Mesoporous materials and processes for preparation thereof

Patent metadata

Field	Value
Publication number	US-2016151767-A1
Application number	US-201414891218-A
Country	US
Kind code	A1
Filing date	May 8, 2014
Priority date	May 13, 2013
Publication date	Jun 2, 2016
Grant date	—

Abstract

A process for preparing a mesoporous material, e.g., transition metal oxide, sulfide, selenide or telluride, Lanthanide metal oxide, sulfide, selenide or telluride, a post-transition metal oxide, sulfide, selenide or telluride and metalloid oxide, sulfide, selenide or telluride. The process comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic or lyotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to form the mesoporous material. A mesoporous material prepared by the above process. A method of controlling nano-sized wall crystallinity and mesoporosity in mesoporous materials. The method comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic or lyotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to control nano-sized wall crystallinity and mesoporosity in the mesoporous material. Mesoporous materials and a method of tuning structural properties of mesoporous materials.

First claim

1 - 383 . (canceled)

384 . A process for preparing a mesoporous material, said process comprising:
preparing an acidic mixture by mixing one or more metal precursors, an interface modifier, a hydrotropic or lyotropic ion precursor, and a surfactant; aging the acidic mixture at a temperature and for a period of time sufficient to form a powder, film or gel; and heating the powder, film or gel at a temperature and for a period of time sufficient to form the mesoporous material.

385 . The process of claim 384 wherein the mesoporous material comprises an oxide, a sulfide, a selenide or a telluride of the following:
a transition metal selected from the group consisting of Cr, Zr, Nb, Hf and Ta; a Lanthanide selected from the group consisting of Nd, Sm, Ce and Gd; a post-transition metal comprising Sn; or a mixed metal or a solid acid selected from the group consisting of P—Zr, W—Zr, S—Ti, Sn—Zr and S—Zr.

386 . The process of claim 384 wherein the mesoporous material comprises: a transition metal oxide selected from the group consisting of Cr 2 O 3 , ZrO 2 , Nb 2 O 5 , HfO 2 and Ta 2 O 5 ; a post-transition metal oxide comprising SnO 2 ; and a Lanthanide oxide selected from the group consisting of CeO 2 , Nd 2 O 3 , Sm 2 O 3 and Gd 2 O 3 .

387 . The process of claim 384 wherein the mesoporous material is selected from the group consisting of a transition metal oxide, sulfide, selenide or telluride; a Lanthanide metal oxide, sulfide, selenide or telluride; a post-transition metal oxide, sulfide, selenide or telluride; a metalloid oxide, sulfide, selenide or telluride; and mixtures thereof.

388 . The process of claim 387 wherein the transition metal oxide, sulfide, selenide or telluride comprises a Group 3-12 transition metal oxide, sulfide, selenide or telluride.

389 . The process of claim 388 wherein the Group 3-12 transition metal oxide, sulfide, selenide or telluride is selected from the group consisting of a Sc, Y, La, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd and Hg oxide, sulfide, selenide or telluride.

390 . The process of claim 387 wherein the transition metal oxide is selected from a Group 6-12 transition metal oxide, sulfide, selenide or telluride.

391 . The process of claim 390 wherein the Group 6-12 transition metal oxide, sulfide, selenide or telluride is selected from the group consisting of a Cr, Mo, W, Mn, Tc, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd and Hg oxide, sulfide, selenide or telluride.

392 . The process of claim 387 wherein the Lanthanide metal oxide, sulfide, selenide or telluride is selected from the group consisting of a La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu oxide, sulfide, selenide or telluride.

393 . The process of claim 387 wherein the post-transition metal oxide, sulfide, selenide or telluride is selected from the group consisting of an Al, Ga, In, TI, Sn, Pb and Bi oxide, sulfide, selenide or telluride.

394 . The process of claim 387 wherein the metalloid oxide, sulfide, selenide or telluride is selected from the group consisting of a B, Si, Ge, As, Sb, Te, Po and At oxide, sulfide, selenide or telluride.

