Chitosan and chitosan quaternary ammonium salt composite magnetic microspheres and preparation method thereof

A chitosan quaternary ammonium salt, composite magnetic technology, applied in chemical instruments and methods, alkali metal compounds, alkali metal oxides/hydroxides, etc., can solve the problems of low degree of protonation and easy solubility in water, etc. , to achieve the effect of large ion exchange capacity, easy separation and high mechanical strength

Active Publication Date: 2016-05-11
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem that the degree of protonation of chitosan is not high under neutral conditions in the prior art, and the chitosan quaternary ammonium salt itself is easily soluble in water, and provide a method for removing negatively charged pollutants in water with high efficiency. chitosan and chitosan quaternary ammonium salt composite magnetic microspheres

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  • Chitosan and chitosan quaternary ammonium salt composite magnetic microspheres and preparation method thereof
  • Chitosan and chitosan quaternary ammonium salt composite magnetic microspheres and preparation method thereof
  • Chitosan and chitosan quaternary ammonium salt composite magnetic microspheres and preparation method thereof

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Embodiment 1

[0035] A preparation method of chitosan and chitosan quaternary ammonium salt composite magnetic microspheres, comprising the steps of:

[0036] (1) prepare water phase, claim 0.6g chitosan, 1.8g chitosan quaternary ammonium salt, 0.4g porogen PEG600, stirring and dissolving in 40mL volume concentration is in the acetic acid aqueous solution of 2%, add 0.6g particle diameter 0.01~1μm Fe 3 o 4 Magnetic particles, stir and add ultrasound (40kHz, 300W) for 20min to obtain the water phase; the molecular weight of chitosan is 2.0×10 4 -2.0×10 5 , the degree of deacetylation is 80.0%-85.0%; the molecular weight of chitosan quaternary ammonium salt is 1.0×10 5 -3.0×10 5 , the degree of substitution is 95%;

[0037] (2) To prepare the oil phase, take 100mL of liquid paraffin and 1mL of Span80, stir at 40°C at a speed of 200rpm for 40min to obtain the oil phase;

[0038] (3) Add the water phase to the oil phase dropwise under stirring, and stir for 60 min at 360 rpm to obtain a l...

Embodiment 2

[0042] A preparation method of chitosan and chitosan quaternary ammonium salt composite magnetic microspheres, comprising the steps of:

[0043] (1) Prepare the water phase, claim 1.2g chitosan, 1.2g chitosan quaternary ammonium salt, 0.4g PEG2000, stir and dissolve in 40mL volume concentration of 2% acetic acid aqueous solution, add 0.6g particle diameter is 0.1~10μm γ-Fe 2 o 3 Magnetic particles, stir and add ultrasound (40kHz, 300W) for 20min to obtain the water phase; the molecular weight of chitosan is 2.0×10 5 -3.0×10 5 , the degree of deacetylation is 85.0%-95.0%; the molecular weight of chitosan quaternary ammonium salt is 3.0×10 5 -5.0×10 5 , the degree of substitution is 103%;

[0044](2) To prepare the oil phase, take 200 mL of n-hexane and 4 mL of Span80, and stir at 40° C. at a speed of 200 rpm for 40 min to obtain the oil phase;

[0045] (3) Add the water phase to the oil phase dropwise under stirring, and stir for 60 min at 360 rpm to obtain a liquid mixtu...

Embodiment 3

[0049] A preparation method of chitosan and chitosan quaternary ammonium salt composite magnetic microspheres, comprising the steps of:

[0050] (1) Prepare the water phase, claim 1.8g chitosan, 0.6g chitosan quaternary ammonium salt, 0.6g PEG4000, stir and dissolve in 40mL volume concentration of 2% acetic acid aqueous solution, add 0.6g particle diameter of 1-10 μm Stainless steel powder magnetic particles, stirring and ultrasonic (40kHz, 300W) for 10min to obtain the water phase; the molecular weight of chitosan is 2.0×10 4 -2.0×10 5 , the degree of deacetylation is 80.0%-85.0%; the molecular weight of chitosan quaternary ammonium salt is 3.0×10 5 -5.0×10 5 , the degree of substitution is 80%;

[0051] (2) Prepare the oil phase, take 100mL corn oil, 2mL Span80, stir at 40°C at a speed of 200rpm for 40min to obtain the oil phase;

[0052] (3) Add the water phase to the oil phase dropwise under stirring, and stir for 40 min at 400 rpm to obtain a liquid mixture;

[0053]...

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Abstract

The invention discloses a chitosan and chitosan quaternary ammonium salt composite magnetic microsphere and a preparation method thereof. The method comprises the steps of preparing a water phase, stirring and dissolving chitosan, chitosan quaternary ammonium salt and a pore-foaming agent PEG or PVP according to a ratio in an acetic acid aqueous solution, and adding magnetic particles for stirring and ultrasonic treatment; preparing an oil phase, and stirring liquid paraffin and Span80 to obtain the oil phase; gradually adding the water phase into the oil phase drop by drop while stirring is carried out to obtain a liquid mixture; adding a sodium polyphosphate aqueous solution into the liquid mixture drop by drop, carrying out stirring, and adding a glutaraldehyde aqueous solution for reaction; carrying out centrifugation and washing to obtain the chitosan and chitosan quaternary ammonium salt composite magnetic microsphere. The composite magnetic microsphere disclosed by the invention is higher in adsorption to electronegative materials such as humic acid, anionic dyes, arsenate ions, phosphate anions and nitrate ions, is higher in pH adaptability, magnetic separation property and regeneration performance, and is high in exchange capacity, high in adsorption speed and easy to separate.

Description

technical field [0001] The invention relates to chitosan and chitosan quaternary ammonium salt magnetic microspheres and a preparation method. Background technique [0002] Chitosan, a natural polymer material, contains a large number of amino groups and hydroxyl groups in its molecular chain, which enables it to capture organic matter, heavy metals and various anion substances in water through chemical bonds such as hydrogen bonds and coordination bonds, and ion exchange, and has good adsorption properties. With the advantages of non-toxicity, biocompatibility, non-toxicity, biodegradability, and no secondary pollution, it has become a promising environment-friendly material and is widely used in water treatment. Currently, magnetic resins made of chitosan have been extensively studied, such as the disclosed chitosan magnetic microsphere resins such as CN101805037A, CN102107980A and CN102134334A, which have a high adsorption capacity for organic pollutants in water and have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30B01J41/12
CPCB01J20/267B01J20/28009B01J20/3085B01J41/12B01J2220/445B01J2220/4812
Inventor 王亮张宏伟赵威许金明马树双陈倩倩李明德赵斌张朝晖王冠宁李想乐于凯
Owner TIANJIN POLYTECHNIC UNIV
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