Techniques
(Cont.):

3- Pan coating:
1- Solid particles are mixed with a dry coating
material.
2- The temperature is raised so that the coating material melts and
encloses the core particles, and then is solidified by cooling        .

Or, the coating material can be gradually applied to core particles
tumbling in a vessel rather than being wholly mixed with the core
particles from the start of encapsulation.
Pan coating:
Microencapsulation Techniques
(Cont.):

4- Co-Extrusion:
1- A dual fluid stream of liquid core and shell materials is
   pumped through concentric tubes and forms droplets
   under the influence of vibration.
2-The shell is then hardened by chemical cross linkings,
   cooling, or solvent evaporation.
- Different types of extrusion nozzles have been
   developed in order to optimize the process
Schematic presentation of the Co-extrusion process
Co-extrusion Process
Microencapsulation Techniques
 (Cont.):

 5- Spinning Disk:
Steps
 :
:
1- Suspensions of core particles in liquid shell material are poured into
a rotating disc.
2- Due to the spinning action of the disc, the core particles become
coated with the shell material.
3- The coated particles are then cast from the edge of the disc by
centrifugal force.
4- After that the shell material is solidified by external means (usually
cooling).
 - This technology is rapid, cost-effective, relatively simple and has
high production efficiencies.
Microencapsulation by spinning disc
Microencapsulation

