IP Library Granted Patent US 12,697,606
Granted Patent B2
US 12,697,606 · App. 18/097,439 · Granted Aug 4, 2026

Method of preparing electrocatalysts for converting carbon dioxide to chemicals

Inventors: Di-Jia Liu (Elmhurst, IL); Tao Xu (Naperville, IL); Jianxin Wang (Chicago, IL)
Assignees: UCHICAGO ARGONNE, LLC; BOARD OF TRUSTEES OF NORTHERN ILLINOIS UNIVERSITY
B01J23/78B01J23/14B01J23/72B01J35/618B01J37/0081B01J37/0228B01J37/04C07C29/154
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Quick Facts
Patent No.
US 12,697,606
App. No.
18/097,439
Filed
Jan 16, 2023
Granted
Aug 4, 2026
Kind
B2
Art Unit
1732
USPC
502/352
Abstract

Electrocatalysts composed of single atoms or metal clusters dispersed over porous carbon support were prepared by a lithium-melt method. The new catalysts demonstrated high selectivity, high Faradic efficiency and low overpotential toward to the electrocatalytic reduction of carbon dioxide to chemicals such as glycerol or isopropanol.

Claims (32)

1 . A method of synthesizing a catalyst comprising:

adding a catalytic metal selected from the group consisting of Sn and Cu in its metallic form to molten lithium metal, wherein a ratio of Cu to Li ranges from 0.5% to 2% or the relative ratio of Sn to Li ranges from 4% to 40%;

atomically dispersing the catalytic metal in the molten lithium metal;

forming a lithium catalytic metal-solid;

converting a portion of lithium in the lithium catalytic metal solid to lithium hydroxide forming a catalytic metal-lithium hydroxide solid;

mixing said catalytic metal-lithium hydroxide solid with a conductive support material to form a mixture, the conductive support material being carbonaceous with a porous network and having catalytic metal decorated throughout the porous network with a specific surface area of 1200 to 2000 m 2 /g;

removing lithium hydroxide from the mixture leaving a mixture of catalytic metal and the conductive support material; and

drying the mixture of catalytic metal and the conductive support material to produce the catalyst containing the catalytic metal atomically dispersed over the conductive support material.

2 . The method of claim 1 , wherein converting the portion of the lithium-catalytic metal solid to catalytic metal-lithium hydroxide solid comprises reacting lithium in the lithium catalytic metal solid with moist air.

3 . The method of claim 2 , further comprising mixing the catalytic metal-lithium hydroxide solid with the conductive support material using a mechanical method.

4 . The method of claim 1 , wherein the molten lithium metal has a temperature of 300° C. or less.

5 . The method of claim 1 , wherein removing the lithium hydroxide comprises a drop-wise washing of the catalytic metal-lithium metal hydroxide solid with water thereby removing lithium.

6 . The method of claim 5 , wherein the washing comprises forming an alkaline water solution and modifying the carbonaceous support with oxygenated species serving as anchoring sites for the catalytic metal.

7 . The method of claim 1 , wherein the catalytic metal comprises Cu.

8 . The method of claim 1 , wherein a loading range for the catalytic metal on the conductive support material is 0.2 wt % to 20 wt %.

9 . The method of claim 8 , wherein the loading range is 0.2 wt % to 1 wt %.

10 . The method of claim 8 , wherein the loading range is 0.4 wt % to 2 wt %.

11 . The method of claim 1 , wherein the catalytic metal comprises Sn.

12 . The method of claim 11 , wherein a loading range for the catalytic metal on the conductive support material is 0.5 wt % to 20 wt %.

13 . The method of claim 11 , wherein the loading range is 0.5 wt % to 2 wt %.

14 . The method of claim 11 , wherein the loading range is 10 wt % to 20 wt %.

15 . The method of claim 11 wherein the loading range is 10 wt % to 40 wt %.

16 . A process for forming glycerol comprising:

providing a catalyst having catalytic metal, comprising Sn or Cu, atomically dispersed as 0.2 wt % to 20 wt % over a carbonaceous conductive support material having a surface area of 1200-2000 m 2 /g;

exposing carbon dioxide to the catalyst; and

forming glycerol.

17 . The process of claim 16 , wherein the glycerol is formed at a Faradaic efficiency of at least 90%.

18 . A process for forming isopropanol comprising:

providing a catalyst having catalytic metal, comprising Sn atomically dispersed over a carbonaceous conductive support material having a surface area of 1200-2000 m 2 /g;

exposing carbon dioxide to the catalyst; and

forming isopropanol.

