DECLARATION OF DAVID A. ROCKSTRAW, PH.D., P.E.
`DECLARATION OF DAVID A. RoCKsTRAw, PH.D., P.E.
`UNITED STATES PATENT NO. 8,962,059
`UNITED STATES PATENT No. 8,962,059
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`HYDRITE EXHIBIT 1005
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`TABLE OF CONTENTS
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`Page
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`George R. Alther article, “Put the Breaks on: Removal of fats,
`oil, and greases is necessary to recycle water and meet
`discharge limits.” Chemical Engineering, Vol. 5, No. 3, March
`
`U.S. Patent No. 4,662,990 (“Bonanno”) May 5, 1987 (Ex.
`
`Qualifications and Professional Experience ........................................ 1
`I.
`Information Considered In Forming My Opinions ............................. 2
`II.
`Scope Of Opinions ............................................................................... 3
`III.
`IV. Background of the ’059 Patent ............................................................ 3
`V.
`Legal Principles ................................................................................... 8
`A.
`Prior Art and Person of Ordinary Skill in the Art ..................... 8
`B.
`Obviousness ............................................................................... 9
`VI. Chemistry and Terminology .............................................................. 12
`A.
`Functionalized ......................................................................... 12
`B.
`Alkylate ................................................................................... 12
`C.
`Alkoxylate ............................................................................... 15
`D.
`Surfactants ............................................................................... 16
`E.
`Polysorbates ............................................................................. 16
`VII. Relevant Prior Art .............................................................................. 18
`A. U.S. Patent Application Publication No. 2008/0110577
`(“Winsness”) May 15, 2008 (Ex. 1012) .................................. 18
`B.
`1998 (“Alther”) (Ex. 1007) ..................................................... 19
`C.
`1006) ........................................................................................ 20
`D. U.S. Patent No. 5,283,322 (“Martin”) Feb. 1, 1994 (Ex. 1010)
` ................................................................................................. 21
`E.
`1011) ........................................................................................ 22
`F.
`(“Scheimann”) Sep. 13, 2007 (Ex. 1014) ................................ 23
`G. U.S. Patent No. 7,309,602 (“David”) December 18, 2007 (Ex.
`1013) ........................................................................................ 23
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`U.S. Patent No. 5,558,781 (“Buchold”) Sept. 24, 1996 (Ex.
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`U. S. Patent Application Publication US2007/0210007 A1
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`The HLB System: a time-saving guide to emulsifier selection
`
`IUPAC-IUB Commission on Biochemical Nomenclature, The
`Nomenclature of Lipids, Biochem. J. (1978) 171, 21–35
`
`V. K. Babayan. “Specialty Lipids and their Biofunctionality.”
`
`International Union of Pure and Applied Chemistry,
`“Compendium of Chemical Terminology,” Second Edition, pp.
`
`Surfactant Systems,” Nat. Stand. Ref. Data Ser., Nat. Bur.
`Stand. (U.S.), 36,227 pages , pages 1–7 (Feb. 1971)
`
`TABLE OF CONTENTS
`(continued)
`H.
`(ICI Americas, Inc.) 1980 (“ICI”) (Ex. 1008) ......................... 24
`I.
`(“Biochem”) (Ex. 1018) .......................................................... 26
`J.
`Lipids. (1987) 22(6), 417–420 (“Babayan”) (Ex. 1019) ......... 26
`K. McCutcheon’s Volume 1: Emulsifiers & Detergents, North
`American Edition, 1997 (“McCutcheon’s”) (Ex. 1016) ......... 27
`L.
`16, 166 (1997) (“IUPAC”) (Ex. 1017) .................................... 28
`M. Mukerjee et al., “Critical Micelle Concentrations of Aqueous
`(“Mukerjee”) (Ex. 1009) ......................................................... 28
`VIII. Statements And Basis Of Opinions ................................................... 29
`A. Ground 1: Claims 1–5, and 9 are obvious in view of Winsness
`1008). ....................................................................................... 29
`B.
