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(12) United States Patent (10) Patent No.: US 9,096.974 B2 Ranocchia Et Al

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(12) United States Patent (10) Patent No.: US 9,096.974 B2 Ranocchia Et Al US009096974B2 (12) United States Patent (10) Patent No.: US 9,096.974 B2 Ranocchia et al. (45) Date of Patent: Aug. 4, 2015 (54) PROCESS FOR PRODUCING MODIFIED (58) Field of Classification Search CELLULOSE PULPS, CELLULOSE PULP USPC ................ 162/10, 141, 140, 168.3, 175, 178, THUS OBTANED AND USE OF 162/1811, 1812, 1818, 158, 164.1 BOPOLYMER FOR PRODUCING See application file for complete search history. CELLULOSE PULPS (56) References Cited (75) Inventors: Romolo Ranocchia, São Paulo-SP (BR): U.S. PATENT DOCUMENTS Ademilson Massoquete, Aracruz-ES (BR); Danilo Oyakawa, São Paulo-SP 4,756,801 A 7, 1988 Joinen et al. 4,927.498 A 5/1990 Rushmere (BR) 7,303,654 B2 * 12/2007 Tokarz et al. .............. 162,181.8 (73) Assignee: Fibria Cellulose S/A, Aracruz (BR) FOREIGN PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this EP O 148 647 A1 7, 1985 patent is extended or adjusted under 35 EP 1 08O 271 B1 3, 2001 WO WO 2004/046464 A1 6, 2004 U.S.C. 154(b) by 0 days. WO WO 2007/078247 A1 7/2007 (21) Appl. No.: 13/636,075 OTHER PUBLICATIONS (22) PCT Filed: Mar. 21, 2011 International Search Report and Written Opinion for International Application No. PCT/BR2011/000071, mailed Sep. 14, 2011. (Under 37 CFR 1.47) International Preliminary Report on Patentability for International Application No. PCT/BR2011/000071, mailed Sep. 17, 2012. (86). PCT No.: PCT/BR2O11AOOOOT1 International Preliminary Reporton Patentability for Application No. S371 (c)(1), PCT/BR2010/000081 dated Sep. 25, 2012. (2), (4) Date: Aug. 2, 2013 * cited by examiner (87) PCT Pub. No.: WO2011/113126 Primary Examiner — Mark Halpern PCT Pub. Date: Sep. 22, 2011 (74) Attorney, Agent, or Firm — Alston & Bird LLP (65) Prior Publication Data (57) ABSTRACT US 2013/0228297 A1 Sep. 5, 2013 The present invention relates to an improved process for producing chemical cellulose pulp wherein biopolymers are (30) Foreign Application Priority Data added immediately before, during or after a bleaching step, depending on pulp characteristics and on process conditions Mar. 19, 2010 (WO)................ PCT/BR2O1 O/OOOO81 used. The biopolymers according to the present invention are starch by an etherification reaction. This treatment results in a differentiated pulp having improved physical, chemical and (51) Int. Cl. mechanical properties when compared with cellulose pulps D2 IIH 7/28 (2006.01) obtained by traditional processes. The use of said biopolymer D2C3/22 (2006.01) alters the relations between important pulp properties render D2C5/02 (2006.01) ing their application in papermaking process advantageous. D2IC 9/00 (2006.01) This differentiation increases the possibilities of use and also D2IC 9/10 (2006.01) of new applications, including for the Substitution of pulps D2 IIH 7/2 (2006.01) produced from other cellulose sources. Thus, the present D2 IIH 7/24 (2006.01) invention also relates to a process for the preparation of paper, (52) U.S. Cl. Such as printing, writing, decorative, special or tissue-type CPC ................ D2IH 17/28 (2013.01); D21C3/222 papers, through the use of the cellulose pulps modified by the (2013.01); D2IC5/025 (2013.01); D2IC 9/005 above process. (2013.01); D2IC 9/1036 (2013.01); D21H 17/21 (2013.01); D21H 17/24 (2013.01) 5 Claims, 9 Drawing Sheets U.S. Patent Aug. 4, 2015 Sheet 1 of 9 US 9,096.974 B2 in a rar as AcEra: -e-Aletics 50 so to Tensile index the FIG. 1 - - - A -- AlcBranco re- Alesio-1,5% G 70 B Tensile index (Nm/g) FIG 2 2 r - r s - Actrarco O -- AlcBio 1-t,5% . Cls O t O C) B O 8O Tensile index (Ning FIG. 3 U.S. Patent Aug. 4, 2015 Sheet 2 of 9 US 9,096.974 B2 A Achite area. AcBio2-15% 456 1, s 50 SO 7 Tensile index Nim? ) * * * * * * Ace -- AcBio21.5% SO SO Tensile index Ning) F.G. 5 is e i A is is AcWhite -ieran AcBio2-15% U.S. Patent Aug. 4, 2015 Sheet 3 of 9 US 9,096.974 B2 wa-how to Bict Akt : ** "A" AcWhite i X g9 9 ---. Elo Aic 23 3. 3. Tensile index , Nantg U.S. Patent Aug. 4, 2015 Sheet 4 of 9 US 9,096.974 B2 -0-1's BioAc o 35 40 Tensile index , Nimig --&- - - AtkWhite -a- 1% Biof Alc 3S 40 45 Tensile index , Nmig FIG 11 -8-1.2% bio3Ac g af g 35 40 45 SO Tensile index , Nmg FIG. 12 U.S. Patent Aug. 4, 2015 Sheet 5 Of 9 US 9,096.974 B2 -8-1.2%Bio3AC 45 SO Tensile index Nim?g FIG. 13 - er AcWhite -O-2%. Bio3Act SO 55 B 35 U.S. Patent Aug. 4, 2015 Sheet 6 of 9 US 9,096.974 B2 resistance (gfiSOmm) x pulp type MD CD 800 reference 0,5% BP 1,0% BP 1.0% BP+ starch FIG. 15 0 reference o 0.5% biopolymer a 1.0% biopolymer A 1.0% biopolymer + starch 90 88 86 0 86O 87 84 82 78 78 76 74. 