DETAILED ACTION
Continued Examination Under 37 CFR 1.114
1. A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on 2/19/26 has been entered.
Response to Amendment
2. In response to the amendment received on 2/19/26:
claims 1, 2, and 4-10 are presently pending
all prior art grounds of rejection based on MAGNAN, SNYDACKER, HIAI, CR11 and SASAKI are withdrawn in light of the amendments to the claims
new prior art grounds of rejection based on MAGNAN, SNYDACKER, HIAI, CR11 and SASAKI are set forth as contained herein
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claim(s) 1 is/are rejected under 35 U.S.C. 103 as being unpatentable over US Pub. No. 2016/0032471 to Magnan et al., (hereinafter referred to as “MAGNAN”) in view of US Pub. No. 2019/0256987 to Snydacker et al., (hereinafter referred to as “SNYDACKER”) and US Pub. No. 2010/0116093 to Hiai et al., (hereinafter referred to as “HIAI”).
Regarding claim 1, MAGNAN teaches a method for producing lithium hydroxide (see generally MAGNAN at Abstract discussing the disclosed process for obtaining lithium hydroxide by electrodialysis under conditions to convert a lithium compound to lithium hydroxide, and Fig. 1 depicting the process including purity removal steps, followed by an ion exchange step, followed by a membrane electrolysis step; see also MAGNAN at ⁋98 generally teaching the starting lithium containing materials including lithium chloride, i.e. LiCl; see also MAGNAN at ⁋101 and ⁋110 generally discussing the electrodialysis of LiCl; see also MAGNAN at ⁋147-⁋149 generally teaching a purity removal step; see also MAGNAN at ⁋154-⁋157 generally teaching the ion exchange step; see also MAGNAN at ⁋171-⁋215 disclosing an exemplary process using lithium sulphate and starting with a leached ore solution, which is illustrative of the process for a lithium chloride starting material and which the rejection herein is based), comprising:
adding an alkali to a first lithium chloride containing liquid to obtain a post-neutralization liquid (see MAGNAN at ⁋147-⁋149 and at ⁋177, ⁋182 and ⁋183 teaching the addition of an alkali, i.e. NaOH, to precipitate out impurities from the lithium containing material);
bringing the post-neutralization liquid into contact with an ion-exchange resin to obtain a second lithium chloride containing liquid (see MAGNAN at ⁋154-⁋157 and at ⁋191 teaching the use of an ion exchange step to further remove impurities and which would result in a further purified lithium containing material); and
electrodialyzing the second lithium chloride containing liquid to obtain a lithium hydroxide containing liquid (see MAGNAN at ⁋98, ⁋101, ⁋110 and at ⁋212 teaching the eventual electrodialysis in order to produce lithium hydroxide from the purified lithium chloride containing material), wherein
the ion exchange resin is regenerated by immersing it in a liquid having a hydrogen concentration of acid of 0.3 mol/L or more and 2.0 mol/L or less (see MAGNAN at ¶192 teaching the method including a regeneration step included in the processing; and see MAGNAN at ¶194 teaching the treatment of the ion exchange resin with 2 M HCl which would have H+ ions at a concentration of 2 mol/L as claimed).
MAGNAN fails to explicitly teach: (1) the obtaining of the lithium containing material by bringing a lithium adsorbent obtained from lithium manganate into contact with a low lithium content liquid to obtain a post-adsorption lithium manganate, and bring the post-adsorption lithium manganate into contact with a hydrochloric acid solution to obtain the first lithium chloride containing liquid that is then purified before going through the purification and electrodialysis process of MAGNAN to produce the lithium hydroxide product; and (2) the SV and BV values of the post-neutralization liquid passing through the column as claimed.
As to (1), while MAGNAN teaches the starting lithium containing material being from any of a number of different sources and comprising a number of various lithium compounds (see MAGNAN at ⁋98), MAGNAN fails to explicitly teach the obtaining of the lithium containing material by bringing a lithium adsorbent obtained from lithium manganate into contact with a low lithium content liquid to obtain a post-adsorption lithium manganate, and bring the post-adsorption lithium manganate into contact with a hydrochloric acid solution to obtain the first lithium chloride containing liquid that is then purified before going through the purification and electrodialysis process of MAGNAN to produce the lithium hydroxide product.
However, SNYDACKER teaches methods of extracting lithium from liquid resources such as natural and synthetic brines (see SNYDACKER at Abstract). Specifically, SNYDACKER teaches the use of a lithium ion exchange materials including various types of lithium manganese oxides or combinations thereof (see SNYDACKER at ⁋329) to remove lithium from the brine solutions being treated (see SNYDACKER at ⁋325-⁋327 reading on the step of bringing the lithium adsorbent into contact with a low lithium content liquid as claimed) and then be washed with hydrochloric acid in order to release the stored lithium (see SNYDACKER at ⁋329 teaching the step of obtaining the first lithium chloride containing liquid as claimed).
