CN104910445A - Chitosan-coated ferroferric oxide magnetic nano composite particle and preparation method thereof - Google Patents
Chitosan-coated ferroferric oxide magnetic nano composite particle and preparation method thereof Download PDFInfo
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- CN104910445A CN104910445A CN201510320100.7A CN201510320100A CN104910445A CN 104910445 A CN104910445 A CN 104910445A CN 201510320100 A CN201510320100 A CN 201510320100A CN 104910445 A CN104910445 A CN 104910445A
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Abstract
The invention discloses a chitosan-coated ferroferric oxide magnetic nano composite particle and a preparation method thereof. The preparation method comprises the following steps: (1) adding FeSO4.7H2O, FeCl3.6H2O and polyethyleneglycol into deionized water to obtain a dispersion solution; (2) adding NH3.H2O and sodium citrate into the dispersion solution to obtain a citric-acid-modified Fe3O4 magnetic colloid; (3) neutralizing; (4) carrying out magnetic separation; (5) adding the citric-acid-modified Fe3O4 magnetic particle into a chitosan solution, stirring, sucking out magnetic particles with a magnet, adding into a glutaric dialdehyde ethanol solution, crosslinking, cleaning, and drying to obtain the chitosan-coated Fe3O4 magnetic nano composite particle. The chitosan-coated ferroferric oxide magnetic nano composite particle has the advantages of uniform particle size distribution, high stability and favorable biocompatibility, and can be combined with enzymes, antibodies, cells and other biological active substances. The method is simple to operate, and has the advantages of mild conditions, small pollution, short synthesis time and high safety.
Description
Technical field
The present invention relates to field of nano material preparation, particularly relate to a kind of Fe of Chitosan-coated
3o
4the preparation method of magnetic nanometer composite material.
Background technology
Magnetic nanometer composite material, refers to and by suitable preparation method, organic polymer is combined with inorganic magnetic particle, forms the composite particles with certain magnetic and special construction.Due to the quantum effect of nano material, small-size effect, powerful specific surface area, the effects such as quantum tunneling, give its much special character.Magnetic Nano composite particles has magnetic responsiveness and special surface functional group, can with the combinations such as other small molecules, macromole or cell, then some response is made under the influence of a magnetic field, therefore, magnetic Nano composite particles is widely used in clinical diagnosis, contrast imaging, targeted drug, biomarker and is separated and the field such as enzyme immobilizatio.But because the affinity of organism and inorganics is poor, being evenly dispersed in by magnetic-particle in polymer particles is a more difficult job, therefore the preparation of magnetic Nano composite particles is the focus of research always.
Chitosan (chitosan), also known as chitosan, is the product that chitin takes off N-ethanoyl, and chemical name is Chitosan (1-4)-2-amino-B-D glucose.Chitosan is unique basic natural polysaccharides, and having easy film forming, corrosion-resistant, readily biodegradable, good biocompatibility, germ resistance, the advantage such as nontoxic, is one of natural polymer of excellent performance.From 1859, after first Frenchman Rouget obtains chitosan, the premium propertiess such as the biological functionality of this natural polymer and consistency, blood compatibility, security, microbic resolvability, by all trades and professions extensive concern, achieve major progress in the applied research of the numerous areas such as medicine, food, makeup, water treatment, METAL EXTRACTION and recovery, chemical industry and biomedical engineering.
Have active hydroxyl and amino in chitosan macromole, they have stronger chemical reaction ability, at present, although there is the Fe of people's Chitosan-coated
3o
4prepare magnetic Nano material, but the material granule of preparation is uneven, poor stability, poor biocompatibility, can not meet the needs of biological field application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of particle size distribution evenly, the ferroferric oxide magnetic nano composite particles of the dispersed and good Chitosan-coated of stability.
Second object of the present invention is to provide a kind of preparation method of ferroferric oxide magnetic nano composite particles of Chitosan-coated.
