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1. The document describes a study to enhance the strength of paper using cellulose nanomaterials (CNF) and starch nanoparticles. CNF was derived from both hardwood and softwood, and was modified using glycidyltrimethylammonium chloride to impart a positive charge. Starch nanoparticles used were Ecosphere 2777. 2. Handsheets were formed from pulp, CNF, and additives using a standardized procedure. Physical testing showed that adding 5-10% CNF-GTMAC or 10% CNF-g-pAPTAC increased the dry and wet tensile strength of paper by over 20% compared to untreated pulp.

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1 Performance Enhanced Pulp by Cellulose Nanomaterials Eugenia Chan, Jeremy Kim Mentor: Dr. Yao http://www.mseco.com/wp-content/uploads/2014/07/paper_large.jpg
Purpose • Collaboration with Ecosynthetix • Renewable chemicals company with a focus on alternatives to petroleum-based products • Goal • Enhance paper’s dry and wet tensile strength using cellulose nanomaterials (CNF) and starch nanoparticles (Ecosphere) on the order of 20% greater than unmodified paper products 2
Materials Used in this Project • Pulp • Brazil • BCTMP • CNF • Hardwood • Softwood • Starch Nanoparticles • Ecosphere 2777 3
Pulp and Paper Industry • Origin of papermaking dates back to ~100 AD China • Rags, hemp and grass were beat against stone mortars to break down its fibres • Pulping wood was developed ~1800s • More abundant fibre source • Still used in modern pulp & paper manufacturing • In modern times, papermaking is a large integration operation including: • Foresting • Lumbermilling • Pulp & Paper Manufacturing • Conversion 4 Teschke K. (2011). Paper and Pulp Industry: General Profile. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry
Pulp • Main component is cellulose • Strong H-bonds that holds the fibres together • 600 to 1500 repeating alternating D- glucose molecules • Modified using additives • Different types of woods have different proportions of components • Our project involves Softwoods and Hardwoods pulp 5 Keefe A. & Teschke K. (2011). Paper and Pulp Industry: Fibre Sources for Pulp and Paper. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry Royal Society of Chemistry (2013). Paper Conservation Cellulose Acid Hydrolysis. Education in Chemistry Magazine. Retrieved from: http://www.rsc.org/education/eic/issues/2013March/paper-conservation-cellulose-acid-hydrolysis.asp Table 1. Chemical Compositions of Pulp and its Sources (Keefe & Teschke (2011)
Pulping • Process of exposing fibrous structures of pulp by rupturing bonds within wood structure • Mechanical • Chemical • Pulping process was already done and pulp was provided by: • Suzano Papel e Celulose (Brazil) • West Fraser (BCTMP) 6 Anderson J., Anastrakianakis G. & Keefe A. (2011). Paper and Pulp Industry: Pulping. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry
Properties of Pulp Brazil 7 • 0.0176 mM/g of COOH content • Hardwood from Eucalyptus trees • Shorter fiber length, lower pulp strength BCTMP • 0.024 mM/g of COOH content • Zeta potential: -25.3 mV • Softwood • Longer fiber length
Bleached Chemical Thermo-Mechanical Pulp (BCTMP) • Softwood • Used to manufacture coated boards, printing/writing paper and paper towel/napkin grades • From Lodgepole Pine and White Spruce trees • Advantages • Produce 2x the yield of pulp compared to other chemical pulps (85% vs. 42%) • More environmentally friendly → chlorine-free bleaching 8 CANNELL, E. (2000, May 1). PULP & PAPER MAGAZINE:The Future of BCTMP. Retrieved from http://legacy.risiinfo.com/magazines/May/2000/PP/pulp-paper/magazine/may/2000/The-Future-of-BCTMP.html Softwood BCTMP provided by West Fraser
Optical Microscopy Images of BCTMP • Long fibers that are a couple of mm in length • Small amount of fibrillated fibers 9
What is CNF? • Referred to as Cellulose Nanofibers (CNF) or Microfibrillated Cellulose (MFC) • Size: 20-50 nm • Nanocomponent of cellulose, acquired by mechanical methods (shearing) using high pressure homogenizer • Contains amorphous and crystalline regions • Our project involved 2 different types of CNF samples: • CNF from Hardwood (CNF-H) • CNF from Softwood (CNF-S) 10 Nasirpour A., Fathi M. & Rezzei A. (2015). Application of Cellulosic Nanofibers in Food Science Using Electrospinning and Its Potential Risk. Comprehensive Review in Food Science and Food Safety. Vol 14-3. Retrieved from: http://onlinelibrary.wiley.com/doi/10.1111/1541-4337.12128/pdf
Properties of CNF • Lightweight material • Renewable resource and biodegradable • High surface area and high tensile strength (138 GPa) compared to pulp fiber (2 GPa) • Hydroxyl groups on the surface allow for various chemical modifications • Negatively charged 11 CNC 5-20 nm Mircofibrillated Cellulose (CNF/MFC) 20-50 nm Elementary fibrils 5 nm Chemical structure Amorphous regionCrystalline region Pulp Fibers
CNF-Hardwood • 0.048 mM/g of COOH content • Zeta Potential: -36.1 mV 12 CNF-H
CNF-Softwood • 0.064 Mm/g of COOH content • Zeta Potential: -22.5 mV 13 CNF-S
Optical Microscopy Images of CNF-H • Few long fibers that are mm in length • Most fibers are hundred microns in length 14
Optical Microscopy Images of CNF-S • Some long fibers that are mm in length • Considerable amount of fibrillated fibers that are hundred microns in length 15
Starch Nanospheres • Starch • natural, renewable, and biodegradable polymer • consists of linear amylose (~75%) and branched amylopectin (~25%) • contains both amorphous and crystalline regions 16 Corre, D. L., Bras, J., & Dufresne, A. (2010). Starch Nanoparticles: A Review. Biomacromolecules, 11(5), 1139-1153. doi:10.1021/bm901428y
Ecosphere 2777 • Starch particles cationically modified by quaternary amine • Zeta potential: 16.9 mV • Size measured by DLS: Rh = 92.5 nm 17 Ecosphere 2777
Traditionally Used Wet Strength Agents • Urea-Formaldehyde (UF) resin • network created by self-crosslinking • not environmental friendly • Polyamide Epichlorohydrin (PAE) • formation of covalent bonds between PAE and cellulose fibers • negatively impacts environment due to organic chloride → limited use in paper mills now 18 Espy, H. H. (1995). The mechanism of wet-strength development in paper: a review. Tappi Journal, 78(4), 90-100.