Moreover, one of ordinary skill in the art would have recognized that the lithium salt solution collected by the process of SNYDACKER (see SNYDACKER at ⁋329) after the treatment with HCl would be a LiCl containing solution which would then be ready for further processing. One of ordinary skill in the art would have appreciated that the process of MAGNAN could be used to get the lithium in a useable form, such as by further purification and then conversion to lithium hydroxide as taught by MAGNAN.
Consequently, one of ordinary skill in the art would have been motivated to have used the first part of the process of SNYDACKER in order to obtain a lithium containing solution to be used by the process MAGNAN, which is taught as being suitable on a wide array of lithium containing materials (see MAGNAN at ⁋98). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used the initial process of SNYDACKER, as set forth, in order to obtain a first lithium chloride containing liquid for treatment by the purification and conversion process of MAGNAN so as to arrive at having the predictable result of a process as claimed.
As to (2), while MAGNAN as modified by SNYDACKER teaches the ion exchange portion of the process being performed with a column (see MAGNAN at ⁋192 and ⁋194 teaching the ion exchange resin being in columns), MAGNAN in view of SNYDACKER fails to explicitly teach the SV and BV values of the post-neutralization liquid passing through the column as claimed.
However, it is noted that HIAI teaches a column ion exchange process for silver recovery in which the parameters of the ion exchange are conducted at an SV of 5 or less and a BV value of 10-20 (see HIAI at ⁋13, ⁋45, and ⁋47). As such, HIAI shows that it is known in the art to have the parameters for an ion exchange process set within the values as claimed. Moreover, MAGNAN teaches a person of ordinary skill in the art would recognize, and is aware of, the need to vary and adjust parameters such as flow rates, retention time, bed volumes, etc. based on the nature of the materials, level of purity and would be motivated to adjust the conditions in order to allow for the best impurity removal balanced against time for the processing (MAGNAN at ¶99).
Therefore, it would have been obvious to one of ordinary skill in the art to have set the SV and BV values within the ranges as claimed as taught HIAI in the process of MAGNAN; or, alternatively, to have optimized the conditions so as to arrive at values that allow for the effective removal of impurities while also allowing for the process to be conducted in a reasonable time frame.
Claim(s) 2 is/are rejected under 35 U.S.C. 103 as being unpatentable over MAGNAN in view of SNYDACKER.
Regarding claim 2, MAGNAN teaches a method for producing lithium hydroxide (see generally MAGNAN at Abstract discussing the disclosed process for obtaining lithium hydroxide by electrodialysis under conditions to convert a lithium compound to lithium hydroxide, and Fig. 1 depicting the process including purity removal steps, followed by an ion exchange step, followed by a membrane electrolysis step; see also MAGNAN at ⁋98 generally teaching the starting lithium containing materials including lithium chloride, i.e. LiCl; see also MAGNAN at ⁋101 and ⁋110 generally discussing the electrodialysis of LiCl; see also MAGNAN at ⁋147-⁋149 generally teaching a purity removal step; see also MAGNAN at ⁋154-⁋157 generally teaching the ion exchange step; see also MAGNAN at ⁋171-⁋215 disclosing an exemplary process using lithium sulphate and starting with a leached ore solution, which is illustrative of the process for a lithium chloride starting material and which the rejection herein is based), comprising:
adding an oxidant to a first lithium chloride containing liquid to obtain a post-oxidation liquid (see MAGNAN at ⁋176 teaching a primary impurity removal step which includes adjusting the pH and sparging air, i.e. containing O2 as the oxidant, into the lithium salt solution that is being treated so as to precipitate out Fe);
adding an alkali to a first lithium chloride containing liquid to obtain a post-neutralization liquid (see MAGNAN at ⁋147-⁋149 and at ⁋177, ⁋182 and ⁋183 teaching the addition of an alkali, i.e. NaOH, to precipitate out impurities from the lithium containing material);
bringing the post-neutralization liquid into contact with an ion-exchange resin to obtain a second lithium chloride containing liquid (see MAGNAN at ⁋154-⁋157 and at ⁋191 teaching the use of an ion exchange step to further remove impurities and which would result in a further purified lithium containing material); and
electrodialyzing the second lithium chloride containing liquid to obtain a lithium hydroxide containing liquid (see MAGNAN at ⁋98, ⁋101, ⁋110 and at ⁋212 teaching the eventual electrodialysis in order to produce lithium hydroxide from the purified lithium chloride containing material), wherein
the ion exchange resin is regenerated by immersing it in a liquid having a hydrogen concentration of acid of 0.3 mol/L or more and 2.0 mol/L or less (see MAGNAN at ¶192 teaching the method including a regeneration step included in the processing; and see MAGNAN at ¶194 teaching the treatment of the ion exchange resin with 2 M HCl which would have H+ ions at a concentration of 2 mol/L as claimed).