`1011), and ICI (Ex. 1008). ...................................................... 41
`C.
`and Scheimann (Ex. 1014). ..................................................... 48
`D. Ground 4: Claim 8 is obvious in view of Winsness (Ex. 1012),
`Scheimann (Ex. 1014) and Mukerjee (Ex. 1009). ................... 50
`E.
`1008), and Bonanno (Ex. 1006). ............................................. 53
`
`(Ex. 1012), Alther (Ex. 1007), Martin (Ex. 1010) and ICI (Ex.
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`Ground 2: Claims 13–16 are obvious in view of Winsness (Ex.
`1012), Alther (Ex. 1007), Martin (Ex. 1010), Buchold (Ex.
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`Ground 3: Claims 6–7 are obvious in view of Winsness (Ex.
`1012), Alther (Ex. 1007), Martin (Ex. 1010), ICI (Ex. 1008),
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`Alther (Ex. 1007), Martin (Ex. 1010), ICI (Ex. 1008),
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`Ground 5: Claims 10 and 12 are obvious in view of Winsness
`(Ex. 1012), Alther (Ex. 1007), Martin (Ex. 1010), ICI (Ex.
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`Ground 6: Claim 11 is obvious in view of Winsness (Ex.
`1012), Alther (Ex. 1007), Martin (Ex. 1010), ICI (Ex. 1008),
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`TABLE OF CONTENTS
`(continued)
`Page
`F.
`Bonanno (Ex. 1006), and David (Ex. 1013). .......................... 58
`G. Ground 7: Claims 1 and 6 are obvious in view of Bonanno (Ex.
`1006) and ICI (Ex. 1008). ....................................................... 60
`H. Ground 8: Claims 2 and 3 and 10 are obvious in view of
`Bonanno (Ex. 1006), Martin (Ex. 1010) and ICI (Ex. 1008). . 65
`I.
`Martin (Ex. 1010), ICI (Ex. 1008), and David (Ex. 1013). .... 69
`IX. Conclusion ......................................................................................... 70
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`Ground 9: Claim 11 is obvious in view of Bonanno (Ex. 1006),
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`I, David A. Rockstraw, declare:
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`I. Qualifications and Professional Experience
`1.
`I am the Robert Davis Distinguished Professor, a New Mexico State
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`University Distinguished Achievement Professor, and Academic Department
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`Head of Chemical & Materials Engineering at New Mexico State University
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`(“NMSU”).
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`2.
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`I completed a B.S. in chemical engineering at Purdue University in 1986,
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`followed by a Ph. D. in chemical engineering at The University of
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`Oklahoma in 1989.
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`3.
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`I have over 25 years of experience in the chemical arts including experience
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`with chemical separation technologies.
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`4.
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`I have specific experience in ethanol manufacture, which began in the
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`summer of 1986 at which time my employ with Kraft, Inc. sent me to
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`Melrose, MN, where I was assigned the task of collecting material and
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`energy balance data from an ethanol production facility using a feedstock
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`from cheese processing. I have continued to study ethanol manufacture as a
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`member of the NMSU faculty, using corn ethanol as the basis for the 2004
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`design problem of my senior class in process design, analysis, and
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`simulation. I directed laboratory research in 2013 for producing transgenic
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`alfalfa plants with high protein and low fiber in the leaves and stem, and
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`with increased cellulose content and low lignin content to test for the
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`increased fermentability potential to ethanol.
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`5.
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`Additional details of my qualifications are listed in my curriculum vitae,
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`which is attached.
`
`II.
`6.
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`Information Considered In Forming My Opinions
`In forming my opinions, I have relied upon the documents discussed in my
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`declaration. I have also considered my own personal education, training,
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`experience, and skills in the relevant arts in forming my opinions. My
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`opinions are based on the information reviewed to date, and I reserve the
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`right to amend or modify these opinions if additional information is provided
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`to me.
