# US 10,369,544 B1 · Method of synthesizing novel adsorbent titanosilicate material (UPRM-5) using NR4+ type cations

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- Number: US 10,369,544 B1
- Document ID: US10369544B1
- Status: Granted
- Kind: B1
- Application number: 13/893,284
- Filed: 2013-05-13
- Granted: 2019-08-06
- Earliest claimed: 2011-03-24
- Assignees: University of Puerto Rico
- Applicants: Arturo J. Hernandez-Maldonado; Marietta E. Marcano-Gonzalez; Jose N. Primera-Pedrozo
- Inventors: Arturo J. Hernandez-Maldonado; Marietta E. Marcano-Gonzalez; Jose N. Primera-Pedrozo
- Web page: https://patentgrep.com/patent/US10369544B1

## CPC

- B01J 20/3057: {Use of a templating or imprinting material (molecularly imprinted polymers B01J20/268); filling pores of a substrate or matrix followed by the removal of the substrate or matrix}
- B01J 20/10: comprising silica or silicate
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- C01B 39/02: Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B 39/04: using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
- C01B 39/085: {Group IVB- metallosilicates}
- B01D 53/02: by adsorption, e.g. preparative gas chromatography {(solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01)}
- B01D 2257/504: Carbon dioxide
- Y02C 20/40: of CO2
- Y02P 20/151: Reduction of greenhouse gas [GHG] emissions, e.g. CO2
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

The invention employs tetrapropylammonium (TPA+) and tetrabutylammonium (TBA+) as structure directing agents (SDAs), respectively for the preparation of the flexible titanium silicate UPRM-5. Both UPRM-5 variants are detemplated and modified to include extraframework Sr2+ and produce materials for carbon dioxide adsorption.

## Claims

### Claim 1

A method of synthesizing a titanosilicate material comprising:
adding a structure directing agent selected from the group consisting of: tetrapropylammonium (TPA+) and tetrabutylammonium (TBA+), that allows the formation of a porous adsorbent material, to a gel solution containing titanium (III) chloride solution in HCl and stirring for 30 minutes to prepare a gel mixture and crystallizing said gel mixture to form a titanosilicate porous material having structural faults introduced by said structure directing agent;
removing said structure directing agent from said titanosilicate porous material via ion exchange with NH4+ to form a detemplated material; and
functionalizing said detemplated material with strontium cation via ion exchange to form a titanosilicate porous material having a micropore area that varies as a function of thermal activation temperature due to said structural faults introduced by the structure directing agent, wherein the titanosilicate material having an unit cell selected from the group consisting of |Sr2+3.0Na+3.3OH−2.31|[Si11.4Ti8.3O37]:23H2O and |Sr2+2.4Na+3.9OH−1.5|[Si9.3Ti7.1O37]:20H2O.

### Claim 2 (depends on 1)

The method of claim 1, wherein said gel mixture comprises a composition having a formula of 3.4(TBA)2O: 7.3Na2O:1.2 K2O: 1.3TiO2: 10SiO2: 201.5H2O.

### Claim 3 (depends on 1)

The method of claim 1, wherein said gel mixture comprises a composition having a formula of 3.4(TPA)2O: 7.3Na2O:1.2 K2O: 1.3TiO2: 10SiO2: 201.5H2O.

### Claim 4 (depends on 1)

The method of claim 1, wherein said functionalized detemplated material exhibits selectivity for CO2.