DETAILED ACTION
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 .
Response to Arguments
With respect to the rejection of Claims 1-9 and 18-20 under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite, as understood the traversal relies on amendments. Claim 1 has been canceled and the dependency of claims 2-9 and 18-20 has been changed to Claim 10. Claim 10 recites process steps which require using a solid adsorbent which cures the indefiniteness of remaining Claims 2-9 and 18-20. The rejections have been WITHDRAWN.
With respect to the rejection of Claim 18 under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite, as understood the traversal relies on amendments. Claim 18 has been amended to specify that the solvent in the washing step is water which sures the indefiniteness issues raised. The rejection has been WITHDRAWN.
With respect to the rejection of claims 1-7 and 9-20 under 35 U.S.C. 102(a)(1) as being anticipated by Wu et al., as understood the traversal relies on amendments. Applicant argues “As no objection was raised against the first three pre- treatments of claim 11, which are now recited in claim 10, claim 10 and all claims dependent therefrom are believed to be free of the applied prior art.” [Remarks, Page 11, Paragraph 2]. This is unpersuasive. It is understood that adding water to a non-protic solvent would not only affect the polarity of the solvent but also the pH, which is the first pre-treatment of Claim 10 (previously Claim 11). This is because water is relatively acidic (pKa = 14) compared to organic solvents such as toluene (pKa = 43). The rejections have been MAINTAINED.
With respect to the rejection of claims 1 and 8 under 35 U.S.C. 102(a)(1) as being anticipated by Kumar et al., as understood the traversal relies on amendments. Applicant argues “The rejection based on Kumar is believed to be overcome by rewriting claim 10 in independent form, as claim 10 was not rejected based on Kumar.” [Remarks, Page 10, Paragraph 6]. This is unpersuasive. Kumar teaches at least the second pre-treatment step of homogenizing the solution “The sodium doped composite adsorbent and prior art alumina as prepared in example 1-3 were tested for organometallic catalyst residue pick in a fixed polyethylene melt purification solution adsorber of commercial solution polymerization unit during linear low density polyethylene (LLDPE) manufacture.” [0054]. It is understood that LLDPE precipitates out of solution at room temperature and therefore keeping it in a melt solution is equivalent to homogenizing the solution. The rejection has been MAINTAINED.
Claim Rejections - 35 USC § 102
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.
Claim(s) 2-7 and 9-20 is/are rejected under 35 U.S.C. 102(a)(1) as being anticipated by US 2008/0020928 A1 Wu et al. Claim 10 requires “A method for recovering a spent metal-containing homogeneous catalyst using a solid adsorbent selected from bleaching agents, filter aids and mixtures thereof, comprising the following steps:”. Wu et al. discloses a homogeneous catalyst removed by a solid sorbent “In yet another preferred embodiment, the catalyst system can be any single site catalyst or other constraint geometry catalyst or any other homogeneous catalysts that can be absorbed by proper solid sorbent.” [0009]. Regarding the identity of the sorbent Wu et al. discloses “Particularly preferred sorbents useful in the process of the invention include silica, alumina, activated alumina, di-atomaceous earth filter aid, zeolites of different pore size, MCM41, natural or synthetic clay materials, micro crystalline material or powdered cellulose material with hydroxyl group. These material are available from commercial solid sorbent suppliers with different trade names. Examples suitable for this applications include Celite 545, Celite 577, Hyflow, Perlite, Hyflo-SuperCelTM Celite, etc. Powered cellulose may have many different trade names. Examples are Solka-Floc® and Alpha-CelTM brand powdered cellulose.” [0065]. These are understood to be filter aids.
Claim 10 further requires “(A) providing a solution containing said spent metal- containing homogeneous catalyst, said solution containing at least one solvent selected from water and an organic solvent,”. Wu et al. discloses “Solvents for polymerization process can be any common paraffinic or aromatic hydrocarbons, such as pentanes, hexanes, heptane, Norpar™ or Isopar solvent, benzene, toluene, xylenes, ethylbenzene, propylbenzene, i- or t-butylbenzene, etc. Other solvents that are compatible with the homogenous or colloidal catalyst systems can also be used. Examples are methylene chloride, chloroform, chlorobenzene, etc.” [0019].
Claim 10 further requires “(B) adding to said provided solution said solid adsorbent to obtain a suspension of a solid and a solvent,”. Wu et al. discloses in Example 1 “1.5 wt % of a solid material Hyflo-SuperCelTM from Celite, which is a kind of diatomaceous earth solid, was added to the reactor effluent. The slurry was stirred at room temperature for 15 minutes.” [0074]. It is understood that a slurry is a suspension of a solid in a liquid solvent.