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`7.
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`This report and the opinions contained within are subject to revision based
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`on any additional information, materials, and testimony I may receive that,
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`in my professional opinion, warrant such changes. Moreover, I may
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`comment on, or testify in response to, the opinions or the testimony of other
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`witnesses, including witnesses who testify on behalf of Hydrite. I reserve the
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`right to respond to arguments raised by Solenis and its expert witnesses.
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`8.
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`Throughout this report, I may refer to “the Solenis Patent” or “the ’059
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`Patent” to describe the patent in question in this case: U.S. Patent No.
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`8,962,059.
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`III. Scope Of Opinions
`9.
`I have been asked to consider and form opinions as to validity of the ’059
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`Patent, considering the prior art relative to the ’059 Patent and the degree to
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`which the claimed invention would have been obvious to one skilled in the
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`art in light of the prior art at the time of the claimed invention.
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`IV. Background of the ’059 Patent
`10.
` According to the description of the ’059 Patent (Ex. 1001), “it is desired to
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`increase the value of byproduct streams from the production of ethanol from
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`bio-based sources [and] one manner of increasing the value is to separate the
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`oil, which has greater value as a separate byproduct stream, from the stillage
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`stream.” Ex. 1001, 3:42–45. The ’059 Patent states that one “manner of
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`increasing the value of the byproduct streams is to enhance the efficiency by
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`which the oil is separated from the byproduct stream.” Ex. 1001, 3:49–52.
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`11. The purported “invention” of the ’059 Patent is the “use of an oil
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`concentrator on the whole stillage byproduct stream or a secondary
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`byproduct stream derived therefrom [as] a means for increasing the value of
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`the byproduct streams.” Ex. 1001, 3:52–55. Claim 1 of the ’059 Patent
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`recites the steps of “mixing an ethoxylated sorbitan ester with the byproduct
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`stream; centrifuging the mixture of the ethoxylated sorbitan ester and the
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`byproduct stream; and separating the oil from the mixture.” Ex. 1001, Claim
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`1.
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`12. However, the solution to the oil recovery inefficiency problems noted in
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`the ’059 Patent has been known to one of ordinary skill in the art well before
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`the time of the purported invention of the ’059 Patent, and has been
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`described in open and published literature in a variety of contexts. In
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`addition, overall market demands and incentives were driving increased
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`efficiencies and oil recovery in the corn to ethanol industry well before the
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`time of the purported invention of the ’059 Patent.
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`13. Winsness (Ex. 1012) recognizes the need for more efficient and economical
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`manners of recovering oil from byproducts created during the dry milling of
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`corn to produce ethanol. Figure 2 and paragraphs [0043] and [0044] of
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`Winsness describe an apparatus and method for recovering oil from
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`byproducts created during the dry milling of corn to produce ethanol. The
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`whole stillage leftover after deriving the ethanol can be mechanically
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`separated into distillers wet grains, and thin stillage using a centrifugal
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`decanter. The resulting thin stillage is then introduced to an evaporator to
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`create a syrup. The resulting syrup is delivered to a disk stack centrifuge
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`which recovers usable oil. The leftover syrup from the centrifuge is
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`recombined with the distillers wet grains and dried.
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`14. Winsness further recognizes that “efforts to recover usable oil from the
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`byproducts of the dry milling process used to create ethanol have not been
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`terribly successful in terms of efficiency.” A problem with one previous
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`approach is that the spinning of thin stillage using a centrifuge creates an
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`emulsion phase that requires further processing. Ex. 1012, ¶ [0007]. Thus, at
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`the time of the invention of Claim 1 of the ’059 Patent, Winsness had
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`recognized a problem caused by the creation of an emulsion phase in a
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`centrifuge used to recover oil from the byproducts of corn to ethanol
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`production. One skilled in the art would seek to solve this problem and
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`thereby increase the efficiency of the Winsness systems and methods.
