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 .
Priority
Acknowledgment is made of applicant’s claim for foreign priority under 35 U.S.C. 119 (a)-(d). A certified copy of Application No. CN-2022109354843, filed 04 August 2022, has been received.
Information Disclosure Statement
The Information Disclosure Statement (IDS), filed 05 March 2024, has been reviewed and considered by the examiner.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 1-10 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention.
The claims are generally narrative and indefinite, failing to conform with current U.S. practice. They appear to be a literal translation into English from a foreign document and are replete with grammatical and idiomatic errors. Specific examples of indefinite claim language include:
Claim 1 recites the limitation, “a certain flow rate,” in line 6. What would be considered an appropriate flow rate is undefined, and no basis for which what is encompassed by the scope is provided, thus rendering the claim indefinite.
Claim 1 recites the limitation, “the aluminum salt function material gel,” in lines 12-13, step 1A. There is insufficient antecedent basis for this limitation in the claim.
Claim 3 recites the limitation, “the solid content,” in line 3. There is insufficient antecedent basis for this limitation in the claims. For the purposes of examination and based on the specification, the solid content is interpreted to include the added polyaluminum, lithium source, and additive (as per Embodiments 1 and 17 of the instant specification).
Claim 4 recites the limitation, “the feeding time,” in line 3. There is insufficient antecedent basis for this limitation in the claim.
Claim 4 recites the limitation, “the feeding flow rate,” in line 2. There is insufficient antecedent basis for this limitation in the claim.
Claim 5 recites the limitation, “the additive in step 1 is any one of diatomite, titanium dioxide, zirconia and graphene, and the addition amount is 0% - 10% of the solid mass.” However, claim 1 appears to require an additive. Therefore, it is not clear whether the additive is an optional reagent or is required by the claims.
Claim 6 recites the limitation, “the reaction temperature,” in line 2. There is insufficient antecedent basis for this limitation in the claim because the reaction of step 1 was previous defined as, “constant-temperature stirring reaction” and it is unclear if claim 6 is referring to the constant-temperature stirring reaction or another reaction within claim 1.
Claim 9 recites the limitation, “the particle size D50 of grinding powder in step 2,” in line 2. There is insufficient antecedent basis for this limitation in the claim.
Claims 2-10 are rejected over their dependence on rejected claim 1.
Claim Rejections - 35 USC § 103
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.
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.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 1, 7, 8, and 10 are rejected under 35 U.S.C. 103 as being unpatentable over Chinese Patent Publication No. CN113926419A (published 14 Jan 2022, citations herein made to the English translation provided).
In regard to claim 1, Patent Publication CN113926419A (herein referred to as CN ‘419A) teaches a preparation method for a functional material for extracting lithium from an aluminum salt (LiCl·mAl(OH)3·nH2O), comprising preparation of an aluminum salt functional material precursor slurry by mixing polyaluminum, a lithium source and water in proportion [n0016], adding an additive [n0018], performing ultrasonic stirring to obtain a mixed salt solution [n0016], adding an alkali liquor into the mixed salt solution at a certain flow rate ([n0018] and lines 2-4, [n0019]), adjusting the pH value [n0018], and then performing constant-temperature reaction to obtain a lithium-intercalated aluminum salt functional precursor slurry (i.e. hydrothermal reaction, [n0021]); and preparation of aluminum salt functional material powder via A) preparation of gel: The lithium-intercalated aluminum salt functional precursor slurry obtained in step 1 is subjected to solid-liquid separation (line 1 of [n0023]); B) scrubbing: scrubbing the aluminum salt functional material gel obtained in the step A) with deionized water (i.e. rinsing, line 2, [n0023] and [n0026]), and then performing solid-liquid extraction to obtain lithium-intercalated gel (i.e. elution, lines 3-5 [n0023]) and separation (line 5, [n0023]); C) drying and grinding: drying and grinding the lithium-intercalated gel obtained in the step B) to obtain a functional material for extracting lithium from an aluminum salt (lines 5-7, [n0023]).