72 A 72 70 I T t I 200 250 300 350 400 450 500 550 600 GMT (gif|50mm) FG 16 U.S. Patent Aug. 4, 2015 Sheet 7 Of 9 US 9,096.974 B2 GMT thickness reference 222 0,1420 +1.5% -4% 0,5% BP +64% 255 0,1359 -7% 1,0% BP 363 0,1327 1,0% BP+Starch 581 O,12O6 FIG.17 solid content (%) x pulp type es S ka S es C s ors - ada C o reference 0,5% BP 1,0% BP 1,0% BP+starch FIG. 18 U.S. Patent Aug. 4, 2015 Sheet 8 of 9 US 9,096.974 B2 offset paper - industrial test 98.4 912 Standard 1.0% biopolymer FIG. 19 offset paper - industrial test 4,9 Standard 1.0% biopolymer FIG. 20 U.S. Patent Aug. 4, 2015 Sheet 9 Of 9 US 9,096.974 B2 solid content before press 54.3% SS 44,6% C CD - O () O C Standard 1.0% biopolymer FIG 21 US 9,096.974 B2 1. 2 PROCESS FOR PRODUCING MODIFIED this document teaches a polymer that must be added to the CELLULOSE PULPS, CELLULOSE PULP final cellulose pulp very close to the papermachine to keep a THUS OBTANED AND USE OF big formed floc and improve drainage. Examples 2 and 3 of BOPOLYMER FOR PRODUCING this document mention a compoZil additive, that is, a combi CELLULOSE PULPS nation of two products to improve flocculation alone. Document U.S. Pat. No. 4,756,801 teaches the addition of cationic starch in particular to the papermaking process to This application is a 371 of PCT/BR11/00071 filed 21 Mar. obtain a bonding agent in order to use different kinds of pulps 2011 and fillers in the paper production. The examples contained in this document again mentions additives as retention aids, FIELD OF THE INVENTION 10 which is its well known application for polymers in paper making processes. The present invention relates to a process for the produc Document EP1080271 exclusively refers to a papermaking tion of cellulose pulps for enhancing said bleached pulps process and to the use of polysaccharides as a retention aid, quality and applicability, especially their mechanical strength where a secondary effect could be the strength. Besides, these and drainability properties, by incorporating biopolymers 15 polysaccharides must to have an aromatic hydrophobic specifically developed as additive into producing process group. This patent is also related to a minimum conductivity recipe of said differentiated cellulose pulp. suspension. It is also the case of document EP0148647, which discloses a papermaking process. In the example 1, the appli BACKGROUND OF THE INVENTION cation of polymer was carried out for softwood (long fibers) and starch was added just before the paper sheet formation. In addition to forest developments and treatments directed The result obtained in accordance to that example was reten to paper manufacturing process for developing mechanical tion of the pulp Suspension during the paper sheet formation. strength and other equally important properties, in the last Example 2 in turn mentions the combination of products in few years, researchers of the sector have been working on order to improve retention also using softwood as fiber fur additives association as the most promising means to enhance 25 nish. Thus, this document refers to a polymer is used as these properties in cellulose manufacturing process itself. additive to attach fines and fillers to form flocs and improve Among the additives that have been used for manufacturing retention. paper are the longer fibers, glues, dry and wet strength agents, Document WO2004/046464 mentions the treatment of cel starch, and others. lulosic material with clay and the secondary use of starch or Document WO 00/28141 describes a method for treating 30 other products as a retention aid. The main objective of this lignocellulosic fibrous materials for enhancing the mechani document is to produce cellulose with filler, were the second cal strength and humidity properties of the final product, ary additives are only to become it possible. which comprises fibrous materials, in which paper is the In view of the above, it can be seen that it is already known major example. The treatment involves the application of for prior art to use polymers such as starch but as retention lignin derivatives in a solvent system with secondary addi 35 aids in the production of paper. tives which consist of a broad scope of Sugars and natural Accordingly, the object of the present invention is the use polymers.
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