Advantages of CNF and Cationic Ecosphere • High surface area of CNF and Ecospheres → increases the number of bonds between the pulp fibers • CNF can be modified to have positive charges on the surface • Negatively charged pulp will have electrostatic interaction with cationic Ecospheres and modified CNF 19
Forming Handsheets for Physical Testing • TAPPI T-205 “Forming Handsheets for Physical Tests of Pulp” • Disintegration (mixing and dispersion of pulp fibres) • Sheetmaking (filtration of pulp) • Couching (Blotting and rolling of fresh sheet) • Pressing • Drying • Testing of sheets (Tensile strength) • Followed this stepwise procedure, making appropriate alterations • Included procedure in adding additives to pulp 20
Disintegration • Process of breaking and dispersing pulp fibres into smaller components • Guidelines from Pulp Company: • Dilute to 4-8 wt% (we used 4%), mix for minimum of 20 minutes • Even after several hours, still chunky consistency • Sheets were not homogenous • Guidelines from TAPPI T 205: • Dilute to 1.2 wt% (we used 1.5%), mix at high rpm • Dilute to 0.3 wt%, stir at high rpm until properly mixed • Starting at a lower consistency produced more homogenous sheets • Final procedure: Mix at 1.5 wt% for 1 hour, dilute to 0.3 wt% and mix for 30 mins 21 Disintegration of pulp
Sheetmaking • Glass Filtration • screening trial of sheetmaking • Pros: • Setup was stable  allowed for more homogenous filtration • Cons: • Sheets were too small  could not be properly tested 22 Glass filtration setup
Sheetmaking • Buchner Funnel • Pros: Larger diameter, allows for larger sheets • Cons: Membrane was not completely flat, resulted in non-homogenous areas • Different types of filter membrane used  led to sheet sticking to it • Cloth + metal mesh membrane was made to avoid sticking 23 Buchner funnel setup Cloth + metal mesh
Sheetmaking • Filtration • Set-up designed and made by Dr. Yao • Wire mesh (size: 200 mesh) used instead of cloth or filter paper to eliminate problem with sheet sticking • Solution diluted by adding additional 1250 mL of water, mixed and allowed to settle before applying vacuum • More homogenous sheets 24 Current filtration set-up Wire mesh
Couching/Pressing • Filter papers were used as blotters, rolled to soak up excess water on sheets • Preliminary pressing step • More homogenous sheets, prevented wrinkling and greater tensile strength • Implemented a standard pressing procedure • Hydraulic press at 50 psi for 5 mins, then again for 2 mins after replacing blotters 25 Hydraulic press
Modifying Pulp • Created modified pulp solution by mixing pulp and additive • Initial attempt: • Combined 0.3 wt% pulp and 0.3 wt% additive together and mixed for 10 mins • Sheets were not homogenous due to formation of aggregates • Decreased additive from 0.3 wt% to 0.1 wt%, added dropwise and mixed for 30 mins • Allowed for better dispersion of additive within pulp solution • More homogenous sheets26 Additive Modified Pulp Solution
Drying • Hotplate method • Sheet was placed between glass plates and heated on hotplate at 90oC with weight placed on top for 5 min, then air dried • Heat was not distributed evenly onto sheet, bottom was heated but top was not • Very inefficient when drying multiple sheets 27 Hotplate method of drying
Drying • Current method • Multiple handsheets are placed between glass plates and dried overnight in oven at 70o C • Weights placed on top of plates to prevent wrinkling 28 Oven drying method
Testing • Tensile Strength (TS): Maximum applied tensile force a specimen can withstand before rupturing • Force (NZ) per unit width (m), NZ/m • Force is applied through the z-axis by UMT machine, width of strip is 0.015m • Factors affecting: fibre strength, fibre length and bonding • TS = FZ/(width of strip) • Tensile Index (TI): Relates the strength of the specimen with the amount being loaded • Provides relative strength of sheet • Tensile strength (NZ/m) divided by grammage (g/m2) • TI = TS/(mass of strip/Area of strip) 29 Muchorski D. (2006). Tensile properties of paper and paperboard. TAPPI (2), T 494. Retrieved from: http://www.tappi.org/content/sarg/t494.pdf
Testing • 5 15mm x 60mm strips are cut and weighed from each handsheet and tested • Universal Testing Machine is used to apply a stretching force to the z-axis • Machine usage provided by Dr. Boxin Zhao • 5 dry tests and 5 wet tests • Wet test: 30 µL is dropped onto middle of strip prior to test • Water affects tensile strength by affecting the swelling behaviour of fibres 30 Strips cut from handsheet Testing using UTM
