Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
DETAILED ACTION
Claims 11-20 of M. Merget et al., App. No. 18/280,693 (Mar. 24, 2021) are pending and are rejected.
Election/Restrictions
Pursuant to the election of species requirement Applicant elected, without traverse, the
(1) a species of organopolysiloxanes (A), wherein the organopolysiloxanes (A) comprise units of the formula (I)
RaQbSiO(4-a-b)/2 (I),
Applicant elects α,ω-divinyl-terminated dimethylpolysiloxane, wherein Applicant indicates the units of the formula (I) are as follows:
wherein R, as defined within claim 11, is methyl,
wherein Q, as defined within claim 11, is vinyl,
wherein a, as defined within claim 11, is 2, and
wherein b, as defined within claim 11, is 0 or 1,
(2) a species of organopolysiloxanes (B), wherein the organopolysiloxanes (B) comprise units of the formula (II)
R2d(OR1)fSiO(4-d-f)/2 (II),
Applicant elects α,ω-dihydroxy-terminated dimethylpolysiloxane, wherein the units of formula (II) are as follows:
wherein R1, as defined within claim 11, is a hydrogen atom,
wherein R2, as defined within claim 11, is methyl,
wherein d, as defined within claim 11, is 2, and
wherein f, as defined within claim 11, is 0 or 1,
(3) a species of catalysts (D), Applicant elects the alkali metal hydroxides; and
(4) a species of organopolysiloxane compounds (C), wherein the optional organopolysiloxane compounds (C) comprise at least one structural unit per molecule of the general formula (III)
O3-(e+g)/2R3eQ1gSi-Y(SiR3eQ1gO3-(e+g)/2)c (III)
Applicant elects a star polymer (C1), wherein the units of formula (III) are as follows:
wherein R3, as defined within claim 11, is methyl,
wherein g, as defined within claim 11, is 0,
wherein Q1, as defined within claim 11, is not present,
wherein Y, as defined within claim 11, is a divalent ethanediyl group (-CH2-CH2-),
wherein e, as defined within claim 11, is 1, and
wherein c, as defined within claim 11, is 1,
for prosecution on the merits to which the claims shall be restricted if no generic claim is finally held to be allowable.
In the Reply, Applicant indicates that claims 11-20 all read on the elected species. The elected species was searched and determined to be unpatentable per §§ 102 and 103 with respect to the elected species of α,ω-divinyl-terminated dimethylpolysiloxane. The search/examination was further extended to the full scope of claims 11-20. MPEP § 803.02 (III)(C)(2). MPEP § 803.02 (III)(C)(2). The provisional election of species requirement is given effect and no claims are withdrawn from consideration as not reading on the elected species. MPEP § 803.02(III)(A).
The Claimed Invention
The chemical formulae are drafted using shorthand siloxane nomenclature.1
The claim 11 reaction process is summarized by the Examiner as follows.
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Understanding the method of claim 11 is aided by review of specification working Examples 1-3, directed to preparing the claim 11 product. Working Examples 1-3 are summarized by the Examiner below. The specification first describes the preparation of a species of optional organopolysiloxane compound (C), summarized by the Examiner as follows:
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Specification at page 16. In Examples 1-3, the specification teaches preparation of three species of organopolysiloxanes having unsaturated groups, in each case, where component A should correspond to α,ω-divinylterminated dimethylpolysiloxane and component B (comprising units of formula (I) R2d(OR1)fSiO(4-d-f)/2) is α,ω-dihydroxy-terminated dimethylpolysiloxane, octamethylcyclotetrasiloxane or decamethylcyclopentasiloxane
Working Example 1 is summarized by the Examiner as follows.
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Specification at pages 16-17. Working Example 2 is summarized by the Examiner as follows.
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Specification at page 17.
Working Example 3 is summarized by the Examiner as follows.
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Specification at page 17.
Specification at pages 16-17. In each case, the working Examples teach that 2-butyloctanoic acid (claim 11 component E) is added at the reaction temperature.
Claim Rejections - 35 USC § 102 (AIA )
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale or otherwise available to the public before the effective filing date of the claimed invention.