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Microencapsulation

  • 2. Microencapsulation: Definition: It is the process by which individual particles or droplets of solid or liquid material (the core) are surrounded or coated with a continuous film of polymeric material (the shell) to produce capsules in the micrometer to millimetre range, known as microcapsules.
  • 3. Microencapsulation (Cont.): Morphology of Microcapsules: The morphology of microcapsules depends mainly on the core material and the deposition process of the shell. 1- Mononuclear (core-shell) microcapsules contain the shell around the core. 2- Polynuclear capsules have many cores enclosed within the shell. 3- Matrix encapsulation in which the core material is distributed homogeneously into the shell material. - In addition to these three basic morphologies, microcapsules can also be mononuclear with multiple shells, or they may form clusters of microcapsules.
  • 5. Microencapsulation (Cont.): Coating material properties: •Stabilization of core material. •Inert toward active ingredients. •Controlled release under specific conditions. •Film-forming, pliable, tasteless, stable. •Non -hygroscopic, no high viscosity, economical. •Soluble in an aqueous media or solvent, or melting. •The coating can be flexible, brittle, hard, thin etc.
  • 6. Microencapsulation (Cont.): Coating materials: Gums: Gum arabic, sodium alginate, carageenan. Carbohydrates: Starch, dextran, sucrose Celluloses: Carboxymethylcellulose, methycellulose. Lipids Bees wax, stearic acid, phospholipids. : Proteins: Gelatin, albumin.
  • 7. Microencapsulation (Cont.): Benefits of Microencapsulation: 1- microorganism and enzyme immobilization. - Enzymes have been encapsulated in cheeses to accelerate ripening and flavor development. The encapsulated enzymes are protected from low pH and high ionic strength in the cheese. • The encapsulation of microorganisms has been used to improve stability of starter cultures.
  • 8. Benefits of Microencapsulation (Cont.): 2-Protection against UV, heat, oxidation, acids, bases (e.g.colorants and vitamins). e.g. Vitamin A / monosodium glutamate appearance (white) protection (water, T, ligth) 3- Improved shelf life due to preventing degradative reactions (dehydration, oxidation). 4-Masking of taste or odours. 5- Improved processing, texture and less wastage of ingredients. - Control of hygroscopy - enhance flowability and dispersibility - dust free powder - enhance solubility
  • 9. Benefits of Microencapsulation (Cont.): 6-Handling liquids as solids 7-There is a growing demand for nutritious foods for children which provides them with much needed vitamins and minerals during the growing age. Microencapsulation could deliver the much needed ingredients in children friendly and tasty way. 8- Enhance visual aspect and marketing concept.
  • 10. Benefits of Microencapsulation (Cont.): 9- Carbonless copy paper was the first marketable product to employ microcapsules . A coating of microencapsulated colorless ink is applied to the top sheet of paper, and a developer is applied to the subsequent sheet. When pressure is applied by writing, the capsules break and the ink reacts with the developer to produce the dark color of the copy.
  • 11. Benefits of Microencapsulation (Cont.): 10-Today's textile industry makes use of microencapsulated materials to enhance the properties of finished goods. One application increasingly utilized is the incorporation of microencapsulated phase change materials (PCMs). Phase change materials absorb and release heat in response to changes in environmental temperatures. When temperatures rise, the phase change material melts, absorbing excess heat, and feels cool. Conversely, as temperatures fall, the PCM releases heat as solidifies, and feels warm. it This property of microencapsulated phase change materials can be harnessed to increase the comfort level for users of sports equipment, clothing, building materials, etc.
  • 12. Benefits of Microencapsulation (Cont.): 11- Pesticides are encapsulated to be released over time, allowing farmers to apply the pesticides less amounts than requiring very highly concentrated and toxic initial applications followed by repeated applications to combat the loss of efficacy due to leaching, evaporation, and degradation.
  • 13. Benefits of Microencapsulation (Cont.): 12- Ingredients in foods are encapsulated for several reasons. Most flavorings are volatile; therefore encapsulation of these components extends the shelf-life of these products. Some ingredients are encapsulated to mask taste, such as nutrients added to fortify a product without compromising the product’s intended taste. Alternatively, flavors are sometimes encapsulated to last longer, as in chewing gum.
  • 14. Benefits of Microencapsulation (Cont.): 13- Controlled and targetted release of active ingredients. Many varieties of both oral and injected pharmaceutical formulations are microencapsulated to release over longer periods of time or at certain locations in the body. Aspirin, for example, can cause peptic ulcers and bleeding if doses are introduced all at once. Therefore aspirin tablets are often produced by compressing quantities of microcapsules that will gradually release the aspirin through their shells, decreasing risk of stomach damage. 14- Microencapsulation allows mixing of incompatible compounds.
  • 15. Microencapsulation Technologies
  • 16. Microencapsulation processes with their relative particle size ranges. Physico - Chemical Physico - mechanical Processes Processes Coacervation (2 – 1200 um) Spray-drying (5 – 5000 um) Polymer-polymer incompatibility Fluidized- bed technology (0.5 – 1000 um) (20 – 1500 um) Solvent evaporation Pan coating (600 – 5000 um) (0.5 – 1000 um) Encapsulation by supercritical Spinning disc (5 – 1500 um) fluid Co-extrusion Encapsulation by Polyelectrolyte (250 – 2500 um) multilayer (0.02 – 20 um)
  • 17. Microencapsulation processes with their relative particle size ranges (cont.). Physico-Chemical Chemical Processes Processes (cont.) Hydrogel microsphere Interfacial polymerization (0.5 – 1000 um) Phase Inversion (0.5 — 5.0 um) In situ polymerization (0.5 – 1100 um) Hot Melt (1 — 1000 um)
  • 18. Microencapsulation Techniques (Cont.): I. Physico-Chemical Processes: 1- Coacervation: - Two methods for coacervation are available, namely simple and complex processes. -In simple coacervation , a desolvation agent is added for phase separation. - Whereas complex coacervation involves complexation between two oppositely charged polymers.
