PULP FIBER QUALITY AND THE RELATIONSHIP WITH PAPER TISSUE PROPERTIES. Roland J. Trepanier, PhD. OpTest Equipment Inc. Hawkesbury, ON K6A3S3, Canada

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PULP FIBER QUALITY AND THE RELATIONSHIP WITH PAPER TISSUE PROPERTIES Roland J. Trepanier, PhD OpTest Equipment Inc. Hawkesbury, ON K6A3S3, Canada Introduction Tissue papers include a wide range of products with different properties and quality demands. Key properties include: strength, absorbency, grammage, thickness (bulk), brightness, stretch, appearance and softness [1]. Recovered fibers now represent over 50% of the industry s raw materials. However, using fibers from recovered paper makes it more difficult to maintain machine runnability and product quality. Frequently, the relationship between tissue properties and pulp fiber quality (morphology) is counter-intuitive. It is also grade specific. Knowledge about this relationship holds the key to maximising tissue quality and lowering costs, whilst managing the variability of virgin and recovered fiber. This relationship is sufficiently important that most major tissue manufacturers have obtained patents on the means of generating and controlling fiber curl [15-19]. This report investigates the relationships between fiber morphology and tissue paper properties. This includes the impact on tissue properties of daily variations in fiber quality. The relationships are explained and guidance is provided as to the preferred method to measure fiber quality and how to modify it. Figure 1: A diagrammatic representation of a curled fiber with 2 definitions of length Two common measures of fiber shape are curl and kink. Curl is the gradual and continuous curvature of a fiber and is defined by [2,5] : Curl Index = (L/l)-1. Kink is the abrupt (bend) change in the fiber curvature and is defined by Kibblewhite's Kink Index [4]. This index is a weighted sum of the number, Nx, of kinks within a range of "x" kink angles: Kink Index=[2N(21-45 )+ 3N(46-90 )+4N(91-180 )]/LTOTAL Fiber Morphology and Tissue Sheet Strength The relation between sheet strength and fiber length is well known [6]. Increasing fiber length will tend to increase tensile strength (in-plane force) and tear strength (out-of-plane force). This arises from the longer fibers presenting more bonding opportunities/fiber. The relation holds over a range of sheet densities [2] as shown in Figures 2. Fiber Morphology Definitions Fiber quality is often defined in terms of fiber length and shape [2,3,4]. Fiber length is normally described as either the fiber contour length, L, or the end-to-end (projected) length, l, Figure 1. Figure 2: Increasing avg. fiber length from 1.47 to 2.70 mm increases tensile strength, at fixed bulk, for softwood Kraft pulp. Trepanier Tappi Tissue 2017 1

Fiber curl opens up the fiber network which reduces the opportunities for inter-fiber bonding and it places more stress on fiberfiber bonds. Consequently, fiber curl decreases tensile strength [2], Figure 3. Figures 2 and 3 reveal that increasing fiber length, or decreasing fiber curl, delivers the same sheet strength at a higher sheet bulk. To increase absorbency and bulk, a more open fiber network is advantages. In the absence of other effects, increasing the fiber curl increases the sheet bulk, Figure 5, and absorbency. Figure 3: Increasing avg. fiber Curl Index from 12% to 25% decreases tensile strength for a range of pulps from Kraft to TMP [2]. Conversely, increasing fiber curl increases wet web stretch, Figure 4. In the wet web inter-fiber bonding is negligible and the curlier fiber entangle more and resist being pulled apart. Figure 5: Increasing Curl Index and the Kink Index increases sheet bulk for softwood Kraft. Softness Softness, often reported as a single value, is difficult to measure. It is considered a compound property subjectively combining several more basic properties [1] such as surface smoothness [7], bulk, and flexibility. The relationship between fiber curl and tissue softness was reported by Borrego [8],Figure 6. In general increasing fiber curl and kink tends to increase tissue softness. Figure 4: Increasing %-Curl Index increases wet web stretch for both Kraft and TMP pulps. Out-of-plane tear increases with increasing fiber curl [6]. More energy is required to pull fibers out than to break them. Thus, out-ofplane tear increases with fiber curl. Absorbency & Bulk Absorbency and bulk are important properties for most tissue paper grades and perhaps the most important for products like paper towels. Figure 6: Increasing %-Curl Index increases softness for ONP/OMG pulps. Trepanier Tappi Tissue 2017 2