(a)(2) the claimed invention was described in a patent issued under section 151, or in an application for patent published or deemed published under section 122(b), in which the patent or application, as the case may be, names another inventor and was effectively filed before the effective filing date of the claimed invention.
§ 102(a)(1)/(2) Rejection over D. Kosal et al., US 4,625,011 (1986) (“Kosal”)
Claims 11-14, 16, 17 and 20 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by D. Kosal et al., US 4,625,011 (1986) (“Kosal”). Kosal teaches a process of manufacturing relatively high molecular weight organopolysiloxanes with a viscosity of 10 to 500,000 centipoises at 25 C by polymerization of relatively low molecular weight organopolysiloxanes in the presence of an alkali metal catalyst including the step of neutralizing the alkali metal catalyst subsequent to polymerization using an effective amount of an organic carboxylic acid to neutralize the alkali metal catalyst subsequent to polymerization. Kosal at lines bridging cols. 2-3.
In working Examples 1-3 Kosal teaches preparation of dimethylvinylsiloxy endblocked dimethylpolysiloxane. Kosal at cols. 7-8. Kosal Example 3 (performed in the manner of Example 2, using different neutralization agents, including oleic acid, undecylenic acid, and cyclohexane carboxylic acid) is summarized by the Examiner as follows:
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Kosal’s vinyl-terminated poly(dimethylsiloxane) polymer reactant meets the claim 11 limitations of organopolysiloxanes (A) that comprise units of the formula (I) RaQbSiO(4-a-b)/2, when b is zero as follows and where per claim 11 “the organopolysiloxanes (A) have at least one radical Q”:
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.
Note that Kosal’s vinyl-terminated poly(dimethylsiloxane) polymer reactant is the same polysiloxane structure employed in instant specification working Examples 1-3.
And Kosal’s above cyclic siloxane meets the limitations of organopolysiloxanes (B) comprise2 units of the claim 11 formula (II) R2d(OR1)fSiO(4-d-f)/2, where claim 11 variable f is zero, as follows:
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Note that this is the same polysiloxane structure employed in instant specification working Example 2.
Kosal Example 3 employes potassium silanolate as the basic catalyst in the reaction mixture and thus meets the claim 11 limitation of:
Claim 11 . . . wherein in a first step organopolysiloxanes (A), organopolysiloxanes (B), catalysts (D) and optionally organopolysiloxane compounds (C) are provided and mixed together . .
wherein the basic catalysts (D), are selected from the group of alkali metal hydroxides, alkali metal alkoxides and alkali metal siloxanolates . . .
Kosal Example 3 heats the mixture to 165 °C and thus meets the claim 11 limitation of:
Claim 11 . . . wherein in a second step the mixture obtained in the first step is allowed to react at temperatures of 80 to 170 °C . . .
Kosal Example 3 neutralizes the reaction mixture with each of oleic acid, undecylenic acid, and cyclohexane carboxylic acid (in separate runs) and thus meets the claim 11 limitation of:
Claim 11 . . . wherein in a third step the reaction mixture obtained in the second step is neutralized with carboxylic acid derivatives having at least 4 carbon atoms (E).
In sum, Kosal meets each and every limitation of claim 11, which is anticipated.
Respecting claims 12 and 13, Kosal employs 19.3 g of the vinyl-terminated poly(dimethylsiloxane) polymer reactant (corresponding to claim 11 component (A)) and 405 g of cyclicpolysiloxane (corresponding to claim 11 component (B)) for a total of 4.5% by weight ratio component (A) and 95% by weight ratio of component (B) thereby meeting the limitations of claims 12 and 13.
Claim 14 is anticipated by Kosal Example 3 because Kosal’s linear polydimethylsiloxane meets the limitations of claim 11 organopolysiloxane (C), when R3 is methyl, e is 2, g is zero, Y is a carbon, and c is 1.
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The further limitations of claim 16 are clearly met by either of Kosal’s oleic acid or undecylenic acid.
The limitations of claim 17 are met because Kosal carries out the reaction at ambient pressure (about 1 atm), which is 1013 hPa.
