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(12) United States Patent (10) Patent No.: US 9,109,118 B2 Joyce Et Al

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(12) United States Patent (10) Patent No.: US 9,109,118 B2 Joyce Et Al US009 109118B2 (12) United States Patent (10) Patent No.: US 9,109,118 B2 Joyce et al. (45) Date of Patent: *Aug. 18, 2015 (54) CELLULOSIC INCLUSION 5,075.359 A * 12/1991 Castagna et al. ................ 524, 13 THERMOPLASTC COMPOSITION AND 5,346,773 A * 9/1994 Simoens ........ ... 428,476.9 5,403,667 A * 4/1995 Simoens ..... ... 428/479.6 MOLDING THEREOF 5,882,745 A * 3/1999 Miet al. .......................... 428/15 5.948,524 A 9/1999 Seethamraju et al. (71) Applicants: Innovative Plastics and Molding, 6,270,883 B1* 8/2001 Sears et al. ................. 428,292.1 Lambertville, MI (US); RheTech, Inc., 6,294,602 B1* 9/2001 Shimo et al. ... ... 524,394 6,376,584 B1 * 4/2002 Galbo et al. ....... ... 524/102 Whitmore Lake, MI (US) 6,682,789 B2 * 1/2004 Godavarti et al. .............. 428/34 6,835,764 B2 * 12/2004 Leckey et al. ................... 524/15 (72) Inventors: Robert C. Joyce, Lambertville, MI 7,862,746 B2 * 1/2011 Kaspers et al. ... ... 252/.397 (US); Andrew Hopkins, Sylvania, OH 8,122,996 B2 * 2/2012 Kajihara et al. ... ... 181,169 (US); Harutun George Karian, 8,546,470 B2 * 10/2013 Joyce et al. ..................... 524/14 Brighton, MI (US) 2003/0022962 A1* 1/2003 Cook et al. ..... ... 523, 164 2004/0122133 A1* 6/2004 Mohanty et al. ................ 524/35 2004/O126515 A1* 7, 2004 Yarmoska ...... ... 428/34.1 (73) Assignee: RHETECH, INC., Labertville, MI (US) 2005/0154094 A1* 7/2005 Maeda et al. ................... 524/35 2006/0084764 A1* 4/2006 Hanna et al. ... 525/242 (*) Notice: Subject to any disclaimer, the term of this 2006/0091578 A1* 5, 2006 Bravo et al. .... ... 264,122 patent is extended or adjusted under 35 2007/0027234 A1* 2/2007 Sigworth et al. ................ 524, 13 U.S.C. 154(b) by 12 days. (Continued) This patent is Subject to a terminal dis claimer. FOREIGN PATENT DOCUMENTS DE 2427080 12, 1975 (21) Appl. No.: 14/037,453 EP O319589 6, 1989 (22) Filed: Sep. 26, 2013 (Continued) OTHER PUBLICATIONS (65) Prior Publication Data Injection Molding Handbook: The Complete Molding Operation US 2014/0O24746A1 Jan. 23, 2014 Technology, Performance, Economics Edited by Donald V. Rosato and Dominick V. Rosato, Champman & Hall, Norwell, Massachu Related U.S. Application Data setts, 2nd Edition, 1999. The Efficiency of Cellulosic Fillers in Common Thermoplastics. Part (63) Continuation of application No. 13/158,742, filed on 1. Filling Without Processing Aids or Coupling Agents, C. Klason, J. Jun. 13, 2011, now Pat. No. 8,546,470, which is a Kub, H-E Stormvall, International Journal of Polymric Materials, continuation-in-part of application No. 12/321,093, 10(3), pp. 159-187, 1984. filed on Jan. 15, 2009, now Pat. No. 7,994,241, which Wood-Plastic Composites as Promising Green-Composities for Automotive Industries Alireza Ashori, Bioresource Technology 99, is a continuation-in-part of application No. pp. 4661-4667, 2008. 12/354,310, filed on Jan. 15, 2009, now abandoned. The Nature of Adhesion in Composites of Modified Cellulose Fibers and Polypropylene Johan M. Felix and Paul Gatenholm, Journal of (60) Provisional application No. 61/021,234, filed on Jan. Applied Polymer Sciene 42, pp. 609-620, 1991. 