Curl does increase the risk of fibers protruding out of the fiber network in the z-direction of the sheet. When fibers protrude out, it is important that these protruding fibers be soft and supple. Accurately Measuring Fiber Length & Shape producing fully bleached Kraft softwood (FBK Swd) and hardwood (FBK Hwd) pulp. Figure 8 reveals the fiber length variation during this 18 day period. The 2-sigma Lw %-variation of the FBK Swd was about twice as large as the FBK Hwd. Research performed at FP Innovations (Paprican), the University of British Columbia and OpTest Equipment Inc. resulted in a new design of cytometric flow cell that orients fibers precisely for proper analysis [9,11] of length, curl and kink. Figure 7: Cytometric flow cell The flow cell, Figure 7, has a 33 mm² cross section. The fibers flow in a thin (<0.5 mm) middle laminar layer which is flanked by 2 clear water layers. This design prevents flow cell contamination and plugging by highly curled and kinked fibers typically found in recycled pulps. With the fibers correctly oriented it is essential that the entire fiber be measured without interference by air bubbles or dirt specks. This is best be achieved by using circular polarised light [9,10]. Advanced image analysis software then measures the two dimensional morphology on fibers properly oriented and illuminated. This technology is embodied in a commercial device call the Fiber Quality Analyzer, FQA. Figure 8: FBK pulp process variations of average fiber length over an 18 day period However, the Curl Index %-variation, Figure 9, was over 3 times greater than the corresponding Lw variation. The impact of the Curl variation on tissue strength and bulk is estimated in Table 1. Figure 9: FBK pulp process variations of average fiber curl over an 18 day period Over the 18 day period the tensile strength would vary as much a 37% and bulk as much as 12% for tissue made of 100% FBK softwood. Table 1: The impact of fiber curl process variations on tissue made from 100% FBK Swd pulp Process Variation of Length and Curl and Impact on Tissue Fiber length and curl was measured 8 times daily, for 18 days by a fiber quality analyzer, in a mill Trepanier Tappi Tissue 2017 3

Changing Curl & Kink Any mechanical action on fibers [12-14] performed at high consistency (>10%) can introduce curl into chemical and recycled pulps. Even at lower consistencies changes in fiber morphology, brought on by refining, impacts tissue properties [8,12]. This behaviour is sufficiently important that most major tissue manufacturers have obtained patents on the means of generating and controlling fiber curl [15-19]. It is often necessary to reduce excessive fiber curl. In general, low intensity- low consistency (LC/LI) refining helps remove curl and kink from chemical pulps as shown in Figures 10 and 11. The fiber quality analyzer results in these figures are for an 80% hardwood and 20% softwood bleached pulp. Figure 11 shows that from 0 to 60 kwh/bdmt the fiber curl and kink decreases by over 16%. Then from 60 kwh/bdmt to 130 kwh/bmtd the fiber curl and kink decreases by about 7%. The LC/LI refining study demonstrates how excessive curl and kink may be lowered without sacrificing fiber length. This method may be used to target curl and kink levels that provide desired tissue properties as discussed above. The process stages of washing and bleaching a northern softwood Kraft pulp are presented in Figures 11 and 12. The fiber length, curl and kink were measure by a fiber quality analyzer. Figure 12: Northern softwood fiber length change during washing and bleaching Figure 10: Effect on fiber length due increase Refining Energy on a blended Hwd/Swd pulp Figure 10 reveals that from 0 to 60 kwh/bdmt the fiber length changes by less than 1%. Then from 60 kwh/bdmt to 130 kwh/bdmt the average fiber length decreases by 6%. However, the reduction in fiber Curl and Kink is significantly greater from 0 to 60 kwh/bdmt. Figure 12 finds that the reduction in fiber length over the entire process was less than 4%. However, there was significant increase in both curl and kink indices after each bleaching and washing stage. The Curl index increased from 0.075 entering the bleach plant to 0.175 exiting the last washer, or an increase of 131% Figure 13: Northern softwood fiber curl and kink change during washing and bleaching Figure11: Effect on fiber Curl and kink due increase Refining Energy on a blended Hwd/Swd pulp Trepanier Tappi Tissue 2017 4

