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‘Available online at werw.sciencedirectcom ‘Cement sod Concrete Resch 342004) 1229-1234 Pergamon Use of pulp and paper mill residual solids in production of cellucrete Tarun R. Naik"*, Thomas S. Friberg, Yoon-moon Chun" Contr for By-Products ition, Deparment of Ct Egaeig an Machanis,Cllege of Emcring and Appl Sine Univers of Micon Mibwaulee, PO. Boe 784, Mibwadee, WI 53201, USA "Weyerhaeuser Company, PO. Box 9777, Federal Way. WA 980839777, USA Reccved$ Febrary 2003; accepted 1 December 2003 Abstract, Fibrous residuals generated from pulp and paper mils were included in concrete. Carefully proportioned concrete mixtures containing some of the residuals showed higher compressive and splitingensile strengths than concrete without the residuals. Over, a high ‘correlation was observed between density and strength of conerete containing the residuals, By achieving equivalent density, conerte ‘containing the residuals may be produced equivalent in strength to the concrete without the residuals ‘© 2004 Elsevier Ltd All rights reserved. Keywonts Comprenive strength: Ftc riaforcoment: Paper mill rou esis, Tense properies; Waste manageeat 1. Introduction Pulp and paper mill wastewater-reatment plan residuals are the solid residue removed from mill wastewater before the water is discharged into the environment or reused in the rill, Residuals are removed via a two-step process of treating the wastewater 1-4]. ‘The primary residual isthe solid residue removed from the primary clarifier. The primary clarification is usually carried out by sedimentation and sometimes by dissolved air flotation. The primary residual consists mainly of cellulose fibers, papermaking fillers (kaolnitic clay, calcium carbon- ate, and/or titanium dioxide), and water. In some cases, ash gencrated at mils and inert solids rejected during chemical recovery processes become part ofthe primary residual. The ‘water clarified by the primary treatment is passed on to the secondary treatment, ‘The secondary treatment is usually a biological process in which microorganisms convert soluble organic matter to carbon dioxide and water while consuming oxygen. The ‘secondary residual is mainly microbial biomass (also called biosolids) grown during this process and removed through clarification, Compenig uh, Te: 14142294096 fx #1414229 on a obi: wre (ER Nak). 0008-81468 ~ ce font mater © 2004 Elev Ld. ll ight reserved. 0.10165 ceomconres 2008.12.013 Many times, primary and secondary residuals are com bined to facilitate handling. In most cases, the residuals are dewatered before they are being used or disposed of. In 1995, the US. pulp and paper industry generated about $3 million metic tons of mill wastewater-reatment residuals (on oven-dry basis), which is equivalent to sbout 15 milion metric tons of dewatered (moist) residuals. About half ofthis was disposed in landillslagoons, a quarter was ‘bumed, one-eighth was applied on furmland/forest, onc- sixtonth was reusedecycled in mills, and the rest, onc- sixtoenth, was used in other ways [5] Due to increasing cost of landfiling, increasingly stin- ‘gent environmental regulations, and potential long-term ‘environmental ibiltes the percentage of the residuals that are disposed of in landfills has decreased considerably over the past several decades [1,2,5]- However, as amount of residuals stil ned to be diverted from landfilling. ‘Numerous projects have been conducted on the use of cellulose fibers as reinforcement in pressed cement and/or sorta sheets. Cellulose fiber-reinforced cement-based sheet composites showed considerably higher flexural toughness than plain cement-based sheets [6.7]. Use of cellulose fibers reduced the extent of shrinkage cracking of mortar [8} and improved the resistance of cement-based composites to freezing and thawing [9] Being very fine and slender, cellulose fibers can be placed uniformly in concrete and can effectively bridge, suppress, and stabilize microcracks (10). It has been reported that the use of proprietary (processed) virgin cellulose fibers is effective in reducing plastic-shrinkage cracking [11] as well as drying-shrinkage cracking [12]. ‘Concrete is weak in tension (3-9 MPa). Wood celli- lose fiber is strong in tension (300-900 MP2) [13] ‘Therefore, the use of wood fibers in conerete should improve the usefulness of conerete, The fibrous residuals from pulp and paper mills could become an economical source of wood fibers for microfiber reinforcement of ‘concrete ‘No research results have been reported in any technical Jjoumals or conference proceedings, on the use of pulp and ‘paper mill residuals in structural-grade concrete. This report summarizes the results of a small-seale research project conducted on the use of the residuals in concrete. Results of an extensive research project, which was conducted later, are available elsewhere [14,15]. 