Testing • Tensile strength of different types of sheets are compared to a 100% pulp sheet  control group • Literature value of raw pulp is given in table • Preliminary testing of pulp done with a 100% BCTMP sample • Dry tensile index of 25.97 Nm/g • Confirms that data is agreeable and reproducible 31 Hsieh J. & Yoo S. (2010). Enzyme-Assisted Preparation of Fibrillated Cellulose Fibers and Its Effect on Physical and Mechanical Properties of Paper Sheet Composites. Ind Eng Chem Res. Vol 49 Issue 5. Retrieved from: http://pubs.acs.org/doi/abs/10.1021/ie901621n
Current Additives to Pulp • CNF-GTMAC • CNF-g-pAPTAC and CNF + pAPTAC • Ecosphere 2777 32
CNF-GTMAC • CNF is modified with cationic Glycidyltrimethylammonium chloride (GTMAC) • Carried out in an aqueous solution instead of using an organic solvent such as DMSO • safer, easier to scale up for a large scale process 33
CNF-GTMAC • Procedure: Dissolved CNF in NaOH solution and stirred the mixture at 50°C for 4 hours, dropwise added GTMAC over 1 hour and stirred the mixture at 60°C • Zeta potential: 39.7 mV, higher than CNF (-26.1 mV). • Positively charged so it will better adhere to negatively charged pulp • After 1 week of storage, CNF-GTMAC is more stable than CNF 34 CNF-GTMAC (left) and unmodified CNF (right)
Preliminary Tensile Index Results using CNF- GTMAC • at both 5% and 10%, the addition of CNF- GTMAC to pulp increased the dry and wet tensile index over 20% 35 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 CNF-GTMAC 5% 36.87 2.72 54.20 28.30 10% 38.04 3.09 79.80 45.80
Polymerization of (3- acrylamidopropyl)triethylammonium (APTAC) • Free radical polymerization using ammonium persulfate (APS) as initiator • Procedure: Mixed CNF with initiator APS and bubbled the mixture with N2 gas for 1 hr, added APTAC in dropwise fashion, then stirred the mixture at 70°C overnight.36 CNF APTAC
pAPTAC • In 125 mg of CNF-g-pAPTAC, 0.8 wt% is the polymer • 0.038 mM/g • Zeta potential: • CNF-g-pAPTAC (grafted): –20.8 mV • CNF-pAPTAC (mixed) (1:0.01): –20.8 mV • no difference in zeta potential when pAPTAC is grafted or mixed with CNF 37
Preliminary Tensile Index Results using pAPTAC • only the samples with 10% CNF-g-pAPTAC added to the pulp showed a 20% increase for both the dry and wet tensile index38 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 CNF-g- pAPTAC 5% 35.58 2.13 49.80 0.50 10% 43.55 2.89 105.80 36.30 CNF:pAPTAC (1:0.5) 5% 23.63 1.52 6.70 -28.30 10% 29.85 2.27 41.10 7.10
Ecosphere 2777 • both 5% and 10% Ecosphere 2777 added to the pulp showed much greater than 20% increase for both the dry and wet tensile index 39 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 Ecosphere 2777 5% 41.23 3.74 94.80 76.40 10% 38.06 5.15 79.90 142.90
Ecosphere 2777:CNF-S • zeta potential of the mixture of Ecosphere 2777 and CNF-S increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 0.140 Eco2777:CNF-S Zeta potential (mV) 0 -22.5 0.1 15.2 0.25 14.9 0.5 16.0 1 16.7 2 16.9 3 20.2 5 16.6
TEM Image of Ecosphere 2777:CNF-S (1:1) • dark coloured circles embedded on fibers show that ecosphere particles have bonded to CNF-S 41
Tensile Index Results of Ecosphere 2777:CNF- S (1:1) • when more than 3% of Ecosphere 2777 mixed with CNF-S at 1:1 ratio is added to the pulp, the dry and wet tensile index increased by more than 20% • however, standard deviation is high, more homogenous sheets need to be made42 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 25.17 2.81 1.87 0.56 Ecosphere 2777:CNF-S (1:1) 1% 30.18 3.20 19.93 13.97 5.14 0.97 3% 34.05 3.39 35.30 20.62 2.28 1.24 5% 43.16 4.03 71.49 43.44 6.06 1.22 8% 41.26 3.87 63.96 37.82 5.13 0.56
Tensile Index Results of Ecosphere 2777:CNF- S (1:2) • when more than 1% of Ecosphere 2777 mixed with CNF-S at 1:2 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • however, the trend is not consistent, perhaps due to formation of large aggregates43 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 24.20 2.29 1.22 0.26 Ecosphere 2777:CNF-S (1:2) 1% 29.34 2.82 21.24 23.38 5.61 0.52 3% 32.53 2.84 34.43 24.25 6.95 1.17 5% 51.21 3.42 111.60 49.50 7.38 0.73 8% 39.81 3.14 64.50 37.47 12.83 0.24
Ecosphere 2777:CNF-H • zeta potential of the mixture of Ecosphere 2777 and CNF-H increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 144 Eco2777: CNF-H Zeta potential (mV) 0 -36.1 0.1 10.1 0.25 10.5 0.5 12.4 1 16.7 2 19.1 3 18.8 5 19.4
TEM Image of Ecosphere 2777:CNF-H (1:1) • dark coloured circles embedded on fibers show that Ecosphere particles have bonded to CNF-H 45