15, 2008. Role of Maleated Coupling Agents on the Interface Adhesion of Polyproplene-Wood Compsites, C.A. Correa, C.A. Razzino and E. (51) Int. Cl. Hage, Jr., Journal of Thermoplastic Composite Materials 20, pp. COSL 97/02 (2006.01) 323-339, 2007. COSL I/O (2006.01) (Continued) C08G 18/38 (2006.01) COSR 7/14 (2006.01) Primary Examiner — Liam J Heincer COSL 77/02 (2006.01) (74) Attorney, Agent, or Firm — Blue Filament Law PLLC; COSL 77/06 (2006.01) Avery N. Goldstein (52) U.S. Cl. CPC ............. C08L97/02 (2013.01); C08G 2120/00 (57) ABSTRACT (2013.01); C08K 7/14 (2013.01); C08L 77/02 A cellulosic inclusion-thermoplastic composition that (2013.01); C08L 77/06 (2013.01) includes cellulosic inclusions and a thermoplastic polyolefin (58) Field of Classification Search that forms a matrix in which the cellulosic inclusions are CPC .......... C08L97/02: C08L 23/12: C08L 23/06 dispersed. A maleated polymer and a polar thermoplastic USPC ...................................................... 524/13, 14 polymer resin of a polyamide or polyester are provided to See application file for complete search history. improve adhesion between the cellulosic inclusions and the thermoplastic polyolefin. The polar thermoplastic polymer (56) References Cited resin is characterized by a melting temperature greater than that of the thermoplastic polyolefin. The composition as pro U.S. PATENT DOCUMENTS vided has increased break tensile strength relative to a com position devoid of the polar thermoplastic polymer resin but 3,864,427 A * 2/1975 Nakane et al. ................ 52.5/17O 4.323,625. A * 4, 1982 Coran et al. ..... ... 428.361 otherwise is unchanged. The break tensile is measured at 23° 4,403,007 A * 9/1983 Coughlin ..... ... 428/95 Celsius and at an elongation rate of 50 millimeters perminute. 4,438,228 A * 3/1984 Schenck .. 524/109 5,030,662 A * 7/1991 Banerjie ...................... 521, 43.5 25 Claims, 7 Drawing Sheets US 9,109,118 B2 Page 2 (56) References Cited Janos Moczo and Bela Pukanszky, Polymer Eng. & Sci. 47, pp. 1246-1255, 2007. U.S. PATENT DOCUMENTS Wood Flour Filled PPComposites: Compatibilization and Adhesion, Livia Danyadi, Tunde Janecska, Zoltan Szabo, Gabor Nagy, Janos 2007/0208110 A1* 9/2007 Sigworth et al. ................ 524f13 Moczo and Bela Pukanszky, Composities Science and Technology 2009/0182071 A1* 7/2009 Joyce ............. ... 524/13 2009/0321981 A1* 12/2009 Hopkins et al. ............... 264/128 67, pp. 2838-2846 2007. 2010.0062670 A1 3/2010 Bastioli et al. ................ 442/327 Polypropylene/Polyamide-6 Blends: Influence of Compatibilizing 2011/0245380 A1* 10/2011 Joyce et al. ..................... 524f13 Agent on Interferance Domains, J. Roeder, R.V.B. Oliveria, M.C. Goncalves, V. Soldi and A.T.N. Pires, Polymer Testing 21, pp. 815 FOREIGN PATENT DOCUMENTS 821 2003. Wood/Plastic Composities(WPC) With Glass Fiber EP O540O26 5, 1993 Reinforcement(GRF), Ghaus M. Rizvi and Hamid Semeralul, Antec EP O586212 3, 1994 2006, pp. 224-227. FR 2270311 12, 1975 The Effect of Wood Extractives on the Thermal Stability of Different FR 2344101 1Of 1977 Wood Species, A.N. Shebani, A.J. van Reenen and M. Meincken. FR 2365 019 4f1978 Thermochimica Acta 471, 43-50, 2008. FR 2564374 11, 1985 Effects of Wood Fiber Characteristics on Mechanical Properties of GB 2036148 6, 1980 Wood/Polypropylene Composites, Nichole M. Stark and Robert GB 2104903 3, 1983 GB 217 1953 9, 1986 Rowlands, Wood and Fiber Science 35(21), pp. 167-174, 2003. GB 218665.5 8, 1987 Effect of Particle Size on Properties of