2. Materials and defloceulation of the residuals 2. Cement, fine and coarse aggregates, and chemical ‘admixture ‘Type I portland cement, fine aggregate (Sand), and coarse aggregate (pea gravel with a 9.5-mm maximum size) sup- plied by a local ready-mixed concrete producer were used in this research, The cement and the aggrogates met the requirements of ASTM C 150 and C 33, respectively. The high-range water-reducing admixture (ARWRA) used in this research was an aqueous solution of 2 modified naph- thalene sulfonate and met the requirements of ASTM C 494 for Type F (HRWRA). The manufacturer’s recommended dosage rate for the HRWRA was 0,39-1.3 liter100 kg of ‘cement, 2.2. Pulp and paper mill residuals A total of three sources of fibrous residuals trom pulp and paper mills were used—one each from a de-ink paper mill in the USA, a pulp mill in the USA, and a pulp mill in Canada, Properties of the residuals are presented in Tables 1 and 2. In the research [14,15] TR. Naik to. / Coment and Conrese Research 34 2008) 1229-1286 Table? Oxides composition of ah if ter ignition of esis Resi w F x an cor 36 Dar 17a Oxide (6? Sid; 416 me sa as ALO, wa 25 98 163 co 34 ss na 267 Mo 20 16 10 49 Fas os 16 47 2a To; 49 o1 oe i 0 os 07 44 is Nn0 07 14 2 1s ™ Pest of ove-dy (105 °C) mass of rsdn, * escent of ah (1000 °C) by mas conducted later using other various sources of residuals, the properties of most of the residuals were relatively uniform and consistent. 23, Defloceulation (or “repulping”) of residuals ue to flocculation and dewatering, the as-received residuals contained moist fibrous clumps that consisted of | wood fibers, kuolin-type clay (residual N), and other par- ticles—calcium carbonates, silica (residuals F and K), and carbon (Fesidual F). These clumps may be considered as ‘weaker spots in concrete compared with well-dispersed individual fibers and particles. In addition, in order for the fibers to function efficiently as fibers, they must be sepa rated into individual fibers as much as possible. ‘Therefore, the fibrous residuals were defloceulated, or “repulped,” into separated wood fibers and particulates before they were introduced into a concrete mixture. The “spulper” used for this purpose in the laboratory consisted of a 19-lter plastic bucket and a high-speed mixer with a rotor positioned above the bottom of the bucket. Mechan- ical repulping was performed by immersing the fibrous residuals in room-temperature water with prescribed amount of HRWRA in the bucket and subjecting the mixture to a high-speed rotation by the rotor blades for not less than 20 min, HRWRA was used with the assump- tion that it would help “repulp” the residuals. However, in the research conducted later (14,15), it was shown that the “Types, physical proper, las on ignition at $90 °C ad wood fiber content of sida Residuals ‘Type of —‘ypeot Fiber Moise ‘Aveage fier Loss on ipniion Weed foe residual sign sonient(6)" Sent (asm) 890 °C content 4 x pinay pe reayled 7 146 @ a6 F Primary pulp vise 1s . a “0 x Pimy pulp ve Be 1st 8 5 ‘aerige 7 2 = M7 tt Ey 56 * erect af ove-dry (105 °C) mass of eda, Lengt-weightd everage fie length, f= 2 Notable, "Cool nt rn... 6 to slves andlor lage pricks" mdf 3, al ing Kaj F200. TTR Nath eal /Comont and Concrete Research 34 2004) 1229-1234 na ‘bles More proprtins and fresh eonctepropatis (cnt (CN) Mixure sams © ®t w SS a ra Ne Ww Resins asseecved (wo) v 2 a os 06 o7 0 12 (Gh of cone by mas) ‘Woot ier fom sia (kn) 0 uw 23 26 30 aa 39 a FHRWRA (/100 br cement) 06 to to is 22 ao aa a Resins, aereeced (mois) pla") 45 92 wos bas ba 160 a7 HRWRA (in) 23 34 35 49 69 eo 7a na Cement (ein) Po a 40 an sa 238 so 236 Sind, SSD (kp) us 190 eo us a8, or no ol Pea gave, 9 $n maximum, 1080 m8 ona sz oo 6 wm 6 ‘SSD (kgm) Ware den) 166 bs ro bs fied m2 ns 7 Wateicemon, wie 04 at os oat 04s oat oats Stamp (1) 2s as 5 ss as bs uo 0 ‘Ase cntet (4) im 86 52 >to >10 210 “ 210 Deasiy (km) zag masa 2300212020700 ™ Asrecsived moist ir wore wed The quai of he fib shown ae on oven Bass HRWRA was not helpful in repulping the residuals; a high-speed mixing of residuals in room-temperature water ‘was shown to be the most practical and satisfactory means of repulping