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Propagation of Interfacially Active Nanohybrids
              Stability of Dispersions


                 ASL AN M AL EKI




                                             2/19/2013
Agenda
 Methods

 Measuring Tools

 Stability Experiments:
    Experiment 1: 200 ppm PVP-40K & 1600 ppm HEC-10 & 100 ppm P/MWNT

    Experiment 2: 200 ppm PVP-40K & 1600 ppm Gum Arabic & 100 ppm P/MWNT

    Experiment 3: 200 ppm Gum Arabic & 1600 ppm HEC-10 & 100 ppm P/MWNT

 Xanthan Gum Preparation

 Conclusion

 Future Works

                                    2
Method of preparation
                                     Intermediate Dispersion:
                                   P/MWNT & Primary Polymer

Sequential Dispersion                     Sonicate 2 hr.
    Preparation
 Purified Multi-walled CNTs        Add Secondary Polymer
 Polymer Dispersants
 Brine (8% NaCl & 2% CaCl2)            Sonicate 30 min.
   10%, API

                                   Centrifuge 2 hr. @ 2000 rpm


                                        Filtration @ 1 um

                                       Final Dispersion:
                                     PMWNT + 2 Polymers

                               3
Measuring Tools
Testing Dispersion Stability:
         Measurement of particle loss as a function of time
         Quantify loss with turbidity or UV-Vis

                               Initial Reading
                               1. 1st Hour
                               2. 3rd Hour
                               3. 12th Hour
                               4. 24th Hour
                               5. 1st Day
                               6. 2nd Day
                               7. 3rd Day
                               8. 5th Day
                               9. 7th Day
                               10. 1st Week
                               11. 2nd Week



                                       4
Experiment 1 – with Turbidity


Polymers:         API Brine Based
     Primary – 200 ppm PVP-40K
     Secondary – 1600 ppm HEC-10

P/MWNT – 100 ppm




                            5
Experiment 1 - Data
200 ppm PVP-40K
1600 ppm HEC-10
100 ppm P/MWNT                                50C (Turbidity vs. Time)
                  9


                  8


                  7


                  6
 TURBIDITY (MΩ)




                  5


                  4


                  3


                  2


                  1


                  0
                      0   15   30   45   60    75    90       105        120   135   150   165   180   195   210
                                                          TIME (HOURS)




                                                             6
Experiment 1 – with UV-Vis

Polymers:         API Brine Based
     Primary – 200 ppm PVP-40k
     Secondary – 1600 ppm HEC-10

P/MWNT – 100 ppm




                          7
Experiment 1 - Data
200 ppm PVP-40K
1600 ppm HEC-10
100 ppm P/MWNT
              3.000

              2.900

              2.800
                                             Absorbance Room
              2.700
                                             Absorbance (50C)
 ABSORBANCE




              2.600

              2.500

              2.400

              2.300

              2.200

              2.100

              2.000
                      0    100   200   300           400        500   600   700   800
                                               TIME (HOURS)




                                                 8
Experiment 2 - Description

Polymers:         API Brine Based
     Primary – 200 ppm PVP-40k
     Secondary – 1600 ppm Gum Arabic

P/MWNT – 100 ppm




                           9
Experiment 2 - Data
200 ppm PVP-40k
1600 ppm Gum Arabic
100 ppm P/MWNT




                           10
Experiment 3 - Description
Polymers:                API Brine Based
     Primary – 200 ppm Gum Arabic
     Secondary – 1600 ppm HEC-10

P/MWNT – 100 ppm




                             11
Experiment 3 - Data




               12
Xanthan Gum Preparation

              2000 ppm Xanthan Gum @ 10% API

Method:
1. 8 min @ high speed
2. 8 min @ med. speed (Wait 24 Hours) then 8 min @ med. speed
3. 8 min @ med. Speed, then sonicate 30 min.
4. 8 min @ med. Speed, then sonicate 1 hr.

                                         No gel or cake formation
Filter each at 1 um                      observed on filter for any
                                         method




                              13
Viscosity




            14
Conclusions

 Dispersion Stability
   UV-Vis  less fluctuation in data than turbidity
   Negligible difference in stability at 50oC
   All samples stable for 2 weeks


Xanthan Gum Preparation
   Highest viscosity with lowest change after filtration:
     med speed 8 min (wait 24 hr) med speed 8 min




                            15
Future Work

Dispersion Stability
   PVP-40k only dispersion
     • Compare DI vs. 10% Brine @ Room Temp & 50oC
   Xanthan Gum as secondary dispersant


Polymer Thermo-Stability
   Effect of temperature on polymer viscosity to
    determine time/temperature at which degradation
    occurs.