Tensile Index Results of Ecosphere 2777:CNF- H (1:1) • when more than 1% of Ecosphere 2777 mixed with CNF-H at 1:1 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • however, standard deviation is high, more homogenous sheets need to be made46 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 25.17 2.81 1.87 0.56 Ecosphere 2777:CNF-H (1:1) 1% 30.50 3.50 21.17 24.66 3.42 0.30 3% 41.36 4.14 64.34 47.19 5.69 0.53 5% 37.59 4.34 49.36 54.40 3.37 0.49 8% 39.62 4.48 57.42 59.55 3.70 0.84
Tensile Index Results of Ecosphere 2777:CNF- H (1:2) • when more than 3% of Ecosphere 2777 mixed with CNF-H at 1:2 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • trend is consistent, however standard deviation is high, more homogenous sheets need to be made 47 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 24.20 2.29 1.22 0.26 Ecosphere 2777:CNF-H (1:2) 1% 25.15 2.70 3.92 18.09 2.86 0.37 3% 34.42 2.79 42.22 22.00 6.87 0.79 5% 38.59 2.96 59.47 29.46 4.24 0.31 8% 41.34 4.24 70.84 85.44 13.15 0.43
Comparison of Ecosphere 2777:CNF (1:1 and 1:2) • Comparing the % increase in tensile index of Ecosphere 2777:CNF at ratios of 1:1 and 1:2, adding more CNF did not increase the tensile index very much and in some cases had an even lower tensile index48 Samples % increase Samples % increase Dry Wet Dry Wet Ecosphere 2777:CNF-S (1:1) 1% 19.93 13.97 Ecosphere 2777:CNF-S (1:2) 1% 21.24 23.38 3% 35.30 20.62 3% 34.43 24.25 5% 71.49 43.44 5% 111.60 49.50 8% 63.96 37.82 8% 64.50 37.47 Ecosphere 2777:CNF-H (1:1) 1% 21.17 24.66 Ecosphere 2777:CNF-H (1:2) 1% 3.92 18.09 3% 64.34 47.19 3% 42.22 22.00 5% 49.36 54.40 5% 59.47 29.46 8% 57.42 59.55 8% 70.84 85.44
Ecosphere 2777:CNC • zeta potential of the mixture of Ecosphere 2777 and CNC increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 249 Eco2777:CNC Zeta potential (mV) 0 -41.45 0.1 -20.4 0.25 -18.3 0.5 -13.3 1 12.55 2 15.45 3 16.85 5 15.85
TEM Image of Ecosphere 2777:CNC (1:2) • dark coloured circles are Ecosphere particles, light coloured rods are CNC • appears that Ecosphere particles mixed well with CNC 50
Tensile Index Results of Ecosphere 2777:CNC (2:1) • only the samples with 8% Ecosphere 2777:CNC at 2:1 ratio added to the pulp showed a 20% increase for both the dry and wet tensile index • wet tensile index even decreased due to CNC’s ability to disperse well in water  when the paper absorbed water, CNC lost it’s adhesion capability 51 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 20.37 3.06 1.63 0.07 Ecosphere 2777:CNC (2:1) 1% 23.96 2.65 17.62% -13.59% 4.68 0.28 3% 24.07 3.01 18.16% -1.74% 4.38 0.49 5% 38.1 2.93 87.04% -4.35% 7.38 0.79 8% 30.95 3.95 51.94% 29.01% 1.24 0.34
Conclusion • From the results gathered so far • Ecosphere 2777 mixed with CNF-H and CNF-S and added to pulp reach the goal of increasing the dry and wet tensile index by 20% • CNF-GTMAC added to pulp also shows promising preliminary results and can further be tested as necessary • CNC will not be used again since results did not reach goal and also more expensive compared to CNF 52
Conclusion • Next steps • Handsheet making process can be further improved in order to make more homogenous sheets to decrease standard deviation and produce more reliable results • Make and test sheets: • Ecosphere 2777:CNF-H/S at 2:1 ratio • CNF-H and CNF-S • Ecosphere 2777 mixed with CNF-S dry product provided by company 53
54 THANKS FOR LISTENING http://www.mseco.com/wp-content/uploads/2014/07/paper_large.jpg

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final-ppt

  • 1.
    1 Performance Enhanced Pulpby Cellulose Nanomaterials Eugenia Chan, Jeremy Kim Mentor: Dr. Yao http://www.mseco.com/wp-content/uploads/2014/07/paper_large.jpg
  • 2.
    Purpose • Collaboration withEcosynthetix • Renewable chemicals company with a focus on alternatives to petroleum-based products • Goal • Enhance paper’s dry and wet tensile strength using cellulose nanomaterials (CNF) and starch nanoparticles (Ecosphere) on the order of 20% greater than unmodified paper products 2
  • 3.
    Materials Used inthis Project • Pulp • Brazil • BCTMP • CNF • Hardwood • Softwood • Starch Nanoparticles • Ecosphere 2777 3
  • 4.
    Pulp and PaperIndustry • Origin of papermaking dates back to ~100 AD China • Rags, hemp and grass were beat against stone mortars to break down its fibres • Pulping wood was developed ~1800s • More abundant fibre source • Still used in modern pulp & paper manufacturing • In modern times, papermaking is a large integration operation including: • Foresting • Lumbermilling • Pulp & Paper Manufacturing • Conversion 4 Teschke K. (2011). Paper and Pulp Industry: General Profile. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry
  • 5.