A kind of Fe of Chitosan-coated
3o
4the preparation method of magnetic Nano composite granules, comprises the steps:
(1) by FeSO
47H
2o, FeCl
36H
2o, polyoxyethylene glycol join in deionized water, at 50-80 DEG C, stir 10-20 minute, obtain dispersion liquid under rotating speed 400-800r/min; Described FeSO
47H
2o, FeCl
36H
2the ratio of O, polyoxyethylene glycol and deionized water is 1mol:1.5-2.5mol:0.1-0.4mol:4-7L;
(2) in the dispersion liquid of 50-80 DEG C, under the stirring of rotating speed 400-800r/min, NH is added
3h
2o, then add Trisodium Citrate, continue to stir 40-80 minute under 50-80 DEG C of condition, obtain the Fe of citric acid modification
3o
4magnetic colloid, naturally cools to room temperature; Described FeSO
47H
2o, Trisodium Citrate and NH
3h
2the ratio of O is 1mol:0.1-0.3mol:1.2-2.0L;
(3) with the Fe of hydrochloric acid by citric acid modification
3o
4magnetic colloid is neutralized to neutrality;
(4) inhale with magnet the neutral magnetic colloid solution that step (3) obtains, isolate the Fe of citric acid modification
3o
4magnetic-particle, with deionized water and ethanol purge 3-5 time;
(5) Fe of citric acid modification step (4) obtained
3o
4magnetic-particle, joining mass concentration is in the chitosan solution of 1%, stirred at ambient temperature 1.5-2.5h, use magnet sucking-off magnetic-particle again, magnetic-particle being added to volumetric concentration is in the glutaraldehyde ethanolic soln of 5%, the crosslinked 1.5-3h of vibration, with deionized water and ethanol purge 3-5 time, drying, namely obtains the Fe of Chitosan-coated
3o
4magnetic Nano composite granules, the solvent of described chitosan solution to be volumetric concentration be 1% aqueous hydrochloric acid; FeSO
47H
2the ratio of O, described chitosan solution and described glutaraldehyde ethanolic soln is 1mol:15-20L:7.5-12L.
The Fe of Chitosan-coated prepared by aforesaid method
3o
4magnetic Nano composite granules.
The ferroferric oxide magnetic nano composite particles of Chitosan-coated prepared by method of the present invention, even particle size distribution, particle diameter is about 12.5nm, good stability.And particle surface has active hydroxyl and amino, the biologically active substances such as desmoenzyme, antibody, cell can be carried out by covalent linkage, there is good biocompatibility; Method of the present invention is easy and simple to handle, mild condition, and pollute little, generated time is short, and security is high, and technology difficulty is low, is applicable to large-scale commercial and produces.
Accompanying drawing explanation
Fig. 1 is the Fe of Chitosan-coated prepared by embodiment 1
3o
4the XRD figure of magnetic Nano composite granules.
Fig. 2 is the Fe of Chitosan-coated prepared by embodiment 1
3o
4the SEM figure of magnetic Nano composite granules.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.The following examples understand the present invention better to enable those skilled in the art to, but do not impose any restrictions the present invention.
Embodiment 1
A preparation method for the ferroferric oxide magnetic nano composite particles of Chitosan-coated, comprises the steps:
(1) by 1mol FeSO
47H
2o, 2molFeCl
36H
2o, 0.25mol Polyethylene glycol-2000 joins in 5.5L deionized water, at 65 DEG C, stirs 15 minutes, obtain dispersion liquid under rotating speed 600r/min;
(2) in the dispersion liquid of 65 DEG C, under the stirring of rotating speed 600r/min, slowly 1.6L NH is added
3h
2o, then adds 0.2mol Trisodium Citrate, continues to stir 60 minutes under 65 DEG C of conditions, obtains the Fe of citric acid modification
3o
4magnetic colloid, naturally cools to room temperature;
(3) with the Fe of hydrochloric acid by citric acid modification
3o
4magnetic colloid is neutralized to neutrality;
(4) inhale with magnet the neutral magnetic colloid solution that step (3) obtains, isolate the Fe of citric acid modification
3o
4magnetic-particle, also uses ethanol purge 4 times 4 times by washed with de-ionized water;
(5) Fe of citric acid modification step (4) obtained
3o
4magnetic-particle, joining 18L mass concentration is in the chitosan solution of 1%, stirred at ambient temperature 2h, use magnet sucking-off magnetic-particle again, magnetic-particle being added to 10L volumetric concentration is in the glutaraldehyde ethanolic soln of 5%, and the crosslinked 2.5h of vibration, also uses ethanol purge 4 times 4 times by washed with de-ionized water, drying, namely obtains the Fe of Chitosan-coated
3o
4magnetic Nano composite granules (see Fig. 1 and Fig. 2), the solvent of described chitosan solution to be volumetric concentration be 1% aqueous hydrochloric acid.
