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Magnetic microsphere capable of adsorbing diclofenac sodium

A technology of diclofenac sodium and magnetic microspheres, which is applied in the field of analytical chemistry, can solve the problems of low utilization rate of raw materials, uneven adsorption performance of magnetic microspheres, low mixing ratio of water phase and oil phase, etc., so as to facilitate separation and recovery , Excellent magnetic response, enhanced dispersion effect

Active Publication Date: 2018-01-16
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing technology such as Chinese invention patent authorization document, authorization announcement number is CN104258822B, this invention discloses a kind of chitosan and chitosan quaternary ammonium salt composite magnetic microsphere and preparation method, method steps are: prepare water phase, proportional , take chitosan, chitosan quaternary ammonium salt, porogen PEG or PVP, stir and dissolve in acetic acid aqueous solution, add magnetic particles, stir and add ultrasound; prepare the oil phase, take liquid paraffin, Span80, and stir to obtain the oil phase; Under stirring, add the water phase to the oil phase drop by drop, and stir to obtain a liquid mixture; add sodium polyphosphate aqueous solution to the liquid mixture drop by drop, stir, add glutaraldehyde aqueous solution, and react; centrifuge and wash to obtain chitosan Sugar and chitosan quaternary ammonium salt composite magnetic microspheres, the composite magnetic microspheres of the invention have high adsorption to negatively charged substances such as humic acid, anionic dyes, arsenate ions, phosphate ions and nitrate ions in water , and has strong pH adaptability, magnetic separation and reproducibility; large exchange capacity, fast adsorption speed, and easy separation, but the mixing ratio of the water phase and the oil phase in the preparation process of the magnetic microspheres is low, making the raw materials The utilization rate is low, and the adsorption performance of the prepared magnetic microspheres is not uniform

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0014] A kind of magnetic microsphere of adsorption sodium diclofenac, its preparation process comprises the following steps:

[0015] 1) Nano Fe 3 o 4 Preparation: Take FeCl with a concentration of 0.1mol / L 2 and FeCl 3 The solution is mixed, the Fe in the mixture 2+ / Fe 3 + The molar ratio is 1:1.4, the total weight of the mixed solution is 9.6 parts, add 90 parts of NH 3 ·H 2 0 and 0.12 parts of diethyl malonate were ultrasonically emulsified and dispersed at 70°C, cooled to room temperature, separated, washed, and vacuum-dried to obtain nano-Fe 3 o 4 Magnetic particles, under the preparation conditions, Fe in water 2+ and Fe 3+ The utilization rate of the nano-Fe is high, and the obtained particles have strong superparamagnetism, and the addition of diethyl malonate can reduce the concentration of nano-Fe 3 o 4 The surface energy of the magnetic particles improves the agglomeration phenomenon, significantly enhances the dispersion of the nanoparticles, and impr...

Embodiment 2

[0021] A kind of magnetic microsphere of adsorption sodium diclofenac, its preparation process comprises the following steps: first nanometer Fe 3 o 4 Preparation: Take FeCl with a concentration of 0.1mol / L 2 and FeCl 3 The solution is mixed, the Fe in the mixture 2+ / Fe 3+ The molar ratio is 1:1.5, the total weight of the mixture is 10 parts, add 92 parts of NH 3 ·H 2 0 and 0.12 parts of diethyl malonate were ultrasonically emulsified and dispersed at 69°C, cooled to room temperature, separated, washed, and vacuum-dried to obtain nano-Fe 3 o 4 Magnetic particles; followed by SiO 2 Coated magnetic nanoparticles Fe 3 o 4 @SiO 2 Preparation: take 0.48 parts of nano-Fe 3 o 4 For magnetic particles, add 80 parts of ethanol / water mixture with a volume ratio of 1:0.21, ultrasonically mix and disperse, add 4.1 parts of TEOS ethanol solution and 3.1 parts of 25% ammonia water, stir for reaction, filter, and wash with absolute ethanol and distilled water , Fe was obtained ...

Embodiment 3

[0024] A kind of magnetic microsphere of adsorption sodium diclofenac, its preparation process comprises the following steps: first nanometer Fe 3 o 4 Preparation: Take FeCl with a concentration of 0.1mol / L 2 and FeCl 3 The solution is mixed, the Fe in the mixture 2+ / Fe 3+ The molar ratio is 1:1.6, the total weight of the mixed solution is 10.1 parts, add 97 parts of NH 3 ·H 2 0 and 0.16 parts of diethyl malonate were ultrasonically emulsified and dispersed at 71°C, cooled to room temperature, separated, washed, and vacuum-dried to obtain nano-Fe 3 o 4 Magnetic particles; followed by SiO 2 Coated magnetic nanoparticles Fe 3 o 4 @SiO 2 Preparation: take 0.52 parts of nano-Fe 3 o 4 For magnetic particles, add 81 parts of ethanol / water mixture with a volume ratio of 1:0.25, ultrasonically mix and disperse, add 4.6 parts of TEOS ethanol solution and 3.8 parts of 25% ammonia water, stir for reaction, filter, and wash with absolute ethanol and distilled water , Fe was ...

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PUM

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Abstract

The invention provides a magnetic microsphere capable of adsorbing diclofenac sodium. The magnetic microsphere is prepared by the following steps: preparing nano Fe3O4 by a co-precipitation method, preparing a SiO2 coated magnetic nano particle Fe3O4@SiO2, preparing a chitosan compounded Fe3O4@SiO2 magnetic material, and preparing an ethylene diamine modified magnetic material. According to the preparation method, chitosan and magnetic particles are combined, then the microsphere is modified by ethylene diamine; the magnetic microsphere has more amino groups, the effect of adsorbing and removing diclofenac sodium in water is improved, moreover, the chitosan microsphere has a good magnetic responding performance, so the microsphere can be conveniently separated and recovered, and the magnetic microsphere is a green and sustainable absorbent.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a magnetic microsphere for absorbing diclofenac sodium. Background technique [0002] As a rheumatoid and osteoarthritis drug, diclofenac sodium is a commonly used drug in human life. It is also one of PPCPs (​drugs and personal care products), which has certain hidden dangers to human health. In this study, chitosan-based magnetic particles were used as adsorption materials to remove diclofenac sodium from water. The material is magnetic for easy and quick removal. [0003] Existing technology such as Chinese invention patent authorization document, authorization announcement number is CN104258822B, this invention discloses a kind of chitosan and chitosan quaternary ammonium salt composite magnetic microsphere and preparation method, method steps are: prepare water phase, proportional , take chitosan, chitosan quaternary ammonium salt, porogen PEG or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30C02F1/28C02F1/48C02F101/36
Inventor 杨立业欧阳小琨胡兆红
Owner ZHEJIANG OCEAN UNIV
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