# US 9,434,621 B2 · Mesoporous composite titanium oxide and a preparation method

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- Number: US 9,434,621 B2
- Document ID: US9434621B2
- Status: Granted
- Kind: B2
- Application number: 13/393,014
- Filed: 2009-08-28
- Published: 2012-07-19
- Granted: 2016-09-06
- Earliest claimed: 2009-08-28
- Assignees: Nanjing University of Technology; Nanjing Taiwei Technology Co., Ltd.
- Applicants: Zhuhong Yang; Yudan Zhu; Xiaohua Lu; Changsong Wang; Licheng Li; Linghong Lv; Wei Zhuang; Chang Liu; Xin Feng
- Inventors: Zhuhong Yang; Yudan Zhu; Xiaohua Lu; Changsong Wang; Licheng Li; Linghong Lv; Wei Zhuang; Chang Liu; Xin Feng
- Web page: https://patentgrep.com/patent/US9434621B2

## CPC

- C01G 23/047: Titanium dioxide
- B01J 21/063: {Titanium; Oxides or hydroxides thereof}
- B01J 29/0308: {Mesoporous materials not having base exchange properties, e.g. Si-MCM-41}
- B01J 35/613: {10-100 m2/g}
- B01J 35/615: {100-500 m2/g}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/647: {2-50 nm}
- C04B 38/009: {Porous or hollow ceramic granular materials, e.g. microballoons (C04B18/027, C04B20/002 take precedence)}
- H01M 4/131: Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/364: {as mixtures}
- H01M 4/366: {as layered products}
- H01M 4/485: of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy (H01M4/505, H01M4/525 take precedence)
- H01M 10/052: Li-accumulators
- C01P 2006/12: Surface area
- C01P 2006/14: Pore volume
- C01P 2006/16: Pore diameter
- H01M 2004/021: {Physical characteristics, e.g. porosity, surface area}
- Y02E 60/10: Energy storage using batteries
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- 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)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A mesoporous composite titanium oxide, which is composed of a mesoporous titanium oxide, the outside surface and the wall of pores of the mesoporous titanium oxide are modified by inorganic matters; inorganic matter contains at least one element selected from carbon, silicon, sulphur, phosphorus and selenium in an amount of 0.01%-25%, on amount of the element mass, of the mass of said mesoporous composite titanium oxide material; at least one mean pore size of pore distribution of the mesoporous compound titanium oxide material is 3-15 nm, the specific surface area is 50-250 m2/g, and the pore volume is 0.05-0.4 cm3/g. As a catalyst carrier, the rate of conversion of the hydrodesulfurization reaction of the material reaches as high as 98 percent, and as a lithium ion battery cathode material, the specific capacity of the lithium ion battery cathode material reaches as high as 220 mAh/g.

## Claims

### Claim 1

A mesoporous composite titanium oxide material for a catalyst carrier or a lithium ion battery cathode comprising:
a mesoporous titanium oxide, which has a specific surface area of 90-250 m2/g and a pore volume 0.05-0.4 cm3/g;
wherein an outside surface of the mesoporous titanium oxide and wall surfaces of pores of the mesoporous titanium oxide are modified by a process to form a mesoporous titanium oxide having a composite layer on its outside surface and pores with composite layer on their wall surfaces;
the process is as follows:
dissolving a precursor containing at least one element of Si, C, S, P and Se in water or organic solvent to form solution,
adding mesoporous titanium oxide into the solution and stirring for 1-72 hours then filtering and washing with water or organic solvent, and
carrying out sintering in an atmosphere at 300-900° C.;
mass of the at least one element of Si, C, S, P and Se is in an amount of 0.01%-25% of a mass of said mesoporous composite titanium oxide material;
at least one mean pore size of pore distribution of the mesoporous composite titanium oxide material is 3-15 nm, a specific surface area is 90-250 m2/g, and a pore volume is 0.05-0.4 cm3/g;
morphology of the mesoporous composite titanium oxide material presents crystal whiskers, fiber or particles with the diameter of 0.1-10μm.

### Claim 2 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein the mesoporous titanium oxide in the mesoporous composite titanium oxide material is one or more selected from anatase phase titanium oxide, TiO2(B) phase titanium oxide and rutile phase titanium oxide.

### Claim 3 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein a mean pore size of the added mesoporous titanium oxide is 3-15 nm, a pore volume is 0.05-04 cm3/g, a specific surface area is 90-250 m2/g, and crystal form of the mesoporous titanium oxide is at least one of anatase phase titanium oxide, TiO2 (B) phase titanium oxide and rutile phase titanium oxide.

### Claim 4 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein the precursor is acid, alkali, soluble inorganic salt or organic matter containing at least one element selected from C, Si, S, P and Se.

### Claim 5 (depends on 4)

The mesoporous composite titanium oxide material according to claim 4, wherein the precursor is C4-C20 carbohydrate, C4-C20 alcohol, C4-C20 mercaptan, C4-C20 silane, and C4-C20 organic phosphonic acid or selenate.

### Claim 6 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein the atmosphere used in the sintering process is one gas or at least two gases with different proportions selected from N2, O2, Ar, H2O, He, H2, CO and CO2.

### Claim 7 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein a concentration of the precursor in water or organic solvent is 0.001-10 mol/L, and a molar ratio of the precursor to the mesoporous titanium oxide is 0.001-1.

### Claim 8 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein the organic solvent used for washing is non-polar or weak-polar solvent or strong-polar solvent.

### Claim 9 (depends on 1)

The mesoporous composite titanium oxide material according to claim 1, wherein the organic solvent used for dissolution is non-polar or weak-polar solvent or strong-polar solvent.