The limitations of claim 20 are met for the following reasons. Kosal does not quantitate the FTU (Formazine Turbidity Unit) of the product. However, Kosal’s product is prepared using the same methods and reactants as instantly disclosed. It is therefore asserted that Kosal’s dimethylvinylsiloxy endblocked dimethylpolysiloxane of Example 3 falls within the claimed range of 0 to 65 FTU. Once a reference teaching product appearing to be substantially identical is made the basis of a rejection, and the examiner presents evidence or reasoning to show inherency, the burden of production shifts to the applicant. MPEP § 2112(V) (citing In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433-34 (CCPA 1977).
Claim Rejections - 35 USC § 103
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries set forth in Graham v. John Deere Co., 383 U.S. 1, 148 USPQ 459 (1966), that are applied for establishing a background for determining obviousness under AIA 35 U.S.C. 103(a) are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
Claims 11-18 and 20 are rejected under AIA 35 U.S.C. 103 as being unpatentable over D. Kosal et al., US 4,625,011 (1986) (“Kosal”).
Claim 19 is obvious over Kosal as above in further view of L. Tolentino, US 4,382,057 (1983) (“Tolentino”) and/or L. Lewis et al., US 5,015,691 (1991) (“Lewis”).
D. Kosal et al., US 4,625,011 (1986) (“Kosal”)
Kosal teaches a process of manufacturing relatively high molecular weight organopolysiloxanes with a viscosity of 10 to 500,000 centipoises at 25 C by polymerization of relatively low molecular weight organopolysiloxanes in the presence of an alkali metal catalyst including the step of neutralizing the alkali metal catalyst subsequent to polymerization using an effective amount of an organic carboxylic acid to neutralize the alkali metal catalyst subsequent to polymerization. Kosal at lines bridging cols. 2-3.
In working Examples 1-3, Kosal teaches preparation of dimethylvinylsiloxy endblocked
dimethylpolysiloxane. Kosal at cols. 7-8. Kosal Examples 1-3 are summarized by the Examiner as follows:
In Example 1, Kosal teaches heating a mixture of [(CH3)2SiO]x cyclics, where x is 4 to 6 with (CH3)2(CH2=CH)Si-O[(CH3)2SiO]nSi(CH=CH2)(CH3)2 (where n is 0-12, with an average value of about 6) to a temperature of 150° C., under nitrogen, for about 2.3 hours in the presence of potassium silanolate as the basic alkali metal catalyst, followed by reaction mixture neutralization with either CO2 or propionic acid (in different samples). Kosal at col. 7, lines 1-19. Kosal teaches isolation of the product, dimethylvinylsiloxy end-blocked dimethylpolysiloxane, by filtration of the reaction mixture. Kosal at col. 7, lines 25-50. Working Example 1 (run where propionic acid is the neutralization agent) is summarized by the Examiner as follows:
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In Examples 2 and 3, Kosal teaches heating a mixture of (CH3)2(CH2=CH)Si-O[(CH3)2SiO]nSi(CH=CH2)(CH3)2 (19.3 g, where n is 0-12, with an average value of about 6); (CH3)3SiO[(CH3)2SiO]mSi(CH3)3 (72.6 g, where m has an average value of 13-14); [(CH3)2SiO]x cyclics (405 g, where x is 4 to 6); and the basic catalyst potassium silanolate (2.4 g) to a temperature of 165° C, for about 2.5 hours followed by neutralization with propionic acid in Example 2 and additional runs with oleic acid, undecylenic acid, and cyclohexane carboxylic acid in Example 3. Kosal at cols. 7-8. Kosal Examples 2-3 are collectively summarized by the Examiner as follows:
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Kosal at cols. 7-8. As discussed in the § 102 rejection above, Kosal Example 3 (employing either oleic acid or undecylenic acid as the neutralization agent) meets each and every limitation (both chemical structures and method steps) of claims 11-14, 16, 17 and 20.