395 . The process of claim 384 wherein the one or more metal precursors are selected from the group consisting of a metal halide, a metal phosphate, a metal acetate, a metal nitrate, a metal alkoxide, and a M x O y oxide that is capable of dissolving in HNO 3 ; the interface modifier comprises an aliphatic, alicyclic or aromatic hydrocarbon of between about 1 and about 20 carbon atoms, or mixtures thereof; the hydrotropic ion precursor comprises HNO 3 , NaNO 3 , KNO 3 , metal iodides, metal thiocyanides, or mixtures thereof; and the surfactant comprises an anionic, cationic, non-ionic, or zwitterionic surfactant, or mixtures thereof.

396 . The process of claim 384 wherein the powder, film or gel is heated at a temperature from about 150° C. to about 700° C. for a period from about 1 to about 12 hours.

397 . The process of claim 384 wherein the powder, film or gel is heated sequentially as follows: at a temperature from about 75° C. to about 150° C. for a period from about 1 to about 12 hours; and at a temperature from about 40° C. to about 80° C. for a period from about 1 to about 12 hours.

398 . The process of claim 384 wherein the powder, film or gel is heated sequentially as follows: at a temperature from about 100° C. to about 200° C. for a period from about 2 to about 20 hours; at a temperature from about 200° C. to about 300° C. for a period from about 1 to about 10 hours; at a temperature from about 300° C. to about 400° C. for a period from about 1 to about 8 hours; at a temperature from about 400° C. to about 500° C. for a period from about 0.5 to about 4 hours; and at a temperature from about 500° C. to about 600° C. for a period from about 0.1 to about 2 hours.

399 . The process of claim 384 wherein the powder, film or gel is heated sequentially as follows: at a temperature of about 150° C. for a period of about 12 hours; at a temperature of about 250° C. for a period of about 4 hours; at a temperature of about 350° C. for a period of about 3 hours; at a temperature of about 450° C. for a period of about 2 hours; and at a temperature of about 550° C. for a period of about 1 hour.

400 . A mesoporous material produced by the process of claim 384 .

401 . A mesoporous material particulate having nano-sized wall crystallinity, a particle size between about 1 and about 500 nm, a BET surface area between about 50 and about 1000 m 2 /g, a pore volume (BJH) between about 0.05 and about 2 cm 3 /g, a monomodal pore size (BJH desorption) distribution between about 1 and 25 nm, and optionally a wall thickness (2d/√3−PD, where d is the d-spacing and PD is the pore diameter) between about 2 and about 20 nm; wherein the mesoporous material particulate exhibits thermal stability up to a temperature of about 800° C.

402 . The mesoporous material particulate of claim 401 which is selected from the group consisting of a transition metal oxide, sulfide, selenide or telluride particulate, a Lanthanide metal oxide, sulfide, selenide or telluride particulate, a post-transition metal oxide particulate, a metalloid oxide, sulfide, selenide or telluride particulate, and mixtures thereof.

403 . The mesoporous material particulate of claim 402 wherein the transition metal oxide, sulfide, selenide or telluride particulate comprises a Group 3-12 transition metal oxide, sulfide, selenide or telluride particulate.

404 . The mesoporous material particulate of claim 403 wherein the Group 3-12 transition metal oxide, sulfide, selenide or telluride particulate is selected from the group consisting of a Sc, Y, La, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd and Hg oxide, sulfide, selenide or telluride particulate.

405 . The mesoporous material particulate of claim 402 wherein the transition metal oxide, sulfide, selenide or telluride particulate is selected from a Group 6-12 transition metal oxide, sulfide, selenide or telluride particulate.

406 . The mesoporous material particulate of claim 405 wherein the Group 6-12 transition metal oxide, sulfide, selenide or telluride particulate is selected from the group consisting of a Cr, Mo, W, Mn, Tc, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd and Hg oxide, sulfide, selenide or tellur

Assignees

• Univ Connecticut

Inventors

• Suib Steven L
• Poyraz Altug Suleyman
• Jin Lei
• Kuo Chung-Hao

Classifications

• C01P2006/12

  Surface area · CPC title

• C01P2006/37

  Stability against thermal decomposition · CPC title

• C01G1/02

  Oxides · CPC title

• B01J21/18

  Carbon · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title