Chitosan and chitosan quaternary ammonium salt composite magnetic microsphere 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 good regeneration performance

Active Publication Date: 2015-01-07
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 s...

Method used

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

Examples

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Effect test

Embodiment 1

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

[0036] (1) Prepare the aqueous phase, weigh 0.6g chitosan, 1.8g chitosan quaternary ammonium salt, 0.4g porogen PEG600, stir and dissolve in 40mL acetic acid aqueous solution with a volume concentration of 2%, add 0.6g particle size 0.01~1μm Fe 3 O 4 Magnetic particles, stir and ultrasonic (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) Prepare the oil phase, take 100 mL of liquid paraffin, 1 mL of Span80, and stir at 40° C. and 200 rpm for 40 minutes to obtain the oil phase;

[0038] (3) Under stirring, add the water phase dropwise to the oil phase, stir at 360 rpm for 60 minutes to obtain a liquid mixture;

[0039...

Embodiment 2

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

[0043] (1) Prepare the water phase, weigh 1.2g chitosan, 1.2g chitosan quaternary ammonium salt, 0.4g PEG2000, stir and dissolve in 40mL acetic acid aqueous solution with a volume concentration of 2%, and add 0.6g with a particle size of 0.1-10μm γ-Fe 2 O 3 Magnetic particles, stir and ultrasonic (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) Prepare the oil phase, take 200 mL of n-hexane, 4 mL of Span80, and stir at 40°C and 200 rpm for 40 minutes to obtain the oil phase;

[0045] (3) Under stirring, add the water phase dropwise to the oil phase, stir at 360 rpm for 60 minutes to obtain a liquid mixture;

[0046]...

Embodiment 3

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

[0050] (1) Prepare the water phase, weigh 1.8g chitosan, 0.6g chitosan quaternary ammonium salt, 0.6g PEG4000, stir and dissolve in 40mL acetic acid aqueous solution with a volume concentration of 2%, and add 0.6g with a particle size of 1-10μm Magnetic particles of stainless steel powder, stir 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 100 mL corn oil, 2 mL Span80, and stir at 40°C and 200 rpm for 40 min to obtain the oil phase;

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

...

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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 a chitosan and chitosan quaternary ammonium salt magnetic microspheres and a preparation method. Background technique [0002] The molecular chain of chitosan, a natural polymer material, contains a large number of amino groups and hydroxyl groups, which enables it to capture organics, heavy metals and a variety of anions in water through hydrogen bonds, coordination bonds and other chemical bonds and ion exchange, and has good adsorption It has become a promising environmentally friendly material and has been widely used in water treatment with its advantages such as compatibility, non-toxicity, biodegradability, and no secondary pollution. At present, magnetic resins using chitosan as materials have been studied a lot, such as CN101805037A, CN102107980A and CN102134334A disclosed chitosan magnetic microsphere resins. Such resins have high adsorption capacity for organic pollutants in water and have good Economic and environmental...

Claims

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Application Information

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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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