Claim 10 further requires “(C) separating said suspension to obtain a purified solvent and said solid adsorbent containing said spent metal-containing homogeneous catalyst adsorbed thereon.”. Wu et al. discloses “The slurry was filtered to remove solid sorbent. The effluent contained less than 1 ppm of metal catalyst components-Al, Zr, Si and B.” [0074].
Claim 10 further requires “wherein, prior to step (B), at least one of the following pre-treatments is performed:- the pH of the solution provided in step (A) is adjusted to a basic, neutral or acidic pH,- the solution provided in step (A) is homogenised,- the solution provided in step (A) is submitted to at least one liquid-solid separation to remove optional precipitates contained in the solution.”. Wu et al. discloses adding a protic solvent prior to adding the sorbent “The effluent was treated with 250 ppm water (or alcohol). Then, 1.5 wt % of a solid material Hyflo-SuperCelTM from Celite, which is a kind of diatomaceous earth solid, was added to the reactor effluent.” [0074]. Although Wu et al. does not explicitly disclose that the pH of the solution is adjusted to a basic, neutral or acidic pH one of ordinary skill in the art would know that non-protic solvents used by Wu et al., such as toluene, have a very high pH due to having a high pKa (43) and that adding water (pKa = 14) would adjust the pH to be more acidic. Regardless of whether the final pH results in a solution that is acidic, basic, or neutral the water addition step would fall within the range claimed. Although toluene was used as an example the same logic would apply to any of the solvents used by Wu et al.
Claim 2 requires “the solid adsorbent is selected from bleaching earths, perlites, diatomaceous earths and mixtures thereof.”. Wu et al. discloses perlites, diatomaceous earths and mixtures thereof (“Particularly preferred sorbents useful in the process of the invention include …, di-atomaceous earth filter aid …, Perlite, … These solid sorbent material can be used by itself or mixed with other sorbents to make them more effective.” [0065].).
Claim 3 requires “the solid adsorbent is a solid composition comprising from 50.0 to 95.0 wt% of silicium oxide (SiO2), from 5.0 to 50.0wt% of one or more oxides selected from aluminium oxide (Al2O3), iron III oxide (Fe2O3), potassium oxide (K2O), calcium oxide (CaO), sodium oxide (Na2O) and magnesium oxide (MgO).”. Wu et al. does not disclose the atomic composition of the solid adsorbents used. However, it is understood from the instant application specification that perlite has an atomic composition of “Perlite may comprise from 50.0 to 80.0 wt% of silicium oxide (SiO2), from 4.0 to 18.0 wt% of aluminium oxide (Al2O3), from 0.0 to 2.5 wt% of iron III oxide (Fe2O3), from 0.5 to 7.0 wt% of potassium oxide (K2O), from 0.0 to 2.5wt% of calcium oxide (CaO), , from 0.2 to 5.0 wt% of sodium oxide (Na2O) and from 0.1 to 1wt% or from 20 to 35wt% of magnesium oxide (MgO).” [Page 9, Lines 18-22] which reads on the range claimed. Wu et al. discloses perlite (“Particularly preferred sorbents useful in the process of the invention include …, Perlite” [0065].).
Claim 4 requires “the solid adsorbent is a solid composition comprising from 50.0 to 75.0 wt% of silicium oxide (SiO2), from 1.0 to 40.0 wt% of a compound or mixture of compounds selected from aluminium oxide (Al2O3) and magnesium oxide (MgO), from 0.5 to 5.0wt% of iron III oxide (Fe2O3), from 0.5 to 6.0 wt% of potassium oxide (K2O), from 0.0 to 6.0wt% of a compound or mixture of compounds selected from calcium oxide (CaO) and sodium oxide (Na2O).”. Similarly to Claim 3 the composition of perlite reads on the ranges presented and Wu et al. discloses perlite (“Particularly preferred sorbents useful in the process of the invention include …, Perlite” [0065].).
Claim 5 requires “the solid adsorbent is a solid composition comprising from 50.0 to 80.0 wt% of silicium oxide (SiO2), from 4.0 to 18.0 wt% of aluminium oxide (Al2O3), from 0.0 to 2.5 wt% of iron III oxide (Fe2O3), from 0.5 to 7.0 wt% of potassium oxide (K2O), from 0.0 to 2.5wt% of calcium oxide (CaO), , from 0.2 to 5.0 wt% of sodium oxide (Na2O) and from 0.1 to 1wt% or from 20 to 35wt% of magnesium oxide (MgO).”. This is understood to be equivalent to perlite. Wu et al. discloses perlite (“Particularly preferred sorbents useful in the process of the invention include …, Perlite” [0065].).
