# US 10,118,151 B2 · Composite with synergistic effect of adsorption and visible light catalytic degradation and preparation method and application thereof

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- Number: US 10,118,151 B2
- Document ID: US10118151B2
- Status: Granted
- Kind: B2
- Application number: 15/643,813
- Filed: 2017-07-07
- Published: 2018-01-11
- Granted: 2018-11-06
- Earliest claimed: 2016-07-08
- Assignees: Soochow University
- Applicants: Soochow University
- Inventors: Jun Jiang; Jianmei Lu; Najun Li; Dongyun Chen
- Web page: https://patentgrep.com/patent/US10118151B2

## CPC

- B01J 20/0259: {Compounds of N, P, As, Sb, Bi}
- B01J 20/264: {derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers}
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- B01J 23/18: Arsenic, antimony or bismuth
- B01J 35/39: Photocatalytic properties
- B01J 35/45: Nanoparticles
- B01J 37/0219: {the coating containing organic compounds}
- C02F 1/288: {using composite sorbents, e.g. coated, impregnated, multi-layered}
- C02F 1/30: by irradiation
- C02F 1/725: {by catalytic oxidation}
- C02F 2101/308: {Dyes; Colorants; Fluorescent agents}
- C02F 2305/10: Photocatalysts
- Y02W 10/37: using solar energy
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

The invention discloses a composite with an adsorption-visible light catalytic degradation synergistic effect and a preparation method and application thereof. The preparation method includes the specific steps that firstly, a bismuth oxyiodide/bismuth oxychloride composite nano-particle loaded activated carbon fiber composite ACF@BiOIxCl1-x is synthesized; then, the fiber surface is grafted with polyethyleneimine, and the end composite PEI-g-ACF@BiOIxCl1-x is obtained. The composite can rapidly adsorb pollutants in water, and meanwhile the pollutants are efficiently degraded with a photocatalyst loaded on the surface of the composite; besides, the purpose of recycling and reusing the photocatalyst is achieved, the comprehensive treatment capability of the composite is improved, the service life of the composite is prolonged, and the use cost is lowered.

## Claims

### Claim 1

A preparation method of a composite with synergistic effect of adsorption and visible light catalytic degradation, which comprises the steps as below:
1) preparation of activated carbon fibers with bismuth oxyiodide/bismuth oxychloride composite nanoparticles immobilized on:
dissolving bismuth nitrate pentahydrate and activated carbon fiber in solvent to obtain solution A; dissolving potassium iodide and potassium chloride in solvent to obtain solution B; adding solution B to solution A under stirring, mixing evenly, then moving the reaction mixture to a hydrothermal reactor and reacting for 10 to 16 hours at 120 to 180° C., after the completion of the reaction, the reaction vessel is taken out, cooled and opened, and the fibrous product is collected by filtration, washed and dried to obtain bismuth oxyiodide/bismuth oxychloride composite nanoparticles immobilized activated carbon fiber composite;
wherein,
the molar ratio of bismuth nitrate pentahydrate, potassium iodide and potassium chloride is 1:x:(1−x), and 0<x<1;
the ratio of bismuth nitrate pentahydrate and activated carbon fiber is 1 mol:25˜50 g;
2) the graft of polyethyleneimine:
dispersing the bismuth oxyiodide/bismuth oxychloride composite nanoparticles immobilized activated carbon fiber composite obtained in step 1) in solvent, adding silane coupling agent, reacting for 4 to 8 hours at 60 to 80° C. while stirring, then adding polyethyleneimine solution, continue stirring to react for 4 to 6 hours, after the reaction, the mixture is cooled and filtered to collect the fibrous product, washed and dried to obtain a composite material with synergistic effect of adsorption and visible light catalytic degradation;
wherein,
the ratio of said bismuth oxyiodide/bismuth oxychloride composite nanoparticles immobilized activated carbon fiber composite, silane coupling agent and polyethyleneimine solution is 50 mg:50 μL:1˜10 g.

### Claim 2 (depends on 1)

The preparation method according to claim 1, wherein:
in step 1), said solvent is either of water, ethyl alcohol, ethylene glycol, glycerol or any mixture thereof.

### Claim 3 (depends on 1)

The preparation method according to claim 1, wherein:
in step 2), said solvent is either of acetonitrile, N,N-Dimethylformamide, N,N-Dimethylethanolamine or any mixture thereof.

### Claim 4 (depends on 1)

The preparation method according to claim 1, wherein:
in step 2), said silane coupling agent is (3-bromopropyl) trimethoxysilane or (3-chloropropyl) trimethoxysilane.

### Claim 5 (depends on 1)

The preparation method according to claim 1, wherein:
in step 2), the mass concentration of said polyethyleneimine solution is 10%, wherein the Mw of polyethyleneimine is 600˜10000.

### Claim 6 (depends on 1)

A composite with synergistic effect of adsorption and visible light catalytic degradation, which is obtained according to the preparation method according to claim 1.

### Claim 7 (depends on 6)

An application of the composite with synergistic effect of adsorption and visible light catalytic degradation according to claim 6 for removing organic contaminant with negative charge in water.

### Claim 8 (depends on 7)

The application according to claim 7, wherein:
said organic contaminant with negative charge is anionic dye.