Differences between Kosal and the Claims
As discussed in the § 102 rejection above, Kosal Example 3 (employing either oleic acid or undecylenic acid as the neutralization agent) meets each and every limitation (both chemical structures and method steps) of claims 11-14, 16, 17 and 20.
Kosal differs from claim 15 as follows. Kosal Example 3 employs potassium silanolate as the basic catalyst and therefore does not teach the claim 15 limitation of “the alkali metal hydroxides are used as the catalysts (D)”.
With respect to claim 18, Kosal does not specify the order of reagent addition in Example 3 and further differs from claim 18 because Kosal performs Example 3 at a temperature of 165 °C therefore does not specifically teach the claim 18 limitations is strikeout text below.
18. (Previously Presented) The method of claim 11, wherein
in the first step the organopolysiloxanes (A), the organopolysiloxanes (B) and the optional organopolysiloxane compounds (C) are initially charged at room temperature
wherein in the second step the mixture obtained in the first step is allowed to react
wherein in the third step the reaction mixture obtained in the second step is neutralized with carboxylic acid derivatives (E) at a temperature of 100 to 160°C.
With respect to claim 19, Kosal does not teach the further limitations of claim 19 because Kosal Example 3 does perform a distillation.
Claims 11-20 Are Obvious over the Cited Art
Claim 11-14, 16, 17 and 20 are obvious in view of Kosal because one of ordinary skill is motivated to perform Kosal Example 3 using any of oleic acid, undecylenic acid, and cyclohexane carboxylic acid as a neutralization reagent, as specifically taught by Kosal, thereby meeting each and every claim limitation as discussed above in the § 102 section.
Alternatively, claims 11-13, 16, 17 and 20 are obvious in view of Kosal because one of ordinary skill is motivated to perform Kosal Example 1 using any of oleic acid, undecylenic acid, and cyclohexane carboxylic acid as a neutralization reagent, as specifically taught by Kosal, thereby meeting each and every claim limitation. In this alternative rationale, Kosal’s Example 1 polysiloxane reagent (CH3)2(CH2=CH)Si-O[(CH3)2SiO]nSi(CH=CH2)(CH3)2, corresponds to claim 11 organopolysiloxane (A), Kosal’s Example 1 polysiloxane reagent [(CH3)2SiO]x cyclics, where x is 4 to 6, corresponds to organopolysiloxane (B), and Kosal’s Example 1 potassium silanolate corresponds to catalyst (D). The same matching of claim elements for claims 11-13, 16, 17 and 20 as set forth in the above § 102 rejection also applies under this alternative rationale.
Claim 15 is obvious because one of ordinary skill is motivated to replace the Kosal Example 1 or Example 3 potassium silanolate with an alkali metal hydroxides (e.g. potassium hydroxide) so as to arrive at each and every limitation of claim 15. Kosal teaches the equivalency of alkali metal silanolates and an alkali metal hydroxides. Kosal at col. 4, lines 24-49; Id. at col. 4, lines 48-49 (“[p]referred alkali metal catalysts are potassium silanolate and potassium hydroxide”).
Claim 18 is obvious for the following reasons. Claim 18 recites:
18. (Previously Presented) The method of claim 11, wherein
in the first step the organopolysiloxanes (A), the organopolysiloxanes (B) and the optional organopolysiloxane compounds (C) are initially charged at room temperature and the catalyst (D) is metered in at a temperature of 20 to 90°C and are mixed with one another;
wherein in the second step the mixture obtained in the first step is allowed to react at temperatures of 90 to 150°C and a pressure of 20 to 1100 hPa; and
wherein in the third step the reaction mixture obtained in the second step is neutralized with carboxylic acid derivatives (E) at a temperature of 100 to 160°C.
Kosal does not specify the order of reactant/catalyst addition for Examples 1 and 3; rather Kosal states Example 3 was performed in the manner of Kosal Example 2, where Example 2 states as follows:
A mixture containing. . . 19.3 g of (CH3)2(CH2=CH)Si-O[(CH3)2SiO]nSi(CH=CH2)(CH3)2, where n is 0-12, with an average value of about 6); 72.6 g of (CH3)3SiO[(CH3)2SiO]mSi(CH3)3 (viscosity of 10 cs at 25° C) where m has an average value of 13-14), 405 g of [(CH3)2SiO]x cyclics, where x is 4 to 6), and 2.4 g of potassium silanolate catalyst as heated to a temperature of 165° C, for about 2.5 hours in a closed system.
