# US 11,111,255 B1 · Zirconium-based metal-organic framework material UiO-66(Zr), rapid room-temperature preparation method and application thereof > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,111,255 B1 - Document ID: US11111255B1 - Status: Granted - Kind: B1 - Application number: 16/934,066 - Filed: 2020-07-21 - Published: 2021-09-09 - Granted: 2021-09-07 - Earliest claimed: 2020-03-06 - Assignees: Tongji University - Applicants: Tongji University - Inventors: Fengting Li; Yinan Wu - Web page: https://patentgrep.com/patent/US11111255B1 ## CPC - C07F 7/003: {without C-Metal linkages} - B01J 20/226: {Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF] (preparation of metal complexes containing carboxylic acid moieties C07C51/418; MOF's per se C07F)} - C02F 1/285: {using synthetic organic sorbents} - C02F 2101/14: Fluorine or fluorine-containing compounds - C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes) ## Abstract A zirconium-based metal-organic framework material UiO-66(Zr) and a rapid room-temperature preparation method and application thereof are provided. The preparation method includes: (1) mixing a zirconium source and an organic ligand uniformly, then placing in methanol and stirring at room temperature, centrifuging and then discarding a supernatant to obtain a transparent gel-like intermediate product; and (2) heating and drying the intermediate product to obtain UiO-66(Zr). Compared with the prior art, the present invention excludes the use of N,N-dimethylformamide and other toxic organic solvents that are necessary in the traditional solvothermal method, and only needs to stir in methanol at room temperature and dry to obtain UiO-66(Zr). The method has mild conditions and a high yield. Moreover, the product purity is extremely high, and the product activation step can be omitted. The product has good adsorption to fluoride ion in water, and can be applied to the adsorption treatment of fluorine-containing wastewater. ## Claims ### Claim 1 A rapid room-temperature preparation method of a zirconium-based metal-organic framework material UiO-66(Zr), comprising the following steps: (1) mixing a zirconium source and an organic ligand uniformly to obtain a mixture, then placing the mixture in methanol to obtain a mixed solution and stirring the mixed solution at room temperature, centrifuging the mixed solution to obtain a centrifuged product and then discarding a supernatant of the centrifuged product to obtain a transparent gel-like intermediate product; and (2) heating and drying the transparent gel-like intermediate product obtained in step (1) to obtain the zirconium-based metal-organic framework material UiO-66(Zr); wherein the zirconium source is zirconium oxychloride octahydrate. ### Claim 2 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein the organic ligand is one selected from the group consisting of terephthalic acid, 2-bromoterephthalic acid and aminoterephthalic acid. ### Claim 3 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein a molar ratio of the zirconium source to the organic ligand is (1-2):(2-1). ### Claim 4 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein in step (1), a mass ratio of a mixture of the zirconium source and the organic ligand to the methanol is 1:(10-100). ### Claim 5 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein in step (1), a time for the stirring is 0.5-2 h. ### Claim 6 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein in step (2), a temperature for the heating and drying is 40-120° C. ### Claim 7 (depends on 1) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 1, wherein in step (2), a time for the heating and drying is 0.5-4 h. ### Claim 8 (depends on 1) A zirconium-based metal-organic framework material UiO-66(Zr), wherein the zirconium-based metal-organic framework material UiO-66(Zr) is obtained by using the rapid room-temperature preparation method according claim 1. ### Claim 9 (depends on 8) A method of using the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, comprising applying the zirconium-based metal-organic framework material UiO-66(Zr) in water containing fluoride ion pollutants. ### Claim 10 (depends on 2) The rapid room-temperature preparation method of the zirconium-based metal-organic framework material UiO-66(Zr) according to claim 2, wherein a molar ratio of the zirconium source to the organic ligand is (1-2):(2-1). ### Claim 11 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein the organic ligand is one selected from the group consisting of terephthalic acid, 2-bromoterephthalic acid and aminoterephthalic acid. ### Claim 12 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein a molar ratio of the zirconium source to the organic ligand is (1-2):(2-1). ### Claim 13 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein in step (1), a mass ratio of a mixture of the zirconium source and the organic ligand to the methanol is 1:(10-100). ### Claim 14 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein in step (1), a time for the stirring is 0.5-2 h. ### Claim 15 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein in step (2), a temperature for the heating and drying is 40-120° C. ### Claim 16 (depends on 8) The zirconium-based metal-organic framework material UiO-66(Zr) according to claim 8, wherein in step (2), a time for the heating and drying is 0.5-4 h.