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United States Patent (10) Patent No.: US 9.458,297 B2 Miller (45) Date of Patent: Oct

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United States Patent (10) Patent No.: US 9.458,297 B2 Miller (45) Date of Patent: Oct USOO9458297B2 (12) United States Patent (10) Patent No.: US 9.458,297 B2 Miller (45) Date of Patent: Oct. 4, 2016 (54) MODIFIED FIBER, METHODS, AND 4,898,642 A 2f1990 Moore SYSTEMS 4,900,324 A 2f1990 Chance 4,935,022 A 6, 1990 Lash (71) Applicant: WEYERHAEUSERNR COMPANY., 4,936,8651538 A S366, 1990 WelchWE Federal Way, WA (US) 5,049,235 A 9, 1991 Barcus 5,137,537 A 8, 1992 Herron (72) Inventor: Charles E. Miller, Federal Way, WA 5,5,160,789 183,707 A 11/19922f1993 BarcusHerron (US) 5, 190,563 A 3/1993 Herron 5,221,285 A 6/1993 Andrews (73) Assignee: WEYERHAEUSERNR COMPANY., 5,225,047 A 7, 1993 Graef Federal Way, WA (US) 5,247,072 A 9/1993 Ning et al. 5,366,591 A 11, 1994 Jewell (*) Notice: Subject to any disclaimer, the term of this 3.222 A 8.32 Shiki patent is extended or adjusted under 35 5,496.476 A 3/1996 Tang U.S.C. 154(b) by 0 days. 5,496.477 A 3/1996 Tang 5,536,369 A 7/1996 Norlander (21) Appl. No.: 14/320,279 5,549,791 A 8/1996 Herron 5,556,976 A 9, 1996 Jewell 1-1. 5,562,740 A 10, 1996 Cook (22) Filed: Jun. 30, 2014 5,698,074. A 12/1997 Barcus 5,705,475 A 1, 1998 T (65) Prior Publication Data 5,728,771 A 3, 1998 E. 5,843,061 A 12/1998 Chauvette US 2015/0376347 A1 Dec. 31, 2015 5,873,979 A 2f1999 Naieni 5,981,739 A 11/1999 Anderson (51) Int. Cl. 5.998,511 A 12/1999 Westland C08 3/24 (2006.01) 6,300,259 B1 10/2001 Westland BOI, I/24 (2006.01) 2. R. 39 I - w ae D2IC 9/00 (2006.01) 6,620,865 B2 9, 2003 Westland (52) U.S. Cl. 2002/0090511 A1* 7, 2002 Smith ............... A61F 13,15203 CPC ............... C08J 3/24 (2013.01); B01J 19/2405 428/392 (2013.01); D21C 9/00 (2013.01); B01.J. 2003/O121623 A1* 7/2003 Westland ................ A61L F5 2219/24 (2013.01); C08.J 2301/02 (2013.01); 2006/0142478 A1 6/2006 Luo et all C08J 2333/02 (2013.01) 2011/0077354 A1 3/2011 Stoyanov et al. (58) Field of Classification Search CPC ... C08J 3/24: CO8J 2301/02: C08J 2333/02: OTHER PUBLICATIONS B01J 19/2405; B01J 2219/24 See application file for complete search history. Black Clawson Pulping Machines and Systems, 1985, p. 1-12.* (56) References Cited * cited by examiner U.S. PATENT DOCUMENTS Primary Examiner — Robert Jones, Jr. (74) Attorney, Agent, or Firm — Christensen O'Connor 3,224,926 A 12/1965 Bernardin Johnson Kindness PLLC 3.241,533 A 3, 1966 Balmer 3.241,553 A 3/1966 Steiger 3,440,135 A 4/1969 Chung (57) ABSTRACT 3,526,048 A 9, 1970 Rowland 3,658,613 A 4/1972 Steiger Methods of forming crosslinked cellulose include mixing a 3,664,795. A 5, 1972 Heinz et al. crosslinking agent with an aqueous mixture of cellulose 3,756,923 A 9, 1973 Dahms fibers containing little to no excess water (e.g., Solids content 3,819,470 A 6, 1974 Shaw of 25-55%), drying the resulting mixture to 85-100% solids, 3,932.209 A 1/1976 Chatterjee 4,035,147 A 7/1977 Sangenis then curing the dried mixture to crosslink the cellulose 4,285,690 A 8, 1981 North fibers. Systems include a mixing unit to form, from an 4.332.586 A 6, 1982 North aqueous mixture of unbonded cellulose fibers having a 4,391,878 A 7, 1983 Drach Solids content of about 25-55% and a crosslinking agent, a 4,396,391 A 8, 1983 North Substantially homogenous mixture of non-crosslinked, 4.420,368 A 12/1983 Drach unbonded cellulose fibers and crosslinking agent; a drying 4,431,481 A 2f1984 Drach 4,455,416 A 6/1984 Floyd unit to dry the Substantially homogenous mixture to a 4,505,712 A 3/1985 Floyd consistency of 85-100%; and a curing unit and to cure the 4,689,118 A 8, 1987 Makoui crosslinking agent to form dried and cured crosslinked 4,820,307 A 4, 1989 Welch cellulose fibers. Intrafiber crosslinked cellulose pulp fibers 4,822,453 A 4, 1989 Dean 4,853,086 A 8, 1989 Graef produced by Such methods and/or systems have a chemical 4,888,093 A 12/1989 Dean on pulp level of about 2-14% and an AFAQ capacity of at 4,889,595 A 12/1989 Herron least 12.0 g/g. 4,889,596 A 12/1989 Schoggen 4,889,597 A 12/1989 Bourbon 28 Claims, 5 Drawing Sheets U.S. Patent US 9,458,297 B2 U.S. Patent Oct. 4, 2016 Sheet 2 of 5 US 9,458,297 B2 Anslubuopueun?uansuonn?osAnsluauojovedu? 3/8 'exed nunupceW U.S. Patent Oct. 4, 2016 Sheet 3 of 5 US 9.458,297 B2 |SS300.Jdqu?Jun0, NA?NwSS300/d % 8 ???????????????????????????????????????????????????? ‘dOO 3/3 "Aloedeo ov-w U.S. Patent Oct. 4, 2016 Sheet 4 of 5 US 9.458,297 B2 uo??n?OS%0Zw uO??n?OS%99zL. ___________________________________________%0?7V7|UO!?