    Pulp • Main componentis cellulose • Strong H-bonds that holds the fibres together • 600 to 1500 repeating alternating D- glucose molecules • Modified using additives • Different types of woods have different proportions of components • Our project involves Softwoods and Hardwoods pulp 5 Keefe A. & Teschke K. (2011). Paper and Pulp Industry: Fibre Sources for Pulp and Paper. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry Royal Society of Chemistry (2013). Paper Conservation Cellulose Acid Hydrolysis. Education in Chemistry Magazine. Retrieved from: http://www.rsc.org/education/eic/issues/2013March/paper-conservation-cellulose-acid-hydrolysis.asp Table 1. Chemical Compositions of Pulp and its Sources (Keefe & Teschke (2011)
  • 6.
    Pulping • Process ofexposing fibrous structures of pulp by rupturing bonds within wood structure • Mechanical • Chemical • Pulping process was already done and pulp was provided by: • Suzano Papel e Celulose (Brazil) • West Fraser (BCTMP) 6 Anderson J., Anastrakianakis G. & Keefe A. (2011). Paper and Pulp Industry: Pulping. Encyclopedia or Occupational Health and Safety. Chapter 72. Retrieved from http://www.iloencyclopaedia.org/part-x-96841/paper-and-pulp-industry
  • 7.
    Properties of Pulp Brazil 7 •0.0176 mM/g of COOH content • Hardwood from Eucalyptus trees • Shorter fiber length, lower pulp strength BCTMP • 0.024 mM/g of COOH content • Zeta potential: -25.3 mV • Softwood • Longer fiber length
  • 8.
    Bleached Chemical Thermo-MechanicalPulp (BCTMP) • Softwood • Used to manufacture coated boards, printing/writing paper and paper towel/napkin grades • From Lodgepole Pine and White Spruce trees • Advantages • Produce 2x the yield of pulp compared to other chemical pulps (85% vs. 42%) • More environmentally friendly → chlorine-free bleaching 8 CANNELL, E. (2000, May 1). PULP & PAPER MAGAZINE:The Future of BCTMP. Retrieved from http://legacy.risiinfo.com/magazines/May/2000/PP/pulp-paper/magazine/may/2000/The-Future-of-BCTMP.html Softwood BCTMP provided by West Fraser
  • 9.
    Optical Microscopy Imagesof BCTMP • Long fibers that are a couple of mm in length • Small amount of fibrillated fibers 9
  • 10.
    What is CNF? •Referred to as Cellulose Nanofibers (CNF) or Microfibrillated Cellulose (MFC) • Size: 20-50 nm • Nanocomponent of cellulose, acquired by mechanical methods (shearing) using high pressure homogenizer • Contains amorphous and crystalline regions • Our project involved 2 different types of CNF samples: • CNF from Hardwood (CNF-H) • CNF from Softwood (CNF-S) 10 Nasirpour A., Fathi M. & Rezzei A. (2015). Application of Cellulosic Nanofibers in Food Science Using Electrospinning and Its Potential Risk. Comprehensive Review in Food Science and Food Safety. Vol 14-3. Retrieved from: http://onlinelibrary.wiley.com/doi/10.1111/1541-4337.12128/pdf
  • 11.
    Properties of CNF •Lightweight material • Renewable resource and biodegradable • High surface area and high tensile strength (138 GPa) compared to pulp fiber (2 GPa) • Hydroxyl groups on the surface allow for various chemical modifications • Negatively charged 11 CNC 5-20 nm Mircofibrillated Cellulose (CNF/MFC) 20-50 nm Elementary fibrils 5 nm Chemical structure Amorphous regionCrystalline region Pulp Fibers
  • 12.
    CNF-Hardwood • 0.048 mM/gof COOH content • Zeta Potential: -36.1 mV 12 CNF-H
  • 13.
    CNF-Softwood • 0.064 Mm/gof COOH content • Zeta Potential: -22.5 mV 13 CNF-S
  • 14.
    Optical Microscopy Imagesof CNF-H • Few long fibers that are mm in length • Most fibers are hundred microns in length 14
  • 15.
    Optical Microscopy Imagesof CNF-S • Some long fibers that are mm in length • Considerable amount of fibrillated fibers that are hundred microns in length 15
  • 16.
    Starch Nanospheres • Starch •natural, renewable, and biodegradable polymer • consists of linear amylose (~75%) and branched amylopectin (~25%) • contains both amorphous and crystalline regions 16 Corre, D. L., Bras, J., & Dufresne, A. (2010). Starch Nanoparticles: A Review. Biomacromolecules, 11(5), 1139-1153. doi:10.1021/bm901428y
  • 17.
    Ecosphere 2777 • Starchparticles cationically modified by quaternary amine • Zeta potential: 16.9 mV • Size measured by DLS: Rh = 92.5 nm 17 Ecosphere 2777
  • 18.
    Traditionally Used WetStrength Agents • Urea-Formaldehyde (UF) resin • network created by self-crosslinking • not environmental friendly • Polyamide Epichlorohydrin (PAE) • formation of covalent bonds between PAE and cellulose fibers • negatively impacts environment due to organic chloride → limited use in paper mills now 18 Espy, H. H. (1995). The mechanism of wet-strength development in paper: a review. Tappi Journal, 78(4), 90-100.
  • 19.