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`15. Alther (Ex. 1007) teaches that “[s]ome of the havoc caused by emulsions can
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`be avoided if emulsions are broken.” Ex. 1007, p. 82, col. 1, ¶ 4. Alther
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`further teaches that centrifugal separators use centrifugal force to separate
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`oil from water and that emulsion breakers can be added to a centrifugal
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`separator. Ex. 1007, p. 86, col. 1, last two paragraphs. Alther teaches that
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`“[d]epending on the emulsion, a strongly hydrophilic surfactant, such as
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`Polysorbate 80 [i.e., Tween 80] . . . can break the emulsion.” Ex. 1007, p. 83,
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`col. 2, ¶ 5.
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`16. Martin (Ex. 1010) describes the use of TWEEN polysorbates for dewatering
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`in the processing of corn products. Martin shows the structure of TWEEN
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`polysorbates and lists commercially available options: TWEEN 20, TWEEN
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`21, TWEEN 40, TWEEN 60, TWEEN 61, TWEEN 80 and TWEEN 85.
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`17. McCutcheon’s (Ex. 1016), at page 211, discloses that “Tween” is a trade
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`name for a series of nonionic ethoxylated sorbitan ester surfactants sold by
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`ICI Surfactants more than ten years before the filing date of the ’059 Patent.
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`McCutcheon’s lists commercially available options: TWEEN 20, TWEEN
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`21, TWEEN 40, TWEEN 60, TWEEN 61, TWEEN 65, TWEEN 80,
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`TWEEN 81, and TWEEN 85, along with the HLB for each surfactant.
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`18.
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`ICI (Ex. 1008) teaches that use of a TWEEN ethoxylated sorbitan ester with
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`an HLB value greater than the HLB of a corn oil/water mixture will
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`demulsify the mixture including corn oil and water thereby separating an
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`aqueous liquid phase from an organic liquid phase. See, e.g., ICI (Ex. 1008),
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`pp. 2, 13 (Figures 3 and 4).
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`19. Thus, adding the claimed “ethoxylated sorbitan ester” (see independent
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`Claim 1 of the ’059 Patent) or the claimed “polyoxyethylene (20) sorbitan
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`ester” (see independent Claim 13 of the ’059 Patent) to a corn to ethanol
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`byproduct stream that is centrifuged to separate oil and water phases is not
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`inventive. It is merely the addition of a known, commercial chemical
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`additive (e.g., Polysorbate 80 recognized as an emulsion breaker in Alther)
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`to a known, commercial process (the Winsness corn oil recovery process), to
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`achieve a known, expected result (improved corn oil separation).
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`20. Furthermore, Bonanno (Ex. 1006) describes a process for continuously
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`drying solids wet with an aqueous phase for a system that also includes an
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`oil that may be naturally present in the mixture being processed. In the
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`Bonanno process, oil and surfactant are added to the aqueous solids to
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`promote the exhaustive drying (complete removal of water by evaporation)
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`from the solid and oil. In Examples I and II, Bonanno runs tests on corn
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`stillage that one skilled in the art would understand show the effect that a
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`surfactant has to promote the water/oil separation. The separation step of this
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`process removes pure water from a crude mixture of oil and solids,
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`recovering the oil with the surfactant. Bonanno uses a centrifuge to assist in
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`recovery of the natural oil. Bonanno teaches the surfactant used in the
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`apparatus and process may be “polyoxyethylene sorbitan fatty acid esters
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`sold under the tradename TWEEN by ICI of the United States, Inc.” Ex.
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`1006, 5:8–10.
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`21. Thus, adding the claimed “ethoxylated sorbitan ester” (see independent
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`Claim 1 of the ’059 patent), or the claimed “polyoxyethylene (20) sorbitan
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`ester” (see independent Claim 13 of the ’059 patent) to a corn to ethanol
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`byproduct stream that is centrifuged to separate oil and water phases is
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`explicitly taught in Bonanno.