The last stage of the process was the LC/LI refining which reduces the Curl Index to the target value of 0.12 (or 12%). Conclusion It has been shown that typical process variations may drastically change fiber curl and kink without significantly affecting fiber length. The investigations in this report reveal that changes in fiber curl and kink can significantly impact important tissue paper properties. Consequently precisely measuring fiber length, curl and kink is required to monitor and control the amount of curl and kink. This is the key to maximising tissue quality and lowering costs, whilst managing the variability of virgin and recovered fiber. [15] Carlisle et al. (Procter&Gamble): US Patent No. 5137537 (1992) [16] Hu (Kimberly-Clark): US Patent No. 6413362 (2002) [17] Lee (Georgia-Pacific): US Patent No. 6899790 (2005) [18] Hu (Kimberly-Clark): US Patent No. 6984447 (2006) [19] Reeb et al. (Georgia-Pacific): US Patent Application No. 20100032113 References [1] Hsieh, J., Liu, J., Tappi J., 3(4):4(2004) [2] Page, DH, Seth, RS, Jordan, BD, Barbe, MC, "Paper Making Raw Materials", ed. J. Bender, Mechanical Engineering Publications Ltd., London, UK (1985) [3] Heitanen, S, Ebeling, K, Paperi ja Puu, 72(2):158(1990) [4] Kibblewhite, RP, Brookes, D, Appita, 28(4):227(1975) [5] Jordan, BD, Page, DH, Proc. Tappi Intl. Paper Physics Conf., p.105 (1979) [6] Seth, R.S., Page, D.H., Fiber and Tearing Resistance, International Paper Physics Conference, p.9 (1987) [7] Trepanier, R.J., Tissue World, p. 43, Oct/Nov (2009) [8] Borrego, A., "Kneading Technology Field Experience in Deinking Lines for tissue", Proceedings of TissueWorld 2009, Nice, France (March 2009) [9] Olson, J.A., Robertson, A.G., Finnigan, T.D., Turner, R.H.R., J.P.P.S., 21(11):J367(1995) [10] Trepanier, R.J., Tappi J., 81(6):153(1998) [11] Robertson, G., Olson, J., Allen, P., Chan, B., Seth, R., Tappi J., 82(10):93(1999) [12] Gogac, J., Fiserova, M., Tappi.J., p28, Aug.28 (2008) [13] Page, D.H., Barbe, M.C., Seth, R.S., Jordon, B.D., JPPS, 10(3):74 (1984). [14] Peakes, D. E., Combined High and Low Consistency Refining of Bleached Kraft Pulp, Tappi J., 50(9) 1967. Trepanier Tappi Tissue 2017 5

PULP FIBER QUALITY AND THE RELATIONSHIP WITH PAPER TISSUE PROPERTIES Roland J. Trepanier OpTest Equipment Inc. Hawkesbury, ON Canada 1

Topics: Introduction & definitions Fiber morphology & tissue properties Accurately measuring fiber length & shape Impact of fiber variations on tissue quality Modifying fiber curl & kink Meeting the Int l Standards Conclusion 2

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurate measuring Fiber Length & Shape Impact of Fiber Variations on Tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 3

Introduction & Definitions Fiber length alone is a poor predictor of final product quality Virgin and recovered fibers may have the same lengths, but different shapes will significantly affect tissue properties such as strength, bulk & softness Several US patents have been issued to major tissue manufacturers on the topic of fiber curl and tissue making 4

Introduction & Definitions Definition of curl and kink: Curl Index = (L/l) - 1 L L = Contour Length l l = End-to-end [Projected] Length Kink is an abrupt change in curvature 47 o Kink Index = {2N (21-45 ) + 3N (46-90 ) + 4N (91-180 ) }/Total L N = Number of kinks counted within a range of angles 5

Topics: Introduction & Definitions Fiber morphology & tissue properties Accurate measuring Fiber Length & Shape Impact of Fiber Variations on Tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 6

Fiber Morphology & Tissue Dry tensile strength as a function of length and curl: Strength loss with shorter & curlier fibers

Fiber Morphology & Tissue Dry tensile strength & fiber length: 8

Fiber Morphology & Tissue properties Dry tensile strength & fiber curl: Curl & kink reduces effective fiber length * 9 * Curl & kink place more strain on fiber bonds