    Advantages of CNFand Cationic Ecosphere • High surface area of CNF and Ecospheres → increases the number of bonds between the pulp fibers • CNF can be modified to have positive charges on the surface • Negatively charged pulp will have electrostatic interaction with cationic Ecospheres and modified CNF 19
  • 20.
    Forming Handsheets forPhysical Testing • TAPPI T-205 “Forming Handsheets for Physical Tests of Pulp” • Disintegration (mixing and dispersion of pulp fibres) • Sheetmaking (filtration of pulp) • Couching (Blotting and rolling of fresh sheet) • Pressing • Drying • Testing of sheets (Tensile strength) • Followed this stepwise procedure, making appropriate alterations • Included procedure in adding additives to pulp 20
  • 21.
    Disintegration • Process ofbreaking and dispersing pulp fibres into smaller components • Guidelines from Pulp Company: • Dilute to 4-8 wt% (we used 4%), mix for minimum of 20 minutes • Even after several hours, still chunky consistency • Sheets were not homogenous • Guidelines from TAPPI T 205: • Dilute to 1.2 wt% (we used 1.5%), mix at high rpm • Dilute to 0.3 wt%, stir at high rpm until properly mixed • Starting at a lower consistency produced more homogenous sheets • Final procedure: Mix at 1.5 wt% for 1 hour, dilute to 0.3 wt% and mix for 30 mins 21 Disintegration of pulp
  • 22.
    Sheetmaking • Glass Filtration •screening trial of sheetmaking • Pros: • Setup was stable  allowed for more homogenous filtration • Cons: • Sheets were too small  could not be properly tested 22 Glass filtration setup
  • 23.
    Sheetmaking • Buchner Funnel •Pros: Larger diameter, allows for larger sheets • Cons: Membrane was not completely flat, resulted in non-homogenous areas • Different types of filter membrane used  led to sheet sticking to it • Cloth + metal mesh membrane was made to avoid sticking 23 Buchner funnel setup Cloth + metal mesh
  • 24.
    Sheetmaking • Filtration • Set-updesigned and made by Dr. Yao • Wire mesh (size: 200 mesh) used instead of cloth or filter paper to eliminate problem with sheet sticking • Solution diluted by adding additional 1250 mL of water, mixed and allowed to settle before applying vacuum • More homogenous sheets 24 Current filtration set-up Wire mesh
  • 25.
    Couching/Pressing • Filter paperswere used as blotters, rolled to soak up excess water on sheets • Preliminary pressing step • More homogenous sheets, prevented wrinkling and greater tensile strength • Implemented a standard pressing procedure • Hydraulic press at 50 psi for 5 mins, then again for 2 mins after replacing blotters 25 Hydraulic press
  • 26.
    Modifying Pulp • Createdmodified pulp solution by mixing pulp and additive • Initial attempt: • Combined 0.3 wt% pulp and 0.3 wt% additive together and mixed for 10 mins • Sheets were not homogenous due to formation of aggregates • Decreased additive from 0.3 wt% to 0.1 wt%, added dropwise and mixed for 30 mins • Allowed for better dispersion of additive within pulp solution • More homogenous sheets26 Additive Modified Pulp Solution
  • 27.
    Drying • Hotplate method •Sheet was placed between glass plates and heated on hotplate at 90oC with weight placed on top for 5 min, then air dried • Heat was not distributed evenly onto sheet, bottom was heated but top was not • Very inefficient when drying multiple sheets 27 Hotplate method of drying
  • 28.
    Drying • Current method •Multiple handsheets are placed between glass plates and dried overnight in oven at 70o C • Weights placed on top of plates to prevent wrinkling 28 Oven drying method
  • 29.
    Testing • Tensile Strength(TS): Maximum applied tensile force a specimen can withstand before rupturing • Force (NZ) per unit width (m), NZ/m • Force is applied through the z-axis by UMT machine, width of strip is 0.015m • Factors affecting: fibre strength, fibre length and bonding • TS = FZ/(width of strip) • Tensile Index (TI): Relates the strength of the specimen with the amount being loaded • Provides relative strength of sheet • Tensile strength (NZ/m) divided by grammage (g/m2) • TI = TS/(mass of strip/Area of strip) 29 Muchorski D. (2006). Tensile properties of paper and paperboard. TAPPI (2), T 494. Retrieved from: http://www.tappi.org/content/sarg/t494.pdf
  • 30.
    Testing • 5 15mmx 60mm strips are cut and weighed from each handsheet and tested • Universal Testing Machine is used to apply a stretching force to the z-axis • Machine usage provided by Dr. Boxin Zhao • 5 dry tests and 5 wet tests • Wet test: 30 µL is dropped onto middle of strip prior to test • Water affects tensile strength by affecting the swelling behaviour of fibres 30 Strips cut from handsheet Testing using UTM
  • 31.
    Testing • Tensile strengthof different types of sheets are compared to a 100% pulp sheet  control group • Literature value of raw pulp is given in table • Preliminary testing of pulp done with a 100% BCTMP sample • Dry tensile index of 25.97 Nm/g • Confirms that data is agreeable and reproducible 31 Hsieh J. & Yoo S. (2010). Enzyme-Assisted Preparation of Fibrillated Cellulose Fibers and Its Effect on Physical and Mechanical Properties of Paper Sheet Composites. Ind Eng Chem Res. Vol 49 Issue 5. Retrieved from: http://pubs.acs.org/doi/abs/10.1021/ie901621n
  • 32.
