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    Determination of Grafting Degree of Maleic Anhydride On PP

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    李万福
    The document reports on tests performed to determine the grafting degree of maleic anhydride (MAH) on polypropylene (PP). Two samples of PP grafted with MAH were tested using Fourier-transform infrared spectroscopy (FTIR) and back titration. FTIR found the grafting degree was 1.97% for the untreated sample and 1.46% for the purified sample, indicating 0.51% was unreacted MAH. Back titration calculated a grafting degree of 1.598% for the purified sample. The results show FTIR and back titration are comparable methods for determining grafting degree, with the purified sample giving a more accurate measurement by removing unreact

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    Determination of Grafting Degree of Maleic Anhydride On PP

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    李万福
    88 views6 pages
    The document reports on tests performed to determine the grafting degree of maleic anhydride (MAH) on polypropylene (PP). Two samples of PP grafted with MAH were tested using Fourier-transform infrared spectroscopy (FTIR) and back titration. FTIR found the grafting degree was 1.97% for the untreated sample and 1.46% for the purified sample, indicating 0.51% was unreacted MAH. Back titration calculated a grafting degree of 1.598% for the purified sample. The results show FTIR and back titration are comparable methods for determining grafting degree, with the purified sample giving a more accurate measurement by removing unreact

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    Determination of Grafting Degree of Maleic Anhydride on PP

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    The document reports on tests performed to determine the grafting degree of maleic anhydride (MAH) on polypropylene (PP). Two samples of PP grafted with MAH were tested using Fourier-transform infrared spectroscopy (FTIR) and back titration. FTIR found the grafting degree was 1.97% for the untreated sample and 1.46% for the purified sample, indicating 0.51% was unreacted MAH. Back titration calculated a grafting degree of 1.598% for the purified sample. The results show FTIR and back titration are comparable methods for determining grafting degree, with the purified sample giving a more accurate measurement by removing unreact

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    88 views6 pages

    Determination of Grafting Degree of Maleic Anhydride On PP

    Uploaded by

    李万福
    The document reports on tests performed to determine the grafting degree of maleic anhydride (MAH) on polypropylene (PP). Two samples of PP grafted with MAH were tested using Fourier-transform infrared spectroscopy (FTIR) and back titration. FTIR found the grafting degree was 1.97% for the untreated sample and 1.46% for the purified sample, indicating 0.51% was unreacted MAH. Back titration calculated a grafting degree of 1.598% for the purified sample. The results show FTIR and back titration are comparable methods for determining grafting degree, with the purified sample giving a more accurate measurement by removing unreact

    Copyright:

    © All Rights Reserved
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    of 6

    20.2.

    2019

    Material Report
    DETERMINATION OF GRAFTING DEGREE OF MALEIC ANHYDRIDE ON PP

    The aim of this report is, to show that our Methods of Grafting Degree Determination are versatile and
    accurate.

    MATERIALS USED

    For this report, we used scrap PP that was grafted with MAH at Graft Polymer. Matrix material was provided
    by Customer.

    TESTS PERFORMED

    For the determination of grafting degree, we used:

     Fourier Transformation Infrared Spectrometer (FTIR, picture on


    right)
     Back Titration with KOH and HCl

    We tested two samples:

     Stored in LDPE bags, as prepared – FTIR Only


     Chemically purified samples -

    Purification was performed in two steps:

     Dissolving grafted polymer


     Elimination of unreacted MAH

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com
    Material Report

    PROCESS

    We dissolve 5 gr of PP-g-MAH in boiling xylene (Isomeric mixture) in a reflux (left)


    After that we let it cool (right)

    The solution is precipitated using acetone – acetone also dissolves unreacted MAH away (left)

    The sample is dried in a fume hood for 3 hours and in an oven at 60°C for 2 hours (right)

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com
    Material Report

    After the sample is dried, we dissolve 1 g again in boiling xylene and add 5 mL of the base KOH (0,1 M)

    Reaction with anhydride and KOH occurs, using up all anhydride groups

    We added KOH in excess, in order to titrate it with HCl

    We add 2 drops of the indicator phenolphthalein to the solution – it is pink because the solution is basic

    We titrate the leftover KOH with HCl (0,05 M)

    Titration is finished when the solution is colorless

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com
    Material Report

    RESULTS

    FTIR RESULTS

    PURIFIED SAMPLE

    SAMPLE FROM STORAGE

    On the above picture, we can see the comparison between “raw” (Purple spectra) and purified (Red spectra)
    samples. Maleic anhydride is seen in the area of 1850 cm-1 and 1780 cm-1, according to the x axis. The relevant
    area is circled.

     Calculated MAH on the sample from storage is: 1,97% MAH (Including unreacted MAH)
     Calculated MAH on the purified sample is: 1,46% MAH (No unreacted MAH)

    TITRATION RESULTS

    For the determination of grafting degree, we used the following formula:

    𝑐(𝐾𝑂𝐻)∗𝑉(𝐾𝑂𝐻 𝑙𝑒𝑓𝑡𝑜𝑣𝑒𝑟)∗𝑀(𝑀𝐴𝐻)
    𝐺𝐷 (𝑀𝐴𝐻 ) = = 1,598%
    𝑚(𝑠𝑎𝑚𝑝𝑙𝑒)

    c (KOH) – KOH Concentration [mol/L]

    V(KOH leftover) - KOH, that wasn’t used for neutralizing HCl [L]

    M(MAH) – Molar mass of grafted MAH [=99,07 g/mol]

    m(sample) – mass of the purified polymer sample [g]

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com
    Material Report

    CONCLUSIONS

     Grafting degree, measured with FTIR before purification is higher than that of purified sample, which

    means that 0,51% of MAH was unreacted

     By purifying the sample, we determined the grafting degree of the sample to be around 1,5%

     The difference between the methods is only around 0,138%

     When increasing the number of samples, the deviation grows smaller

     FTIR and titration are COMPARABLE METHODS

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com
    Material Report

    CONTACTS

    MANAGEMENT

    CEO/CTO | Victor Bolduev +386 40 534 739

    Executive Director / CMO | Pavel Kobzev +386 40 867 937

    Pavel@graftpolymer.com

    GRAFT POLYMER D.O.O (OFFICE)

    Emonska Cesta 8, Ljubljana Slovenia.

    Company Num. 8056200000,

    VAT. SI 30561345

    Tel +386 1 777 6561

    office@graftpolymer.com

    www.graftpolymer.com

    GRAFT POLYMER D.O.O (PRODUCTION/WAREHOUSE)

    Mejaceva ulica 2, 1353 Borovnica Slovenia

    Company Num. 8056200000,

    VAT. SI 30561345

    office@graftpolymer.com

    www.graftpolymer.com

    GRAFT POLYMER (UK) LTD

    Central Working Victoria Eccleston Yards 25,

    Eccleston Pl, London, UK, SW1W 9NF.

    Company Num. 10776788, VAT. 281712016

    www.graftpolymer.com

    GRAFT POLYMER D.O.O. GRAFT POLYMER UK LTD


    Emonska Cesta 2, Ljubljana Slovenia Central Working Victoria Eccleston Yards 25,
    Company Num. 8056200000, VAT. SI 30561345 Eccleston Pl, London, UK, SW1W 9NF.
    Phone Num. +38640867937 Company Num. 10776788, VAT. 281712016
    office@graftpolymer.com www.graftpolymer.com

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