Preparation method and application of magnetic cellulose microspheres with core-shell structure

A technology of cellulose microspheres and core-shell structure, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc. Large and other problems, to achieve excellent chelation, low non-specific adsorption, reduce the effect of loss

Inactive Publication Date: 2020-01-14
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing magnetic cellulose microspheres with a core-shell structure that is simple and mild in conditions. The magnetic material is used as the core and the cellulose composite base is used as the shell, which can not only realize rapid separation under the action of an external magnetic field and reuse, and the design of the core-shell structure increases the specific surface area of ​​the adsorbent, thereby increasing its adsorption capacity; and the amino group is introduced through the silane coupling agent on the surface of the magnetic cellulose, and the carboxyl group is introduced through the amidation reaction. It solves the problems of cellulose easy to swell and poor water dispersibility, and avoids the problems of incomplete reaction caused by cellulose esterification and experimental conditions of high temperature and high pressure

Method used

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  • Preparation method and application of magnetic cellulose microspheres with core-shell structure
  • Preparation method and application of magnetic cellulose microspheres with core-shell structure
  • Preparation method and application of magnetic cellulose microspheres with core-shell structure

Examples

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Effect test

Embodiment 1

[0033] (1) Dissolve ferric chloride hexahydrate and ferric dichloride tetrahydrate in deionized water at a molar ratio of 1:1, heat to 70°C, condense and reflux for 3 hours, then add ammonia solution, in which FeCl3 The mass ratio of the three, deionized water and ammonia water is 1:6:1; after cooling to room temperature, the magnetic particles produced are collected with a magnet, and the product is washed 3-5 times with distilled water to obtain Fe 3 o 4 magnetic core;

[0034] (2) After dissolving microcrystalline cellulose in 7% NaOH / 12% urea mixed solution solvent, a cellulose solution with a concentration of 4% was obtained; the above-mentioned magnetic core was mixed with the prepared cellulose solution and ultrasonically mixed for 15 minutes and continuously stirred for 24 hours , wherein the mass ratio of the magnetic inner core to the middle layer cellulose is 1:5, then collect the product with a magnet, wash the product 3-5 times with distilled water and ethanol res...

Embodiment 2

[0038] (1) Dissolve ferric chloride hexahydrate and ferric dichloride tetrahydrate in deionized water at a molar ratio of 1.5:1, heat to 80°C, condense and reflux for 2 hours, and then add ammonia solution; where FeCl 3 The mass ratio of the three, deionized water and ammonia water is 1:4.5:1. After cooling to room temperature, the magnetic particles produced are collected with a magnet, and the product is washed 3-5 times with distilled water to obtain Fe 3 o 4 magnetic core;

[0039] (2) after dissolving the hydroxyethyl cellulose material in lithium chloride / dimethylacetamide (LiCl / DMAc) mixed solution solvent, the obtained concentration is a 4% cellulose solution; take the above-mentioned magnetic inner core and the obtained The cellulose solution was mixed and ultrasonically stirred for 22 minutes and continuously stirred for 16 hours, wherein the mass ratio of the magnetic inner core to the middle layer of cellulose was 1:3, then the product was collected with a magnet,...

Embodiment 3

[0043] (1) Dissolve ferric chloride hexahydrate and ferric dichloride tetrahydrate in deionized water at a molar ratio of 2:1, heat to 90°C, condense and reflux for 1 hour, then add ammonia solution, in which FeCl 3 The mass ratio of the three, deionized water and ammonia water is 1:3:1; after cooling to room temperature, the magnetic particles produced are collected with a magnet, and the product is washed 3-5 times with distilled water to obtain Fe 3 o 4 magnetic core;

[0044] (2) After dissolving hydroxymethylcellulose in the tetrabutylammonium fluoride hydrate / DMSO mixed solution solvent, a cellulose solution with a concentration of 4% was obtained; the above-mentioned magnetic inner core was mixed with the prepared cellulose solution and ultrasonically Stir continuously for 30 minutes for 8 hours, wherein the mass ratio of the magnetic inner core to the middle layer cellulose is 1:1, then collect the product with a magnet, wash the product 3-5 times with distilled water...

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Abstract

The invention relates to a preparation method and application of magnetic cellulose microspheres with a core-shell structure. According to the preparation method,a Fe3O4 magnetic core is prepared by using a chemical coprecipitation method; magnetic cellulose modified by a silane coupling agent is preparedby using an in-situ compounding method; and the magnetic cellulose modified by a silane coupling agent is enabled to react with diethylenetriamine pentaacetic acid, so as to obtain carboxy-modified magnetic cellulose microspheres. An amino group is grafted ontothe surface of cellulose by usingthe silane coupling agent, chemical modification of carboxylation is implemented through an amidation reaction, the prepared core-shell structure with Fe3O4 as a magnetic core can not only achieve rapid separation and reuse under the action of an external magnetic field, but also increase the specific surface area of an adsorbent. The prepared microspheres are adopted to remove heavy metal ions in water, research shows that the adsorbent has a very good adsorption effect on Hg<2+> and Cr<6+> particularly, and the adsorption capacities are up to 5.98mmol / g and 6.97mmol / g, respectively. The preparation method is simple and is applicable to large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of adsorption materials, and relates to a preparation method and application of magnetic cellulose microspheres with a core-shell structure. Background technique [0002] The adsorption method has always been a hot spot in the research of wastewater treatment due to the advantages of simple equipment, low operating cost, and good treatment effect. Therefore, the development of efficient, cheap, and environmentally friendly adsorbents has attracted much attention. As a natural material with abundant sources, low price, non-toxic environmental protection, good biocompatibility and complete degradability, cellulose has great economic and social value in sewage water treatment. [0003] Cellulose is a natural hydrophilic polymer with the characteristics of good biocompatibility, non-toxicity, chemical modification and degradable regeneration, and is an ideal adsorbent material. However, natural cellulose a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30C02F1/28C02F101/20
CPCB01J20/06B01J20/24B01J20/28009B01J20/28016C02F1/281C02F1/286C02F2101/20
Inventor 张利刘涉江张楠王宇晶苗辰
Owner TIANJIN UNIV
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