Kosal at col. 7, lines 53-62. Here, the claimed order of reagent addition does not distinguish claim 18 from Kosal Example 3 under § 103, rather it is merely a design choice. MPEP § 2144.04(IV)(C).3 The specification provides no guidance regarding the meaning of “meter in”; and the specification working examples simply mix the siloxane reagents and catalyst together with no specification of addition order. Here, “metered in” is broadly and reasonably interpreted, consistently with the specification, as simply adding the catalyst into a mixture of reactants. MPEP § 2111. This aspect of claim 18 is obvious because the specification indicates no criticality with respect to reagent/catalyst addition order; one of ordinary skill is motivated to perform Kosal Example 3 by initially mixing the siloxane reagents at room temperature and then adding the catalyst potassium silanolate to this initial mixture, simply as a convenient addition protocol. One of ordinary skill thereby meets the order-of-reagent-addition limitations of claim 18. MPEP § 2144.04(IV)(C), see footnote 3.
Kosal Example 3 further differs from claim 18 because Kosal performs Example 3 at a temperature of 165 °C.
Claim 18 . . . wherein in the second step the mixture obtained in the first step is allowed to react at temperatures of 90 to 150°C and a pressure of 20 to 1100 hPa; and
Note that the claim 18 pressure limitations are met because Kosal carries out the Example 3 reaction at ambient pressure (about 1 atm), which is 1013 hPa and falls within the claim 18 pressure range. The claim 18 temperature range of 90 to 150°C is obvious for the following reasons. Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. MPEP § 2144.05(II)(A).4 Kosal Example 3’s temperature of 165 °C is close to the claim 18 upper temperature limit of 150 °C. A prima facie case of obviousness exists where the claimed ranges or amounts do not overlap with the prior art but are merely close. MPEP § 2144.05(I). More significantly Kosal teaches a similar reaction in Example 1, where the polymerization is carried out at 150 °C, which falls within the claim 18 temperature range. Kosal at col. 7, lines 5-10. Notably, Kosal further implicates a polymerization temperature range of about 80 °C to 200 °C. Kosal at col. 4, lines 39-43. In sum, Kosal teaches a temperature ranges that fall within and/or overlap with the claim 18 range of 90 to 150°C. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP § 2144.05(I).
The final claim 18 limitation of:
Claim 18 . . . wherein in the third step the reaction mixture obtained in the second step is neutralized with carboxylic acid derivatives (E) at a temperature of 100 to 160°C.
is obvious because Kosal teaches:
The temperature at which the neutralization takes place will normally be, for convenience sake, the temperature of the polymerization reaction which is normally less than about 200 °C. The neutralization temperature is preferably about 100-175° C. and most preferably about 150-175° C. Naturally, other neutralization temperatures may be employed.
Kosal at col. 5, lines 37-44. In sum, each and every limitation of claim 18 is taught by Kosal.
Claim 19 is obvious as above, in further view of L. Tolentino, US 4,382,057 (1983) (“Tolentino”) and/or L. Lewis et al., US 5,015,691 (1991) (“Lewis”). Claim 19 recites “distillation” in the following context.
19. The method of claim 11, wherein the reaction mixture after completion of the third step is worked up by distillation, the distillation being carried out at temperatures of 140 to 170°C and a pressure of 1 to 50 hPa.
The specification working examples teach distillation in the context of removing volatiles (i.e., cyclic siloxanes) rather than distillation of the product itself. See, specification at page 17, Examples 1-3. The specification generally teaches that these methods are known in the art:
The reaction mixture obtained in the third step can now - if desired - be worked up by any methods known to date. For example, it can be freed from volatile constituents, especially cycles, by distillation. If the reaction mixture is to be worked up by distillation after completion of the third step, the distillation is preferably carried out at temperatures of 140 to 170°C and a pressure of 1 to 50 hPa.
