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Solvent Systems Screening for Soy Cellulose Fibers  Eugene F. Douglass Richard Kotek North Carolina State University, College of Textiles College of Textiles August 11, 2010 1
Objectives - ,[object Object],[object Object],[object Object],[object Object],College of Textiles 2
1 - Introduction College of Textiles 3
[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],College of Textiles Membranes – what are they? 4
Cellulosic sources ,[object Object],[object Object],College of Textiles Figure 1-  Molecular structure of cellulose. 11   5
[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],College of Textiles 6
Amines and thiocyanate processes   Amine and counter ion dissolution ,[object Object],[object Object],[object Object],College of Textiles Zn +2  > Li +  > Ca +2  > Mg +2  > Ba +2  > Na +  > NH 4 +  > K + SCN -  > I -  > PO 4 -3  > Br -  > Cl -  > NO 3 -  > SO 4 -2  > ClO 3 - Order of decreasing swelling of cellulose   2 7 Figure 2 – Swollen cellulose – crystal structure
Ionic interactions assisting dissolution   Amine and metal salt association College of Textiles 8 Figure 3 – Coordination of ED and KSCN in solution 9  Frey
2 - Development of porous cellulose membranes College of Textiles 9
Objective:  Dissolution of cellulose  (DP 450) ,[object Object],College of Textiles 10 Figure 4 - 7% free flowing ED/KSCN cellulose (DP = 450) solution Figure 5 – Dissolution apparatus
3 - Characterization of porous cellulose membranes College of Textiles 11
[object Object],College of Textiles 12 Figure 6 – SEM micrographs of porous cellulose membrane 500 x 5000 x
[object Object],[object Object],College of Textiles 13 Figure 7 – Raw wood pulp Figure 8 – Cellulose membrane WAXS of ED/ KSCN cellulose from wood pulp and membrane
Khare and Douglass Tensile properties compared College of Textiles 14 Table 1 – Tensile property comparison of cellulose membranes
Characterization using Water absorbency College of Textiles 15 Table 2 – Douglass membranes water absorption after 24 hour immersion in 25 o  C deionized water, compared to never dried water swollen membrane (top)
4 - Development  and Characterization of cellulose blend membranes College of Textiles 16
Development of cellulose / soy protein blend membranes ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],College of Textiles 17
5 – Characterization of cellulose / soy protein blend membranes College of Textiles 18
SEM cross section micrographs of 50/50 cellulose – soy protein blends College of Textiles 19 Figure 9 – 50/50 Cellulose/brim membrane, 5000x Figure 10 – 50/50 Cellulose/Profam 974 membrane, 5000x
TGA Analysis - cellulose membrane compared to cellulose/brim soy protein blend  College of Textiles 20 Figure 11 - Cellulose membrane:  Onset 332º C, end 371º C, ash about 28% Figure 12 - Cellulose / brim blend membrane:  Onset 241º C, end 342º C, ash about 28%  20 o  C 20 o  C 710 o  C 710 o  C 100 30
College of Textiles 21 Figure 13 - Cellulose membrane:  Onset 332º C, end 371º C, ash level about 28% Figure 14 - Cellulose / Profam 974 blend membrane:  Onset 284º C, end 344º C, ash level about 9% TGA Analysis - cellulose membrane compared to cellulose/Profam 974 soy protein blend  20 o  C 710 o  C 100 30
Summary of TGA results for soy protein / cellulose blend membranes College of Textiles 22 Table 3 -  Comparison of TGA results between membranes Materials Start temperature  (ºC) Onset temperature(s) (ºC) Char level @  710º C  (%) Cellulose  fiber 242 350 11 Cellulose membrane 257 332 28 Profam 974 189 276 27 Brim soy protein 193, 285 235, 310 25 Cellulose / Profam 974 mixed 185 290, 362 18 Cellulose / Profam 974 membrane 200 283 9 Cellulose / brim mixed 201, 280 234, 355 19 Cellulose / brim membrane 178 241 28
Wide Angle X-ray Scattering of Profam 974 blend membrane ,[object Object],[object Object],College of Textiles 23 Figure 15 – Cellulose membrane Figure 16 – Cellulose / Profam 974 membrane
[object Object],[object Object],Wide Angle X-ray Scattering of Stretched Soy Protein blend membranes College of Textiles 24 Figure 17 – Cellulose / Brim blend Figure 18 – Cellulose / Profam 974 blend Notice Notice
Tensile Properties Summary College of Textiles 25 Table 4 – Comparison of Tensile properties for soy blend membranes Samples Tensile modulus (kgf/mm 2 ) Failure stress  (kgf/mm 2 ) Failure strain  (%) Thickness  (mm) Cellulose membrane 75 ± 12 2.5 ± 1.2 36 ± 12 0.047 ± 0.015 Cellulose / brim membrane 157 ± 52 3.2 ± 1.6 27 ± 12 0.029 ± 0.003 Cellulose / Profam 974 membrane 200 ± 75 4.7 ± 1.2 16 ± 8.0 0.026 ± 0.001 Cell / PF 40% 220 ± 53 5.0 ± 2.0 29 ± 12 0.026 ± 0.001 Cell / PF 30% 204 ± 74 4.3 ± 2.3 27 ± 12 0.031 ± 0.005 Cell / PF 20% 195 ± 69 2.4 ± 1.8 20 ± 12 0.034 ± 0.003
Water absorbency summary College of Textiles 26 Table 5 – Comparison of water absorbency for soy blend membranes Material Dry mass  (g) Wet mass  (g) Wet mass increase  (%) Wet cellulose membrane (coagulated & kept wet ) 0.28 (after) 4.70 (before) 94 decrease to dry, 1580 increase Dried cellulose membrane 0.49 1.03 110 50% Cellulose / 50% brim membrane 0.18 0.81 350 50 % Cellulose / 50% Profam 974 membrane 0.18 0.81 350 Cell / PF 40% 0.07 0.26 370 Cell / PF 30% 0.11 0.52 470 Cell / PF 20% 0.19 0.60 320
6 – Possible Future work College of Textiles 27
Suggested future work ,[object Object],[object Object],College of Textiles 28
7 - Conclusions College of Textiles 29
[object Object],[object Object],Conclusions College of Textiles 30
8 - References College of Textiles 31
[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],College of Textiles 32

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Soy Membrane Presentation

  • 1. Solvent Systems Screening for Soy Cellulose Fibers Eugene F. Douglass Richard Kotek North Carolina State University, College of Textiles College of Textiles August 11, 2010 1
  • 2.