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`V. Legal Principles
`22.
`In developing my opinions on the invalidity of the ’059 Patent, I have relied
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`upon the following framework, which has been provided to me by counsel.
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`A.
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`Prior Art and Person of Ordinary Skill in the Art
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`23. For purposes of my analysis, I have assumed that the time of the invention of
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`the ’059 Patent was on or before May 27, 2011, which is the earliest filing
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`date listed for U.S. Patent No. 8,962,059.
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`24. My analysis also includes the scope and content of the prior art and the
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`knowledge of one of ordinary skill in the art at the relevant timeframe.
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`25. A hypothetical person of ordinary skill in the art would therefore, in my
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`opinion, be one holding a degree
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`in chemical engineering with
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`approximately five years of post-graduation experience in the design and
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`application of chemical processes, and having before him/her all of the
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`relevant prior art.
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`26.
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`I am an individual of more than ordinary skill in the art and was so at the
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`time of the ’059 Patent. Nevertheless, I have performed my analysis, as I
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`believe a hypothetical person of ordinary skill in the art would have, at the
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`relevant time of the ’059 Patent.
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`27. The term “prior art” refers to the state of the art prior to the ’059 Patent. I
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`understand that prior art evidence can be used to establish that an invention
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`claimed in a patent is either not novel or obvious, in which case the patent
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`claim is invalid. Prior art can take a number of different forms, including a
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`U.S. or foreign patent, a U.S. or foreign publication, and the knowledge of
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`one of ordinary skill in the relevant art.
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`B. Obviousness
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`28.
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`I also understand that a patent claim may be invalid if it can be demonstrated
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`that, even though the claimed subject matter was not identically disclosed or
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`described in a single reference, the differences between the claimed subject
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`matter and the prior art are such that the claimed subject matter, as a whole,
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`would have been obvious at the time the invention was made to a person of
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`ordinary skill in the art to which the invention pertains.
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`29.
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`I further understand that obviousness of a claim requires that the claim be
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`obvious from the perspective of a person of ordinary skill in the relevant art
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`at the time the invention was made. In analyzing obviousness, I understand
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`that it is important to comprehend the scope of the claims, the level of skill
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`in the relevant art, the scope and content of the prior art, the differences
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`between the prior art and the claims, and any secondary considerations. I
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`also understand that a claim of a patent is obvious if it is directed, for
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`example, to:
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`30.
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`(A) combining prior art elements according to known methods to yield
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`predictable results;
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`31.
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`(B) a simple substitution of one known element for another to obtain
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`predictable results;
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`32.
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`(C) use of a known technique to improve similar devices, methods, or
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`products in the same way;
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`33.
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`(D) applying a known technique to a known device, method, or product
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`ready for improvement, to yield predictable results;
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`34.
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`(E) being “obvious to try”— i.e. choosing from a finite number of identified,
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`predictable solutions, with a reasonable expectation of success;
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`35.
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`(F) known work in one field of endeavor may prompt variations of it for use
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`in either the same field or a different field based on design incentives or
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`other market forces, if the variations are predictable to one of ordinary skill
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`in the art; and/or
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`36.
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`(G) some teaching, suggestion, or motivation in the prior art that would have
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`led one of ordinary skill to modify the prior art reference, or to combine
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`prior art reference teachings to arrive at the claimed invention.
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`37.
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`I understand that other rationales supporting a conclusion of obviousness
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`may be relied upon.
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`38.
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`I understand that there must be some reason to combine the elements of the
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`prior art to show a teaching of the claimed invention in the patent at issue.
