Magnetic microsphere resin with high specific surface area and preparation method and application thereof

A high specific surface area, magnetic microsphere technology, applied in the direction of microsphere preparation, magnetic materials, magnetic objects, etc., can solve the problems of inability to effectively prepare magnetic polymer materials, obtain magnetic materials, and contaminate membranes, etc., to achieve convenience Separation method, high adsorption capacity, effect of enhancing lipophilicity

Active Publication Date: 2012-06-27
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Membrane emulsification-suspension polymerization is a relatively easy technology to develop microspheres, but so far, magnetic polymer materials cannot be effectively prepared using this method (Q.C. Yuan, R.A. Williams, China Particuology 5 (2007) 26)
The reason is that it is difficult for magnetic nanoparticles to pass through the membrane with complex pores during the membrane emulsification process, which not only fails to obtain magnetic materials, but also contaminates the membrane.

Method used

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  • Magnetic microsphere resin with high specific surface area and preparation method and application thereof
  • Magnetic microsphere resin with high specific surface area and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Using 20g FeCl 2 4H 2 O and 100g FeCl 3 ·6H 2 O prepared magnetic nanoparticles, modified with 20g oleic acid. The oil phase consists of 50g of high-purity divinylbenzene (99.99%), 10g of n-heptane, 15g of toluene, and 1.6g of benzoyl peroxide. Dissolve 10g of gelatin in 500ml of water to form the water phase. The oil phase and the magnetic nanoparticles are ultrasonically mixed, and the SPG membrane with a pore size of 2 μm is selected to pass through the membrane under a nitrogen pressure of 0.045 MPa to form a uniform emulsion. Transfer the emulsion into a three-necked bottle, stir slowly, raise the temperature to 75°C to initiate the reaction, polymerize for 8 hours, then gradually raise the temperature to 90°C, and react for 10 hours. Centrifuge the obtained microspheres, wash with water, ethanol, and acetone, add dichloroethane to swell after drying, put in ferric chloride with 80% resin mass under nitrogen protection, and react at 80°C for 12 hours, ethanol,...

Embodiment 2

[0035] Using 4.5g FeCl 2 4H2 O and 27g FeCl 3 ·6H 2 O prepared magnetic nanoparticles, modified with 5g oleic acid. The oil phase is composed of 50 g of high-purity divinylbenzene, 100 g of n-hexane, 0.5 g of azobisisobutyronitrile, and 1 g of benzoyl peroxide. Dissolve 10g of gelatin and 10g of polyvinyl alcohol in 500ml of water to form the water phase. The oil phase and the magnetic nanoparticles are ultrasonically mixed, and a SPG membrane with a pore size of 5 μm is selected to form a uniform emulsion under a nitrogen pressure of 0.03 MPa. Transfer the emulsion into a three-necked bottle, stir slowly, raise the temperature to 70°C to initiate the reaction, polymerize for 6 hours, then gradually raise the temperature to 85°C, and react for 14 hours. Centrifuge the obtained microspheres, wash with water, ethanol and acetone, add nitrobenzene to swell after drying, put in zinc chloride with 20% resin mass under the protection of nitrogen, react at 90°C for 16 hours, wash...

Embodiment 3

[0038] Using 23.3g FeCl 2 4H 2 O and 63g FeCl 3 ·6H 2 O prepared magnetic nanoparticles, modified with 15g oleic acid. The oil phase consisted of 50 g of high-purity divinylbenzene, 50 g of isobutanol, and 0.5 g of azobisisobutyronitrile. Dissolve 5g of hydroxyethyl cellulose and 10g of polyvinyl alcohol in 500ml of water to form an aqueous phase. The oil phase and the magnetic nanoparticles are ultrasonically mixed, and a SPG membrane with a pore size of 10 μm is selected to form a uniform emulsion under a nitrogen pressure of 0.01 MPa. Transfer the emulsion into a three-necked bottle, stir slowly, raise the temperature to 65°C to initiate the reaction, polymerize for 10 hours, then gradually raise the temperature to 90°C, and react for 8 hours. Centrifuge the obtained microspheres, wash with water, ethanol, and acetone, add nitrobenzene to swell after drying, put in aluminum chloride with a resin mass of 30% under nitrogen protection, react at 90°C for 16 hours, wash wi...

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Abstract

The invention discloses a magnetic powdered resin with high specific surface area and a preparation method and application thereof, and belongs to the field of resin materials. The average particle size of the magnetic powdered resin is 1 to 60mum, the specific saturation magnetization degree is 0.1 to 20emu/g, and the specific surface area is 800 to 1,600m<2>/g. The resin is prepared by adopting a membrane emulsification-suspension polymerization method, divinyl benzene is used as a reaction monomer, magnetic particles are modified by oleic acid and then subjected to membrane filtering emulsification together with the oil phase, emulsion is suspended and polymerized to form the magnetic microsphere resin, and the specific surface area of microspheres is further enlarged by post cross-linking reaction. Magnetic nano particles in the magnetic microsphere resin prepared by the method are distributed uniformly and have excellent separation performance; the particle size of the resin is small and uniform, so the resin has good adsorption dynamics performance and can realize quick enrichment; and due to the high specific surface area and a rich pore structure, the resin has large adsorption capacity for various polar and non-polar organic substances.

Description

technical field [0001] The invention relates to a resin material and its preparation method and application, more specifically a high specific surface area magnetic microsphere resin and its preparation method and application. Background technique [0002] Tetracyclines are widely used worldwide as antibacterial drugs and animal growth promoters. Only a small part of tetracycline is absorbed and utilized during use, and most of it is excreted through feces and urine. Tetracyclines entering into the environmental system have brought greater ecological risks and promoted the spread of drug-resistant bacteria. Therefore, tetracyclines, as an important part of micro-polluting organic matter in water bodies, have attracted the attention of researchers. In order to solve the problem of tetracycline pollution, it is necessary to grasp the existence and fate of tetracyclines in the environment, and then it is necessary to accurately analyze and detect tetracyclines in water. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L25/02C08K9/04C08K3/16C08F112/36C08J9/28C08J7/02C08J3/24B01J47/00B01J13/02C02F1/42H01F1/42
CPCC08J3/24H01F1/0063C08J2323/16B01J13/02H01F1/42C08J7/02C02F1/42C08F112/36C08K9/04C08J2325/16C08J9/20C08J9/008C08K3/16C08L25/02C08J9/0066C08J9/28B01J47/00C02F1/488B01J20/28009B01J20/28064B01J20/28066
Inventor 李爱民周庆张满成双陈冬王梦乔周扬江野立徐子潇
Owner NANJING UNIV
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