Magnetic polymer adsorption material, preparation method therefor and application thereof

Patent metadata

Field	Value
Publication number	US-11602729-B2
Application number	US-201816954210-A
Country	US
Kind code	B2
Filing date	Jan 11, 2018
Priority date	Dec 18, 2017
Publication date	Mar 14, 2023
Grant date	Mar 14, 2023

Abstract

A magnetic polymer adsorption material, preparation method and use thereof, which relate to the field of magnetic polymer materials. The preparation method comprises: (1) preparing magnetic nanoparticles; (2) dissolving the magnetic nanoparticles in a pore-forming agent, adding N-vinylpyrrolidone, divinylbenzene and an initiator respectively, and mixing uniformly; (3) adding an emulsifier and a dispersant into an aqueous solution; adding a part of the oil phase solution prepared in step (2) at the temperature below 60° C., and adding the rest of the oil phase solution when the temperature rises to 60° C. or above, reacting with stirring, precipitating and filtering the reacted solution, washing and drying the precipitate, and finally obtaining the magnetic polymer adsorption material. The material has the particle size of 2-100 μm, the magnetization of 5-19.5 emu/g and the specific surface area of 210-950 m2/g, and can be applied to the adsorption of inorganic and organic matters in solutions, the controlled release of inorganic and organic matters, and the separation of different substances.

First claim

What is claimed is:

1. A method for preparing a magnetic polymer adsorption material, comprising the following steps:
(1) preparing magnetic nanoparticles;
(2) formulating a first solution comprising the steps of: dissolving the magnetic nanoparticles prepared in step (1) in an agent, adding N-vinylpyrrolidone, divinylbenzene and an initiator respectively, and mixing uniformly under the condition of ice bath; and
(3) synthesizing the magnetic polymer adsorption material comprising the steps of: adding an emulsifier and/or a dispersant into an aqueous solution; adding a part of the first solution prepared in step (2) at the temperature below 60° C. into said aqueous solution, and adding the rest of the first solution when the temperature rises to 60° C. or above, wherein the volume of the first solution added each time accounts for 10-90% of the total volume of the total first solution, reacting with stirring, then precipitating and filtering the reacted solution, washing and drying the precipitate, and finally obtaining the magnetic polymer adsorption material.

2. The method for preparing a magnetic polymer adsorption material according to claim 1 , wherein the magnetic nanoparticles are Fe 3 O 4 organic acid nanoparticles, and the preparation process comprises: formulating soluble salts of Fe 2+ and Fe 3+ into a solution, mixing, introducing nitrogen for protection, adding a precipitating agent and an organic acid at 60-100° C., reacting for 0.5-12 h, adjusting the pH of the solution to be acidic, and washing and drying the product to obtain the magnetic Fe 3 O 4 organic acid nanoparticles.

3. The method for preparing a magnetic polymer adsorption material according to claim 1 , wherein in step (3), the stirring is performed at 100-1500 rpm for 12-80 h, and the reaction with stirring is performed at 60-95° C.

4. The method for preparing a magnetic polymer adsorption material according to claim 1 , wherein the mass of the N-vinylpyrrolidone accounts for 10-90% of the total mass of the N-vinylpyrrolidone and the divinylbenzene.

5. The method for preparing a magnetic polymer adsorption material according to claim 1 , wherein the volume of the agent is 0.05-2 times that of the aqueous solution; the mass of the emulsifier or dispersant accounts for 0.1-10% of the total mass of the N-vinylpyrrolidone and the divinylbenzene; and the mass of the initiator accounts for 0.1-5% of the total mass of the N-vinylpyrrolidone and the divinylbenzene.

6. The method for preparing a magnetic polymer adsorption material according to claim 2 , wherein the initiator is an azo or benzoyl compound; the agent is one or more of methanol, toluene, cyclohexanol, Dimethylformamide and Dimethyl sulfoxide; the emulsifier is an anionic surfactant; the dispersant is one or more of Polyvinylpyrrolidone, Hydroxyethylcellulose and Polyethylene glycol; the molar ratio of the soluble salt of Fe 2+ to the soluble salt of Fe 3+ is 1:(0.23-5.5); the mass of the organic acid is 0.5-5 times that of the magnetic Fe 3 O 4 nanoparticles; and the precipitating agent is an alkaline solution.

Assignees

• Nanjing University Of Technology
• Jiangsu Guochuang Enviro Protection Tech Co Ltd

Inventors

• Zhou Qing
• Yao Zhijian
• Li Aimin
• Jiao Wei
• Shuang Chendong
• Li Qimeng
• Sun Jie

Classifications

• B01J20/261 Primary

  obtained by reactions only involving carbon to carbon unsaturated bonds (macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds per se C08F) · CPC title

• C02F1/281

  using inorganic sorbents · CPC title

• C02F1/285

  using synthetic organic sorbents · CPC title

• B01J20/3064

  Addition of pore forming agents, e.g. pore inducing or porogenic agents · CPC title

• B01J20/28021

  Hollow particles, e.g. hollow spheres, microspheres or cenospheres · CPC title