most of the residuals that were used in the second research 3. Mixture proportions, test results, and discussions 4.1. Mixture proportions Mixture proportions and fresh properties of the concrete mixtures produced in the laboratory are shown in Tables 3 nd 4, The amount of as-received residuals in concrete ranged from 0.2% to 1.2% (by mass) for residual N and from 0.2% to 0.8% for residuals F and K. The amount of ‘wood fibers in conerete ranged from 1.1 to 6.1 kgim® for residual N, from 0.9 to 3.3 kg/m’ for residuals F, and from 1.7 to 6.3 kg/m’ for residual K (When converted to oven-dry mas). Overall, water-cement ratio (wie), slump, air content, and density were in the ranges of 0.40-0.52, 65-260 mm, 1.1->10%, and 2000-2420 kg/m’, respectively. Control mixture C and mixtures F] and F2 showed very high slump (235, 25S, and 260 mm, respectively). Mixtures NI and N3 showed high slump (185 and 165 mm). If the quantities of the mixing water in mixtures C, Fl, F2, NI, and N3 had bbeen reduced, the slump would have been lower and the Tes Mice proportions and fet concrete proper K) Mine name 7 ® 5 Fe xi @ 1m xe Resid, asreeived (ais) 02 a 06 08 2 a we ws (Gh of coneret by ras) Wood Fibers fom esis kp)? os in 23 a3 i 33 as «3 THRWRA (1100 he coment) 10 10 1 ‘0 uo 16 1 13 Resi, stecivl (sia) kgm) 48 os Ma 184 48 96 Be m1 HRWRA (im) 36 36 38 35 so sa 62 66 (Comoe tk’) 3365 33 ast 346 39 386 ue ae ‘Sand, SSD en?) 9 am a 16 = ma mr ™ Pea gavel, 93a maximum, wor 053 nests 10K0 Tn 934 SSD sin’) ‘Water (kg) 1 16 Ma 19 169 sr 13 m Wiateisemert, wie oa ost 0 a6 ost oar os” ost Samp ea) as 20 ko us uo 6s 100 M0 Air content) 12 Mt 35 47 22 20 ar 35 Density gi") ao 2380 6028802200800 ™ Asressned moist fer wer wed. Te quate of th les shown ae on oven as a2 TR Nai to / Come ad Concrete Research 34 (2006) 1229-1286 Mitre ane KD KS KS Fig. 1. Compressive seat of concrete 2128 dys, strength higher. Concrete mixtures containing residual N showed very high air contents and low densities, In general the density of the concrete decreased as the amount of residuals increased. Density values of residual N’ mixtures ‘were considerably lower than that of the control mixture. Density values of residuals F and K mixtures were some- What lower than that of the control mixture. 4.2. Compressive and spliting-tensile strengths Compressive and spliting-tensile strengths of concrete were determined at 28 days by testing three 100 > 200-mm cylinders for each test type. Test results are presented in Figs. 1 and 2, Most of the F and K mixtures were equivalent (o the control conerete in compressive strength and spliting-tensie strength. Within each group of resid- uals Nand K concrete mixtures, compressive and split ting—tensile strengths generally decreased as the amount of residuals increased, probably due to the reduction in the density of the conerete. In addition, a considerable retar- dation of concrete mixture N7 was noted for about 3 days, due fo the use of excessive amount of HRWRA (4.1 vs, 1.3 | [the recommended maximum]/100 kg of cement). Rela- tively large doses of HRWRA in mixtures N4, NS, and N6 ‘might also have caused some delays in the setting of the concrete, On the other hand, the quantities of HRWRA used in mixtures C, NI, N2, FI, F2, F3, and F4 were lower (© NUND ND NONS KGNT FLED FD FUKI KD KS KS Fig 2. Spitinganile strength af concrete a 28 dys 5 2-day spliting tense strength MHP) > 1 » 0 0 09 @ 28-day compressive strength (MPa) Fig. 3, Relation between the 28-ay compressive and sping esl seen of cone than the maximum recommended by the manufacturer, and no considerably delayed settings of these mixtures are suspected. ixtures F3 and F4 showed higher compressive strength than mixtures FI and F2, respectively. This may be aitrib- uted to lower wle of F3 and F mixtures compared with EL and F2 mixtures, respectively. Spliting-tensile strength values of mixtures F3 and F4 were higher than that of mixture F2 and were nearly equivalent to that of mixture FI If less water had been used in mixtures FI and F2, higher strengths of these concrete mixtures would have been ‘obiained; also, the slump would have been comparable to that of mixtures F3 and F4, Overall, the compressive strength and splitting tensile strength of conerete showed a very good correlation (Fig. 3). In general, compressive and spitting-tensle strengths of Concrete containing the residuals were proportional to the density of concrete (Figs. and 5). To make the strength of é 0.7708 a 2 50 4 wa :

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