CN ‘419A does not explicitly teach that the aging process or hydrothermal reaction are conducted with stirring. Example 1 indicates that the first aging step is conducted with the solution being stationary (line 8, [n0043]), but does not specify whether the subsequent hydrothermal reaction is conducted with or without stirring (lines 8-10, [n0043]). Identifying a reliable means of producing an effective lithium adsorbent is of importance in the art, as identified by CN ‘419 [n004] & [n007]. Conducting the constant-temperature reaction with or without stirring constitutes a finite number of ways in which the reaction could be conducted, both of which a person of ordinary skill would have identified as acceptable reaction conditions which predictably yield the resulting slurry, albeit with different physical characteristics. A person of ordinary skill would have found it obvious to try the constant-temperature reaction discussed by CN ‘419A (the hydrothermal reaction) with and without stirring to yield the constant temperature stirring reaction instantly claimed.
CN ‘419A does not explicitly teach solid-liquid separation after scrubbing the aluminum salt functional material gel with DI water in step B as instantly claimed. Instead, CN ‘419A teaches that after scrubbing (i.e. washing) the precursor is dried, ground, and added to a solvent for elution. Then, separation is performed and the solution is again dried and ground to obtain a powdered Keggin chain structure aluminum-based lithium adsorbent. Elution is a form a solid-liquid extraction, not solid-liquid separation, but constitutes the addition and subsequent removal of a solvent from a solid phase. Herein, elution serves the same functional purpose as other traditional means of solid-liquid separation, wherein a liquid phase is removed from a solid phase by gravity, vacuum, etc. A person of ordinary skill in the art could readily envision modifying the procedure taught by CN ‘419A to use solid-liquid separation in lieu of elution in step B as the two procedures are functionally equivalent. Therefore, a person of ordinary skill in the art, at the relevant time, would have found it obvious to replace the method of elution after scrubbing with solid-liquid separation to yield the process as instantly claimed as the two processes are functionally equivalent within the overall preparation method.
In regard to claim 7, CN ‘491A teaches that the method of solid-liquid separation employed in step 2 may be centrifugal filtration/centrifugation or vacuum filtration as instantly claimed [n0028].
In regard to claim 8, CN ‘419A teaches that the drying method in step 2 is vacuum drying as instantly claimed [n0023].
In regard to claim 10, CN ‘419A teaches a functional material for extracting lithium prepared according to the procedure of claim 1 [n0009] & [n0023].
Claims 2-5, and 9 are rejected under 35 U.S.C. 103 as being unpatentable over CN '419A as applied to claim 1 above, and further in view of Harrison et al. (US Patent No. 8,637,428, published 28 Jan 2014).
In regard to claim 2, CN ‘419A teaches that the polyaluminum in step 1 may be polyaluminum chloride [n0024]. CN ‘419A further teaches that the lithium source may be lithium nitrate, lithium sulfate, or lithium chloride [n0025] and that the alkali source in the aqueous solution may be sodium hydroxide, potassium hydroxide, or ammonia [n0026]. CN ‘419A teaches that the polyaluminum utilized is mostly a byproduct of industrial processes [n0008]-[n0009] and may not necessarily be industrial, drinking water, or food-grade polyaluminum chloride. However, Harrison et al. teaches that in the synthesis of lithium aluminum intercalate particles, polyaluminum hydroxyl chloride (KPAX-XL 19) was purchased from Kemira chemical manufacturing (Col. 8, lines 61-62). It would be obvious to one of ordinary skill in the art to employ an industrial grade polyaluminum chloride, as taught by Harrison et al., instead of polyaluminum chloride from a waste stream, as taught by CN ‘419A, to ensure there was no contamination of the final product.
In regard to claim 3, CN ‘419A teaches that the polyaluminum and lithium source are added together in an Al:Li molar ratio of 0.2-10:1, which overlaps the instantly claimed ratio of 1.5-9:1 Al:Li; that the pH value may be adjusted to 3-12, which overlaps the claimed pH range of 5-9; and that the time for constant temperature stirring reaction is 0.5-48 hours, which overlaps the claimed time range of 0.2-4 hours.
