# US 11,299,400 B2 · Hierarchical porous ZrO2 material, method of preparing the same, and application thereof

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- Number: US 11,299,400 B2
- Document ID: US11299400B2
- Status: Granted
- Kind: B2
- Application number: 16/826,032
- Filed: 2020-03-20
- Published: 2020-10-15
- Granted: 2022-04-12
- Earliest claimed: 2019-04-15
- Assignees: Shaanxi University of Science and Technology
- Applicants: Taotao Qiang; Lei Tian; Runtong Zhu; Lu Chen
- Inventors: Taotao Qiang; Lei Tian; Runtong Zhu; Lu Chen
- Web page: https://patentgrep.com/patent/US11299400B2

## CPC

- C01G 25/02: Oxides
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/03: obtained by SEM
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/12: Surface area
- C01P 2006/16: Pore diameter
- C01P 2006/17: Pore diameter distribution
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method for preparing a hierarchical porous ZrO2 includes the following steps: S1, dissolving a triblock copolymer in an organic solvent to obtain a solution A, dissolving a tannin extract in distilled water to obtain a solution B, mixing the solution A and the solution B and stirring to obtain a mixed solution; S2, adding a zirconium salt to the mixed solution obtained in step S1 and stirring; S3, heating the mixed solution obtained in step S2 in an oven to obtain ZrO2, promoting the conversion of the crystal form of ZrO2; S4, calcining ZrO2 at a high temperature to obtain the hierarchical porous ZrO2.

## Claims

### Claim 1

A method for preparing a hierarchical porous ZrO2 comprising the following steps:
S1, dissolving a triblock copolymer in an organic solvent to obtain a solution A, dissolving a tannin extract in distilled water to obtain a solution B, mixing the solution A and the solution B and stirring to obtain a mixed solution;
S2, adding a zirconium salt to the mixed solution obtained in step S1 and stirring;
S3, heating the mixed solution obtained in step S2 in an oven to obtain ZrO2, promoting the conversion of the crystal form of ZrO2; and
S4, calcining ZrO2 at a high temperature to obtain the hierarchical porous ZrO2.

### Claim 2 (depends on 1)

The method of claim 1, wherein the triblock copolymer is Pluronic P123, Pluronic F127 or Pluronic F108.

### Claim 3 (depends on 1)

The method of claim 1, wherein the tannin extract is a sulfonated Acacia mangim tannin extract.

### Claim 4 (depends on 1)

The method of claim 1, wherein the zirconium salt is zirconium chloride, zirconium sulfate, zirconium nitrate, zirconium phosphate, or zirconium oxalate.

### Claim 5 (depends on 1)

The method of claim 1, wherein the organic solvent is methanol, ethanol, ethylene glycol, or glycerin.

### Claim 6 (depends on 1)

The method of claim 1, wherein a molar ratio of the triblock copolymer:the tannin extract:the zirconium salt is 0.015-0.05:0.01-0.05:0.1-1.0.

### Claim 7 (depends on 1)

The method of claim 1, wherein in step S2, the mixed solution is stirred for 3-6 hours; in step 3, the mixed solution is heated at 40° C. for 24-96 hours; and in step S4, ZrO2 is calcined at 200-250° C. for 60-120 minutes and then at 550-700° C. for 240-360 minutes.