# US 12,766,218 B2 · Hemostatic, antibacterial, and healing-promoting clay mineral-based biomaterial and preparation method thereof

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- Number: US 12,766,218 B2
- Document ID: US12766218B2
- Status: Granted
- Kind: B2
- Application number: 18/415,669
- Filed: 2024-01-18
- Published: 2024-09-19
- Granted: 2026-10-20
- Earliest claimed: 2023-03-13
- Assignees: China University of Geosciences (Wuhan)
- Applicants: China University of Geosciences (Wuhan)
- Inventors: Huaming Yang; Ying Chen; Weimin Xie; Yiting Yuan
- Web page: https://patentgrep.com/patent/US12766218B2

## CPC

- A61L 26/008: {Hydrogels or hydrocolloids}
- A61L 26/0004: {containing inorganic materials}
- A61L 26/0052: {Mixtures of macromolecular compounds}
- C08L 5/08: Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
- C08L 39/06: Homopolymers or copolymers of N-vinyl-pyrrolidones
- A61L 2300/102: Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L 2400/12: Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
- A61L 2430/34: for soft tissue reconstruction
- A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)

## Abstract

A method for preparing for preparing the hemostatic, antibacterial, and healing-promoting clay mineral-based hydrogel in the present disclosure includes: dissolving chitosan uniformly in a dilute acid, adding a preset amount of a crosslinking agent to obtain a first mixture, and stirring the first mixture to allow complete dissolution; and adding a kaolinite@Prussian blue (PB) composite to obtain a second mixture, thoroughly stirring the second mixture, and drying a resulting system at room temperature to obtain the hemostatic, antibacterial, and healing-promoting clay mineral-based hydrogel, where the kaolinite@PB composite includes nano-kaolinite and PB in-situ growing on the nano-kaolinite. The present disclosure combines the kaolinite@PB composite with the chitosan, which can not only effectively overcome the defect that simple chitosan exhibits unsatisfactory antibacterial and healing-promoting effects, but also overcome the problem that a simple kaolinite@PB composite powder can hardly be used in practical applications.

## Claims

### Claim 1

A method for preparing a hemostatic, antibacterial, and healing-promoting clay mineral-based hydrogel, comprising the following steps:
dissolving chitosan uniformly in a dilute acid to obtain a chitosan solution, adding a preset amount of a crosslinking agent to obtain a first mixture, and stirring the first mixture to allow complete dissolution; and
adding a kaolinite and Prussian blue (PB) composite to obtain a second mixture, thoroughly stirring the second mixture, and drying a resulting system at room temperature to obtain the hemostatic, antibacterial, and healing-promoting clay mineral-based hydrogel, wherein the kaolinite and PB composite comprises nano-kaolinite and PB in-situ growing on the nano-kaolinite;
wherein a method for preparing the kaolinite and PB composite comprises the following steps:
adding potassium ferricyanide and polyvinylpyrrolidone (PVP) to dilute hydrochloric acid, and subjecting a resulting mixture to stirring and an ultrasonic treatment at a room temperature to obtain a homogeneous solution; and
adding the nano-kaolinite to the homogeneous solution to obtain a mixed solution, subjecting the mixed solution to an ultrasonic treatment and thorough stirring, and allowing a resulting system to stand to obtain the blue kaolinite and PB composite.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the nano-kaolinite is obtained through intercalation and stripping of pharmaceutical-grade kaolinite.

### Claim 3 (depends on 1)

The method according to claim 1, wherein a concentration of the kaolinite and PB composite in the chitosan solution is 0.5 mg/mL to 2 mg/mL.

### Claim 4 (depends on 1)

The method according to claim 1, wherein a method for preparing the nano-kaolinite comprises:
subjecting kaolinite to intercalation with dimethyl sulfoxide (DMSO) and urea successively,
subjecting a resulting system to an ultrasonic treatment and centrifugation, and
washing a resulting precipitate to obtain the nano-kaolinite.

### Claim 5 (depends on 1)

The method according to claim 1, wherein a mass percentage of the PB in the kaolinite and PB composite is 10% to 50%.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the kaolinite and PB composite has a particle size of 200 nm to 500 nm.

### Claim 7 (depends on 1)

The method according to claim 1, wherein a mass percentage of the chitosan in the chitosan solution is 1% to 5%; a volume percentage of the dilute acid is 0.5% to 2%, and the dilute acid is one selected from a group consisting of an acetic acid and a hydrochloric acid; a mass of the crosslinking agent is 10% to 20% of a mass of the chitosan solution; the crosslinking agent is one or a combination of two or more selected from the group consisting of gelatin, glycerin, pectin, and polyvinyl alcohol (PVA); and a viscosity of the chitosan solution is at least 400 Mpa·s.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the resulting system is allowed to stand for 15 h to 24 h in an oil/water bath at 60° C. to 90° C.; a mass ratio of the nano-kaolinite to the potassium ferricyanide is 1:3 to 4:3; and a mass ratio of the nano-kaolinite to the PVP is 1:60 to 4:60.

### Claim 9 (depends on 1)

A hemostatic, antibacterial, and healing-promoting clay mineral-based hydrogel prepared by the method according to claim 1.