    Current Additives toPulp • CNF-GTMAC • CNF-g-pAPTAC and CNF + pAPTAC • Ecosphere 2777 32
  • 33.
    CNF-GTMAC • CNF ismodified with cationic Glycidyltrimethylammonium chloride (GTMAC) • Carried out in an aqueous solution instead of using an organic solvent such as DMSO • safer, easier to scale up for a large scale process 33
  • 34.
    CNF-GTMAC • Procedure: DissolvedCNF in NaOH solution and stirred the mixture at 50°C for 4 hours, dropwise added GTMAC over 1 hour and stirred the mixture at 60°C • Zeta potential: 39.7 mV, higher than CNF (-26.1 mV). • Positively charged so it will better adhere to negatively charged pulp • After 1 week of storage, CNF-GTMAC is more stable than CNF 34 CNF-GTMAC (left) and unmodified CNF (right)
  • 35.
    Preliminary Tensile IndexResults using CNF- GTMAC • at both 5% and 10%, the addition of CNF- GTMAC to pulp increased the dry and wet tensile index over 20% 35 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 CNF-GTMAC 5% 36.87 2.72 54.20 28.30 10% 38.04 3.09 79.80 45.80
  • 36.
    Polymerization of (3- acrylamidopropyl)triethylammonium(APTAC) • Free radical polymerization using ammonium persulfate (APS) as initiator • Procedure: Mixed CNF with initiator APS and bubbled the mixture with N2 gas for 1 hr, added APTAC in dropwise fashion, then stirred the mixture at 70°C overnight.36 CNF APTAC
  • 37.
    pAPTAC • In 125mg of CNF-g-pAPTAC, 0.8 wt% is the polymer • 0.038 mM/g • Zeta potential: • CNF-g-pAPTAC (grafted): –20.8 mV • CNF-pAPTAC (mixed) (1:0.01): –20.8 mV • no difference in zeta potential when pAPTAC is grafted or mixed with CNF 37
  • 38.
    Preliminary Tensile IndexResults using pAPTAC • only the samples with 10% CNF-g-pAPTAC added to the pulp showed a 20% increase for both the dry and wet tensile index38 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 CNF-g- pAPTAC 5% 35.58 2.13 49.80 0.50 10% 43.55 2.89 105.80 36.30 CNF:pAPTAC (1:0.5) 5% 23.63 1.52 6.70 -28.30 10% 29.85 2.27 41.10 7.10
  • 39.
    Ecosphere 2777 • both5% and 10% Ecosphere 2777 added to the pulp showed much greater than 20% increase for both the dry and wet tensile index 39 Samples Tensile index Nm/g % increase Dry Wet Dry Wet 100% pulp 21.16 2.12 Ecosphere 2777 5% 41.23 3.74 94.80 76.40 10% 38.06 5.15 79.90 142.90
  • 40.
    Ecosphere 2777:CNF-S • zetapotential of the mixture of Ecosphere 2777 and CNF-S increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 0.140 Eco2777:CNF-S Zeta potential (mV) 0 -22.5 0.1 15.2 0.25 14.9 0.5 16.0 1 16.7 2 16.9 3 20.2 5 16.6
  • 41.
    TEM Image ofEcosphere 2777:CNF-S (1:1) • dark coloured circles embedded on fibers show that ecosphere particles have bonded to CNF-S 41
  • 42.
    Tensile Index Resultsof Ecosphere 2777:CNF- S (1:1) • when more than 3% of Ecosphere 2777 mixed with CNF-S at 1:1 ratio is added to the pulp, the dry and wet tensile index increased by more than 20% • however, standard deviation is high, more homogenous sheets need to be made42 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 25.17 2.81 1.87 0.56 Ecosphere 2777:CNF-S (1:1) 1% 30.18 3.20 19.93 13.97 5.14 0.97 3% 34.05 3.39 35.30 20.62 2.28 1.24 5% 43.16 4.03 71.49 43.44 6.06 1.22 8% 41.26 3.87 63.96 37.82 5.13 0.56
  • 43.
    Tensile Index Resultsof Ecosphere 2777:CNF- S (1:2) • when more than 1% of Ecosphere 2777 mixed with CNF-S at 1:2 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • however, the trend is not consistent, perhaps due to formation of large aggregates43 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 24.20 2.29 1.22 0.26 Ecosphere 2777:CNF-S (1:2) 1% 29.34 2.82 21.24 23.38 5.61 0.52 3% 32.53 2.84 34.43 24.25 6.95 1.17 5% 51.21 3.42 111.60 49.50 7.38 0.73 8% 39.81 3.14 64.50 37.47 12.83 0.24
  • 44.
    Ecosphere 2777:CNF-H • zetapotential of the mixture of Ecosphere 2777 and CNF-H increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 144 Eco2777: CNF-H Zeta potential (mV) 0 -36.1 0.1 10.1 0.25 10.5 0.5 12.4 1 16.7 2 19.1 3 18.8 5 19.4
  • 45.
    TEM Image ofEcosphere 2777:CNF-H (1:1) • dark coloured circles embedded on fibers show that Ecosphere particles have bonded to CNF-H 45
  • 46.
    Tensile Index Resultsof Ecosphere 2777:CNF- H (1:1) • when more than 1% of Ecosphere 2777 mixed with CNF-H at 1:1 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • however, standard deviation is high, more homogenous sheets need to be made46 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 25.17 2.81 1.87 0.56 Ecosphere 2777:CNF-H (1:1) 1% 30.50 3.50 21.17 24.66 3.42 0.30 3% 41.36 4.14 64.34 47.19 5.69 0.53 5% 37.59 4.34 49.36 54.40 3.37 0.49 8% 39.62 4.48 57.42 59.55 3.70 0.84
  • 47.