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`There is no rigid test for determining the existence of a reason to combine
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`the elements. Factors used to determine the existence of such a reason
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`include: (1) interrelated teachings of multiple patents; (2) the effects of
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`demands known to the design community or present in the marketplace; and
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`(3) the background knowledge and common sense possessed by a person
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`having ordinary skill in the art. Further, any need or problem known in the
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`field of endeavor at the time of invention and addressed by the patent at
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`issue can provide a reason for combining the elements to show a teaching of
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`the claimed invention.
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`39.
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`It is improper, however, to use hindsight in assessing obviousness by, for
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`example, using the claims of the patent at issue as a template for piecing
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`together elements (i.e. components, steps, chemicals elements, etc.) found in
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`separate prior art references. Further, a person skilled in the art must have a
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`reasonable expectation of success that the references combined to establish
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`obviousness would result in teaching the claimed invention. Furthermore,
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`the combination of familiar elements according to known methods is likely
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`to be obvious when it does no more than yield predictable results.
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`40. Accordingly, I understand that where there is a reason to modify or combine
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`the prior art to achieve the claimed invention, the claims may be rejected as
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`obvious provided there is also a reasonable expectation of success.
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`Obviousness does not require absolute predictability, however, at least some
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`degree of predictability is required.
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`VI. Chemistry and Terminology
`A.
`Functionalized
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`41. A functional group1 is as an atom, or a group of atoms, that has similar
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`chemical properties whenever it occurs in different compounds. A functional
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`group defines the characteristic physical and chemical properties of families
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`of organic compounds. The term functionalized may be a verb that refers to
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`the process or action by which a functional group is added to a molecular
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`structure by a chemical reaction.
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`B. Alkylate
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`42. The term alkylate can be used as a noun or a verb. As a noun, alkylate refers
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`to a substance produced by adding alkyl groups (a type of functional group)
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`1 International Union of Pure and Applied Chemistry, “Compendium of Chemical
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`Terminology,” 2nd ed. 1997, p. 16 (Ex. 1017).
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`to a compound.
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`43. Alkyl groups2 are “univalent groups derived from alkanes by removal of a
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`hydrogen atom from any carbon atom – CnH2n+1.” Simply put, an alkyl group
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`is a class of functional groups comprised only of carbon and hydrogen in a
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`defined proportion.
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`44. The verb alkylate is used to describe the reaction of this functionalization
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`process. For example, alcohols can be alkylated to give alkyl ether
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`functional groups (R-O-R):
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`R-OH + R'-X → R-O-R' + H-X
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`45. Alkylate can also be used as a noun, referring to the product (R-O-R) of an
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`alkylation reaction.
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`46. A specific alkylation reaction is an esterification, which involves treating a
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`carboxylic acid (such as a fatty acid) with an alcohol or polyol in the
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`presence of a catalyst.
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`R'OH + RCO2H ⇔ RCO2R' + H2O
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`47. Fatty acids are classified by the nature of the alkylate group of which it is
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`comprised. The IUPAC-IUB Commission on Biochemical Nature published
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`2 Id. at p. 166.
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`a recommendation for naming such groups in 1978.3 The appendix of this
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`publication is provided in Figure 1 below.
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`Figure 1: Names of alkylates classified as fatty acids (Ex. 1018, p. 33).
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`48. Likewise, fatty acids in triglyceride oils (such as corn oil) are also classified
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`using this naming system. Figure 24 below provides compositions of fatty
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`acids in typical food oils where it is seen that the majority of these oils are
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`composed of oleic (18 carbons), linoleic (18 carbons), and palmitic (16
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`3 IUPAC-IUB Commission on Biochemical Nomenclature, “The Nomenclature of
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`Lipids,” Biochem. J., Vol. 171, Issue 1, pp. 21–35 (April 1978) (Ex. 1018).
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`4 V. K. Babayan, “Specialty Lipids and their Biofunctionality.” Lipids. (1987)
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`22(6), 417-420 (Ex. 1019).