Embodiment 2
A preparation method for the ferroferric oxide magnetic nano composite particles of Chitosan-coated, comprises the steps:
(1) by 1mol FeSO
47H
2o, 1.5molFeCl
36H
2o, 0.1mol Polyethylene glycol-2000 joins in 4L deionized water, at 50 DEG C, stirs 20 minutes, obtain dispersion liquid under rotating speed 800r/min;
(2) in the dispersion liquid of 50 DEG C, under the stirring of rotating speed 800r/min, slowly 1.2L NH is added
3h
2o, then adds 0.1mol Trisodium Citrate, continues to stir 80 minutes under 50 DEG C of conditions, obtains the Fe of citric acid modification
3o
4magnetic colloid, naturally cools to room temperature;
(3) with the Fe of hydrochloric acid by citric acid modification
3o
4magnetic colloid is neutralized to neutrality;
(4) inhale with magnet the neutral magnetic colloid solution that step (3) obtains, isolate the Fe of citric acid modification
3o
4magnetic-particle, also uses ethanol purge 3 times 3 times by washed with de-ionized water;
(5) Fe of citric acid modification step (4) obtained
3o
4magnetic-particle, joining 15L mass concentration is in the chitosan solution of 1%, stirred at ambient temperature 1.5h, use magnet sucking-off magnetic-particle again, magnetic-particle being added to 7.5L volumetric concentration is in the glutaraldehyde ethanolic soln of 5%, and the crosslinked 3h of vibration, also uses ethanol purge 3 times 3 times by washed with de-ionized water, drying, namely obtains the Fe of Chitosan-coated
3o
4magnetic Nano composite granules, the solvent of described chitosan solution to be volumetric concentration be 1% aqueous hydrochloric acid.
Embodiment 3
A preparation method for the ferroferric oxide magnetic nano composite particles of Chitosan-coated, comprises the steps:
(1) by 1mol FeSO
47H
2o, 2.5molFeCl
36H
2o, 0.4mol Polyethylene glycol-2000 joins in 7L deionized water, at 80 DEG C, stirs 10 minutes, obtain dispersion liquid under rotating speed 400r/min;
(2) in the dispersion liquid of 80 DEG C, under the stirring of rotating speed 400r/min, 2.0L NH is added
3h
2o, then adds 0.3mol Trisodium Citrate, continues to stir 40 minutes under 80 DEG C of conditions, obtains the Fe of citric acid modification
3o
4magnetic colloid, naturally cools to room temperature;
(3) with the Fe of hydrochloric acid by citric acid modification
3o
4magnetic colloid is neutralized to neutrality;
(4) inhale with magnet the neutral magnetic colloid solution that step (3) obtains, isolate the Fe of citric acid modification
3o
4magnetic-particle, also uses ethanol purge 5 times 5 times by washed with de-ionized water;
(5) Fe of citric acid modification step (4) obtained
3o
4magnetic-particle, joining 20L mass concentration is in the chitosan solution of 1%, stirred at ambient temperature 2.5h, use magnet sucking-off magnetic-particle again, magnetic-particle being added to 12L volumetric concentration is in the glutaraldehyde ethanolic soln of 5%, and the crosslinked 1.5h of vibration, also uses ethanol purge 5 times 5 times by washed with de-ionized water, drying, namely obtains the Fe of Chitosan-coated
3o
4magnetic Nano composite granules, the solvent of described chitosan solution to be volumetric concentration be 1% aqueous hydrochloric acid.