With respect to the ratio of added water to solid reagents, CN ‘419A teaches that 20g and polyaluminum chloride powder and an amount of lithium chloride were added to 400 mL of deionized water. Lithium chloride was added in a range of 4.3 g to 25 g, based on the attempted Al:Li ratios of 0.2-1.2 Li:Al of Fig. 1. At a molar ratio of 1.5:1 Al:Li, 12.8 g of LiCl were added to solution, which accounts for a total solid content of 7.4% ((20g + 12.8g)/(20g + 12.8g + 400g)). CN ‘419A broadly teaches that the lithium-aluminum mixed solution contains 0.01-15 M Li ions and 0.1-10 M aluminum ions, reflecting a large range of starting reagents to water added. The concentration of reagents in solution has a demonstrated impact on particle size and crystal morphology. For example, Harrison et al. teaches that during the production of a lithium-aluminum intercalate loaded onto a substrate, the specific synthesis conditions employed, which includes reagent concentration during the reaction, may impact the size and thickness of lithium aluminum intercalate platelets formed (Col. 7, lines 8-24), the hydration levels of the crystal structure, and/or the crystal plane stacking (Col. 7, lines 25-33), which in turn influence the lithium loading/unloading of the final composition (Col. 7, lines 36-40). Therefore, it would have been obvious to optimize the reaction conditions taught by CN ‘419A to modify the solid content of the aluminum salt precursor slurry from 7-9% to be between 10-50%, as instantly claimed, in order to achieve specific, desired physical properties of the final composition including particle size and crystal geometry.
In regard to claim 4, CN ‘419A does not teach that the feeding time for the alkali liquor to the aluminum-lithium slurry is between 0.1-2 hours. Instead, CN ‘419A generally discloses that the feeding flow rate of an alkali liquor with a concentration of 0.5-20 M to an aluminum-lithium solution may be between 0.5-100 mL/min [n0019]. Within the feeding time window of 0.1-2 hours, the range of addition rates discloses allows for the addition of 3 mL to 12,000 mL of alkali solution.
However, Harrison et al. teaches that the functional material may adopt variations in crystalline geometry based on the synthesis conditions used, wherein the controlled synthesis conditions include the sequence of reactant addition and the amounts of reactants (which is inclusive of water) that are added (Col. 8, lines 38-41). Furthermore, Harrison et al. specifically cites variation in platelet size, crystal hydration, and stacking of elementary crystal planes based on the synthesis conditions used may impact lithium ion loading of the material (Col. 7, lines 8-24 & lines 36-40).
It would have been obvious to one of ordinary skill at the relevant time to optimize the addition rate disclosed to add all of the required alkali liquor in order to achieve the desired adjusted pH within a time window of 0.1-2 hours because the synthesis conditions of the intercalated lithium-aluminum material (i.e. the rate of reaction via basicity) have a direct impact on the crystal structure of the functional material, which in turn affect the lithium loading/unloading capacity of the product.
In regard to claim 5, CN ‘419A does not teach that diatomite, titanium dioxide, zirconia, or graphene are added as additives in an amount equal to 0-10% of the solid mass in step 1. However, Harrison et al. teaches that diatomaceous earth, titanium oxide, zirconia, or carbon-based materials are all acceptable substrates to which a lithium aluminum intercalate can be adhered (Col. 4, lines 8-18). Harrison et al. discloses a lithium aluminum intercalate on diatomaceous earth was prepared by mixing 20 g of diatomaceous earth, 90 g of 50 wt% polyaluminum hydroxyl chloride, and 11.2 g of LiCl, which results in diatomaceous earth accounting for 26.2% of the solid content of the reaction (Col. 8, line 59-Col. 9, line 5). Harrison et al. further discloses that additional polyaluminum hydroxyl chloride may be added to the substrate to reach a steady state of precipitation (Col. 8, lines 52-59).