    Tensile Index Resultsof Ecosphere 2777:CNF- H (1:2) • when more than 3% of Ecosphere 2777 mixed with CNF-H at 1:2 ratio is added to the pulp, the dry and wet tensile index increased more than 20% • trend is consistent, however standard deviation is high, more homogenous sheets need to be made 47 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 24.20 2.29 1.22 0.26 Ecosphere 2777:CNF-H (1:2) 1% 25.15 2.70 3.92 18.09 2.86 0.37 3% 34.42 2.79 42.22 22.00 6.87 0.79 5% 38.59 2.96 59.47 29.46 4.24 0.31 8% 41.34 4.24 70.84 85.44 13.15 0.43
  • 48.
    Comparison of Ecosphere2777:CNF (1:1 and 1:2) • Comparing the % increase in tensile index of Ecosphere 2777:CNF at ratios of 1:1 and 1:2, adding more CNF did not increase the tensile index very much and in some cases had an even lower tensile index48 Samples % increase Samples % increase Dry Wet Dry Wet Ecosphere 2777:CNF-S (1:1) 1% 19.93 13.97 Ecosphere 2777:CNF-S (1:2) 1% 21.24 23.38 3% 35.30 20.62 3% 34.43 24.25 5% 71.49 43.44 5% 111.60 49.50 8% 63.96 37.82 8% 64.50 37.47 Ecosphere 2777:CNF-H (1:1) 1% 21.17 24.66 Ecosphere 2777:CNF-H (1:2) 1% 3.92 18.09 3% 64.34 47.19 3% 42.22 22.00 5% 49.36 54.40 5% 59.47 29.46 8% 57.42 59.55 8% 70.84 85.44
  • 49.
    Ecosphere 2777:CNC • zetapotential of the mixture of Ecosphere 2777 and CNC increased when increasing the amount of 2777 • zeta potential stayed almost unchanged after the ratio exceeded 249 Eco2777:CNC Zeta potential (mV) 0 -41.45 0.1 -20.4 0.25 -18.3 0.5 -13.3 1 12.55 2 15.45 3 16.85 5 15.85
  • 50.
    TEM Image ofEcosphere 2777:CNC (1:2) • dark coloured circles are Ecosphere particles, light coloured rods are CNC • appears that Ecosphere particles mixed well with CNC 50
  • 51.
    Tensile Index Resultsof Ecosphere 2777:CNC (2:1) • only the samples with 8% Ecosphere 2777:CNC at 2:1 ratio added to the pulp showed a 20% increase for both the dry and wet tensile index • wet tensile index even decreased due to CNC’s ability to disperse well in water  when the paper absorbed water, CNC lost it’s adhesion capability 51 Samples Tensile index Nm/g % increase SD Dry Wet Dry Wet Dry Wet 100% pulp 20.37 3.06 1.63 0.07 Ecosphere 2777:CNC (2:1) 1% 23.96 2.65 17.62% -13.59% 4.68 0.28 3% 24.07 3.01 18.16% -1.74% 4.38 0.49 5% 38.1 2.93 87.04% -4.35% 7.38 0.79 8% 30.95 3.95 51.94% 29.01% 1.24 0.34
  • 52.
    Conclusion • From theresults gathered so far • Ecosphere 2777 mixed with CNF-H and CNF-S and added to pulp reach the goal of increasing the dry and wet tensile index by 20% • CNF-GTMAC added to pulp also shows promising preliminary results and can further be tested as necessary • CNC will not be used again since results did not reach goal and also more expensive compared to CNF 52
  • 53.
    Conclusion • Next steps •Handsheet making process can be further improved in order to make more homogenous sheets to decrease standard deviation and produce more reliable results • Make and test sheets: • Ecosphere 2777:CNF-H/S at 2:1 ratio • CNF-H and CNF-S • Ecosphere 2777 mixed with CNF-S dry product provided by company 53
  • 54.

Editor's Notes

  • #6 Lignin acts as a glue to hold the pulp fibres together. cellulose: glucose units alternate in direction when joined
  • #7 Mechanical: grinding and sheering wood between stone or wooden plates. Chemical: Dissolving the lignin that hold the pulp fibres together.
  • #8 pH titration done using 10mM NaOH
  • #9 sodium sulfite for impregnation, fibers are bleached in a conventional peroxide bleach
  • #11 Maine uni - briefly used Amorphous: part where fibres don’t have rigid structure
  • #13 10mM NaOH to 0.25 wt% pulp solution
  • #14 10mM NaOH to 0.25 wt% pulp solution
  • #17 Starch Nanoparticles: A Review, Biomacromolecules 2010, 11, 1139–1153
  • #18 Rh: hydrodynamic radius graph - relaxation time distribution
  • #24 filter membrane: sheets would stick to the membrane. cloth + metal membrane: good lol
  • #25 PICTURE OF METAL MESH
  • #26 PICTURE
  • #41 COPY TABLE FROM OTHER PPT WHEN EXPORTING
  • #42 INSERT PHOTO AGAIN WHEN EXPORTING
  • #45 COPY TABLE FROM OTHER PPT WHEN EXPORTING
  • #46 INSERT PHOTO
  • #50 COPY TABLE FROM OTHER PPT WHEN EXPORTING
  • #51 INSERT IMAGE