ñ|OS 3/3 "Aloedebow-w || | || |-----~l-----!-----i)----)? U.S. Patent Oct. 4, 2016 Sheet S of 5 US 9,458,297 B2 3/3 'Apedeo Ow-w |-~~~~|~~~~~~|~~~~~~~)--~~~~); US 9,458,297 B2 1. 2 MODIFIED FIBER, METHODS, AND crosslinking. The methods further include drying the result SYSTEMS ing mixture to 85-100% solids, then curing the dried mixture to crosslink the cellulose fibers. In some methods, the solids TECHNICAL FIELD content of the aqueous mixture is about 25-55%. Some methods include forming the aqueous mixture, Such as by hydrapulping cellulose fibers from, for example, fibers pro This disclosure relates to methods of and systems for vided in bale or roll form. forming modified fiber, in particular intrafiber crosslinked In one particular, non-limiting example of such a method, cellulose fiber. an aqueous mixture of unbonded cellulose fibers having a solids content of about 40-50% is formed, followed by BACKGROUND 10 mixing a polyacrylic acid crosslinking agent with the aque ous mixture in an amount to achieve a chemical on pulp Traditionally, cellulose fibers from southern pine and level of about 2-14%, wherein said crosslinking agent is other Softwood species are used in absorbent products in mixed at ambient conditions. The resulting mixture is then large part because the morphology of these fibers provides dried and cured as above. good absorbent performance. Compared to hardwood fibers, 15 In another aspect, the present disclosure provides embodi southern pine and other softwood fibers tend to be longer ments of a system for forming crosslinked cellulose prod (e.g., having a length weighted fiber length of about 2.5 mm) ucts, which include a mixer configured to form, from an and more coarse (e.g., having a coarseness greater than aqueous mixture of unbonded cellulose fibers having a about 20 mg/100 m), and form low density pads with Solids content of about 25-55% and a crosslinking agent, a sufficient void volume to hold several times their weight in Substantially homogenous mixture of non-crosslinked, liquid. Hardwood fibers, on the other hand, are known for unbonded cellulose fibers and crosslinking agent, at ambient their performance in paper applications where shorter fiber conditions. The system further includes, downstream of the length (e.g., about 1 mm) and lower coarseness (e.g., less mixer, a dryer configured to dry the Substantially homog enous mixture to a consistency of 85-100% without curing than about 20 mg/100 m) provide a dense structure and the crosslinking agent; and a curing unit coupled to the dryer Smooth paper Surface. 25 that is configured to cure the crosslinking agent, thereby Crosslinked cellulose fibers are usually produced by forming dried and cured crosslinked cellulose fibers. applying a crosslinking agent to a dried sheet or roll of In another aspect, the present disclosure provides intra conventional Softwood pulp fibers, generally at a dilute fiber crosslinked cellulose pulp fibers having a having a concentration to ensure chemical impregnation of the sheet, chemical on pulp level of about 2-14% and an AFAQ followed by wet fiberization in a hammermill to generate 30 capacity of at least 12.0 g/g. In some embodiments, the treated, individualized cellulose fibers. These fibers are then cellulose fibers are, or include, hardwood cellulose pulp dried, such as in a flash drier, and cured, such as in an oven. fibers, such as eucalyptus cellulose pulp fibers. The resulting fibers exhibit intrafiber crosslinking in which The concepts, features, methods, and component configu the cellulose molecules within a cellulose fiber are cross rations briefly described above are clarified with reference to linked. Intrafiber crosslinking generally imparts twist and 35 the accompanying drawings and detailed description below. curl to the cellulose fiber, and also imparts bulk to the fiber, properties that are advantageous in Some absorbent prod BRIEF DESCRIPTION OF THE DRAWINGS uctS. One drawback of this method is the high capital cost of FIG. 1 is a schematic representation of an illustrative, the production process, as well as high energy costs due to 40 non-limiting embodiment of a system suitable for producing drying the fiber prior to curing. Another drawback is that wet crosslinked cellulose fibers in accordance with one aspect of hammermilling can generate fiber and chemical buildup the present disclosure.
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