Claims (2)
1. the Fe of a Chitosan-coated
3o
4the preparation method of magnetic Nano composite granules, is characterized in that comprising the steps:
(1) by FeSO
47H
2o, FeCl
36H
2o, polyoxyethylene glycol join in deionized water, at 50-80 DEG C, stir 10-20 minute, obtain dispersion liquid under rotating speed 400-800r/min; Described FeSO
47H
2o, FeCl
36H
2the ratio of O, polyoxyethylene glycol and deionized water is 1mol:1.5-2.5mol:0.1-0.4mol:4-7L;
(2) in the dispersion liquid of 50-80 DEG C, under the stirring of rotating speed 400-800r/min, NH is added
3h
2o, then add Trisodium Citrate, continue to stir 40-80 minute under 50-80 DEG C of condition, obtain the Fe of citric acid modification
3o
4magnetic colloid, naturally cools to room temperature; Described FeSO
47H
2o, Trisodium Citrate and NH
3h
2the ratio of O is 1mol:0.1-0.3mol:1.2-2.0L;
(3) with the Fe of hydrochloric acid by citric acid modification
3o
4magnetic colloid is neutralized to neutrality;
(4) inhale with magnet the neutral magnetic colloid solution that step (3) obtains, isolate the Fe of citric acid modification
3o
4magnetic-particle, with deionized water and ethanol purge 3-5 time;
(5) Fe of citric acid modification step (4) obtained
3o
4magnetic-particle, joining mass concentration is in the chitosan solution of 1%, stirred at ambient temperature 1.5-2.5h, use magnet sucking-off magnetic-particle again, magnetic-particle being added to volumetric concentration is in the glutaraldehyde ethanolic soln of 5%, the crosslinked 1.5-3h of vibration, with deionized water and ethanol purge 3-5 time, drying, namely obtains the Fe of Chitosan-coated
3o
4magnetic Nano composite granules, the solvent of described chitosan solution to be volumetric concentration be 1% aqueous hydrochloric acid; FeSO
47H
2the ratio of O, described chitosan solution and described glutaraldehyde ethanolic soln is 1mol:15-20L:7.5-12L.
2. the Fe of Chitosan-coated for preparing of the method for claim 1
3o
4magnetic Nano composite granules.
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Cited By (16)
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| CN105195112A (en) * | 2015-10-26 | 2015-12-30 | 福建农林大学 | Preparation method of melamine-modified chitosan-coated magnetic nanocellulose adsorbent and product thereof |
| CN105203752A (en) * | 2015-11-05 | 2015-12-30 | 上海中山医疗科技发展公司 | Magnetic platelet adsorption particle and preparation method thereof |
| CN105195111A (en) * | 2015-10-26 | 2015-12-30 | 福建农林大学 | Preparation method of polyethylenimine modified chitosan-coated magnetic nanocellulose adsorbent and product thereof |
| CN105671029A (en) * | 2016-03-08 | 2016-06-15 | 万香波 | Establishment method of three-dimensional cell model |
| CN106268680A (en) * | 2016-10-12 | 2017-01-04 | 沈阳航空航天大学 | Magnetic Nano microcapsule adsorbent and its preparation method and application |
| CN107896476A (en) * | 2017-10-24 | 2018-04-10 | 当涂县瑞龙果树种植专业合作社 | A kind of magnetic nano-particle microwave absorbing material and preparation method thereof |
| CN107903074A (en) * | 2017-10-24 | 2018-04-13 | 当涂县瑞龙果树种植专业合作社 | A kind of ceramic material sintering aid and preparation method thereof |
| CN107955627A (en) * | 2017-10-24 | 2018-04-24 | 当涂县瑞龙果树种植专业合作社 | A kind of iron producing area soil pollution renovation agent and preparation method thereof |
| CN108060158A (en) * | 2018-02-10 | 2018-05-22 | 成都理工大学 | A kind of chitosan magnetic carries the preparation method of denitrifying bacteria bead |