Claim 6 requires “the solid adsorbent is a solid composition comprising from 80.0 to 95.0 wt% of silicium oxide (SiO2), from 0.1 to 9.0 wt% of aluminium oxide (Al2O3), from 0.1 to 4.5 wt% of iron III oxide (Fe2O3) from 0.0 to 4.5wt% of calcium oxide (CaO) and from 0.0 to 1.5 wt% of magnesium oxide (MgO).”. Wu et al. does not disclose the atomic composition of the solid adsorbents used. However, it is understood from the instant application specification that diatomaceous earth has an atomic composition of “Typically, diatomaceous earths comprise from 80.0 to 95.0 wt% of silicium oxide (SiO2), from 0.1 to 9.0 wt% of aluminium oxide (Al2O3), from 0.1 to 4.5 wt% of iron III oxide (Fe2O3), from 0.0 to 4.5 wt% of calcium oxide (CaO) and from 0.0 to 1.5 wt% of magnesium oxide (MgO).” [Page 9, Lines 26-29]. Wu et al. discloses diatomaceous earth (“Particularly preferred sorbents useful in the process of the invention include …, di-atomaceous earth filter aid” [0065].).
Claim 7 requires “said solid adsorbent is in powder form or in granular form.”. Wu et al. discloses “The sorbent used in slurry phase have fine particle size, from 1 micron to 1000 micron average particle size” [0063]. Fine particles are understood to be a powder.
Claim 9 requires “said spent metal-containing homogeneous catalyst contains one or more metals selected from Ag, Au, Pt, Pd, Rh, Ir, Ru.”. Wu et al. discloses a palladium catalyst “said homogenous or colloidal catalyst is a transition metal complexed with diimide ligands, and wherein said transition metal is selected from the group consisting of Pd, Ni, Co, W, and Мo” [0090].
Claim 11 requires “prior to step (B), the following pre-treatment is performed - the polarity of the solution provided in step (A) is adjusted by addition of a polar solvent.”. Wu et al. discloses adding a polar solvent prior to adding the sorbent “The effluent was treated with 250 ppm water (or alcohol). Then, 1.5 wt % of a solid material Hyflo-SuperCelTM from Celite, which is a kind of diatomaceous earth solid, was added to the reactor effluent.” [0074]. Although Wu et al. does not explicitly disclose that the polarity and/or proticity of the solution is altered one of ordinary skill in the art would know that the addition of water (or alcohol) to a non-polar solvent (such as Norpar or toluene) would adjust both the polarity and proticity of the solvent. In other words Wu et al. implicitly discloses the adjustment of the polarity and proticity of the solvent prior to adding the sorbent.
Claim 12 requires “step (B) is performed at ambient temperature or from 35 °C to Tb-10 °C optionally under stirring, with Tb being the boiling temperature of the solvent(s) of the solution.”. In Example 5 Wu et al. discloses “A distilled polymerization effluent from polymerization method A … was mixed with 1.5% of diatomaceous earth solid sorbent filter aid Hyflo-SuperCelTM from Celite. The slurry was stirred at room temperature for 15 minutes.” [0078].
Claim 13 requires “the solid adsorbent added in the solution represents from 0.1 to 10 wt% of the total suspension.”. Wu et al. discloses “A distilled polymerization effluent from polymerization method A … was mixed with 1.5% of diatomaceous earth solid sorbent filter aid Hyflo-SuperCelTM from Celite.” [0078].
Claim 14 requires “step (C) includes at least one solid-liquid separation step selected from a centrifugation, a filtration and a decantation.”. Wu et al. discloses “The slurry was filtered to remove solid sorbent.” [0078].
Claim 15 requires “the solid adsorbent containing said spent metal-containing homogeneous catalyst adsorbed thereon is submitted to at least one of the following steps, after step (C) or during step (C) : a washing step with a solvent, a steam stripping step, a drying step.”. Wu et al. discloses washing and drying after being used in step C “These sorbent can be further re-activated and regenerated by calcinations or by washing/drying/calcinations. Thus the solid sorbent can be re-used.” [0066].
Claim 16 requires “prior to step (B), the proticity of the solution provided in step (A) is adjusted by addition of a polar solvent.”. Wu et al. discloses adding water prior to the sorbent “The effluent was treated with 250 ppm water (or alcohol). Then, 1.5 wt % of a solid material Hyflo-SuperCelTM from Celite, which is a kind of diatomaceous earth solid, was added to the reactor effluent.” [0074]. This is understood to affect the proticity of the solvent.