                          16
Acknowledgement
         Dr. Ben Shiau

       Dr. Jeffrey Harwell

     Dr. Peter Lohateeraparp

     Master Danny Swatske

      Master3 Tzu-Ping Hsu

         ASL Lab Crew

               17
Questions & Answers
        T H AN K YO U F O R YO U R T IM E




18

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Fall 2012 final research presentation

  • 1. Propagation of Interfacially Active Nanohybrids Stability of Dispersions ASL AN M AL EKI 2/19/2013
  • 2. Agenda  Methods  Measuring Tools  Stability Experiments:  Experiment 1: 200 ppm PVP-40K & 1600 ppm HEC-10 & 100 ppm P/MWNT  Experiment 2: 200 ppm PVP-40K & 1600 ppm Gum Arabic & 100 ppm P/MWNT  Experiment 3: 200 ppm Gum Arabic & 1600 ppm HEC-10 & 100 ppm P/MWNT  Xanthan Gum Preparation  Conclusion  Future Works 2
  • 3. Method of preparation Intermediate Dispersion: P/MWNT & Primary Polymer Sequential Dispersion Sonicate 2 hr. Preparation  Purified Multi-walled CNTs Add Secondary Polymer  Polymer Dispersants  Brine (8% NaCl & 2% CaCl2) Sonicate 30 min. 10%, API Centrifuge 2 hr. @ 2000 rpm Filtration @ 1 um Final Dispersion: PMWNT + 2 Polymers 3
  • 4. Measuring Tools Testing Dispersion Stability: Measurement of particle loss as a function of time Quantify loss with turbidity or UV-Vis Initial Reading 1. 1st Hour 2. 3rd Hour 3. 12th Hour 4. 24th Hour 5. 1st Day 6. 2nd Day 7. 3rd Day 8. 5th Day 9. 7th Day 10. 1st Week 11. 2nd Week 4
  • 5. Experiment 1 – with Turbidity Polymers: API Brine Based Primary – 200 ppm PVP-40K Secondary – 1600 ppm HEC-10 P/MWNT – 100 ppm 5
  • 6. Experiment 1 - Data 200 ppm PVP-40K 1600 ppm HEC-10 100 ppm P/MWNT 50C (Turbidity vs. Time) 9 8 7 6 TURBIDITY (MΩ) 5 4 3 2 1 0 0 15 30 45 60 75 90 105 120 135 150 165 180 195 210 TIME (HOURS) 6
  • 7. Experiment 1 – with UV-Vis Polymers: API Brine Based Primary – 200 ppm PVP-40k Secondary – 1600 ppm HEC-10 P/MWNT – 100 ppm 7
  • 8. Experiment 1 - Data 200 ppm PVP-40K 1600 ppm HEC-10 100 ppm P/MWNT 3.000 2.900 2.800 Absorbance Room 2.700 Absorbance (50C) ABSORBANCE 2.600 2.500 2.400 2.300 2.200 2.100 2.000 0 100 200 300 400 500 600 700 800 TIME (HOURS) 8
  • 9. Experiment 2 - Description Polymers: API Brine Based Primary – 200 ppm PVP-40k Secondary – 1600 ppm Gum Arabic P/MWNT – 100 ppm 9
  • 10. Experiment 2 - Data 200 ppm PVP-40k 1600 ppm Gum Arabic 100 ppm P/MWNT 10
  • 11. Experiment 3 - Description Polymers: API Brine Based Primary – 200 ppm Gum Arabic Secondary – 1600 ppm HEC-10 P/MWNT – 100 ppm 11
  • 12. Experiment 3 - Data 12
  • 13. Xanthan Gum Preparation 2000 ppm Xanthan Gum @ 10% API Method: 1. 8 min @ high speed 2. 8 min @ med. speed (Wait 24 Hours) then 8 min @ med. speed 3. 8 min @ med. Speed, then sonicate 30 min. 4. 8 min @ med. Speed, then sonicate 1 hr. No gel or cake formation Filter each at 1 um observed on filter for any method 13
  • 14. Viscosity 14
  • 15. Conclusions  Dispersion Stability  UV-Vis  less fluctuation in data than turbidity  Negligible difference in stability at 50oC  All samples stable for 2 weeks Xanthan Gum Preparation  Highest viscosity with lowest change after filtration: med speed 8 min (wait 24 hr) med speed 8 min 15
  • 16. Future Work Dispersion Stability  PVP-40k only dispersion • Compare DI vs. 10% Brine @ Room Temp & 50oC  Xanthan Gum as secondary dispersant Polymer Thermo-Stability  Effect of temperature on polymer viscosity to determine time/temperature at which degradation occurs. 16
  • 17. Acknowledgement Dr. Ben Shiau Dr. Jeffrey Harwell Dr. Peter Lohateeraparp Master Danny Swatske Master3 Tzu-Ping Hsu ASL Lab Crew 17
  • 18. Questions & Answers T H AN K YO U F O R YO U R T IM E 18