MAGNAN fails to explicitly teach: (1) the obtaining of the lithium containing material by bringing a lithium adsorbent obtained from lithium manganate into contact with a low lithium content liquid to obtain a post-adsorption lithium manganate, and bring the post-adsorption lithium manganate into contact with a hydrochloric acid solution to obtain the first lithium chloride containing liquid that is then purified before going through the purification and electrodialysis process of MAGNAN to produce the lithium hydroxide product; and (2) the oxidant being sodium hypochlorite, i.e. NaOCl, as claimed.
As to (1), while MAGNAN teaches the starting lithium containing material being from any of a number of different sources and comprising a number of various lithium compounds (see MAGNAN at ⁋98), MAGNAN fails to explicitly teach the obtaining of the lithium containing material by bringing a lithium adsorbent obtained from lithium manganate into contact with a low lithium content liquid to obtain a post-adsorption lithium manganate, and bring the post-adsorption lithium manganate into contact with a hydrochloric acid solution to obtain the first lithium chloride containing liquid that is then purified before going through the purification and electrodialysis process of MAGNAN to produce the lithium hydroxide product.
SNYDACKER teaches methods of extracting lithium from liquid resources such as natural and synthetic brines (see SNYDACKER at Abstract). Specifically, SNYDACKER teaches the use of a lithium ion exchange materials including various types of lithium manganese oxides or combinations thereof (see SNYDACKER at ⁋329) to remove lithium from the brine solutions being treated (see SNYDACKER at ⁋325-⁋327 reading on the step of bringing the lithium adsorbent into contact with a low lithium content liquid as claimed) and then be washed with hydrochloric acid in order to release the stored lithium (see SNYDACKER at ⁋329 teaching the step of obtaining the first lithium chloride containing liquid as claimed).
Moreover, one of ordinary skill in the art would have recognized that the lithium salt solution collected by the process of SNYDACKER (see SNYDACKER at ⁋329) after the treatment with HCl would be a LiCl containing solution which would then be ready for further processing. One of ordinary skill in the art would have appreciated that the process of MAGNAN could be used to get the lithium in a useable form, such as by further purification and then conversion to lithium hydroxide as taught by MAGNAN.
Consequently, one of ordinary skill in the art would have been motivated to have used the first part of the process of SNYDACKER in order to obtain a lithium containing solution to be used by the process MAGNAN, which is taught as being suitable on a wide array of lithium containing materials (see MAGNAN at ⁋98). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used the initial process of SNYDACKER, as set forth, in order to obtain a first lithium chloride containing liquid for treatment by the purification and conversion process of MAGNAN so as to arrive at having the predictable result of a process as claimed.
As to (2), while MAGNAN teaches O2 as the oxidant to assist in the removal of impurities from the lithium concentrate solution (see MAGNAN at ⁋176; see also MAGNAN at ¶169 teaching the starting lithium material being lithium chloride), SNYDACKER also teaches that it is known when removing impurities from a lithium containing solution to remove impurities via oxidation using O2 or NaOCl, i.e. sodium hypochlorite (see SNYDACKER at ¶240). One of ordinary skill would have recognized that besides the addition of O2 as an oxidant, that any known oxidation component could be employed. As such, the use of another known oxidizing agent, such as sodium hypochlorite as taught by SNYDACKER, would have been obvious to one of ordinary skill in the art.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used a sodium hypochlorite oxidant, as taught by SNYDACKER, instead of the O2 oxidant for the removal of hydroxides of Fe, Al, and Si in the method of MAGNAN as modified by SNYDACKER as set forth above.
Claim(s) 4, 5, 6 and 7 is/are rejected under 35 U.S.C. 103 as being unpatentable over MAGNAN in view of SNYDACKER and HIAI as applied to claim 1 above (for claims 4 and 5), or MAGNAN in view of SNYDACKER as applied to claim 2 above (for claims 6 and 7), and further in view of “Product Data Sheet – DIAION CR11” Version No. 01-09-A-0108 publicly accessible on Dec. 2017 (hereinafter referred to as “CR11”).