Claim 17 requires “in step (B), the solid adsorbent added in the solution represents from 1 to 5 wt% of the total suspension.”. Wu et al. discloses “A distilled polymerization effluent from polymerization method A … was mixed with 1.5% of diatomaceous earth solid sorbent filter aid Hyflo-SuperCelTM from Celite.” [0078].
Claim 18 requires “the solvent utilized in said washing step is water.”. Wu et al. discloses “These sorbent can be further re-activated and regenerated by calcinations or by washing/drying/calcinations. Thus the solid sorbent can be re-used. This method is much more efficient than conventional washing method, which generated a large amount of aqueous waste.” [0066]. Considering the disclosure of aqueous waste, one of ordinary skill in the art would understand that water must be the solvent if aqueous waste is generated.
Claim 19 requires “the solid adsorbent is a solid composition comprising from 50.0 to 95.0 wt% of silicium oxide (SiO2), from 5.0 to 50.0wt% of one or more oxides selected from aluminium oxide (Al2O3), iron III oxide (Fe2O3), potassium oxide (K2O), calcium oxide (CaO), sodium oxide (Na2O) and magnesium oxide (MgO).”. It is understood that perlite meets these requirements (see Claim 3). Wu et al. discloses perlite (“Particularly preferred sorbents useful in the process of the invention include …, Perlite” [0065].).
Claim 20 requires “the solid adsorbent is a solid composition comprising from 50.0 to 75.0 wt% of silicium oxide (SiO2), from 1.0 to 40.0 wt% of a compound or mixture of compounds selected from aluminium oxide (Al2O3) and magnesium oxide (MgO), from 0.5 to 5.0wt% of iron III oxide (Fe2O3), from 0.5 to 6.0 wt% of potassium oxide (K2O), from 0.0 to 6.0wt% of a compound or mixture of compounds selected from calcium oxide (CaO) and sodium oxide (Na2O).”. It is understood that perlite meets these requirements (see Claim 4). Wu et al. discloses perlite (“Particularly preferred sorbents useful in the process of the invention include …, Perlite” [0065].).
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 for establishing a background for determining obviousness under 35 U.S.C. 103 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.
Claim(s) 8 is/are rejected under 35 U.S.C. 103 as being unpatentable over US 2008/0020928 A1 Wu et al. in view of US 2013/0341563 A1 Kumar et al. Regarding Claim 8, Wu et al. discloses all of the limitations of Claim 10. Claim 8 further requires “wherein said solid adsorbent has a specific surface area from 150 to 400 m2/g.”. Wu et al. discloses “The Solid Sorbents generally have Surface hydroxyl group or Surface oxygen group to react chemically or to interact physically with the catalyst components and/or catalyst residuals. Generally they should have surface area greater than 0.1 m2/gram” [0063]. Although this range overlaps with the range claimed, it is not sufficiently specific to motivate a surface area of between 150-400 m2/g on its own.
Kumar et al. is similarly directed to methods of recovering spent polyolefin catalysts from post-polymerization solution (“In accordance with the present disclosure, there is provided a solid shaped composite adsorbent for reducing deactivated catalyst residues and contaminants from a post polyolefin solution polymerization mixture” [0016].). Kumar et al. discloses “Typically, the adsorbent has surface area in the range of 150 m2/g to 250 m2/gm.” [0023].
It would have been obvious for one of ordinary skill in the art to have combined the method of Wu et al. with the solid sorbent of Kumar et al. for at least the reason that they are directed to methods of solving the same problem: removal of spent catalyst after the reaction.
The motivation to have combined the sorbent of Kumar et al. with the method of Wu et al. is given by Kumar et al. “A particularly preferred spherical agglomerated composite adsorbent having 8-10 mesh size (Tyler series) has about 270 m2/g surface area, 0.47 cc/g total pore volume, LOI of 2.8 wt % at 280-1000° C. crush strength about 5.5 kgf and bulk density of about 0.80 gm/cc of formed composites spheres. The agglomerated composite spheres have almost Zero attrition compared to activated alumina, which is an important parameter required for a polymerization mixture purification adsorbent in a solution polymerization adsorber.” [0043].
Conclusion
Applicant's amendment necessitated any new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a). A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
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/JOSHUA MAXWELL SPEER/
Examiner
Art Unit 1736
/DANIEL BERNS/Primary Examiner, Art Unit 1736
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