  • 3. 1 - Introduction College of Textiles 3
  • 4.
  • 5.
  • 6.
  • 7.
  • 8. Ionic interactions assisting dissolution Amine and metal salt association College of Textiles 8 Figure 3 – Coordination of ED and KSCN in solution 9 Frey
  • 9. 2 - Development of porous cellulose membranes College of Textiles 9
  • 10.
  • 11. 3 - Characterization of porous cellulose membranes College of Textiles 11
  • 12.
  • 13.
  • 14. Khare and Douglass Tensile properties compared College of Textiles 14 Table 1 – Tensile property comparison of cellulose membranes
  • 15. Characterization using Water absorbency College of Textiles 15 Table 2 – Douglass membranes water absorption after 24 hour immersion in 25 o C deionized water, compared to never dried water swollen membrane (top)
  • 16. 4 - Development and Characterization of cellulose blend membranes College of Textiles 16
  • 17.
  • 18. 5 – Characterization of cellulose / soy protein blend membranes College of Textiles 18
  • 19. SEM cross section micrographs of 50/50 cellulose – soy protein blends College of Textiles 19 Figure 9 – 50/50 Cellulose/brim membrane, 5000x Figure 10 – 50/50 Cellulose/Profam 974 membrane, 5000x
  • 20. TGA Analysis - cellulose membrane compared to cellulose/brim soy protein blend College of Textiles 20 Figure 11 - Cellulose membrane: Onset 332º C, end 371º C, ash about 28% Figure 12 - Cellulose / brim blend membrane: Onset 241º C, end 342º C, ash about 28% 20 o C 20 o C 710 o C 710 o C 100 30
  • 21. College of Textiles 21 Figure 13 - Cellulose membrane: Onset 332º C, end 371º C, ash level about 28% Figure 14 - Cellulose / Profam 974 blend membrane: Onset 284º C, end 344º C, ash level about 9% TGA Analysis - cellulose membrane compared to cellulose/Profam 974 soy protein blend 20 o C 710 o C 100 30
  • 22. Summary of TGA results for soy protein / cellulose blend membranes College of Textiles 22 Table 3 - Comparison of TGA results between membranes Materials Start temperature (ºC) Onset temperature(s) (ºC) Char level @ 710º C (%) Cellulose fiber 242 350 11 Cellulose membrane 257 332 28 Profam 974 189 276 27 Brim soy protein 193, 285 235, 310 25 Cellulose / Profam 974 mixed 185 290, 362 18 Cellulose / Profam 974 membrane 200 283 9 Cellulose / brim mixed 201, 280 234, 355 19 Cellulose / brim membrane 178 241 28
  • 23.
  • 24.
  • 25. Tensile Properties Summary College of Textiles 25 Table 4 – Comparison of Tensile properties for soy blend membranes Samples Tensile modulus (kgf/mm 2 ) Failure stress (kgf/mm 2 ) Failure strain (%) Thickness (mm) Cellulose membrane 75 ± 12 2.5 ± 1.2 36 ± 12 0.047 ± 0.015 Cellulose / brim membrane 157 ± 52 3.2 ± 1.6 27 ± 12 0.029 ± 0.003 Cellulose / Profam 974 membrane 200 ± 75 4.7 ± 1.2 16 ± 8.0 0.026 ± 0.001 Cell / PF 40% 220 ± 53 5.0 ± 2.0 29 ± 12 0.026 ± 0.001 Cell / PF 30% 204 ± 74 4.3 ± 2.3 27 ± 12 0.031 ± 0.005 Cell / PF 20% 195 ± 69 2.4 ± 1.8 20 ± 12 0.034 ± 0.003
  • 26. Water absorbency summary College of Textiles 26 Table 5 – Comparison of water absorbency for soy blend membranes Material Dry mass (g) Wet mass (g) Wet mass increase (%) Wet cellulose membrane (coagulated & kept wet ) 0.28 (after) 4.70 (before) 94 decrease to dry, 1580 increase Dried cellulose membrane 0.49 1.03 110 50% Cellulose / 50% brim membrane 0.18 0.81 350 50 % Cellulose / 50% Profam 974 membrane 0.18 0.81 350 Cell / PF 40% 0.07 0.26 370 Cell / PF 30% 0.11 0.52 470 Cell / PF 20% 0.19 0.60 320
  • 27. 6 – Possible Future work College of Textiles 27
  • 28.
  • 29. 7 - Conclusions College of Textiles 29
  • 30.
  • 31. 8 - References College of Textiles 31
  • 32.