Specification at page 14, lines 19-24 (emphasis added).
L. Tolentino, US 4,382,057 (1983) teaches that such distillation removal of volatiles from the product is standard practice in the art. Tolentino teaches that
It should be noted that these polymers are easily produced and generally comprise taking the appropriate cyclotetrasiloxanes and equilibrating them or reacting them in the presence of vinyl-terminated, low molecular weight linear polymers such as divinyltetramethyl disiloxane, in the presence of an alkali metal hydroxide catalyst. After a sufficient amount of the linear polymers is formed, the catalyst is neutralized and the unreacted cyclics vented off to give the desired polymer. The chain-stopper is generally obtained by the hydrolysis of the appropriate chlorosilanes. For more information as to the production of such polymers, please refer to U.S. Pat. Nos. 4,041,010 and 3,436,366 and the patents referred to therein.
Tolentino at col. 5, lines 30-43 (emphasis added). Claim 19 is obvious because one of ordinary skill is motivated to treat Kosal’s Example 3 product mixture under the claim 19 temperature and reduced-pressure conditions to remove any volatile cyclicsiloxanes (e.g., remaining cyclotetrasiloxanes). The cyclicsiloxanes of Kosal working Example 3 are the same as the those employed in the instant specification’s working examples and one of ordinary skill is motivated to remove them, as taught by Tolentino in the interest of a purer product siloxane. In this regard, Lewis teaches that “[p]referably, excess cyclics are stripped off so that the linear polymer will have a low volatile content and be relatively pure”. Lewis at col. 4, lines 42-44.
Conclusion
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ALEXANDER R. PAGANO
Examiner
Art Unit 1692
/ALEXANDER R PAGANO/Primary Examiner, Art Unit 1692
1 Chemical shorthand nomenclature is often used to represent silicone polymers based upon polymer units. Dow Corning Corporation, Silicone Chemistry Overview, 1-11 (1997) (“Dow Corning”); A. Colas et al., Handbook of Polymer Applications in Medicine and Medical Devices, 131-143 (2013); A. O’Lenick, 3 Journal of Surfactants, 229-236 (2000) (page 231, col. 2, Table 1). Dow Corning provides a description of the short hand nomenclature for siloxane units as follows.
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In these silicone building blocks, the numerator in the subscript "fraction" following the "O" represents the number of oxygen atoms connected to the particular silicon, and the denominator "2" indicates that each of these oxygen atoms are shared between two silicon atoms. Id.; see also, J. Grande et al., 46 Chem. Commun., 4988-4990 (2010) (see page 4990 under “Notes and references”). For example, with SiO4/2, the silicon forms four single bonds to four different oxygen atoms, and each oxygen, in turn, bonds to another silicon through a single bond, i.e., Si(-O-Si-)4. Id.
2 The claim 11 transitional term "comprising", is open-ended and does not exclude additional, unrecited chemical structure. MPEP § 2111.03(I).
3 MPEP § 2144.04 (IV)(C) (citing Ex parte Rubin, 128 USPQ 440 (Bd. App. 1959) (Prior art reference disclosing a process of making a laminated sheet wherein a base sheet is first coated with a metallic film and thereafter impregnated with a thermosetting material was held to render prima facie obvious claims directed to a process of making a laminated sheet by reversing the order of the prior art process steps.). See also In re Burhans, 154 F.2d 690, 69 USPQ 330 (CCPA 1946) (selection of any order of performing process steps is prima facie obvious in the absence of new or unexpected results); In re Gibson, 39 F.2d 975, 5 USPQ 230 (CCPA 1930) (selection of any order of mixing ingredients is prima facie obvious.).
4 MPEP § 2144.05(II)(A) (citing In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955) (claimed process which was performed at a temperature between 40°C and 80°C and an acid concentration between 25% and 70% was held to be prima facie obvious over a reference process which differed from the claims only in that the reference process was performed at a temperature of 100°C and an acid concentration of 10%.)).
Prosecution Insights