19 . The process of claim 18 , wherein the isopropanol is formed at a Faradaic efficiency of at least 80%.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 15, 2026
From: WANG, JIANXIN
To: UCHICAGO ARGONNE, LLC
Reel/Frame 074962/0107 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 14, 2026
From: LIU, DI-JIA
To: UCHICAGO ARGONNE, LLC
Reel/Frame 073473/0345 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 14, 2026
From: XU, TAO
To: BOARD OF TRUSTEES OF NORTHERN ILLINOIS UNIVERSITY
Reel/Frame 073473/0629 →
CONFIRMATORY LICENSE Recorded Feb 15, 2024
From: UCHICAGO ARGONNE LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 066601/0371 →
Continuity (2)
Continuation In Part 17008853 · Sep 1, 2020
Related Publication 20230278014A1 · Sep 7, 2023
References Cited (27)
US 3625768A · Moulton et al. · 1971 [cited by applicant]
US 4201760A · Arendt et al. · 1980 [cited by applicant]
US 5071815A · Wallace et al. · 1991 [cited by applicant]
US 10844501B2 · Liu et al. · 2020 [cited by applicant]
US 10978718B2 · Liu et al. · 2021 [cited by applicant]
US 20140291161A1 · Awazu et al. · 2014 [cited by applicant]
US 20150311522A1 · Fang et al. · 2015 [cited by applicant]
US 20190067706A1 · Liu et al. · 2019 [cited by applicant]
US 20190276943A1 · Liu et al. · 2019 [cited by applicant]
US 20210202955A1 · Liu et al. · 2021 [cited by applicant]
US 20220062864A1 · Liu · 2022 [cited by examiner]
CN 117418269A · 2024 [cited by examiner]
WO WO2013166505A2 · 2013 [cited by applicant]
Abbasi, et al., “Tailoring the Edge Structure of Molybdenum Disulfide toward Electrocatalytic Reduction of Carbon Dioxide,” ACS Nano 11(1), pp. 453-460 (2017). [cited by applicant]
Ahmed & Mao, “Ultrafine Iridium Oxide Nanorods Synthesized by Molten Salt Method toward Electrocatalytic Oxygen and Hydrogen Evolution Reactions,” Electrochimica Acta 212, pp. 686-693 (2016). [cited by applicant]
Barkholtz, et al., “Lithium Assisted ‘Dissolution-Alloying’ Synthesis of Nanoalloys from Individual Bulk Metals,” Chemistry of Materials 28(7), pp. 2267-2277 (2016). [cited by applicant]
Calvinho, et al., “Selective CO2 reduction to C3 and C4 oxyhydrocarbons on nickel phosphides at overpotentials as low as 10 mV,” Energy & Environmental Science 11, pp. 2550-2559 (2018). [cited by applicant]
Duan, et al., “Amorphizing of Cu Nanoparticles toward Highly Efficient and Robust Electrocatalyst for CO2 Reduction to Liquid Fuels with High Faradaic Efficiencies,” Advanced Materials 30(14), 1706194, 7 pages (2018). [cited by applicant]
Kim, et al., “Copper nanoparticle ensembles for selective electroreduction of CO2 to C2—C3 products,” Proceedings of the National Academy of Sciences 114(40), pp. 10560-10565 (2017). [cited by applicant]
Lin, et al., “Direct Synthesis of Bimetallic Pd3Ag Nanoalloys from Bulk Pd3Ag Alloy,” Inorganic Chemistry 51(24), pp. 13281-13288 (2012). [cited by applicant]
Mugavero, et al., “Materials discovery by crystal growth: Lanthanide metal containing oxides of the platinum group metals (Ru, Os, Ir, Rh, Pd, Pt) from molten alkali metal hydroxides,” Journal of Solid State Chemistry 1… [cited by applicant]
Ramierez-Valencia, et al., “From CO2 to Value-Added Products: A Review about Carbon-Based Materials for Electro-Chemical CO2 Conversion,” Catalysts 11(3):351, 67 pages (2021). [cited by applicant]
Wang, et al., “CO2 reduction to acetate in mixtures of ultrasmall (Cu)n,(Ag)m bimetallic nanoparticles,” Proceedings of the National Academy of Sciences 115(2), pp. 278-283 (2018). [cited by applicant]
Xu, et al., “Highly selective electrocatalytic CO2 reduction to ethanol by metallic clusters dynamically formed from atomically dispersed copper,” Nature Energy 5, pp. 623-632 (2020). [cited by applicant]
Xu, et al., “Supplemental Information—Synthesis of Supported Platinum Nanoparticles from Li—Pt Solid Solution,” Journal of the American Chemical Society 132(7), 8 pages (2010). [cited by applicant]
Xu, et al., “Synthesis of Supported Platinum Nanoparticles from Li—Pt Solid Solution,” Journal of the American Chemical Society 132(7), pp. 2151-2153 (2010). [cited by applicant]
Yang, et al., “Atomically dispersed Ni(I) as the active site for electrochemical CO2 reduction,” Nature Energy 3, pp. 140-147 (2018). [cited by applicant]