| CN109879326A (en) * | 2019-03-22 | 2019-06-14 | 信阳师范学院 | A method of ferric oxide nanometer particle is prepared using tealeaves |
| CN112973190A (en) * | 2021-02-22 | 2021-06-18 | 广东省惠州市中药厂有限公司 | Method for removing heavy metal in traditional Chinese medicine extracting solution |
| CN113398848A (en) * | 2021-06-24 | 2021-09-17 | 苏州市德赫亚新纺织科技有限公司 | Preparation method of recyclable oxidized chitosan coated Fe304 magnetic microspheres |
| CN114772676A (en) * | 2022-04-07 | 2022-07-22 | 张胜枚 | Magnetic nano-particle technology applied to environmental management |
| CN114797790A (en) * | 2022-05-10 | 2022-07-29 | 南京信息工程大学 | Preparation method of magnetic nano FeS stabilized by chitosan |
| CN114887058A (en) * | 2022-05-09 | 2022-08-12 | 南京工业大学 | Delivery system based on photosensitive nano-composite and preparation method and application thereof |
| CN116259459A (en) * | 2023-02-22 | 2023-06-13 | 上海蓝载信息科技有限公司 | Super-magnetic citric acid coated iron oxide nanoparticle, and synthesis method and application thereof |
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| CN105195112A (en) * | 2015-10-26 | 2015-12-30 | 福建农林大学 | Preparation method of melamine-modified chitosan-coated magnetic nanocellulose adsorbent and product thereof |
| CN105195111A (en) * | 2015-10-26 | 2015-12-30 | 福建农林大学 | Preparation method of polyethylenimine modified chitosan-coated magnetic nanocellulose adsorbent and product thereof |
| CN105203752A (en) * | 2015-11-05 | 2015-12-30 | 上海中山医疗科技发展公司 | Magnetic platelet adsorption particle and preparation method thereof |
| CN105671029A (en) * | 2016-03-08 | 2016-06-15 | 万香波 | Establishment method of three-dimensional cell model |
| CN106268680A (en) * | 2016-10-12 | 2017-01-04 | 沈阳航空航天大学 | Magnetic Nano microcapsule adsorbent and its preparation method and application |
| CN107896476A (en) * | 2017-10-24 | 2018-04-10 | 当涂县瑞龙果树种植专业合作社 | A kind of magnetic nano-particle microwave absorbing material and preparation method thereof |
| CN107903074A (en) * | 2017-10-24 | 2018-04-13 | 当涂县瑞龙果树种植专业合作社 | A kind of ceramic material sintering aid and preparation method thereof |
| CN107955627A (en) * | 2017-10-24 | 2018-04-24 | 当涂县瑞龙果树种植专业合作社 | A kind of iron producing area soil pollution renovation agent and preparation method thereof |
| CN108060158A (en) * | 2018-02-10 | 2018-05-22 | 成都理工大学 | A kind of chitosan magnetic carries the preparation method of denitrifying bacteria bead |
| CN109879326A (en) * | 2019-03-22 | 2019-06-14 | 信阳师范学院 | A method of ferric oxide nanometer particle is prepared using tealeaves |
| CN112973190A (en) * | 2021-02-22 | 2021-06-18 | 广东省惠州市中药厂有限公司 | Method for removing heavy metal in traditional Chinese medicine extracting solution |
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| CN114772676A (en) * | 2022-04-07 | 2022-07-22 | 张胜枚 | Magnetic nano-particle technology applied to environmental management |
| CN114887058A (en) * | 2022-05-09 | 2022-08-12 | 南京工业大学 | Delivery system based on photosensitive nano-composite and preparation method and application thereof |
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| CN116259459A (en) * | 2023-02-22 | 2023-06-13 | 上海蓝载信息科技有限公司 | Super-magnetic citric acid coated iron oxide nanoparticle, and synthesis method and application thereof |
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