Therefore, it would have been obvious to one of ordinary skill in the art at the relevant time to modify the ratio of additive (i.e. diatomaceous earth, titania, zirconia, etc.) to lithium aluminum intercalate particles so that the additive accounts for 10% or less of the solid mass in step 1 of the preparation method in order to deposit the maximum possible amount of polyaluminum hydroxyl chloride onto the substrate. Furthermore, it would have been obvious to one having ordinary skill in the art at the time the invention was made to choose the instantly claimed addition amount of diatomite, TiO2, ZrO2, or graphene through process optimization, since it has been held that there the general conditions of a claim are disclosed in the prior art, discovering the optimum or workable ranges involves only routine skill in the art. See In re Boesch, 205 USPQ 215.
In regard to claim 9, CN ‘419A does not teach that the functional material for extracting lithium is ground to have a particle diameter D50 of 0.1-20 µm. CN ‘419A teaches that the synthesized functional material generally has smaller dimensions [n0033] and provides an example of a material with an average particle size of 161 µm [n0047]. However, Harrison et al. teaches that smaller particles of lithium aluminum intercalate are preferable because of the positive relationship between the proximity of the intercalated lithium ions to the particle surface and ease of adsorption/desorption (Col. 6, lines 14-24). Furthermore, Harrison et al. teaches that lithium aluminum intercalated particles with an average diameter smaller than 10 µm have an advantageously large surface area and improved adsorption/desorption properties (Col. 7, lines 55-67), and may be loaded onto a porous substrate to prevent a hindered flow of brine during extraction. A person of ordinary skill in the art at the relevant time would readily understand the advantages of a smaller functional material particle size, specifically of an average particle size at or below 10 µm, as taught by Harrison et al. Therefore, it would have been obvious to one of ordinary skill at the relevant time to optimize the final particle size of the functional material of CN ‘419A to have an average particle size (D50) of 10 µm or lower, which is within the claimed range of 0.1-20 µm, in order to maximize the adsorption/desorption rate of lithium ions.
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over CN '419A as applied to claim 1 above, and further in view of Builliard-Sauret et al. (Experimental Thermal and Fluid Science, 2019, 104, pp. 258-271).
In regard to claim 6, CN ‘419A teaches the reaction temperature of the reaction is step 1 may be 10-80°C as instantly claimed [n0016], and that the ultrasonic stirring time is 5-240 min, which overlaps the instantly claimed range of 5-30 min [n0016]. CN ‘419A is silent to frequency employed for ultrasonic stirring in both the general disclosure and specific embodiments. However, it is understood by a person of ordinary skill in the art that low frequency ultrasound agitation (generally 20 kHz to 40 kHz) is a typical low frequency employed for optimal stirring via ultrasound agitation. As taught by Bulliard-Sauret et al., ultrasonic irradiation at 25 kHz was effective at generating acoustic cavitation (i.e. disturbance of a liquid via oscillating gas vapors) which is most often employed as a stirring technique in various industries (pp. 258, Abstract & pp. 259, left col., 2nd paragraph). Therefore, it would have been obvious to one of ordinary skill in the art at the relevant time to select an operating frequency between 20 and 60 kHz, as instantly claimed, to effectively stir the reaction of step 1 because the range described is of routine use in the art and higher frequencies may induce unwanted convection (pp. 269, right col., 5th paragraph).
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure:
Chinese Patent Publication No. CN-106076243A, which describes a microporous lithium extraction material made from an aluminum salt with formula LiCl·2Al(OH)3·H2O, a method of its preparation, and a discussion of the effect of stirring, addition rate, and pH on the physical properties of the final product.
French Patent Publication No. FR-3024445A, which describes a lithium extraction material made from an aluminum salt with formula LiXx·2Al(OH)3·nH2O and a method of its preparation.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to MORDECAI M LEAVITT whose telephone number is (571)272-6637. The examiner can normally be reached Monday-Friday 8AM-5PM.
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/MORDECAI M LEAVITT/Examiner, Art Unit 1742 /CHRISTINA A JOHNSON/Supervisory Patent Examiner, Art Unit 1742
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