Polystyrene Micro Beads

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    Extraction of Polystyrene micro

    beads from EPS with OptimumSolvent Recovery

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    Purpose Of the Project

    EPS- Expanded Polystyrene popularly known as

    Thermocol

    It consists mostly of voids filled with gas and are

    considered as Use-Throw materials

    Polystyrene micro beads are of more economic value

    This project is to obtain a more economic valued

    beads from Thermocol waste with an optimumsolvent recovery

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    Stages Of Project

    1) Extraction Of Micro beads

    Dissolution of EPS in a solvent Phase

    Preparation Of Emulsion

    Separation Of Micro beads from Solvent Phase

    2)Solvent Recovery Process

    Need for most economical way with optimum recovery

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    Solvent Selection

    D-Limonene is preferred as it is obtained from a renewable

    source (citrus oil) and is environment friendly solvent

    Initial stage of experiments are carried with toluene as solvent

    as it is cheaper than D-limonene and it readily dissolves poly

    styrene

    These results can be extended to d-limonene as solvent

    Solubility parameter values should be studied to select a

    suitable solvent for a dissolving polymer

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    Solubility Parameter

    Dissolution of an amorphous polymer in a solvent is governedby the free energy of mixing

    Gm = Hm - TSmwhere Gm is the Gibbs free energy change on mixing, Hm is the

    enthalpy change on mixing, T is the absolute temperature, and Smis the entropy change on mixing.

    The heat of mixing must be smaller than the entropic term forpolymersolvent miscibility

    Gm < 0 The cohesive energy, CED; of a material is the increase in the

    internal energy per mole of the material if all of theintermolecular forces are eliminated

    Cohesive energy density = CED = (Hvap - RT)/V

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    Hildebrand Solubility parameters

    Solubility Parameter is given by square root of CED

    d = (CED)1/2= ((Hvap - RT)/V)1/2

    Hmix = Vmix[(E1/V1)1/2-(E2/V2)

    1/2]*(12)

    Hmix = Vmix[d1 - d2 ]*(12)12 are mole fractions of solute and solvent

    Vmix is Volume of mixture

    E1 is energy of vaporization of specie 1

    V1 is molar volume of specie 1

    Therefore, [d1 - d2] should be small for dissolution.

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    Solubility Parameter Values

    Solubility parameters for some common

    polymers

    Solubility parameters for some common

    Solvents

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    Experiment

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    Prepared samples of different wt% of EPS in toluene (1%,

    2% and 4% of EPS in toluene). Solvents used are water, methanol, 1:1mixture of water and

    methanol.

    Take EPS- Toluene sample of known concentration in a test

    tube which forms the oil phase. To this sample (oil phase) add the solvent, drop by drop until

    the inversion phase occurs.

    Now shake the test tube to ensure proper and uniform

    dispersion and observe the formation of beads and observetheir behaviour (i.e. stability, coagulation etc.).

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    Observations

    For water as solvent, no beads are formed (irrespective of

    concentration of EPS-toluene sample), but the mixture sample

    is retained at the top surface of water. Shaking resulted in

    dispersion of EPS sample into polystyrene beads which

    immediately settled at the surface of water.

    For EPS-Toluene in methanol we got thread like structured

    fibers after immediate drying

    For EPS-toluene in 1:1 methanol/water emulsion, milky

    solution is formed, and slowly beads coalesce to form threadlike structures.

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    Effect Of Concentration

    These results are similar for 1%,2%,5% EPS in toluene

    So as far as concentration change is concerned no significant

    change is observed

    Also for all these concentrations, there was immediateseparation of phases (oil phase at the top and water at the

    bottom)

    So in all the cases of experiments above, we stirred rigorously

    & within no time poured onto flat plate and dried it

    So we need to obtain stability of emulsion to prevent the

    separation of phases

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    Density effects

    When tested with increased concentration of EPS in

    toluene(20%), the results ( Polystyrene Spheres Formation)

    were better with water than the remaining two solvents.

    This could be because of difference of densities of oil phasewith that of solvent phase

    Increasing to 20% w/w of EPS (in toluene) will make the

    density of oil phase approximate to that of water

    Hence the possible dispersion occurs instead of immediatephase separation

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    Take away

    Hence concentration of EPS in Toluene should

    be optimal considering the density and

    viscosity effects

    If possible a third component should be added

    to oil phase which doesnt increase viscosity

    but increases density

    Also for stability of emulsion, addition of

    emulsifier is must

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    What are Emulsifiers

    When there is a problem of making an

    emulsion, emulsifying agent can be used to

    stabilize the emulsion

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    Selection Of Emulsifier- The HLB System

    There are hundreds of emulsifiers which are available in

    industry

    But only the appropriate emulsifiers can serve the

    purpose efficiently The selection of emulsifier can be done on the basis of

    HLB system

    HLB stands for Hydrophile-Lipophile Balance

    All emulsifiers consist of a molecule that combines both

    hydrophilic and lipophilic groups

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    HLB System

    Hydrophile-Lipophile Balance is the balance ofthe size and strength of the hydrophilic (water-loving or polar) and the lipophilic (oil loving ornon-polar) groups of the emulsifier.

    The HLB System enables you to assign a number

    to the ingredient or combination of ingredientsyou want to emulsify, and then to choose anemulsifier or blend of emulsifiers having thissame number

    An emulsifier that is lipophilic in character is

    assigned a low HLB number (below 9.0), and onethat is hydrophilic is assigned a high HLB number(above 11.0). Those in the range of 9-11 areintermediate.

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    Available emulsifiers in lab:

    SLS

    Tween 80 (HLB Value = 15)

    Span 80 (HLB Value = 4.3)

    The emulsifier we

    selected is Tween 80

    Because the HLB

    number matches with

    that of ingredient

    Toluene

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    Taken Ingredients:

    Solvent: Water and Methanol

    Oil phase: Eps in Toluene of different concentrations

    Emulsifier: 4:1 blend of Tween 80 and Span 80

    HLB Value of Blend of two emulsifiers:

    HLB Value of E1 = HLB1

    HLB Value of E2 = HLB2 Volume fraction of E1 = x1 Volume fraction of E2 = x2 HLB Value of Blend = x1 * HLB1 + x2 * HLB2

    For Tween 80 : Span 80 = 4:1

    HLB Value of Blend = 0.8*15 + 0.2*4.3 = 12.86

    Result

    No convincing change

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    Contd..

    Emulsifier: Sodium Lauryl Sulphate

    Result:

    Addition of SLS to water phase:

    Mixed SLS in water and then added the oil phase drop by drop.

    After stirring and drying, we got fibrous structured polystyrene

    Addition of SLS to Oil phase:

    Taken SLS in oil phase and added water drop by drop to the oilphase

    We were able to get relatively good results in this case

    But after the stirring is done, in about 5-10 min and when theemulsion is poured in a flat plate we obtain small beads separatedbut after some time they coalesce

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