Fiber Morphology & Tissue Wet web strength (~ 20%solids): Wet stretch increases with fiber curl Fiber bonding not a factor Mainly fiber entanglement 10

Fiber Morphology & Tissue Bulk & softness as a function of fiber curl Burrego, Tissue World 2009-Nice Curl & kink opens the sheet increasing bulk & softness 11

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurately measuring fiber length & shape Impact of Fiber Variations on Tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 12

3 Requirements to measure accurately: 1. Precisely orient fibers to correctly measure fiber length, width, curl, & kink Also, analyzes fiber bundles without plugging 2. Characterizes only cellulose 3. Measure all values simultaneously on each fiber 13

1. Precisely orient fibers to correctly measure length, width & shape values sandwich of 3 layers with cross section of 33 mm² The thin middle layer is laminar and contains fiber Clean water outer layer cytometric flow cell US Patent No. 5311290 Imaging area Center layer with fibers Clean water outer layer 14

Fiber Quality & Tissue 2. Characterize only cellulose 3 mm rayon fibers, no fines Normal sample De-aired sample Smallest air bubbles cannot be distinguished from fines! 15

2. Characterize only cellulose Using cross polarized light causes air bubbles & non cellulose contaminants to disappear There are 2 types of polarized light: Linear and Circular 16

2. Characterize only cellulose Circular Linear same fiber, different polarization Circular polarized light gives true length in 2-d 17

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurate measuring Fiber Length & Shape Impact of fiber variations on tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 18

Fiber Quality Variations & Tissue Fiber quality analyzer measured variations in Lw & CI over 18 days: -9% +60% 19 Curl Index variation is > 3x greater than Lw The variability was greater for FBK softwood

Fiber Quality Variations & Tissue Tissue made from this FBK softwood would be expected to have noticeable variations in quality. Using the relationships described earlier... 20

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurate measuring Fiber Length & Shape Impact of Fiber Variations on Tissue quality Modifying fiber curl & kink Meeting the Int l Standards Conclusion 21

Modifying Fiber Curl & Kink Any mechanical action on fibers performed at high consistency (>10%) can introduce curl into chemical and recycled pulps. It is often necessary to reduce excessive fiber curl. In general, low intensity-low consistency (LC/LI) refining helps remove curl and kink from chemical pulps 22

Modifying Fiber Curl & Kink Fiber quality analyzer results on an 80% Hwd / 20% Swd blend: 23 Energy Range ΔLw (mm) Δ Curl & Kink 0 60 kwh/bdmt < 1% > 16% 60 130 kwh/bdmt ~ 6% ~ 7%

Modifying Fiber Curl & Kink This LC/LI refining study demonstrates how excessive curl may be lowered without sacrificing fiber length. This method may be used to target curl and kink levels that provide desired tissue properties Consider the process stages of washing and bleaching a northern softwood Kraft pulp 24

Modifying Fiber Curl & Kink - Lw decreases <4% over the entire process - Exiting the last washer, the curl & kink increased >131% - LC/LI Refining brought the curl index to the target value of 12% 25

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurate measuring Fiber Length & Shape Impact of Fiber Variations on Tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 26

Meeting Int l Standards Std. Methods to measures fiber lengths: Tappi T271, PAPTAC B4 & ISO 16065-1 (Reproducibility ~3x better with polarized light!) Std. Methods to measures fiber coarseness: ISO 23713 Common specifications: - flow cell orients fibers to < 0.5 mm thin plane - light & detector spectral sensitivity match >90% - Use cross polarized light (>99% extinction) to detect only cellulose - calculate Ln, Lw, and Lww for each fiber 27

Topics: Introduction & Definitions Fiber Morphology & Tissue properties Accurate measuring Fiber Length & Shape Impact of Fiber Variations on Tissue quality Modifying Fiber Curl & Kink Meeting the Int l Standards Conclusion 28

29 Fiber Quality & Tissue Typical process variations of fiber curl & kink may occur with no appreciable change in fiber length This report shows that changes in curl & kink can significantly impact important tissue properties Precisely measuring fiber length, curl and kink is required and best achieved with technology that: correctly orients, without deforming, fibers for imaging uses circular polarized light for true 2 d analysis Controlling fiber length & curl is key to maximizing tissue quality and lowering costs, whilst managing the variability of virgin and recovered Fiber

30 Thank you Questions?