  • 19. 1- Coacervation (Cont.): Complex coacervation: 1- First the core material (usually an oil) is dispersed into a polymer solution (e.g., a cationic aqueous polymer, gelatin). 2- The second polymer (anionic, water soluble, gum arabic) solution is then added to the prepared dispersion. 3- Deposition of the shell material onto the core particles occurs when the two polymers form a complex. 4-This process is triggered by the addition of salt or by changing the pH, temperature or by dilution of the medium.
  • 20. 1- Coacervation (Cont.): 5- Finally, the prepared microcapsules are stabilized by crosslinking (with formaldehyde), desolvation or thermal treatment. Complex coacervation is used to produce microcapsules containing fragrant oils, liquid crystals, flavors, dyes or inks as the core material.
  • 21.
  • 22. Microencapsulation Techniques (Cont.): 2- Polymer-polymer incompatibility: - Also called phase separation. 1- This method utilizes two polymers that are soluble in a common solvent, yet do not mix with one another in the solution. 2- The polymers form two separate phases, one rich in the polymer intended to form the capsule walls, the other rich in the incompatible polymer meant to induce the separation of the two phases. The second polymer is not intended to be part of the finished microcapsule wall.
  • 23. Microencapsulation Techniques (Cont.): 3- Solvent Evaporation: - It is the most extensively used method of microencapsulation. 1-Prepare an aqueous solution of the drug (may contain a viscosity building or stabilizing agent) 2- Then added to an organic phase consisting of the polymer solution in solvents like dichloromethane or chloroform with vigorous stirring to form the primary water in oil emulsion. 3- This emulsion is then added to a large volume of water containing an emulsifier like PVA or PVP to form the multiple (w/o/w). emulsion 4- The double emulsion is then subjected to stirring until most of the organic solvent evaporates, leaving solid microspheres. 5- The microspheres can then be washed and dried.
  • 24.
  • 25. Microencapsulation Techniques (Cont.): 4- Polymer Encapsulation by Rapid Expansion of Supercritical Fluids: - Supercritical fluids are highly compressed gasses that possess several properties of both liquids and gases. - The most widely used being supercritical CO2 and nitrous oxide (N2O). - A small change in temperature or pressure causes a large change in the density of supercritical fluids .
  • 26. Polymer Encapsulation by Rapid Expansion of Supercritical Fluids (Cont.): Steps : 1-Supercritical fluid containing the active ingredient and the shell material are maintained at high pressure and then released at atmospheric pressure through a small nozzle. 2-The sudden drop in pressure causes desolvation of the shell material, which is then deposited around the active ingredient (core) and forms a coating layer. -Different core materials such as pesticides, pigments, vitamins, flavors, and dyes are encapsulated using this method. -A wide variety of shell materials e.g. paraffin wax and polyethylene glycol are used for encapsulating core substances. -The disadvantage of this process is that both the active ingredient and the shell material must be very soluble in supercritical fluids.
  • 27. Microencapsulation by rapid expansion of supercritical solutions
  • 28. Microencapsulation Techniques (Cont.): 5- Hydrogel microspheres: 1- Microspheres made of gel-type polymers, such as alginate, are produced by dissolving the polymer in an aqueous solution 2-Then, suspending the active ingredient in the mixture 3- Extruding through a precision device, producing micro droplets 4- Then fall into a hardening bath that is slowly stirred. The hardening bath usually contain calcium chloride solution. Advantage: The method involves an all -aqueous system and avoids residual solvents in microspheres. The particle size of microspheres can be controlled by: A- using various size extruders or B- by varying the polymer solution flow rates.
  • 30. Microencapsulation Techniques (Cont.): II Physical Processes: 1- Spray-Drying & spray-congealing : - Microencapsulation by spray-drying is a low-cost commercial process which is mostly used for the encapsulation of fragrances, oils and flavors. Steps : 1- Core particles are dispersed in a polymer solution and sprayed into a hot chamber. 2- The shell material solidifies onto the core particles as the solvent evaporates. - The microcapsules obtained are of polynuclear or matrix type.
  • 33. Microencapsulation Techniques (Cont.): Spray-congealing: - This technique can be accomplished with spray drying equipment when the protective coating is applied as a melt. 1- the core material is dispersed in a coating material melt. 2- Coating solidification (and microencapsulation) is accomplished by spraying the hot mixture into a cool air stream. - e.g. microencapsulation of vitamins with digestable waxes for taste masking.
  • 34. Microencapsulation Techniques (Cont.): 2- Fluidized-Bed Technology: - Different types of fluid-bed coaters include top spray, bottom spray, and tangential spray. - used for encapsulating solid or liquids absorbed into porous particles. Steps : 1-Solid particles to be encapsulated are suspended on a jet of air and then covered by a spray of liquid coating material. 2- The rapid evaporation of the solvent helps in the formation of an outer layer on the particles. 3- This process is continued until the desired thickness and weight is obtained.
  • 35. Schematics of a fluid-bed coater. (a) Top spray; (b) bottom spray; (c) tangential spray
  • 37. Microencapsulation Techniques (Cont.): 3- Pan coating: 1- Solid particles are mixed with a dry coating material. 2- The temperature is raised so that the coating material melts and encloses the core particles, and then is solidified by cooling . Or, the coating material can be gradually applied to core particles tumbling in a vessel rather than being wholly mixed with the core particles from the start of encapsulation.
  • 39. Microencapsulation Techniques (Cont.): 4- Co-Extrusion: 1- A dual fluid stream of liquid core and shell materials is pumped through concentric tubes and forms droplets under the influence of vibration. 2-The shell is then hardened by chemical cross linkings, cooling, or solvent evaporation. - Different types of extrusion nozzles have been developed in order to optimize the process
  • 40. Schematic presentation of the Co-extrusion process
  • 42. Microencapsulation Techniques (Cont.): 5- Spinning Disk: Steps : : 1- Suspensions of core particles in liquid shell material are poured into a rotating disc. 2- Due to the spinning action of the disc, the core particles become coated with the shell material. 3- The coated particles are then cast from the edge of the disc by centrifugal force. 4- After that the shell material is solidified by external means (usually cooling). - This technology is rapid, cost-effective, relatively simple and has high production efficiencies.