Wood-Flour Reinforced WO 9008O20 7, 1990 Polypropylene Composities, Nicole M. Stark and Mark J. Berger 4th, WO 92O7022 4f1992 International Conference on Woodfiber-plastic composites, 1997. Composition of Wood-Plastic Composite Deck Boards: Thermoplas OTHER PUBLICATIONS tics, Anatole A. Klysov, John Wiley & Sons, NY, 1st Edition (2007). Wood Flour Filled Polypropylene Composites: Interfacial Adhesion and Micromechanical Deformations, Livia Danyadi, Karoly Renner, * cited by examiner U.S. Patent Aug. 18, 2015 Sheet 1 of 7 US 9,109,118 B2 t 8808«? g 3. s {& 3%33-333333333s 3:33:33. U.S. Patent Aug. 18, 2015 Sheet 4 of 7 US 9,109,118 B2 -No.?600)- {388: 83-8:333,338. 33.38x3; U.S. Patent US 9,109,118 B2 *------------~--~~~~~*~~~~~~~~*~~~~~~~~~~~&~~~~~~~.~~~~~~------+-------------------&-------------------+-------~--~~~~.~~~~}--~~~~ ************?«$s;& *********3;&#}&&&&&&&&~$$ $$$$$$ $$$$ §§§ 388x33x933-&233:33%; 332.33333; U.S. Patent Aug. 18, 2015 Sheet 6 of 7 388: p33}83-883: 3:3: 2: 3:33, U.S. Patent Aug. 18, 2015 Sheet 7 of 7 US 9,109,118 B2 #-----~~~~);-------------------~*~~~~*~ ~~~~*~~~~~~~~~~~~~~~~ ------------~#~#~~~~---+-----------------+~~~~#~~~~--~~~~*~~~~~~~ - -----~--~~~~);--~~~~~~~~.~~~~)-(< 3 :33:39 x: US 9,109,118 B2 1. 2 CELLULOSIC INCLUSION the molded parts has proved costly and difficult, most com THERMOPLASTC COMPOSITION AND monly being achieved through fiber pre-processing or encap MOLDING THEREOF sulation of the fiber in the thermoplastic. Wood fibers are hydrophilic materials that are poorly wet CROSS-REFERENCE TO RELATED by molten hydrophobic thermoplastic polymers resulting in APPLICATIONS poor flow characteristics, difficult processability, and prema ture fiber pull-out, all of which leads to molded products with This application is a continuation of U.S. patent applica poor appearance and inferior mechanical properties. Property tion Ser. No. 13/158,742 filed Jun. 13, 2011, that in turn is a improvement has been addressed through the use of "com continuation in part of U.S. patent application Ser. No. 10 patibilizing materials that adhere to both the polar fibers and 12/321,093 filed 15 Jan. 2009 and is a continuation in part of the non-polar polymer resin. Most common has been the use U.S. patent application Ser. No. 12/354,310 filed 15 Jan. of a maleic anhydride grafted polypropylene copolymer. See, 2009, both of which in turn claim priority benefit of U.S. Provisional Patent Application Ser. No. 61/021,234 filed Jan. for example, U.S. Pat. No. 5,948,524 and “Wood Flour Filled 15 Polypropylene Composites: Interfacial Adhesion and Micro 15, 2008, these prior applications are incorporated herein by mechanical Deformations’, L. Danyadi et al., Polym. Eng. & reference. Sci. 47(8), pp 1246-1255 (August 2007). Typically, wood FIELD OF THE INVENTION flour-polypropylene composite (WPC) pellets are manufac tured via compounding extrusion equipment followed by The present invention in general relates to a composition thermoplastic post-forming processes such as injection mold containing cellulosic inclusions dispersed in a thermoplastic ing or profile extrusion. The engineering of desirable process polymeric matrix and in particular to Such a composition with ing and physical properties into a WPC is further complicated improved distribution of the cellulosic inclusions and physi by the addition of other substances such as reinforcing glass cal properties.
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