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`carbons) chains: corn (96.7%), peanut (89.5%), safflower (97.3%), soybean
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`(87.6%), and sunflower (93.6%). Corn oil has 12.2% palmitic acid, 0.1%
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`palmitoleic acid, 2.2% stearic acid, 27.5% oleic acid, 57.0% linoleic acid,
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`0.9 linoleneic acid, and 0.1% arachadic acid.
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`Figure 2: Fatty acid compositions of common long chain triglyceride food
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`oils. (Ex. 1019, pp. 417–420)
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`C. Alkoxylate
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`49. The term alkoxylate can also be used as a noun or verb. The noun alkoxylate
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`refers to a specific functional group. An alkoxy functional group (or alkyl
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`oxide) is an alkyl group singular bonded to oxygen (R—O). The simplest
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`alkoxy groups are methoxy (CH3O—), ethoxy (CH3CH2O—), and propoxy
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`(CH3CH2CH2O—). The verb form of alkoxylate means to perform a
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`chemical reaction whereby an alkoxy group is chemically added to a
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`compound. The verb can be expressed with further specificity of the
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`functional group as methoxylate, ethoxylate, or propoxylate.
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`50. The general form of an ethoxylation reaction is given as:
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`ROH + n C2H4O → R(OC2H4)nOH
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`where n is commonly in the range of 5 to 10. The reaction requires a catalyst
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`(a material present that promotes the reaction, but is not itself chemically
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`altered by the reaction) to proceed at an acceptable rate. A polyoxyethylene
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`group (or ethylene oxide group) would have repeat units of oxyethylene
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`(-OC2H4-) and is formed in an ethoxylation reaction using ethyl oxide, an alkyl
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`oxide.
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`D.
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`Surfactants
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`51. The term surfactant is a blend of the words forming the term “surface active
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`agent.” It refers to a broad range of chemical compounds that have both
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`hydrophilic and hydrophobic properties, and thus tend to accumulate at the
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`interface between aqueous (water) and organic (oil) phases. One skilled in the
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`art understands to use an appropriate surfactant to elicit chemistries and
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`physical phenomena to occur at such an interface. See, e.g., Alther (Ex. 1007).
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`E.
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`Polysorbates
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`52. Martin5 describes the use of TWEEN polysorbates (nonionic surfactants) for
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`dewatering. The structure shown in Martin (2:55–64) is a general
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`polysorbate structure in which defining the “R” functional group and the
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`extent of ethoxylation (w+x+y+z) will completely define the nature of the
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`polysorbate. The nature of the functional group designated as –R on the
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`polysorbate structure dictates the identifying number of the polysorbate as
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`illustrated in Figures 7–10.
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`Figure 3: Tween 20 - Polysorbate 20 (polyoxyethylene (20) sorbitan
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`monolaurate)
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`Figure 4: Tween 40 - Polysorbate 40 (polyoxyethylene (20) sorbitan
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`monopalmitate)
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`5 Martin et al., U.S. Patent No. 5,283,322 (Feb. 1, 1994) (Ex. 1010).
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`Figure 5: Tween 60 - Polysorbate 60 (polyoxyethylene (20) sorbitan
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`monostearate)
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`Figure 6: Tween 80 - Polysorbate 80 (polyoxyethylene (20) sorbitan
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`monooleate)
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`VII. Relevant Prior Art
`A. U.S. Patent Application Publication No. 2008/0110577
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`(“Winsness”) May 15, 2008 (Ex. 1012)
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`53. Winsness recognizes the need for more efficient and economical manners of
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`recovering oil from byproducts created during the dry milling of corn to
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`produce ethanol. Figure 2 and paragraphs [0043] and [0044] of Winsness
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`describe an apparatus and method for recovering oil from byproducts created
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`during the dry milling of corn to produce ethanol. The whole stillage leftover
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`after deriving the ethanol can be mechanically separated into distillers wet
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`grains and thin stillage using a centrifugal decanter. The resulting thin
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`stillage is then introduced to an evaporator to create a syrup (concentrated
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`thin stillage). The resulting syrup is delivered to a disk stack centrifuge
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`which recovers usable oil. The leftover syrup from the centrifuge is
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`recombined with the distillers wet grains and dried.