Regarding claims 4, 5, 6, and 7, while MAGNAN as modified by SNYDACKER and HIAI or MAGNAN as modified by SNYDACKER above, teaches the use of a Purolite S950 ion exchange resin in sodium form and also teaches that any ion exchange resin that is suitable for removing divalent cations and/or trivalent metal cations could alternatively be used (see MAGNAN at ⁋191), MAGNAN fails to explicitly teach the ion exchange resin being an iminodiacetic acid type or an iminoacetate type chelating resin in sodium form as claimed.
However, CR11 teaches a commercially available iminodiacetate type chelating resin in sodium form that is highly selective for multivalent metal ions and in particular trivalent metal ions (see CR11 at page 1, first paragraph; and, bottom of section titled “Product” showing the resin in the Na+ or sodium form). As such, one of ordinary skill in the art would have readily recognized CR11 as an alternative resin that could be used in the ion exchange process to further purify and remove divalent and trivalent metal cations. Furthermore, the substituting of one known ion exchange resin for another known ion exchange resin both of which are suitable for the removal of divalent and/or trivalent metal cations as taught by MAGNAN, would have been obvious to one of ordinary skill in the art.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used CR11 as the ion exchange resin, as taught by CR11, for further purifying the lithium chloride containing solution in the process of MAGNAN as modified by SNYDACKER, or MAGNAN as modified by SNYDACKER and HIAI, in order to further remove impurity bivalent and trivalent metal cations.
Claim(s) 8 and 9 is/are rejected under 35 U.S.C. 103 as being unpatentable over MAGNAN in view of SNYDACKER as applied to claim 2 above, and further in view of HIAI.
Regarding claims 8 and 9, while MAGNAN as modified by SNYDACKER teaches the ion exchange portion of the process being performed with a column (see MAGNAN at ⁋192 and ⁋194 teaching the ion exchange resin being in columns), MAGNAN in view of SNYDACKER fails to explicitly teach the SV and BV values of the post-neutralization liquid passing through the column as claimed.
However, it is noted that HIAI teaches a column ion exchange process for silver recovery in which the parameters of the ion exchange are conducted at an SV of 5 or less and a BV value of 10-20 (see HIAI at ⁋13, ⁋45, and ⁋47). As such, HIAI shows that it is known in the art to have the parameters for an ion exchange process set within the values as claimed. Moreover, MAGNAN teaches a person of ordinary skill in the art would recognize, and is aware of, the need to vary and adjust parameters such as flow rates, retention time, bed volumes, etc. based on the nature of the materials, level of purity and would be motivated to adjust the conditions in order to allow for the best impurity removal balanced against time for the processing.
Therefore, it would have been obvious to one of ordinary skill in the art to have set the SV and BV values within the ranges as claimed as taught HIAI in the process of MAGNAN; or, alternatively, to have optimized the conditions so as to arrive at values that allow for the effective removal of impurities while also allowing for the process to be conducted in a reasonable time frame.
Claim 10 is/are rejected under 35 U.S.C. 103 as being unpatentable over MAGNAN in view of SNYDACKER and HIAI as applied to claim 1 above, and further in view of SASAKI.
Regarding claim 10, while MAGNAN as modified by SNYDACKER and HIAI teaches the use of brine solutions from a wide range of sources including natural brine, seawater, a concentrated brine, or other synthetic brines (see SNYDACKER at ⁋27), SNYDACKER fails to explicitly teach the brine being a salt lake brine. However, SASAKI teaches that salt lake brines are known to exist, that the reserves of them are large and that they contain lithium salts and are advantageous resources in terms of production costs (see SASAKI at ⁋4). As such, one of ordinary skill in the art would have recognized that as taught by SNYDACKER that any natural brine which could be used as a low lithium content liquid brine source could and would also include the salt lake brines which are known to have lithium salts therein and be readily available. Furthermore, one of ordinary skill in the art would have been motivated to have used a salt lake brine due to its favorable production costs as mentioned by SASAKI.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used as the low lithium content liquid brine of SNYDACKER the salt lake brine as taught by SASAKI in order to yield the predictable result of having the modified process MAGNAN as claimed.
Response to Arguments
Applicant's arguments filed 2/19/26 have been fully considered but they are not persuasive. Specifically, it is noted that as set forth in the new grounds of rejection above, the Examiner is of the opinion that MAGNAN does teach the newly added limitation contrary to applicant’s assertion (see Remarks at page 7, penultimate paragraph).
Consequently, for at least these reasons the examiner must respectfully disagree with applicant’s assertion.
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to Bryan D. Ripa whose telephone number is (571)270-7875. The examiner can normally be reached Mon-Fri 8:00AM-4:00PM ET.
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/BRYAN D. RIPA/Primary Patent Examiner, Art Unit 1794