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`B. George R. Alther article, “Put the Breaks on: Removal of fats, oil,
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`and greases is necessary to recycle water and meet discharge
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`limits.” Chemical Engineering, Vol. 5, No. 3, March 1998
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`(“Alther”) (Ex. 1007)
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`54. This article appeared in the trade journal “Chemical Engineering” in 1998
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`and describes the use of various technologies to break emulsions. The
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`primary application is to recover water for recycling, but whenever an
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`emulsion is separated, two streams result: water and oil. This article
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`provides general information about the known science and technology of
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`emulsions. Alther provides a list of information (in the form of a series of
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`questions) on page 84 that is important to define the nature of an emulsion.
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`Alther then subsequently uses that information to guide one skilled in the art
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`through a range of potential emulsion breaking methodologies.
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`55.
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`In response to Alther’s questions, the system described by the ’059 Patent is
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`an oil-in-water emulsion composed of single-digit percentages of corn oil.
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`Droplets are small (appearing as a cream), and there are solids present. Oil-
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`soluble structures like corn gluten, phosphatides, and starches serve as
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`hydrophilic surfactants that attract the water to the oil phase.
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`56. Alther later describes how to counteract such an emulsion. It is suggested to
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`“increase the solubility of the surfactant in either bulk phase” to separate
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`these components accumulated at the oil water interface. This suggests the
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`addition of more of the oil phase material to the composition of the emulsion.
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`57. Alther also advises to “disrupt the oriented structure of the emulsifier’s
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`interfacial phase with demulsifiers.” This act is also accomplished by the
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`previous suggestion of adding additional oil phase material. Additionally,
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`Alther provides a simple explanation of how demulsifying agents work,
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`stating, “separation occurs when the agents insert themselves between the
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`surfactant molecules, increasing the intermolecular distance and weakening
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`the binding forces constructed by the emulsifier.”
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`58. Alther explicitly identifies Polysorbate 80 as an emulsion breaker.
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`59. Alther further identifies that pH and temperature affect emulsion stability.
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`C. U.S. Patent No. 4,662,990 (“Bonanno”) May 5, 1987 (Ex. 1006)
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`60. Bonanno describes a process for continuously drying solids wet with an
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`aqueous phase for a system that also includes an oil that may be naturally
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`present or added to the system. In this process, oil and surfactant are added
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`to the aqueous solid to promote the exhaustive drying (complete removal of
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`water by evaporation) from the solid and oil. Bonanno recognizes the effect
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`that a surfactant has to promote the water/oil separation. The separation step
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`of this process removes pure water from a crude mixture of oil and solids,
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`recovering the oil with the surfactant. Then, Bonanno uses a centrifuge to
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`assist in recovery of the natural oil.
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`D. U.S. Patent No. 5,283,322 (“Martin”) Feb. 1, 1994 (Ex. 1010)
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`61. Martin describes the use and selection of a series of polyoxyethylene 20
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`sorbitan fatty esters for the dewatering of the crude materials obtained in the
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`processing of corn. Similar to Bonanno, this patent recognizes the advantage
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`of an appropriately selected surfactant on the ability to separate an aqueous
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`liquid phase from an organic liquid phase in the presence of solids that act to
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`form an emulsion. Martin narrows the window of potential surfactants to use
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`for the specific application when the solids material is composed of glutens
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`from grain processing. In particular, this patent identifies polyoxyethylene
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`20 sorbitan fatty esters with the trade name “TWEEN,” a trade name of ICI
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`Surfactants.
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`62. Martin suggests treatment dosages of 75 to 300 ppm for gluten dewatering.
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`E. U.S. Patent No. 5